WO2012133018A1 - Metal oxide conjugated highly-flat cellulose powder and cosmetic containing same - Google Patents

Metal oxide conjugated highly-flat cellulose powder and cosmetic containing same Download PDF

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Publication number
WO2012133018A1
WO2012133018A1 PCT/JP2012/057110 JP2012057110W WO2012133018A1 WO 2012133018 A1 WO2012133018 A1 WO 2012133018A1 JP 2012057110 W JP2012057110 W JP 2012057110W WO 2012133018 A1 WO2012133018 A1 WO 2012133018A1
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Prior art keywords
metal oxide
cellulose powder
powder
composite high
oxide composite
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PCT/JP2012/057110
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French (fr)
Japanese (ja)
Inventor
増渕　祐二
五十嵐　啓二
村田　東吾
村田　哲雄
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株式会社オーケン
株式会社コーセー
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Application filed by 株式会社オーケン, 株式会社コーセー filed Critical 株式会社オーケン
Priority to JP2013507417A priority Critical patent/JP6069189B2/en
Priority to CN201280015354.2A priority patent/CN103442685B/en
Priority to KR1020137024988A priority patent/KR101600058B1/en
Publication of WO2012133018A1 publication Critical patent/WO2012133018A1/en
Priority to HK13114338.7A priority patent/HK1186687A1/en

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/731—Cellulose; Quaternized cellulose derivatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/0254—Platelets; Flakes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/0283—Matrix particles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27—Zinc; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29—Titanium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02—Preparations containing skin colorants, e.g. pigments
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns

Definitions

  • the present invention relates to a cellulose powder having high flatness composited with a metal oxide and a powder cosmetic containing the same, and more specifically, has a shape having high flatness and the surface thereof is a metal oxide.
  • the present invention relates to a metal oxide-complexed highly flat cellulose powder coated with a cosmetic and a cosmetic containing the same.
  • Powder cosmetics containing a powder component, an oily component, and the like are widely used in the field of cosmetics, and examples thereof include powder foundation, eye shadow, powdered white powder, blusher, and the like.
  • This powder cosmetic is generally produced by filling a powder container of powder components such as extender pigments and pigments and an oil component into a dish-like container and press-molding.
  • Patent Documents 1 to 3 Also known are powder components coated with metal oxide (Patent Documents 1 to 3).
  • Patent Documents 1 and 2 both cover polymer fine powder and spherical resin powder with a fine metal oxide, and Patent Document 3 can be used as cosmetic powder.
  • the substrate was treated with hydroxyapatite and zinc oxide.
  • the powder component has various shapes, and flaky inorganic powders such as mica pieces, sericite, and talc are widely used, but these are all aluminosilicate minerals.
  • flaky inorganic powders such as mica pieces, sericite, and talc are widely used, but these are all aluminosilicate minerals.
  • the properties are slightly different depending on the production area, for example, there is a problem that the oil absorbability is low or the desired physical properties cannot be obtained.
  • flat organic powders have not been reported so much, for example, to the extent that flat cellulose particles obtained by mixing cellulose-based substances and fatty acids and then mechanically pulverizing them are known. (Patent Document 4).
  • Patent Document 5 a technique for treating the surface of crystalline cellulose with hydrogenated lecithin is also known (Patent Document 5).
  • this crystalline cellulose has a major axis / minor axis ratio (L / D) of 3 or less, which is not flat.
  • L / D major axis / minor axis ratio
  • the present inventors have previously developed a flat cellulose powder having an extremely high flatness (aspect ratio) of 20 to 200 (hereinafter referred to as “high flatness cellulose powder”) and a method for producing the same, and applied for a patent.
  • high flatness cellulose powder is obtained by drying the purified cellulose pulp-derived cellulose powder under reduced pressure to sufficiently remove the adsorbed moisture, and then grinding it with a planetary ball mill together with a grinding aid and, if necessary, a hydrophobizing agent. It is obtained by.
  • the resulting high flatness cellulose powder is made of cellulose and has the characteristics of high flatness, so when it is blended as a powder cosmetic ingredient, the amount of oily ingredients is large. However, the agglomeration of the powder is not caused, the characteristics such as the smoothness of the powder itself are maintained, and the caking is difficult to occur even if the powder is pressed.
  • An object of the present invention is to provide a cosmetic powder and a cosmetic using the same.
  • the inventors of the present invention were further researching on the high flatness cellulose powder obtained from the cellulosic material, and added a grinding aid and a metal oxide to the cellulosic material by a specific method.
  • a metal oxide composite high flattened cellulose powder with properties that can hardly be obtained with conventional cosmetic powders is obtained, and by using this, commercial properties of cosmetics such as powder cosmetics are obtained.
  • the present invention has been completed.
  • the present invention is a metal oxide composite high flattened cellulose powder obtained by mechanically grinding a cellulosic material, a grinding aid, and a metal oxide.
  • the present invention is also a cosmetic comprising the metal oxide composite high flattened cellulose powder.
  • the present invention provides a metal oxide composite high flat cellulose powder characterized by adding a grinding aid and a metal oxide to a cellulosic material to form a mixture, and mechanically grinding the mixture. Is the method.
  • the metal oxide composite high flattened cellulose powder of the present invention has a new effect in addition to the effect of the conventional high flattened cellulose powder by combining the metal oxide on the surface thereof. .
  • the composite metal oxide has a thickness of 10 to 100 nm on the powder, an extremely excellent UV blocking effect and a smooth use feeling can be obtained.
  • the composite metal oxide is more than 100 nm and not more than 1000 nm on the powder, natural concealing properties, excellent color developability and a smooth feeling of use can be obtained.
  • the cosmetic compounded with this metal oxide composite high flattened cellulose powder has excellent cosmetic film uniformity and smooth use feeling, as well as excellent UV blocking effect, natural hiding property, and coloring effect. In addition, it has an excellent makeup lasting effect such as no color sink.
  • the cosmetics using the metal oxide composite high flat cellulose powder of the present invention can be suitably used as powder foundation, eye shadow, powdered white powder, blusher and the like.
  • the metal oxide composite high flat cellulose powder of the present invention is one in which fine metal oxide powder is firmly attached and combined on the surface of the high flat cellulose powder.
  • This metal oxide composite high flat cellulose powder is produced by adding a grinding aid and a metal oxide to a cellulose-based material to form a mixture, and mechanically grinding the mixture.
  • the cellulosic material used as a starting material for the metal oxide composite high flattened cellulose powder is not particularly limited, but for example, a woody material such as fibrous or powdery wood powder or wood pulp originating from wood It is preferable to use a cotton-based material such as fibrous or powdered cotton or linter fiber originating from cotton, a woody material, or a fibrous or powdery cellulose material obtained by refining the cotton-based material Alternatively, a purified cellulosic material obtained by acid hydrolysis may be used. In addition, as a cellulosic substance originating in cotton, the thing originating in the cotton which received the organic certification
  • the cellulosic material used as a raw material easily adsorbs or absorbs moisture, and has an adsorbed moisture of about 3 to 10% by mass (hereinafter simply referred to as “%”) in a normal state.
  • % an adsorbed moisture of about 3 to 10% by mass
  • the grinding aid used in the production of the metal oxide-complexed highly flat cellulose powder of the present invention is used for highly flattening the cellulosic material.
  • amphiphilic substances include phospholipids, ceramides, cholesterol or derivatives thereof, phytosterols or derivatives thereof, and the like. These are substances having a common property of being a lipid in vivo or a structure close to that, that is, having a long-chain alkyl structure and a hydrophilic group.
  • phospholipid is a generic term for lipids having a phosphate ester moiety in the structure.
  • Specific phospholipids include those derived from natural products hydrogenated to natural lecithin such as egg yolk lecithin and soybean lecithin, hydrogenated lysolecithin, phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidylinositol, sphingomyelin, etc. And the like.
  • hydrogenated lecithin, phosphatidylcholine, phosphatidylethanolamine, and hydrogenated phosphatidylglycerol are preferable.
  • the ceramide has a non-linear group having one or more long-chain linear and / or branched alkyl or alkenyl groups, at least two hydroxyl groups, and one or more amide groups (and / or amino groups) in the molecule.
  • Specific examples of ceramide include natural ceramides such as ceramide 1, ceramide 2, ceramide 3, ceramide 3B, ceramide 4, ceramide 5, ceramide 6, ceramide 6I, ceramide 6II and the like, which are long-chain fatty acid amides of sphingosine and phytosphingosine. Is mentioned.
  • ceramide 2 and ceramide 3 are preferable. These ceramides may be derived from natural products or synthesized.
  • cholesterol is a white to slightly yellow solid purified by extracting, crystallizing and drying a fraction obtained from saponified animal oil and fat and fish oil, and its molecular formula is C 27 H 46 O.
  • cholesterose derivatives include ester derivatives of saturated fatty acids such as oleic acid, palmitooleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, lauric acid, etc. , Esterified derivatives with a mixture of fatty acids obtained by hydrolyzing oils such as natural vegetable oils such as avocado oil, sesame oil, rice germ oil, macadamia nut oil, and animal oils such as fish oil and butter.
  • preferable cholesterol derivatives include cholesteryl hydroxystearate, polyoxyethylene cholesteryl ether, and the like. Among these cholesterol or derivatives thereof, cholesterol is preferable.
  • phytosterol is a general term for sterol compounds obtained from plants.
  • specific examples of phytosterols include sitosterol, stigmasterol, fucostosterol, spinasterol, and brush castrol.
  • phytosterol derivatives include ester derivatives of saturated or unsaturated fatty acids such as oleic acid, palmitooleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, lauric acid, olive oil, avocado, etc. And esterified derivatives with a mixture of fatty acids obtained by hydrolyzing natural vegetable oils such as oil, sesame oil, rice germ oil and macadamia nut oil.
  • Specific examples of preferred phytosterol derivatives include phytosteryl hydroxystearate, polyoxyethylene phytosterol, polyoxyethylene phytostanol and the like. Among these phytosterols or derivatives thereof, phytosterol is preferable.
  • amino acids include N-acyl amino acids such as N-lauroyl-L-lysine and amino acids such as theanine.
  • fatty acids include saturated fatty acids such as lauric acid, myristic acid, palmitic acid and stearic acid and salts thereof, and unsaturated fatty acids such as oleic acid and salts thereof.
  • the metal oxide used in the production of the metal oxide composite high flat cellulose powder of the present invention can be used in general cosmetics as long as it is blended as a powder component such as extender pigment or colored pigment. It can be used without any particular restrictions.
  • the metal oxide include iron oxide, titanium oxide, zinc oxide, cerium oxide and the like. These metal oxides can also be used singly or in combination of two or more.
  • the particle diameter of the metal oxide is preferably 10 to 10,000 nm, but some of the effects obtained will differ depending on the average particle diameter on the obtained metal oxide composite high flat cellulose powder. In view of this point, it is desirable to select the particle size of the raw metal oxide.
  • the amount of the grinding aid added to the whole of the above components is 0.5 to 5%, preferably 1 to 3%.
  • the total amount of metal oxide is 5 to 50%, preferably 20 to 40%.
  • pulverization aids and metal oxides can be added to the cellulosic material at any time before the pulverization treatment, and the addition method can be added separately even if the pulverization aid and metal oxide are added simultaneously. May be added.
  • a method for adding the grinding aid it may be dissolved in a suitable solvent and then added to the cellulosic material.
  • the solvent used for dissolving the grinding aid include alkanes such as hexane, alcohols such as ethanol, ketones such as acetone, ethers such as tetrahydrofuran, aromatic hydrocarbons such as toluene, and the like.
  • a pulverizing apparatus such as a vibration ball mill, a rotating ball mill, a planetary ball mill, a roll mill, a media mill, a disk mill, a high-speed mixer using high-speed rotating blades, a homomixer, etc., and a planetary ball mill is particularly preferable.
  • the pulverization method is preferably dry pulverization without using a solvent. Note that the crushing energy applied in the crushing process (in the case of a planetary ball mill, the gravitational acceleration applied to the planetary ball mill) is 3 to 20 G, preferably 5 to 15 G.
  • the particle size, thickness, and flatness (aspect ratio) of the metal oxide composite high flattened cellulose powder are important. Since the diameter is also important depending on the application, the pulverization time must be determined in consideration of these. This relationship is related to the target flat cellulose itself, the particle size of the metal oxide as a raw material, and the like, so it is desirable to experimentally determine pulverization conditions, pulverization time, and the like in advance.
  • the purified cellulose pulp-derived cellulose powder is dried under reduced pressure at 30 to 50 ° C. to sufficiently remove the adsorbed moisture to 0.1% or less.
  • This cellulose powder is put into a sealable alumina or zirconia grinding container together with alumina or zirconia grinding balls, and further, a grinding aid and a metal oxide powder are added so as to have the above amount with respect to the cellulose powder.
  • the pulverization container is placed in a planetary ball mill, and pulverization is performed at a rotational speed of 100 to 250 rpm.
  • the pulverization treatment may be repeated for about 2 to 72 cycles continuously, with 5 to 15 minutes of pulverization-5 to 15 minutes of rest, or for about 5 to 120 minutes without interruption. May be.
  • moisture adhering to the metal oxide composite high flattened cellulose powder may be further removed by a known drying means such as air drying, hot air drying, vacuum drying, and reduced pressure drying.
  • the metal oxide composite high flattened cellulose powder obtained as described above has, for example, an average particle diameter of 1 to 50 ⁇ m, preferably 5 to 40 ⁇ m, and an average thickness of 0.1 to 10 ⁇ m, preferably 0. It has a flake shape of 2 to 2 ⁇ m and a flatness of 4 to 200, preferably 10 to 100.
  • the average particle size is the average value of the width and length of the flat cellulose particles measured in a dispersion state in ethanol using a particle size distribution measuring device such as a laser diffraction / scattering type particle size distribution measuring device. (Particle size value of 50% cumulative volume).
  • the average thickness refers to a value obtained by selecting a plurality of particles having the same size as the average particle size obtained above with an electron microscope such as a scanning electron microscope, measuring the thickness, and averaging the values.
  • the flatness is the average particle diameter / average thickness determined as described above.
  • the particle size of the composite metal oxide can also be measured with a scanning electron microscope.
  • the metal oxide composite high flat cellulose powder obtained in this way has a particle size of the metal oxide that is firmly adhered and composited more than 100 nm and not more than 1000 nm (pigment grade size). In some cases, this is a case of 10 to 100 nm (fine particle size), and the properties are slightly different, and the applications are also different. That is, when the composite metal oxide is a fine particle class, an extremely excellent UV blocking effect and uniformity of the decorative film can be obtained. Further, when the composite metal oxide is a pigment grade, excellent color developability can be obtained. Since the particle size of the metal oxide hardly changes before and after the compounding, the particle size of the metal oxide added before the compounding and the particle size of the metal oxide after the compounding are almost the same.
  • this metal oxide composite high flat cellulose powder also has the smooth feeling of use originally possessed by the high flat cellulose powder, the cosmetic compounded with this has an excellent cosmetic film. It has a uniform and smooth use feeling, an excellent UV blocking effect and a color developing effect, and also has an excellent makeup sustaining effect such as no color sink.
  • the resulting metal oxide composite high flattened cellulose powder has a thin flake shape compared to the conventional extender pigments talc and sericite, and has excellent properties such as transparency, softness, elongation, and natural gloss.
  • many cosmetics that use powder examples thereof include various cosmetics such as basic (skin care) cosmetics, makeup cosmetics, sunscreen cosmetics, hair cosmetics, and the like.
  • powder cosmetics such as powder foundation, liquid foundation, eye shadow, cheek red, powdered white powder and the like and sunscreens, cosmetics requiring UV blocking effect such as makeup base.
  • Preparation of a cosmetic compounded with the metal oxide composite high flattened cellulose powder of the present invention is carried out by combining it with a suitable cosmetic base and formulating it.
  • a suitable cosmetic base for example, when the cosmetic is a powder cosmetic, the metal oxide composite high flatness of the present invention is used instead of a part or all of the conventional powder component in the same manufacturing method as that of the conventional powder cosmetic.
  • Cellulose powder may be used.
  • the blending amount of the metal oxide composite high flat cellulose powder in the cosmetic is 1 to 90%, preferably 5 to 90%, particularly preferably 5 to 70%.
  • an oil component as a cosmetic base.
  • the oily ingredients blended in this cosmetic but for example, paraffin wax, ceresin wax, ozokerite, microcrystalline wax, montan wax, fisher trops wax, polyethylene wax, liquid paraffin, squalane, petrolatum, Hydrocarbons such as polyisobutylene and polybutene, natural waxes such as carnauba wax, beeswax, lanolin wax and candelilla, glyceryl tribehenate, rosin acid pentaerythritol ester, jojoba oil, cetyl isooctanoate, isopropyl myristate, trioctanoic acid Esters such as glyceryl, diglyceryl triisostearate, dipentaerythritol fatty acid esters, fatty acids such as stearic acid, behenic acid, 12-hydroxystearic acid Higher alcohols such as cetan
  • inorganic powder such as talc and organic powder such as nylon
  • organic powder such as nylon
  • an inorganic powder or an organic powder may be added and dispersed together with the metal oxide composite high flat cellulose powder of the present invention, and oil may be added as necessary.
  • the above cosmetics include components used in normal cosmetics, for example, surfactants, oil gelling agents, water-soluble components such as polyhydric alcohols and humectants, and ultraviolet absorbers as necessary.
  • preservatives, cosmetic ingredients, fragrances, and the like can be appropriately blended within a range not impairing the effects of the present invention.
  • the properties and dosage forms of the cosmetics are not particularly limited and can be selected according to the purpose.
  • the properties of the cosmetic of the present invention may be any of liquid, powder, solid, emulsion, cream, gel and the like, and the dosage form is aqueous, oily, solubilized, in oil Any dosage form such as a water mold and an oil-in-water mold may be used.
  • FIGS. 1 to 3 are obtained by observing the surface of the product 6 obtained in Example 6 with a scanning electron microscope. In FIG. 1 where the magnification is about 10,000 times, the fine zinc oxide is completely observed. Can not. However, when the magnification is increased to 50,000 times, fine zinc oxide begins to appear white on the surface, and at a magnification of 200,000, fine zinc oxide of about 20 nm is observed on the mother powder.
  • the fine particle zinc oxide does not aggregate on the surface of the metal oxide composite high flat cellulose powder of the present invention, and is relatively primary particles. It can be understood that it is compounded in the state of. That is, on the metal oxide composite high flattened cellulose powder, the presence of the metal oxide in a primary particle state that can exert its action to the maximum is considered to be the reason that the performance is remarkably improved.
  • the reason why the metal oxide is composited in a primary particle state is not yet clear. Since the fine metal oxide powder is present on the spot where it is formed and stirred with a high share, it adheres on the cellulose surface just preferentially formed and has a strong bond. It is understood that there is not.
  • Example 1 Production of Lauroyllysine-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (1) (1) As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL).
  • the average particle diameter, thickness, and flatness of the product 1 were measured as follows. That is, using a laser diffraction / scattering type particle size distribution measuring apparatus (Horiba: LA-920), the average particle diameter (width and length on the apparatus of the width and length) of the obtained powder in a dispersed state in ethanol in a flow cell. The average value was determined. As the average particle size, a particle size value with an integrated volume of 50% was used. In the particle size distribution measurement, a suspension in which 50 mg of the obtained powder was dispersed in 10 mL of ethanol was dropped into a sample circulation tank using ethanol as a medium in the particle size distribution measurement device, and after reaching an appropriate concentration. It was measured. As a result, the average particle size of the powder was 16 ⁇ m.
  • the average thickness of the obtained particles was determined by directly observing the particles using a scanning electron microscope (S-2150, manufactured by Hitachi, Ltd.) and selecting a plurality of particles having a size equivalent to the average particle size obtained above. The thickness was measured and averaged.
  • a scanning electron microscope In observation with a scanning electron microscope, a very small amount of the obtained powder was placed on a sample stage of a scanning electron microscope, dried under reduced pressure, and platinum was deposited to obtain a spectroscopic sample. From the image obtained by observing the microscopic sample at an acceleration voltage of 10 to 25 kV and an enlargement ratio of 500 to 10,000 times, the thickness of particles having a size equivalent to the average particle size measured above was measured, The average thickness was determined from them. As a result, the average thickness was 1.7 ⁇ m.
  • the product 1 has an average particle diameter of 16 ⁇ m, an average thickness of 1.7 ⁇ m, and a flat cellulose particle (lauroyllysine-treated fine particle titanium oxide composite) having a flatness (average particle diameter / average thickness) of 9.4.
  • Flat cellulose powder Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 2 Production of Lauroyllysine-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (2): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) and 28 g of fine titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) were added.
  • the obtained product 2 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle size was 15 ⁇ m
  • the average thickness was 1.0 ⁇ m
  • the particle size / average thickness was 15 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 3 Production of hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder (3): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 14 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) were added.
  • Resinol S-10 manufactured by Nikko Chemicals
  • TTO-S-4 fine particle titanium oxide
  • the obtained product 3 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 16 ⁇ m
  • the average thickness was 1.9 ⁇ m
  • the particle size / average thickness was 8.4. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 4 Production of hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder (4):
  • purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used.
  • cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls.
  • the obtained product 4 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 15 ⁇ m
  • the average thickness was 1.2 ⁇ m
  • the particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 5 Production of Ceramide-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (5):
  • purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used.
  • cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls.
  • 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) were added.
  • the obtained product 5 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 16 ⁇ m
  • the average thickness was 1.2 ⁇ m
  • the particle size / average thickness was 13.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 6 Production of Lauroyllysine-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (6): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL).
  • the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2).
  • the average particle diameter was 16 ⁇ m
  • the average thickness was 1.7 ⁇ m
  • the particle size / average thickness was 9.4. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 7 Production of Lauroyllysine-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (7): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) and 28 g of fine zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) were added.
  • alumina crushing container capacity 500 mL
  • ZnO-610 fine zinc oxide
  • the obtained product 7 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 15 ⁇ m
  • the average thickness was 1.0 ⁇ m
  • the particle size / average thickness was 15 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 8 Production of hydrogenated lecithin-treated fine zinc oxide composite high flat cellulose powder (8): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of fine zinc oxide (ZnO-610 manufactured by Sumitomo Osaka Cement) were added.
  • the obtained product 8 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle size was 15 ⁇ m
  • the average thickness was 1.2 ⁇ m
  • the particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 9 Production of Ceramide-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (9): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) were added.
  • ceramide Ceramide II Wako Pure Chemical Industries, Ltd.
  • ZnO-610 fine particle zinc oxide
  • the obtained product 9 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 15 ⁇ m
  • the average thickness was 1.2 ⁇ m
  • the particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 10 Production of hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (10): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) (average particle size 250 nm) were added.
  • the obtained product 10 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 18 ⁇ m
  • the average thickness was 2.2 ⁇ m
  • the particle size / average thickness was 8.2. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 11 Production of hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (11): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added.
  • the obtained product 11 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 17 ⁇ m
  • the average thickness was 1.5 ⁇ m
  • the particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 12 Production of ceramide-treated titanium oxide composite high flat cellulose powder (12): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added.
  • the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2).
  • the average particle diameter was 18 ⁇ m
  • the average thickness was 2.2 ⁇ m
  • the particle size / average thickness was 8.2. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 13 Production of ceramide-treated titanium oxide composite high flat cellulose powder (13): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added.
  • the obtained product 13 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 17 ⁇ m
  • the average thickness was 1.5 ⁇ m
  • the particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 14 Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (14): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, 41.3 g (59%) of cellulose powder from which adsorbed moisture has been sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C. is placed in an alumina crushing container (capacity 500 mL) in an alumina crushing ball.
  • alumina crushing container capacity 500 mL
  • the obtained product 14 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle size was 17 ⁇ m
  • the average thickness was 1.5 ⁇ m
  • the particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 15 Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (15): In the same manner as in Example 14, purified wood pulp-derived cellulose powder (W-400G) 59%, ceramide (Ceramide II) 1%, titanium oxide (TITANIX JR-800) 38.2%, red iron oxide ( A ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 15) was obtained using 0.45% of Tarox R-516P) and 1.35% of yellow iron oxide (Tarox synthetic iron oxide YP1200P).
  • the obtained product 15 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 17 ⁇ m
  • the average thickness was 1.5 ⁇ m
  • the particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 16 Manufacture of stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (16): In the same manner as in Example 14, 57% of purified wood pulp-derived cellulose powder (W-400G), 3% of stearic acid instead of ceramide, 38.2% of titanium oxide (TITANIX JR-800), red iron oxide (Tarox R-516P) 0.45% and yellow iron oxide (Tarox synthetic iron oxide YP1200P) 1.35% were used to obtain stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 16). It was.
  • the obtained product 16 was measured for the average particle size, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle size was 17 ⁇ m
  • the average thickness was 1.1 ⁇ m
  • the particle size / average thickness was 15.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 17 Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (17): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls.
  • alumina crushing container capacity 500 mL
  • the obtained product 17 was measured for the average particle size, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle size was 17 ⁇ m
  • the average thickness was 1.5 ⁇ m
  • the particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Comparative Example 1 Manufacture of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (1): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added.
  • the obtained ceramide-treated high flattened cellulose powder 60 g
  • 30 g of titanium oxide manufactured by TITANIX JR-800 Teika
  • 1.25 g of red iron oxide Tirox R-516P manufactured by Titanium Industry Co., Ltd.
  • yellow oxide Iron Tearox synthetic iron oxide YP1200P manufactured by Titanium Industry Co., Ltd.
  • ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture Comparative product 1 Got.
  • Example 1 The average particle diameter was 19 ⁇ m, the average thickness was 1.4 ⁇ m, and the flatness ( The average particle diameter / average thickness was 13.6.
  • Comparative Example 2 Manufacture of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (2): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added.
  • the obtained comparative product 2 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 19 ⁇ m
  • the average thickness was 1.4 ⁇ m
  • the flatness The average particle diameter / average thickness was 13.6.
  • Example 2 The average particle diameter was 19 ⁇ m, the average thickness was 1.4 ⁇ m, and the flatness ( The average particle diameter / average thickness was 13.6.
  • Example 2 The average particle diameter was 19 ⁇ m, the average thickness was 1.4 ⁇ m, and the flatness ( The average particle diameter / average thickness was 13.6.
  • Comparative Example 5 Production of hydrogenated lecithin-treated high flattened cellulose (5): As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) was added.
  • the obtained comparative product 5 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 19 ⁇ m
  • the average thickness was 1.4 ⁇ m
  • the flatness The average particle diameter / average thickness was 13.6.
  • Titanium oxide / iron oxide composite cellulose powder (6) 60% by mass of refined wood pulp-derived cellulose powder (W-400G) was put in a planetary ball mill (Misho Industry Co., Ltd.), and 38.2% titanium oxide (TITANIX JR-800), red iron oxide ( Add 0.45% of Tarox R-516P) and 1.35% of yellow iron oxide (Tarox synthetic iron oxide YP1200P), and crush for 40 minutes at a rotation speed of 200 rpm (crushing energy of about 10 G (gravity acceleration)). Then, a titanium oxide / iron oxide composite cellulose powder (Comparative Product 6) was obtained.
  • the obtained comparative product 6 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 18 ⁇ m
  • the average thickness was 2.0 ⁇ m
  • the flatness The average particle size / average thickness was 9.0. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2).
  • the average particle diameter was 7.0 ⁇ m
  • the average thickness was 1.0 ⁇ m
  • the flatness was measured.
  • the degree (average particle diameter / average thickness) was 7.0. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • the obtained comparative product 8 was measured for the average particle diameter, thickness, and flatness in the same manner as in Example 1 (2).
  • the average particle diameter was 7.0 ⁇ m
  • the average thickness was 0.7 ⁇ m
  • the flatness was measured.
  • the degree (average particle diameter / average thickness) was 10.0 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
  • Example 18 UV blocking test (1) The UV blocking ability of the finely divided titanium oxide composite high flat cellulose powder (Product 1 and Product 2) produced in Examples 1 and 2 was examined. In the experiment, 0.04 g of each powder was uniformly applied to a transpore tape (5 cm ⁇ 8 cm) so as to be 1 mg / cm 2, and the UV blocking ability in the region of 300 to 450 nm was measured with an SPF analyzer (manufactured by Sanyo Trading Co., Ltd.). ). For comparison, comparative product 3 was used. The results are shown in Table 1.
  • the products 1 and 2 of the present invention have an SPF value of about 5 times higher than that of the high flat cellulose powder mixed with fine particle titanium oxide (Comparative Product 3), and have a UV blocking ability. It was an excellent powder.
  • Example 19 UV blocking test (2) The UV blocking ability of the fine zinc oxide composite high flat cellulose powder (Products 6 to 9) produced in Examples 6 to 9 was examined in the same manner as in Example 18. For comparison, the comparative product 4 was used. The results are shown in Table 2.
  • the product 6 of the present invention has an SPF value that is about twice or more higher than that of the highly flat cellulose powder mixed with fine zinc oxide (Comparative Product 4). About 3 times higher, the powder of the present invention was excellent in UV blocking ability.
  • Example 20 Color change test The powders prepared in Examples 15 and 16 and Comparative Examples 6 to 8 were tested for color change.
  • each powder was thoroughly mixed with the same weight of oil (glyceryl tri-2-ethylhexanoate) with a spatula to prepare a test sample.
  • the color value (a value; redness / b value; yellowness) is measured with a spectral color difference meter SE-2000 (manufactured by Nippon Denshoku Kogyo Co., Ltd.). ) Respectively.
  • Color changeability ⁇ (( ⁇ a) 2 + ( ⁇ b) 2 )
  • ⁇ a means the difference between a1 and a2
  • ⁇ b means the difference between b1 and b2.
  • the product 15 and the product 16 of the present invention were excellent with little color change even when mixed with oil.
  • comparative product 6 without using a grinding aid comparative product 7 in which dimethylpolysiloxane-treated sericite is the base powder, dimethylpolysiloxane-treated talc Comparative product 8, which is a mother powder, was greatly inferior in color change when mixed with oil.
  • Example 21 Powder foundation (1) Using the finely divided titanium oxide composite high flattened cellulose powders (Products 1 to 5) produced in Examples 1 to 5, powder foundations of the cosmetics 1 to 5 of the present invention were prepared by the formulation shown in Table 4 and the following method. About this powder foundation, UV blocking ability, SPF value, uniformity of makeup film, natural finish (no whitening), makeup lasting, stability (presence of aggregates), and feeling of use (when applying) Smoothness).
  • Test method UV blocking ability and SPF value: The UV blocking ability of the powder foundations produced with the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2 was examined. In the experiment, 0.04 g of each powder was uniformly applied to a transpore tape (5 cm ⁇ 8 cm) so as to be 1 mg / cm 2, and the UV blocking ability in the region of 300 to 450 nm was measured with an SPF analyzer (Sanyo Trading Co., Ltd.). ). In addition, evaluation was implemented by the following determination.
  • Evaluation content A SPF is 25 or more.
  • ⁇ SPF is 20 or more and less than 25.
  • ⁇ SPF is 15 or more and less than 20.
  • X SPF is less than 15.
  • Judgment criteria (Average score): (Judgment) 5.0 or more: ⁇ (very good) 3.5 or more and less than 5.0: ⁇ (good) 1.5 or more and less than 3.5: ⁇ (somewhat poor) Less than 1.5: ⁇ (defect)
  • Stability was evaluated by the presence or absence of aggregates.
  • the surface state after 20 times of surface coating was visually observed using a cosmetic sponge.
  • evaluation was implemented by the following determination.
  • Evaluation content A Aggregates are not observed. ⁇ : Aggregates are observed, but the amount is small. ⁇ : Agglomerates are observed and the amount is large. X: Large aggregates are observed and the amount is large.
  • the powder foundations of the cosmetics 1 to 5 of the present invention have a high SPF value, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), long-lasting makeup ( The powder foundation was excellent in all the items of adhesion and no color change), stability (presence / absence of aggregates), and feeling of use (smoothness during application).
  • the powder foundation of the comparative cosmetic 1 in which the product 1 of the cosmetic 1 of the present invention is replaced with the conventional fine particle titanium oxide composite mica shows agglomeration of the powder, and the uniformity of the cosmetic film, the natural finish, etc. It was inferior.
  • the powder foundation of the comparative cosmetic 2 in which the product 1 of the cosmetic 1 of the present invention is replaced with the comparative product 3 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application). Was inferior.
  • Example 22 Powder foundation (2): Using the fine zinc oxide composite high flat cellulose powder produced in Examples 6 to 9, powder foundations of the cosmetics 6 to 9 of the present invention were prepared according to the formulation shown in Table 5 and the following method. About this powder foundation, it carried out similarly to Example 21, and investigated UV blocking ability, SPF value, the uniformity of a cosmetic film, the natural finish (no powder whiteness), makeup lasting, usability, and stability.
  • the powder foundation of the cosmetics 6 to 9 of the present invention has a high SPF value, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), long-lasting makeup,
  • the powder foundation was excellent in all items of stability (presence / absence of aggregates) and feeling of use (smoothness during application).
  • the powder foundation of the comparative cosmetic 3 in which the product 6 of the cosmetic 6 of the present invention is replaced with the fine particle zinc oxide-coated mica / barium sulfate composite powder shows agglomeration of the powder, uniformity of the cosmetic film and natural The finish was inferior.
  • the powder foundation of the comparative cosmetic 4 in which the product 6 of the cosmetic 6 of the present invention is replaced with the comparative product 4 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application).
  • the powder foundation of the comparative cosmetic 4 in which the product 6 of the cosmetic 6 of the present invention is replaced with the comparative product 4 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application).
  • Example 23 Powder foundation (3) Using the titanium oxide composite high flattened cellulose powders (Products 10 to 13) produced in Examples 10 to 13, powder foundations of the cosmetics 10 to 13 of the present invention were prepared by the formulation shown in Table 6 and the following method. The powder foundation was examined for concealment by the following method, and in the same manner as in Example 21, the uniformity of the cosmetic film, the cosmetic durability and the feeling of use were examined. For comparison, high-flat cellulose powder and titanium oxide (comparative cosmetics 5 and 6) were used separately. The results are also shown in Table 6.
  • Test method 20 panelists specializing in cosmetics evaluation use the powder foundations of the present cosmetics 10 to 13 and comparative cosmetics 5 and 6, and each of them evaluates the “concealment” in 7 levels according to the following evaluation criteria. A rating was given. Next, each product was determined from the average score of all panels according to the following criteria.
  • Judgment criteria (Average score): (judgment) 5.0 or more: ⁇ (very good) 3.5 or more and less than 5.0: ⁇ (good) 1.5 or more and less than 3.5: ⁇ (somewhat poor) Less than 1.5: ⁇ (defect)
  • the powder foundation of the cosmetics 10 to 13 of the present invention is a powder foundation that is excellent in all items of uniformity of the cosmetic film, concealment, makeup lasting, and feeling of use (smoothness during application). It was.
  • the comparative cosmetic 5 in which the titanium oxide having almost the same mass as that of the cosmetic 10 of the present invention is mixed and mixed with other components without treatment is poor in dispersion of titanium oxide, has poor makeup, and has concealment and use.
  • the feeling (smoothness during application) was also inferior.
  • the comparative cosmetic 6 containing double amount of titanium oxide has a concealing property, the feeling of use (smoothness at the time of application), the uniformity of the cosmetic film, and the longevity of the makeup are poor.
  • Example 24 Powder foundation (4) Using the titanium oxide / iron oxide composite high flattened cellulose powder (Products 14 and 15) produced in Examples 14 to 15, the powder foundations of the cosmetics 14 and 15 of the present invention were prepared by the formulation shown in Table 7 and the following method. . The powder foundation was examined for color development by the following method, and in the same manner as in Example 21, the uniformity of the cosmetic film, the cosmetic durability and the feeling of use were examined.
  • Test method Color development: 20 panelists specializing in cosmetics evaluation use the powder foundations of the present cosmetics 14 to 15 and comparative cosmetics 7 and 8, and each of them evaluates their “color development” in 7 stages according to the following evaluation criteria. Was given a score. Next, each product was determined from the average score of all panels according to the following criteria.
  • Judgment criteria (Average score): (judgment) 5.0 or more: ⁇ (very good) 3.5 or more and less than 5.0: ⁇ (good) 1.5 or more and less than 3.5: ⁇ (somewhat poor) Less than 1.5: ⁇ (defect)
  • the powder foundations of the cosmetics 14 and 15 of the present invention are powder foundations that are excellent in all items of uniformity of the cosmetic film, concealment, makeup lasting, and feeling of use (smoothness during application). It was.
  • comparative cosmetics 7 and 8 containing a mixture of titanium oxide or iron oxide mixed with cellulose powder had particularly poor color development and long lasting makeup.
  • Example 25 Powder foundation (5) Using the fine zinc oxide composite high flat cellulose powder (Product 7) produced in Example 7, a powder foundation of the cosmetic 16 of the present invention was prepared according to the formulation shown in Table 8 and the following method.
  • the SPF value was determined by the following method, and in the same manner as in Example 21, UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), makeup retention, stability (of aggregates) Existence) and usability (smoothness during application) were examined.
  • a cosmetic (comparative cosmetic 9) using the flat cellulose powder of Comparative Example 4 and a fine particle zinc oxide mixture was used. The results are shown in Table 8.
  • part the site
  • a test sample was applied to 50 cm 2 of this test site. The coating amount was 2.00 mg / cm 2 ⁇ 2.5% / cm 2 .
  • the test sample application site of the subject was irradiated with ultraviolet rays using a xenon arc solar simulator (manufactured by SOLAR LIGHT) as a light source.
  • This xenon arc simulator has a continuous spectrum similar to that of sunlight in the UV-B and UV-A regions with wavelengths of 290 to 400 nm. Further, ultraviolet rays having a wavelength of 290 nm or less were removed as much as possible using a filter.
  • the occurrence of erythema at the site irradiated with ultraviolet rays was examined in a sufficiently bright room.
  • the minimum amount of ultraviolet irradiation that initially causes slight erythema with a clear boundary at 2/3 or more of the irradiated region was defined as the minimum erythema dose (MED).
  • MED minimum erythema dose
  • SPF value MED (sample application part) / MED (sample non-application part)
  • the powder foundation of the cosmetic 16 of the present invention has a higher SPF measured value than the comparative cosmetic 9, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (powder whiteness) No powder), makeup lasting (no adhesion and no color change), stability (presence of agglomerates), and feeling of use (smoothness during application) were excellent powder foundations.
  • the powder foundation of the comparative cosmetic 9 in which the product 7 of the cosmetic 16 of the present invention is replaced with a lauroyl lysine-treated high flattened cellulose powder / particulate zinc oxide mixture has a slightly low SPF measured value and UV blocking ability, All items, such as a feeling of use (smoothness at the time of application
  • Example 26 Powder foundation (6) Using the pigments of the product 14 prepared in Example 14 and the product 15 prepared in Example 15, powder foundations were prepared by the following method according to the composition described in Table 9 below (Formulations 1 to 3). As a comparison, the one using iron oxide not subjected to special treatment was used (comparison prescription). In addition, as for the total amount of iron oxide in each prescription in a present Example, the composition 1 is the same amount (100%) as a comparison prescription, and the compositions 2 and 3 are 80% of a comparison prescription.
  • Color development For each formulation, the measured a and b values were compared to the comparative formulation a and b values (as and bs) to determine the difference ( ⁇ a and ⁇ b). After ⁇ a and ⁇ b were squared and added, the value was opened with a square root, and the value was used as an evaluation value of “color development”. For this evaluation value, 1 or more was evaluated as ⁇ , 0.5 or more and less than 1 as ⁇ , 0.25 or more and less than 0.5 as ⁇ , and less than 0.25 as ⁇ .
  • Makeup (no color sink): Immediately after application and 2 hours after application, the values of L, a, and b of the appearances of the present invention and comparative formulations were determined. The difference between the measured values immediately after application in each formulation and 2 hours after application ( ⁇ L 0-2 , ⁇ a 0-2 and ⁇ b 0-2 ) was squared, and after adding them, the square root was opened. This value was used as an evaluation value for “long makeup (no color sinking)”. With respect to this evaluation value, 0 or more and 1 or less were evaluated as ⁇ , 1 and 1.5 or less were evaluated as ⁇ , 1.5 or more and 2 or less as ⁇ , and 2 or more as x.
  • the formulation 1 in which the same amount of iron oxide as the comparative formulation was blended in the overall formulation using the product 14 of Example 14 was higher in color development than the comparative formulation, and the application 2 The color settling after time was small and the adhesion was excellent.
  • Formula 2 in which the compounding amount of iron oxide is reduced from Formula 1 and the compounding amount of iron oxide is 80% of the comparative formulation is less than that of the comparative formulation, although the compounding amount of iron oxide is smaller than that of the comparative formulation.
  • Excellent color development and other items were also excellent.
  • the formulation 3 using the product 15 of Example 15 and having the compounding amount of iron oxide 80% of the comparative formulation as in the formulation 2 also had good color development and other items.
  • Example 27 Double layer lotion A two-layer lotion having the following composition was produced by the following method.
  • the obtained two-layer lotion was excellent in powder dispersibility, a smooth feeling in use, and a two-layer lotion excellent in the uniformity of the decorative film.
  • Example 28 Milk liquid: An emulsion having the composition shown below was produced by the following method.
  • the obtained emulsion was excellent in emulsification stability, smooth use feeling, uniformity of decorative film, and excellent UV blocking ability.
  • Example 29 cream A cream having the following composition was produced by the following method.
  • the obtained cream was excellent in emulsification stability, smooth use feeling, uniformity of cosmetic film, and excellent UV blocking ability.
  • Example 30 Beauty liquid A serum having the following composition was produced by the following method.
  • the obtained essence was excellent in stability, smooth sensation of use, uniformity of cosmetic film, and essence excellent in UV blocking ability.
  • Example 31 Pack A pack having the composition shown below was produced by the following method.
  • the obtained pack was excellent in emulsification stability, smooth in feeling of use, and excellent in uniformity of the decorative film.
  • Example 32 Facial wash A face wash having the composition shown below was produced by the following method.
  • the obtained facial cleanser was an excellent facial cleanser.
  • Example 33 Cleansing cream A cleansing cream having the following composition was produced by the following method.
  • the obtained cleansing cream was excellent in emulsification stability and excellent in smooth use feeling.
  • Example 34 Hair wax A hair wax having the following composition was produced by the following method.
  • the obtained hair wax was excellent in emulsification stability and hair styling property, and was a hair wax excellent in smooth use feeling and UV blocking ability.
  • Example 35 Oily eyeliner An oily eyeliner having the following composition was produced by the following method.
  • the obtained oily eyeliner was an oily eyeliner excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.
  • Example 36 Aqueous eyeliner: An aqueous eyeliner having the composition shown below was produced by the following method.
  • the obtained water-based eyeliner was a water-based eyeliner excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.
  • Example 37 Eyebrow An eyebrow having the following composition was produced by the following method.
  • the obtained eyebrow was an eyebrow excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.
  • Example 38 O / W type mascara: An O / W type mascara having the following composition was produced by the following method.
  • the obtained O / W type mascara was excellent in powder dispersibility, and was an O / W type mascara excellent in smooth feeling of use, uniformity of the cosmetic film, and makeup lasting effect.
  • Example 39 Non-aqueous mascara: A non-aqueous mascara having the following composition was produced by the following method.
  • the obtained non-aqueous mascara was a non-aqueous mascara excellent in smooth use feeling, uniformity of the cosmetic film, and a makeup lasting effect.
  • Example 40 Sticky lipstick: A stick-shaped lipstick having the following composition was produced by the following method.
  • the obtained stick-shaped lipstick was a lipstick with a smooth feeling of use, uniformity of the cosmetic film, and excellent makeup lasting effect.
  • Example 41 Liquid Rouge: A liquid rouge having the following composition was produced by the following method.
  • the obtained liquid rouge was a liquid rouge excellent in smooth feeling of use, uniformity of the makeup film, and makeup lasting effect.
  • Example 42 O / W type foundation: An O / W type foundation having the following composition was produced by the following method.
  • the obtained O / W type foundation was excellent in powder dispersibility, and was an O / W type foundation excellent in smooth use feeling, uniformity of cosmetic film, hiding property, UV blocking ability, and makeup lasting effect.
  • Example 43 W / O type foundation A W / O type foundation having the following composition was produced by the following method.
  • the obtained W / O-type foundation was excellent in powder dispersibility, and was a W / O-type foundation excellent in smooth feeling of use, cosmetic film uniformity, hiding properties, UV blocking ability, and makeup lasting effect.
  • Example 44 O / W eye color: An O / W eye color having the following composition was produced by the following method.
  • the obtained O / W type eye color was excellent in powder dispersibility, and was an O / W type eye color excellent in smooth feeling of use, uniformity of the cosmetic film, color developability, and makeup lasting effect.
  • Example 45 Oil solid foundation: An oily solid foundation having the following composition was produced by the following method.
  • the obtained oil-based solid foundation was excellent in powder dispersibility, had a smooth feeling of use, and was excellent in the uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.
  • Example 46 Stick concealer A stick concealer having the following composition was produced by the following method.
  • the obtained stick-like concealer was excellent in powder dispersibility, and was a stick-like concealer excellent in smooth feeling of use, makeup film uniformity, hiding property, UV blocking ability, and makeup lasting effect.
  • Example 47 Body milk: Body milk having the following composition was produced by the following method.
  • the obtained body milk was excellent in emulsification stability, and was excellent in smooth use feeling, uniformity of cosmetic film, UV blocking ability, and makeup lasting effect.
  • Example 48 conditioner A conditioner having the following composition was produced by the following method.
  • the obtained conditioner was excellent in emulsification stability and excellent in smooth use feeling.
  • Example 49 Hair pack A hair pack having the composition shown below was produced by the following method.
  • the obtained hair pack was excellent in emulsification stability and was excellent in smooth usability.
  • Example 50 W / O sunscreen A sunscreen with the composition shown below was produced by the following method.
  • the obtained W / O type sunscreen was excellent in powder dispersibility, and was excellent in smooth use feeling, uniformity of cosmetic film, UV blocking ability, and makeup lasting effect.
  • Example 51 Manicure: A nail polish having the following composition was produced by the following method.
  • the obtained nail polish was excellent in powder dispersibility, smooth maneuverability, uniformity of the cosmetic film, and excellent makeup lasting effect.
  • Example 52 Makeup base A makeup base having the following composition was produced by the following method.
  • the obtained makeup base was excellent in emulsification stability, and was excellent in smooth use feeling, uniformity of makeup film, UV blocking ability, and makeup lasting effect.
  • Example 53 White powder having the following composition was produced by the following method.
  • the obtained white powder was excellent in powder dispersibility, and was excellent in smooth use feeling, uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.
  • Example 54 Solid powder foundation: A solid powder type foundation having the following composition was produced by the following method.
  • the obtained solid powder type foundation was excellent in powder dispersibility, and had a smooth feeling in use, uniformity of a cosmetic film, UV blocking ability, and a makeup lasting effect.
  • Example 55 Solid powder type teak: A solid powder type cheek having the composition shown below was produced by the following method.
  • the obtained solid powder type cheek was excellent in powder dispersibility, excellent in smooth use feeling, uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.
  • Example 56 Solid powder eyeshadow: A solid powder eye shadow having the following composition was produced by the following method.
  • the obtained solid powder type eye shadow was excellent in powder dispersibility, and had a smooth feeling in use, a makeup film uniformity, color development, and a makeup lasting effect.
  • the base cellulose itself is an organic substance and is flat, the surface thereof is composited with extremely fine metal oxide particles.
  • powders made by combining talc and sericite, which are flat inorganic materials, with metal oxides they have higher adhesion, excellent usability, and excellent UV blocking ability and coloring ability due to metal oxides It is.
  • the metal oxide-complexed high flat cellulose powder of the present invention can be used in many cosmetics.
  • cosmetics that easily exhibit the effect include powder foundation, eye shadow, blusher, powdered white powder, etc.
  • cosmetics containing the powder component and the oil component are preferable, and powder foundations and eye shadows are particularly preferable.
  • the cosmetic of the present invention is a powder foundation and eye shadow, there is no powderiness, good wet feeling, good adhesion to the skin, and as a result, it blends naturally with the skin, unevenness, twist, color It will have good makeup without dullness or float.

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Abstract

The purpose of the present invention is to provide a powder for a cosmetic having, when compared to conventional powders for cosmetics, a better skin feel, and high functionality such as a UV blocking ability, and also to provide a cosmetic using the same. The cosmetic is a metal oxide conjugated highly-flat cellulose powder obtained by mechanically grinding a cellulosic material, a grinding aid, and a metal oxide, and combines the same.

Description

金属酸化物複合化高扁平セルロース粉体およびこれを含有する化粧料Metal oxide composite high flat cellulose powder and cosmetics containing the same
　本発明は、金属酸化物で複合された高い扁平度のセルロース粉体およびこれを含有する粉体化粧料に関し、更に詳細には、扁平度の高い形状を有し、かつその表面が金属酸化物で被覆された金属酸化物複合化高扁平セルロース粉体およびこれを含有する化粧料に関する。 The present invention relates to a cellulose powder having high flatness composited with a metal oxide and a powder cosmetic containing the same, and more specifically, has a shape having high flatness and the surface thereof is a metal oxide. The present invention relates to a metal oxide-complexed highly flat cellulose powder coated with a cosmetic and a cosmetic containing the same.
　粉体成分と油性成分等を含む粉体化粧料は、化粧品の分野において広く使用されており、その例として、パウダーファンデーション、アイシャドウ、粉白粉、ほほ紅等が挙げられる。 Powder cosmetics containing a powder component, an oily component, and the like are widely used in the field of cosmetics, and examples thereof include powder foundation, eye shadow, powdered white powder, blusher, and the like.
　この粉体化粧料は、一般には、体質顔料、顔料等の粉体成分と油性成分との粉体混合物を皿状容器に充填し、プレス成形することにより製造される。 This powder cosmetic is generally produced by filling a powder container of powder components such as extender pigments and pigments and an oil component into a dish-like container and press-molding.
　この粉体化粧料に使用される粉体成分としては、皮膚の上での伸びやつきがよいために天然物由来で薄板状の雲母片、セリサイト、タルク等やその表面処理物が体質顔料として使用されてきた。また、体質顔料の皮膚上での滑りや感触を向上させるため、球状有機粉体等が上記体質顔料と共に使用されてきた。更に、顔料としては、酸化チタン等の白色顔料、ベンガラ等の着色顔料、雲母チタン等の光沢顔料が使用されてきた。 As the powder component used in this powder cosmetic, natural pigment-derived thin mica pieces, sericite, talc, etc. and surface treated products thereof are extender pigments because they have good elongation and stickiness on the skin. Has been used as. Further, spherical organic powders and the like have been used together with the above extender pigments in order to improve the slip and feel of extender pigments on the skin. Furthermore, as pigments, white pigments such as titanium oxide, colored pigments such as Bengala, and glossy pigments such as titanium mica have been used.
　また、粉体成分上を金属酸化物で被覆したものも知られている（特許文献１～３）。例えば、特許文献１および２のものは、いずれも高分子微粉末や球状樹脂パウダー上を微細な金属酸化物で被覆するものであり、特許文献３のものは、化粧料の粉体に使用可能な基体上をハイドロキシアパタイトと酸化亜鉛で処理するものであった。 Also known are powder components coated with metal oxide (Patent Documents 1 to 3). For example, Patent Documents 1 and 2 both cover polymer fine powder and spherical resin powder with a fine metal oxide, and Patent Document 3 can be used as cosmetic powder. The substrate was treated with hydroxyapatite and zinc oxide.
　ところで粉体成分には、色々な形状のものがあり、雲母片、セリサイト、タルク等の薄片状の無機系粉体が汎用されているが、これらはいずれもアルミノシリケート系の鉱物であり、また産地により性質が若干異なるため、例えば、油の吸収性が低かったり、目的の物性のものが得られないという問題があった。一方、有機物粉体で扁平状のものはあまり報告されておらず、例えば、セルロース系物質と脂肪酸を混合した後、これを機械的に粉砕して得た扁平セルロース粒子が知られている程度であった（特許文献４）。 By the way, the powder component has various shapes, and flaky inorganic powders such as mica pieces, sericite, and talc are widely used, but these are all aluminosilicate minerals. In addition, since the properties are slightly different depending on the production area, for example, there is a problem that the oil absorbability is low or the desired physical properties cannot be obtained. On the other hand, flat organic powders have not been reported so much, for example, to the extent that flat cellulose particles obtained by mixing cellulose-based substances and fatty acids and then mechanically pulverizing them are known. (Patent Document 4).
　しかし、この特許文献４では、扁平セルロース粒子が開示されているものの、その具体的な使用形態は開示されておらず、化粧品への応用もきわめて簡単に開示されているにすぎないものである。 However, in this Patent Document 4, although flat cellulose particles are disclosed, the specific usage form is not disclosed, and the application to cosmetics is only disclosed very simply.
　一方、結晶セルロースの表面を水素添加レシチンで処理する技術も知られている（特許文献５）。しかし、この結晶セルロースは、長径と短径の比（Ｌ／Ｄ）が３以下と、扁平といえるようなものでなく、実際、未処理のものと比較した場合、化粧持ちの良さでは差があるものの、使用感である「取れ」、「のび」、「仕上がり」ではあまり差がないことが開示されている。 On the other hand, a technique for treating the surface of crystalline cellulose with hydrogenated lecithin is also known (Patent Document 5). However, this crystalline cellulose has a major axis / minor axis ratio (L / D) of 3 or less, which is not flat. In fact, when compared with untreated ones, there is a difference in the goodness of makeup. However, it is disclosed that there is not much difference between “Take”, “Nobi”, and “Finish” that are the feeling of use.
　本発明者らは先に、扁平度（アスペクト比）が２０～２００と極めて高い扁平なセルロース粉体（以下、「高扁平度セルロース粉体」という）およびその製造方法を開発し、特許出願した（特許文献６）。この高扁平度セルロース粉体は、精製した木材パルプ由来のセルロース粉末を減圧乾燥して、吸着水分を十分に除去した後、粉砕助剤および必要により疎水化処理剤と共に遊星型ボールミルで粉砕することで得られるものである。 The present inventors have previously developed a flat cellulose powder having an extremely high flatness (aspect ratio) of 20 to 200 (hereinafter referred to as “high flatness cellulose powder”) and a method for producing the same, and applied for a patent. (Patent Document 6). This high flatness cellulose powder is obtained by drying the purified cellulose pulp-derived cellulose powder under reduced pressure to sufficiently remove the adsorbed moisture, and then grinding it with a planetary ball mill together with a grinding aid and, if necessary, a hydrophobizing agent. It is obtained by.
　そして得られた高扁平度セルロース粉体は、素材自体がセルロースであり、しかも高扁平度という特徴を有するため、これを粉体化粧料の成分として配合した場合、油性成分の配合量が多くても、粉体の凝集を起こさず、粉体自体のサラサラ感等の特性も維持され、また、粉体をプレスしてもケーキングを起こしにくいという特性を有するものである。 The resulting high flatness cellulose powder is made of cellulose and has the characteristics of high flatness, so when it is blended as a powder cosmetic ingredient, the amount of oily ingredients is large. However, the agglomeration of the powder is not caused, the characteristics such as the smoothness of the powder itself are maintained, and the caking is difficult to occur even if the powder is pressed.
特開平３－２００７２１号公報JP-A-3-2000072 特開平８－５９４３３号公報JP-A-8-59433 特開２００２－２０２１８号公報Japanese Patent Laid-Open No. 2002-20218 特開２００４－２３０７１９号公報JP 2004-230719 A 特開２００３－１４６８２９号公報JP 2003-146829 A ＷＯ／２０１０／０２６９２５WO / 2010/026925
　すでに多くの化粧料用粉体が提供されてはいるが、消費者がより良い使用感や、高い使用性の化粧料を求めることは自然成り行きであり、本発明はそのような化粧料の提供することのできる化粧料用粉体およびこれを用いた化粧料の提供をその課題とするものである。 Although many cosmetic powders have already been provided, it is natural for consumers to seek cosmetics with a better feeling of use and higher usability, and the present invention provides such cosmetics. An object of the present invention is to provide a cosmetic powder and a cosmetic using the same.
　本発明者らは、セルロース系物質から得られる高扁平度セルロース粉体について、更に研究を進めていたところ、特定の方法でセルロース系物質に、粉砕助剤と金属酸化物とを加え、これらを複合化させることにより、従来の化粧料用粉体では到底得られない性質の金属酸化物複合化高扁平セルロース粉体が得られ、これを利用することで粉体化粧料等化粧料の商品性を極めて高くすることができることを見出し、本発明を完成した。 The inventors of the present invention were further researching on the high flatness cellulose powder obtained from the cellulosic material, and added a grinding aid and a metal oxide to the cellulosic material by a specific method. By compounding, a metal oxide composite high flattened cellulose powder with properties that can hardly be obtained with conventional cosmetic powders is obtained, and by using this, commercial properties of cosmetics such as powder cosmetics are obtained. The present invention has been completed.
　すなわち本発明は、セルロース系物質と、粉砕助剤と、金属酸化物とを機械的に粉砕処理することにより得られる金属酸化物複合化高扁平セルロース粉体である。 That is, the present invention is a metal oxide composite high flattened cellulose powder obtained by mechanically grinding a cellulosic material, a grinding aid, and a metal oxide.
　また本発明は、前記金属酸化物複合化高扁平セルロース粉体を含有することを特徴とする化粧料である。 The present invention is also a cosmetic comprising the metal oxide composite high flattened cellulose powder.
　更に本発明は、セルロース系物質に、粉砕助剤および金属酸化物を添加して混合物とし、この混合物を機械的に粉砕処理することを特徴とする金属酸化物複合化高扁平セルロース粉体の製造方法である。 Furthermore, the present invention provides a metal oxide composite high flat cellulose powder characterized by adding a grinding aid and a metal oxide to a cellulosic material to form a mixture, and mechanically grinding the mixture. Is the method.
　本発明の金属酸化物複合化高扁平セルロース粉体は、その表面に金属酸化物を複合化したことで、従来の高扁平度セルロース粉体の有する効果に加え、新たな効果を奏するものである。具体的には、複合化した金属酸化物が、粉体上で１０～１００ｎｍとなっている場合は、極めて優れたＵＶ遮断効果となめらかな使用感を得ることができる。また、複合化した金属酸化物が粉体上で１００ｎｍを超え１０００ｎｍ以下となっている場合は、自然な隠蔽性、優れた発色性となめらかな使用感を得ることができる。 The metal oxide composite high flattened cellulose powder of the present invention has a new effect in addition to the effect of the conventional high flattened cellulose powder by combining the metal oxide on the surface thereof. . Specifically, when the composite metal oxide has a thickness of 10 to 100 nm on the powder, an extremely excellent UV blocking effect and a smooth use feeling can be obtained. Further, when the composite metal oxide is more than 100 nm and not more than 1000 nm on the powder, natural concealing properties, excellent color developability and a smooth feeling of use can be obtained.
　そして、この金属酸化物複合化高扁平セルロース粉体を配合した化粧料は、優れた化粧膜の均一性となめらかな使用感を有すると共に、優れたＵＶ遮断効果や自然な隠蔽性、発色効果を有し、更に、色沈みしないなど化粧の持続効果に優れたものである。 The cosmetic compounded with this metal oxide composite high flattened cellulose powder has excellent cosmetic film uniformity and smooth use feeling, as well as excellent UV blocking effect, natural hiding property, and coloring effect. In addition, it has an excellent makeup lasting effect such as no color sink.
　従って、本発明の金属酸化物複合化高扁平セルロース粉体を利用する化粧料は、パウダーファンデーション、アイシャドウ、粉白粉、ほほ紅等として好適に用いることができる。 Therefore, the cosmetics using the metal oxide composite high flat cellulose powder of the present invention can be suitably used as powder foundation, eye shadow, powdered white powder, blusher and the like.
実施例６で得られた製品６の表面を、走査型顕微鏡（１０，０００倍）により観察した写真である。It is the photograph which observed the surface of the product 6 obtained in Example 6 with the scanning microscope (10,000 times). 図１と同じ製品の表面を、走査型顕微鏡（５０，０００倍）により観察した写真である。It is the photograph which observed the surface of the same product as FIG. 1 with the scanning microscope (50,000 times). 図１と同じ製品の表面を、走査型顕微鏡（２００，０００倍）により観察した写真である。It is the photograph which observed the surface of the same product as FIG. 1 with the scanning microscope (200,000 times).
　本発明の金属酸化物複合化高扁平セルロース粉体は、高扁平セルロース粉体の表面上に、微細な金属酸化物粉末が強固に付着、複合化しているものである。 The metal oxide composite high flat cellulose powder of the present invention is one in which fine metal oxide powder is firmly attached and combined on the surface of the high flat cellulose powder.
　この金属酸化物複合化高扁平セルロース粉体は、セルロース系物質に、粉砕助剤および金属酸化物を添加して混合物とし、この混合物を機械的に粉砕処理することにより製造される。 This metal oxide composite high flat cellulose powder is produced by adding a grinding aid and a metal oxide to a cellulose-based material to form a mixture, and mechanically grinding the mixture.
　金属酸化物複合化高扁平セルロース粉体の出発原料として用いられるセルロース系物質としては、特に制限されないが、例えば、木材を起源とする繊維状もしくは粉末状の木粉または木材パルプのような木質材料、綿花を起源とする繊維状もしくは粉末状の木綿またはリンター繊維などの綿系材料、木質材料や、綿花系材料を精製することで得られる繊維状もしくは粉末状のセルロース系物質を用いることが好ましく、酸加水分解によって得られた精製セルロース系物質を用いてもよい。なお、綿花を起源とするセルロース系物質としては、オーガニック認証をうけた綿花を起源とするものでもよい。 The cellulosic material used as a starting material for the metal oxide composite high flattened cellulose powder is not particularly limited, but for example, a woody material such as fibrous or powdery wood powder or wood pulp originating from wood It is preferable to use a cotton-based material such as fibrous or powdered cotton or linter fiber originating from cotton, a woody material, or a fibrous or powdery cellulose material obtained by refining the cotton-based material Alternatively, a purified cellulosic material obtained by acid hydrolysis may be used. In addition, as a cellulosic substance originating in cotton, the thing originating in the cotton which received the organic certification | authentication may be used.
　この原料となるセルロース系物質は、水分を吸着または吸収し易く、通常状態で３～１０質量％（以下、単に「％」という）程度の吸着水分を有している。このセルロース系物質から、効果的に扁平セルロース粉体を得るためには、これを粉砕処理する前に熱風乾燥、真空乾燥、減圧乾燥等により予め乾燥し、吸着水分を除去することが好ましい。 The cellulosic material used as a raw material easily adsorbs or absorbs moisture, and has an adsorbed moisture of about 3 to 10% by mass (hereinafter simply referred to as “%”) in a normal state. In order to effectively obtain a flat cellulose powder from this cellulosic material, it is preferable to dry it beforehand by hot air drying, vacuum drying, reduced pressure drying or the like before removing the adsorbed water before pulverization.
　一方、本発明の金属酸化物複合化高扁平セルロース粉体の製造において用いられる粉砕助剤は、上記セルロース系物質を高扁平化させるために使用されるものであり、その例としては、両親媒性物質、アミノ酸類、脂肪酸類等を挙げることができる。これらは、一種でも、また二種以上配合しても良い。 On the other hand, the grinding aid used in the production of the metal oxide-complexed highly flat cellulose powder of the present invention is used for highly flattening the cellulosic material. And other substances, amino acids, fatty acids and the like. These may be used alone or in combination of two or more.
　このうち、両親媒性物質としては、リン脂質、セラミド、コレステロールもしくはその誘導体、フィトステロールもしくはその誘導体等を挙げることができる。これらは生体内の脂質であるかもしくはそれに近しい構造、すなわち長鎖アルキル構造と親水基を持つという共通の性質を有する物質である。 Among these, examples of amphiphilic substances include phospholipids, ceramides, cholesterol or derivatives thereof, phytosterols or derivatives thereof, and the like. These are substances having a common property of being a lipid in vivo or a structure close to that, that is, having a long-chain alkyl structure and a hydrophilic group.
　上記両親媒性物質のうち、リン脂質は構造中にリン酸エステル部位をもつ脂質の総称である。具体的なリン脂質としては、卵黄レシチン、大豆レシチン等の天然レシチンに水素添加した天然物由来のもの、リゾレシチン、ホスファチジルコリン、ホスファチジルエタノールアミン、ホスファチジルセリン、ホスファチジルグリセロール、ホスファチジルイノシトール、スフィンゴミエリン等を水素添加したもの等が挙げられる。これらのリン脂質の中でも、水素添加レシチン、ホスファチジルコリン、ホスファチジルエタノールアミン、水素添加ホスファチジルグリセロールが好ましい。 Among the above amphiphiles, phospholipid is a generic term for lipids having a phosphate ester moiety in the structure. Specific phospholipids include those derived from natural products hydrogenated to natural lecithin such as egg yolk lecithin and soybean lecithin, hydrogenated lysolecithin, phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidylinositol, sphingomyelin, etc. And the like. Among these phospholipids, hydrogenated lecithin, phosphatidylcholine, phosphatidylethanolamine, and hydrogenated phosphatidylglycerol are preferable.
　また、セラミドは分子中に１個以上の長鎖の直鎖および／もしくは分岐アルキルまたはアルケニル基、更に、少なくとも２個以上の水酸基、１個以上のアミド基（及び／またはアミノ基）を有する非イオン系両親媒性物質の総称である。具体的なセラミドとしては、スフィンゴシン、フィトスフィンゴシンの長鎖脂肪酸アミドであるセラミド１、セラミド２、セラミド３、セラミド３Ｂ、セラミド４、セラミド５、セラミド６、セラミド６I、セラミド６II等の天然セラミド類等が挙げられる。これらのセラミドの中でも、セラミド２、セラミド３が好ましい。また、これらのセラミドは、天然物由来のものであっても、合成したものであってもよい。 In addition, the ceramide has a non-linear group having one or more long-chain linear and / or branched alkyl or alkenyl groups, at least two hydroxyl groups, and one or more amide groups (and / or amino groups) in the molecule. A general term for ionic amphiphiles. Specific examples of ceramide include natural ceramides such as ceramide 1, ceramide 2, ceramide 3, ceramide 3B, ceramide 4, ceramide 5, ceramide 6, ceramide 6I, ceramide 6II and the like, which are long-chain fatty acid amides of sphingosine and phytosphingosine. Is mentioned. Among these ceramides, ceramide 2 and ceramide 3 are preferable. These ceramides may be derived from natural products or synthesized.
　更に、コレステロールは動物油脂をけん化した高級アルコール分や魚油から得られる留分を抽出・結晶化・乾燥して精製される白色ないし微黄色の固体であり、その分子式はＣ27Ｈ46Ｏである。また、コレステロースの誘導体は、上記コレステロールの、オレイン酸、パルミトオレイン酸、パルミチン酸、ステアリン酸、２－エチルヘキサン酸、カプリン酸、ラウリン酸等の飽和脂肪酸または不飽和脂肪酸のエステル誘導体、オリーブ油、アボガド油、ゴマ油、コメ胚芽油、マカデミアナッツ油等の天然の植物性油脂、魚油、バター等の動物性油脂等の油脂を加水分解して得られる脂肪酸の混合物とのエステル化誘導体等である。好ましいコレステロール誘導体の具体例としては、ヒドロキシステアリン酸コレステリル、ポリオキシエチレンコレステリルエーテル等が挙げられる。これらコレステロールまたはその誘導体の中でも、コレステロールが好ましい。 Furthermore, cholesterol is a white to slightly yellow solid purified by extracting, crystallizing and drying a fraction obtained from saponified animal oil and fat and fish oil, and its molecular formula is C 27 H 46 O. . Further, cholesterose derivatives include ester derivatives of saturated fatty acids such as oleic acid, palmitooleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, lauric acid, etc. , Esterified derivatives with a mixture of fatty acids obtained by hydrolyzing oils such as natural vegetable oils such as avocado oil, sesame oil, rice germ oil, macadamia nut oil, and animal oils such as fish oil and butter. Specific examples of preferable cholesterol derivatives include cholesteryl hydroxystearate, polyoxyethylene cholesteryl ether, and the like. Among these cholesterol or derivatives thereof, cholesterol is preferable.
　また更に、フィトステロールは植物から得られるステロール化合物の総称である。具体的なフィトステロールとしては、シトステロール、スチグマステロール、フコステロール、スピナステロール、ブラシカステロール等が挙げられる。また、フィトステロール誘導体は、上記フィトステロールの、オレイン酸、パルミトオレイン酸、パルミチン酸、ステアリン酸、２－エチルヘキサン酸、カプリン酸、ラウリン酸等の飽和脂肪酸または不飽和脂肪酸のエステル誘導体、オリーブ油、アボガド油、ゴマ油、コメ胚芽油、マカデミアナッツ油等の天然の植物性油脂を加水分解して得られる脂肪酸の混合物とのエステル化誘導体等である。好ましいフィトステロール誘導体の具体例としては、ヒドロキシステアリン酸フィトステリル、ポリオキシエチレンフィトステロール、ポリオキシエチレンフィトスタノール等が挙げられる。これらフィトステロールまたはその誘導体の中でもフィトステロールが好ましい。 Furthermore, phytosterol is a general term for sterol compounds obtained from plants. Specific examples of phytosterols include sitosterol, stigmasterol, fucostosterol, spinasterol, and brush castrol. Further, phytosterol derivatives include ester derivatives of saturated or unsaturated fatty acids such as oleic acid, palmitooleic acid, palmitic acid, stearic acid, 2-ethylhexanoic acid, capric acid, lauric acid, olive oil, avocado, etc. And esterified derivatives with a mixture of fatty acids obtained by hydrolyzing natural vegetable oils such as oil, sesame oil, rice germ oil and macadamia nut oil. Specific examples of preferred phytosterol derivatives include phytosteryl hydroxystearate, polyoxyethylene phytosterol, polyoxyethylene phytostanol and the like. Among these phytosterols or derivatives thereof, phytosterol is preferable.
　また粉砕助剤のうち、アミノ酸類としては、Ｎ－ラウロイル－Ｌ－リジン等のＮ－アシルアミノ酸、テアニン等のアミノ酸が挙げられる。 Among the grinding aids, amino acids include N-acyl amino acids such as N-lauroyl-L-lysine and amino acids such as theanine.
　更に脂肪酸類としては、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸等の飽和脂肪酸及びその塩、オレイン酸等の不飽和脂肪酸及びその塩が挙げられる。 Furthermore, examples of fatty acids include saturated fatty acids such as lauric acid, myristic acid, palmitic acid and stearic acid and salts thereof, and unsaturated fatty acids such as oleic acid and salts thereof.
　他方、本発明の金属酸化物複合化高扁平セルロース粉体の製造において用いられる金属酸化物としては、一般の化粧料において、体質顔料や着色顔料などの粉体成分として配合されるものであれば特に制約はなく利用することができる。この金属酸化物の例としては、酸化鉄、酸化チタン、酸化亜鉛、酸化セリウム等を挙げることができる。この金属酸化物も、一種または二種以上で利用することができる。 On the other hand, as the metal oxide used in the production of the metal oxide composite high flat cellulose powder of the present invention, it can be used in general cosmetics as long as it is blended as a powder component such as extender pigment or colored pigment. It can be used without any particular restrictions. Examples of the metal oxide include iron oxide, titanium oxide, zinc oxide, cerium oxide and the like. These metal oxides can also be used singly or in combination of two or more.
　この金属酸化物の粒径は、１０～１００００ｎｍが好ましいが、得られる金属酸化物複合化高扁平セルロース粉体上での平均粒径によって、後記するように得られる効果の一部が相違するので、この点も勘案して原料金属酸化物の粒径を選択することが望ましい。 The particle diameter of the metal oxide is preferably 10 to 10,000 nm, but some of the effects obtained will differ depending on the average particle diameter on the obtained metal oxide composite high flat cellulose powder. In view of this point, it is desirable to select the particle size of the raw metal oxide.
　本発明の金属酸化物複合化高扁平セルロース粉体の製造において、上記した各成分全体中での粉砕助剤の添加量は、０.５～５％であり、好ましくは１～３％である。また、全体中の金属酸化物の量が５～５０％であり、好ましくは２０～４０％である。 In the production of the metal oxide composite high flattened cellulose powder of the present invention, the amount of the grinding aid added to the whole of the above components is 0.5 to 5%, preferably 1 to 3%. . The total amount of metal oxide is 5 to 50%, preferably 20 to 40%.
　これら粉砕助剤や金属酸化物をセルロース系物質に添加する時期は、粉砕処理前であればいつでも良く、また、その添加方法も、粉砕助剤と金属酸化物を同時に加えても、また別個に加えても良い。更に、粉砕助剤の添加方法としては、これを適当な溶媒に溶解した後、セルロース系物質に加えても良い。ここで粉砕助剤の溶解に使用される溶媒としては、例えば、ヘキサン等のアルカン、エタノール等のアルコール、アセトン等のケトン、テトラヒドロフラン等のエーテル、トルエン等の芳香族炭化水素等が挙げられる。 These pulverization aids and metal oxides can be added to the cellulosic material at any time before the pulverization treatment, and the addition method can be added separately even if the pulverization aid and metal oxide are added simultaneously. May be added. Furthermore, as a method for adding the grinding aid, it may be dissolved in a suitable solvent and then added to the cellulosic material. Examples of the solvent used for dissolving the grinding aid include alkanes such as hexane, alcohols such as ethanol, ketones such as acetone, ethers such as tetrahydrofuran, aromatic hydrocarbons such as toluene, and the like.
　前記したセルロース系物質、粉砕助剤および金属酸化物の混合物を機械的に粉砕する処理では、粉砕による圧力や剪断力が一定時間連続して印可する必要がある。そのため、粉砕処理には振動ボールミル、回転ボールミル、遊星型ボールミル、ロールミル、メディアミル、ディスクミル、高速回転羽根による高速ミキサー、ホモミキサー等の粉砕装置を用いることが好ましく、遊星型ボールミルが特に好ましい。粉砕処理方法は、溶媒を用いない乾式粉砕処理が好ましい。なお、粉砕処理を行う場合に印可する粉砕エネルギー（遊星型ボールミルの場合、遊星型ボールミル内に与える重力加速度）は３～２０Ｇ、好ましくは５～１５Ｇが適している。 In the process of mechanically pulverizing the mixture of the cellulose-based substance, the pulverization aid and the metal oxide, it is necessary to continuously apply the pressure and shear force due to the pulverization for a certain period of time. Therefore, it is preferable to use a pulverizing apparatus such as a vibration ball mill, a rotating ball mill, a planetary ball mill, a roll mill, a media mill, a disk mill, a high-speed mixer using high-speed rotating blades, a homomixer, etc., and a planetary ball mill is particularly preferable. The pulverization method is preferably dry pulverization without using a solvent. Note that the crushing energy applied in the crushing process (in the case of a planetary ball mill, the gravitational acceleration applied to the planetary ball mill) is 3 to 20 G, preferably 5 to 15 G.
　また、金属酸化物複合化高扁平セルロース粉体では、その粒径、厚さ、扁平度（アスペクト比）が重要であるが、更にこれに強固に付着、複合化される金属酸化物粉末の粒径も、その用途によっては重要であるので、上記粉砕時間は、これらを勘案しつつ決める必要がある。この関係は、目的とする扁平セルロース自体や、原料である金属酸化物の粒径なども関連するので、予め実験的に粉砕条件、粉砕時間等を決めておくことが望ましい。 In addition, the particle size, thickness, and flatness (aspect ratio) of the metal oxide composite high flattened cellulose powder are important. Since the diameter is also important depending on the application, the pulverization time must be determined in consideration of these. This relationship is related to the target flat cellulose itself, the particle size of the metal oxide as a raw material, and the like, so it is desirable to experimentally determine pulverization conditions, pulverization time, and the like in advance.
　次に本発明の金属酸化物複合化高扁平セルロース粉体を得るための好ましい態様を示す。まず、精製した木材パルプ由来のセルロース粉末を３０～５０℃で減圧乾燥を行い、吸着水分を０.１％以下まで十分に除去する。このセルロース粉末を、密閉可能なアルミナ製やジルコニア製粉砕容器に、アルミナ製やジルコニア製粉砕ボールとともに投入し、更に、セルロース粉末に対して上記量となるように粉砕助剤および金属酸化物粉末を添加する。その後、上記粉砕容器を遊星型ボールミルに設置し、回転数１００～２５０ｒｐｍにて、粉砕処理を行う。粉砕処理は、５～１５分間粉砕－５～１５分間休止を１サイクルとし、連続して２～７２サイクル程度繰り返して行っても良いし、休止を入れずに連続して５～１２０分間程度行っても良い。 Next, a preferred embodiment for obtaining the metal oxide composite high flat cellulose powder of the present invention will be shown. First, the purified cellulose pulp-derived cellulose powder is dried under reduced pressure at 30 to 50 ° C. to sufficiently remove the adsorbed moisture to 0.1% or less. This cellulose powder is put into a sealable alumina or zirconia grinding container together with alumina or zirconia grinding balls, and further, a grinding aid and a metal oxide powder are added so as to have the above amount with respect to the cellulose powder. Added. Thereafter, the pulverization container is placed in a planetary ball mill, and pulverization is performed at a rotational speed of 100 to 250 rpm. The pulverization treatment may be repeated for about 2 to 72 cycles continuously, with 5 to 15 minutes of pulverization-5 to 15 minutes of rest, or for about 5 to 120 minutes without interruption. May be.
　なお、粉砕処理の後は、更に、風乾、熱風乾燥、真空乾燥、減圧乾燥等の公知の乾燥手段により金属酸化物複合化高扁平セルロース粉体に付着した水分等を除去させてもよい。 In addition, after the pulverization treatment, moisture adhering to the metal oxide composite high flattened cellulose powder may be further removed by a known drying means such as air drying, hot air drying, vacuum drying, and reduced pressure drying.
　上記のようにして得られた金属酸化物複合化高扁平セルロース粉体は、例えば、その平均粒径が１～５０μｍ、好ましくは５～４０μｍ、平均厚さが０.１～１０μｍ、好ましくは０．２～２μｍの薄片状のものであり、かつ扁平度が４～２００、好ましくは１０～１００のものである。なお、ここで平均粒径とは、レーザー回折・散乱式粒度分布測定装置等の粒度分布測定装置を用い、エタノール中分散状態で測定された扁平セルロース粒子の幅と長さの装置上の平均値（積算体積５０％の粒径値）をいう。また、平均厚さとは、走査型電子顕微鏡等の電子顕微鏡にて前記で求められた平均粒径と同等の大きさの粒子を複数選択し、その厚さを測定し、それらを平均した値をいう。更に、扁平度は、前記のようにして求められた平均粒径／平均厚さである。また、複合化した金属酸化物の粒径も走査型電子顕微鏡にて測定することができる。 The metal oxide composite high flattened cellulose powder obtained as described above has, for example, an average particle diameter of 1 to 50 μm, preferably 5 to 40 μm, and an average thickness of 0.1 to 10 μm, preferably 0. It has a flake shape of 2 to 2 μm and a flatness of 4 to 200, preferably 10 to 100. Here, the average particle size is the average value of the width and length of the flat cellulose particles measured in a dispersion state in ethanol using a particle size distribution measuring device such as a laser diffraction / scattering type particle size distribution measuring device. (Particle size value of 50% cumulative volume). In addition, the average thickness refers to a value obtained by selecting a plurality of particles having the same size as the average particle size obtained above with an electron microscope such as a scanning electron microscope, measuring the thickness, and averaging the values. Say. Further, the flatness is the average particle diameter / average thickness determined as described above. The particle size of the composite metal oxide can also be measured with a scanning electron microscope.
　斯くして得られる金属酸化物複合化高扁平セルロース粉体は、上記したように、強固に付着、複合化された金属酸化物の粒径が、１００ｎｍを超え１０００ｎｍ以下（顔料級サイズ）である場合と、これが、１０～１００ｎｍ（微粒子級サイズ）である場合で、その性質が若干異なり、その用途も相違する。すなわち、複合化した金属酸化物が、微粒子級の場合は、極めて優れたＵＶ遮断効果と化粧膜の均一性を得ることができる。また、複合化した金属酸化物が顔料級の場合は、優れた発色性を得ることができる。なお、金属酸化物の粒径は複合化の前後で殆ど変化しないため、複合化前に添加した金属酸化物の粒径と複合化した後の金属酸化物の粒径はほぼ同等である。 As described above, the metal oxide composite high flat cellulose powder obtained in this way has a particle size of the metal oxide that is firmly adhered and composited more than 100 nm and not more than 1000 nm (pigment grade size). In some cases, this is a case of 10 to 100 nm (fine particle size), and the properties are slightly different, and the applications are also different. That is, when the composite metal oxide is a fine particle class, an extremely excellent UV blocking effect and uniformity of the decorative film can be obtained. Further, when the composite metal oxide is a pigment grade, excellent color developability can be obtained. Since the particle size of the metal oxide hardly changes before and after the compounding, the particle size of the metal oxide added before the compounding and the particle size of the metal oxide after the compounding are almost the same.
　そして、この金属酸化物複合化高扁平セルロース粉体は、高扁平セルロース粉体が元々有していたなめらかな使用感も具備しているので、これを配合した化粧料は、優れた化粧膜の均一性となめらかな使用感を有すると共に、優れたＵＶ遮断効果や発色効果を有し、更に、色沈みしないなど化粧の持続効果に優れたものである。 And since this metal oxide composite high flat cellulose powder also has the smooth feeling of use originally possessed by the high flat cellulose powder, the cosmetic compounded with this has an excellent cosmetic film. It has a uniform and smooth use feeling, an excellent UV blocking effect and a color developing effect, and also has an excellent makeup sustaining effect such as no color sink.
　得られた金属酸化物複合化高扁平セルロース粉体が従来の体質顔料のタルク、セリサイトに比べ、薄い薄片状であり、透明感、ソフト感、伸び、自然な光沢などに優れた特性を持つ他、使用する油剤との親和性が優れ、かつＵＶ遮断効果や発色効果に優れたものであるため、具体的に、このものを利用できる化粧料としては、粉体を利用する多くの化粧料、例えば、基礎（スキンケア）化粧料、メーキャップ化粧料、日焼け止め化粧料、頭髪化粧料等の各種化粧料等を挙げることができる。特にパウダーファンデーション、リキッドファンデーション、アイシャドウ、ほほ紅、粉白粉等の粉体化粧料や日焼け止め料、化粧下地等のＵＶ遮断効果が必要とされる化粧料での使用が有効であり、好ましい。 The resulting metal oxide composite high flattened cellulose powder has a thin flake shape compared to the conventional extender pigments talc and sericite, and has excellent properties such as transparency, softness, elongation, and natural gloss. In addition, since it has excellent affinity with the oil used, and has excellent UV blocking effect and coloring effect, specifically, as cosmetics that can use this, many cosmetics that use powder Examples thereof include various cosmetics such as basic (skin care) cosmetics, makeup cosmetics, sunscreen cosmetics, hair cosmetics, and the like. Particularly, it is effective and preferable to use in powder cosmetics such as powder foundation, liquid foundation, eye shadow, cheek red, powdered white powder and the like and sunscreens, cosmetics requiring UV blocking effect such as makeup base.
　本発明の金属酸化物複合化高扁平セルロース粉体を配合する化粧料の調製は、これを適当な化粧料基剤と組合せ、製剤化することにより行われる。例えば、化粧料が粉体化粧料である場合は、従来の粉体化粧料と同様の製造方法において、従来の粉体成分の一部または全部に換えて本発明の金属酸化物複合化高扁平セルロース粉体を使用すればよい。なお、上記化粧料における金属酸化物複合化高扁平セルロース粉体の配合量は１～９０％であり、好ましくは５～９０％、特に好ましくは５～７０％である。 Preparation of a cosmetic compounded with the metal oxide composite high flattened cellulose powder of the present invention is carried out by combining it with a suitable cosmetic base and formulating it. For example, when the cosmetic is a powder cosmetic, the metal oxide composite high flatness of the present invention is used instead of a part or all of the conventional powder component in the same manufacturing method as that of the conventional powder cosmetic. Cellulose powder may be used. The blending amount of the metal oxide composite high flat cellulose powder in the cosmetic is 1 to 90%, preferably 5 to 90%, particularly preferably 5 to 70%.
　上記化粧料においては、化粧料基剤として油性成分を配合することが好ましい。この化粧料に配合される油性成分としては、特に制約はないが、例えば、パラフィンワックス、セレシンワックス、オゾケライト、マイクロクリスタリンワックス、モンタンワックス、フィッシャトロプスワックス、ポリエチレンワックス、流動パラフィン、スクワラン、ワセリン、ポリイソブチレン、ポリブテン等の炭化水素系類、カルナウバロウ、ミツロウ、ラノリンワックス、キャンデリラ等の天然ロウ類、トリベヘン酸グリセリル、ロジン酸ペンタエリトリットエステル、ホホバ油、セチルイソオクタネート、ミリスチン酸イソプロピル、トリオクタン酸グリセリル、トリイソステアリン酸ジグリセリル、ジペンタエリトリット脂肪酸エステル等のエステル類、ステアリン酸、ベヘニン酸、１２－ヒドロキシステアリン酸等の脂肪酸類、セタノール、ステアリルアルコール、ベヘニルアルコール等の高級アルコール類、オリーブ油、ヒマシ油、ミンク油、モクロウ等の油脂類、ラノリン脂肪酸イソプロピル、ラノリンアルコール等のラノリン誘導体類、Ｎ－ラウロイルーＬ－グルタミン酸ジ（コレステリル・ベヘニル・オクチルドデシル）等のアミノ酸誘導体類、パーフルオロポリエーテル、パーフルオロデカン、パーフルオロオクタン等のフッ素系油剤類等が挙げられる。これらの油性成分は１種または２種以上を用いることができ、本発明の化粧料で油性成分を配合する場合の配合量は、特に限定されないが、０.１～２５％が好ましい。 In the above cosmetics, it is preferable to blend an oil component as a cosmetic base. There are no particular restrictions on the oily ingredients blended in this cosmetic, but for example, paraffin wax, ceresin wax, ozokerite, microcrystalline wax, montan wax, fisher trops wax, polyethylene wax, liquid paraffin, squalane, petrolatum, Hydrocarbons such as polyisobutylene and polybutene, natural waxes such as carnauba wax, beeswax, lanolin wax and candelilla, glyceryl tribehenate, rosin acid pentaerythritol ester, jojoba oil, cetyl isooctanoate, isopropyl myristate, trioctanoic acid Esters such as glyceryl, diglyceryl triisostearate, dipentaerythritol fatty acid esters, fatty acids such as stearic acid, behenic acid, 12-hydroxystearic acid Higher alcohols such as cetanol, stearyl alcohol and behenyl alcohol, oils and fats such as olive oil, castor oil, mink oil and owl, lanolin derivatives such as lanolin fatty acid isopropyl and lanolin alcohol, N-lauroyl L-glutamate di (cholesteryl and behenyl) -Amino acid derivatives such as octyldodecyl), fluorine oils such as perfluoropolyether, perfluorodecane, and perfluorooctane. These oily components can be used alone or in combination of two or more. The amount of the oily component to be blended with the cosmetic of the present invention is not particularly limited, but is preferably 0.1 to 25%.
　また、上記化粧料においては、従来の粉体成分、例えば、タルクなどの無機粉末やナイロンなどの有機粉末を配合することができる。この場合には、本発明の金属酸化物複合化高扁平セルロース粉体と共に無機粉末や有機粉末を添加し、分散させ、必要に応じて油分を添加して製造すればよい。 Further, in the above cosmetics, conventional powder components, for example, inorganic powder such as talc and organic powder such as nylon can be blended. In this case, an inorganic powder or an organic powder may be added and dispersed together with the metal oxide composite high flat cellulose powder of the present invention, and oil may be added as necessary.
　更に、上記化粧料には、必要に応じて、通常の化粧料に使用される成分、例えば、界面活性剤、油ゲル化剤、多価アルコール類や保湿剤などの水溶性成分、紫外線吸収剤、防腐剤、美容成分、香料等を本発明の効果を損なわない範囲で適宜配合することができる。 Furthermore, the above cosmetics include components used in normal cosmetics, for example, surfactants, oil gelling agents, water-soluble components such as polyhydric alcohols and humectants, and ultraviolet absorbers as necessary. In addition, preservatives, cosmetic ingredients, fragrances, and the like can be appropriately blended within a range not impairing the effects of the present invention.
　上記化粧料の性状や剤型は特に限定されず、目的に応じて選択することができる。本発明の化粧料の性状としては、液状、粉末状、固形状、乳液状、クリーム状、ゲル状等のいずれであってもよく、またその剤型も水性、油性、可溶化型、油中水型、水中油型などのいずれの剤型であってもよい。 The properties and dosage forms of the cosmetics are not particularly limited and can be selected according to the purpose. The properties of the cosmetic of the present invention may be any of liquid, powder, solid, emulsion, cream, gel and the like, and the dosage form is aqueous, oily, solubilized, in oil Any dosage form such as a water mold and an oil-in-water mold may be used.
　以上説明した本発明の金属酸化物複合化高扁平セルロース粉体が、従来の金属酸化物複合化粒子に比べ、格段に優れた性能を有する理由は、金属酸化物が極めて微細な、一次粒子の形態で高扁平セルロース粉体に複合化していることによるためと推定されている。すなわち、図１ないし３は実施例６で得た製品６の表面を走査型電子顕微鏡で観察したものであるが、倍率が約１０,０００倍である図１では、微粒子酸化亜鉛は、全く観察できない。しかしながら、倍率を５０,０００倍に上げると、表面に微粒子酸化亜鉛が白く見え始め、倍率２００,０００倍では、２０ｎｍ程度の微粒子酸化亜鉛が、母粉体上で観察される。そして、微粒子酸化亜鉛の元の粒径は、２０ｎｍ程度であるので、この結果は、本発明の金属酸化物複合化高扁平セルロース粉体表面では、微粒子酸化亜鉛が凝集せず、比較的一次粒子の状態で複合化されていると解することができる。すなわち、金属酸化物複合化高扁平セルロース粉体上では、金属酸化物がその作用を最大限に発揮できる一次粒子の状態で存在することが格段に優れた性能を発揮する理由と考えられる。 The reason why the metal oxide composite high flattened cellulose powder of the present invention described above has much superior performance compared to conventional metal oxide composite particles is that the metal oxide is very fine, This is presumed to be due to the fact that it is combined with the highly flat cellulose powder in the form. That is, FIGS. 1 to 3 are obtained by observing the surface of the product 6 obtained in Example 6 with a scanning electron microscope. In FIG. 1 where the magnification is about 10,000 times, the fine zinc oxide is completely observed. Can not. However, when the magnification is increased to 50,000 times, fine zinc oxide begins to appear white on the surface, and at a magnification of 200,000, fine zinc oxide of about 20 nm is observed on the mother powder. Since the original particle size of the fine particle zinc oxide is about 20 nm, this result shows that the fine particle zinc oxide does not aggregate on the surface of the metal oxide composite high flat cellulose powder of the present invention, and is relatively primary particles. It can be understood that it is compounded in the state of. That is, on the metal oxide composite high flattened cellulose powder, the presence of the metal oxide in a primary particle state that can exert its action to the maximum is considered to be the reason that the performance is remarkably improved.
　このように、本発明の金属酸化物複合化高扁平セルロース粉体で、金属酸化物が一次粒子の状態で複合化される理由については、未だ明らかではないが、セルロース系物質から高扁平セルロース粒子が生成するその場に微細な金属酸化物粉体が存在し、且つ高シェアで攪拌されていることから、これが優先的に生成したばかりのセルロース表面上に付着し、強固な結合を有するためではないかと解される。 As described above, in the metal oxide composite high flat cellulose powder of the present invention, the reason why the metal oxide is composited in a primary particle state is not yet clear. Since the fine metal oxide powder is present on the spot where it is formed and stirred with a high share, it adheres on the cellulose surface just preferentially formed and has a strong bond. It is understood that there is not.
　以下、実施例を挙げて本発明を詳細に説明するが、本発明はこれら実施例に何ら限定されるものではない。 Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.
実　施　例　１
　　　ラウロイルリジン処理微粒子酸化チタン複合高扁平セルロース粉体の
　　　製造（１）：
（１）原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（５５.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、ラウロイルリジン（アミホープＬＬ　味の素社製）を０.７ｇ、微粒子酸化チタン（ＴＴＯ－Ｓ－４　石原産業社製）（粒径　短軸：１０～２０ｎｍ、長軸：５０～１００ｎｍ）を１４ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ラウロイルリジン処理微粒子酸化チタン複合高扁平セルロース粉体（製品１）を得た。 Example 1
Production of Lauroyllysine-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (1):
(1) As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). In addition, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co., Inc.), fine particle titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) (particle diameter minor axis: 10 to 20 nm, major axis: 50 to 100 nm) 14 g was added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine titanium oxide composite high flat cellulose powder. (Product 1) was obtained.
（２）以下のようにして、製品１の平均粒径、厚さ、扁平度を測定した。すなわち、レーザー回折・散乱式粒度分布測定装置（堀場社：ＬＡ－９２０）を用いてフローセルにて、得られた粉体のエタノール中分散状態での平均粒径（幅と長さの装置上の平均値）を求めた。ここでの平均粒径としては、積算体積５０％の粒径値を用いた。また、粒度分布測定は、得られた粉体の５０ｍｇをエタノール１０ｍＬに分散させた懸濁液を、粒度分布測定装置のエタノールを媒体とする試料循環槽に滴下し、適切な濃度になった後に測定した。その結果、粉体の平均粒径は１６μｍであった。 (2) The average particle diameter, thickness, and flatness of the product 1 were measured as follows. That is, using a laser diffraction / scattering type particle size distribution measuring apparatus (Horiba: LA-920), the average particle diameter (width and length on the apparatus of the width and length) of the obtained powder in a dispersed state in ethanol in a flow cell. The average value was determined. As the average particle size, a particle size value with an integrated volume of 50% was used. In the particle size distribution measurement, a suspension in which 50 mg of the obtained powder was dispersed in 10 mL of ethanol was dropped into a sample circulation tank using ethanol as a medium in the particle size distribution measurement device, and after reaching an appropriate concentration. It was measured. As a result, the average particle size of the powder was 16 μm.
　また、得られた粒子の平均厚さは、走査型電子顕微鏡（日立製作所製Ｓ－２１５０）を用いて粒子を直接観察し、前記で求めた平均粒径と同等の大きさの粒子を複数選択し、厚さを測定し、それらを平均することにより求めた。走査型電子顕微鏡による観察では、得られた粉体の極少量を走査型電子顕微鏡の試料台に載せ、減圧にて乾燥後、白金を蒸着して検鏡試料とした。この検鏡試料を加速電圧１０～２５ｋＶで拡大率５００～１０,０００倍にて観察して得た画像から、前記で測定した平均粒径と同等の大きさの粒子における厚さを測定し、それらから平均厚さを求めた。その結果、平均厚さは１.７μｍであった。 The average thickness of the obtained particles was determined by directly observing the particles using a scanning electron microscope (S-2150, manufactured by Hitachi, Ltd.) and selecting a plurality of particles having a size equivalent to the average particle size obtained above. The thickness was measured and averaged. In observation with a scanning electron microscope, a very small amount of the obtained powder was placed on a sample stage of a scanning electron microscope, dried under reduced pressure, and platinum was deposited to obtain a spectroscopic sample. From the image obtained by observing the microscopic sample at an acceleration voltage of 10 to 25 kV and an enlargement ratio of 500 to 10,000 times, the thickness of particles having a size equivalent to the average particle size measured above was measured, The average thickness was determined from them. As a result, the average thickness was 1.7 μm.
　この結果、製品１は平均粒径が１６μｍで、平均厚さが１.７μｍ、扁平度（平均粒径／平均厚さ）が９.４の扁平なセルロース粒子（ラウロイルリジン処理微粒子酸化チタン複合高扁平セルロース粉体）であることが分かった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 As a result, the product 1 has an average particle diameter of 16 μm, an average thickness of 1.7 μm, and a flat cellulose particle (lauroyllysine-treated fine particle titanium oxide composite) having a flatness (average particle diameter / average thickness) of 9.4. Flat cellulose powder). Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　２
　　　ラウロイルリジン処理微粒子酸化チタン複合高扁平セルロース粉体の
　　　製造（２）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、ラウロイルリジン（アミホープＬＬ　味の素社製）を０.７ｇ、微粒子酸化チタン（ＴＴＯ－Ｓ－４　石原産業社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ラウロイルリジン処理微粒子酸化チタン複合高扁平セルロース粉体（製品２）を得た。 Example 2
Production of Lauroyllysine-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (2):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) and 28 g of fine titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine titanium oxide composite high flat cellulose powder. (Product 2) was obtained.
　得られた製品２について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１５μｍ、平均厚さが１.０μｍ、扁平度（平均粒径／平均厚さ）が１５の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 2 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 15 μm, the average thickness was 1.0 μm, and the flatness (average) The particle size / average thickness was 15 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　３
　　　水素添加レシチン処理微粒子酸化チタン複合高扁平セルロース粉体の
　　　製造（３）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（５５.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、水素添加レシチン（レシノールＳ－１０　日光ケミカルズ社製）を０.７ｇ、微粒子酸化チタン（ＴＴＯ－Ｓ－４　石原産業社製）を１４ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、水素添加レシチン処理微粒子酸化チタン複合高扁平セルロース粉体（製品３）を得た。 Example 3
Production of hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder (3):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 14 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder A body (product 3) was obtained.
　得られた製品３について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１６μｍ、平均厚さが１.９μｍ、扁平度（平均粒径／平均厚さ）が８.４の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 3 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 16 μm, the average thickness was 1.9 μm, and the flatness (average) The particle size / average thickness was 8.4. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　４
　　　水素添加レシチン処理微粒子酸化チタン複合高扁平セルロース粉体の
　　　製造（４）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、水素添加レシチン（レシノールＳ－１０　日光ケミカルズ社製）を０.７ｇ、微粒子酸化チタン（ＴＴＯ－Ｓ－４　石原産業社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、水素添加レシチン処理微粒子酸化チタン複合高扁平セルロース粉体（製品４）を得た。 Example 4
Production of hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder (4):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, hydrogenated lecithin-treated fine titanium oxide composite high flat cellulose powder A body (product 4) was obtained.
　得られた製品４について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１５μｍ、平均厚さが１.２μｍ、扁平度（平均粒径／平均厚さ）が１２.５の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 4 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 15 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　５
　　　セラミド処理微粒子酸化チタン複合高扁平セルロース粉体の
　　　製造（５）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ、微粒子酸化チタン（ＴＴＯ－Ｓ－４　石原産業社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理微粒子酸化チタン複合高扁平セルロース粉体（製品５）を得た。 Example 5
Production of Ceramide-treated Fine Titanium Oxide Composite High Flat Cellulose Powder (5):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle titanium oxide (TTO-S-4 Ishihara Sangyo Co., Ltd.) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated fine particle titanium oxide composite high flat cellulose powder ( Product 5) was obtained.
　得られた製品５について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１６μｍ、平均厚さが１.２μｍ、扁平度（平均粒径／平均厚さ）が１３.３の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 5 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 16 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 13.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　６
　　　ラウロイルリジン処理微粒子酸化亜鉛複合高扁平セルロース粉体の
　　　製造（６）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（５５.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、ラウロイルリジン（アミホープＬＬ　味の素社製）を０.７ｇ、微粒子酸化亜鉛（ＺｎＯ－６１０　住友大阪セメント社製）（平均粒径　２０ｎｍ）を１４ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ラウロイルリジン処理微粒子酸化亜鉛複合高扁平セルロース粉体（製品６）を得た。 Example 6
Production of Lauroyllysine-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (6):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co., Inc.) and 14 g of fine zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) (average particle size 20 nm) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine zinc oxide composite high flat cellulose powder. (Product 6) was obtained.
　得られた製品６について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１６μｍ、平均厚さが１.７μｍ、扁平度（平均粒径／平均厚さ）が９.４の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 For the obtained product 6, the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 16 μm, the average thickness was 1.7 μm, and the flatness (average) The particle size / average thickness was 9.4. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　７
　　　ラウロイルリジン処理微粒子酸化亜鉛複合高扁平セルロース粉体の
　　　製造（７）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、ラウロイルリジン（アミホープＬＬ　味の素社製）を０.７ｇ、微粒子酸化亜鉛（ＺｎＯ－６１０　住友大阪セメント社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ラウロイルリジン処理微粒子酸化亜鉛複合高扁平セルロース粉体（製品７）を得た。 Example 7
Production of Lauroyllysine-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (7):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) and 28 g of fine zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) were added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, lauroyllysine-treated fine zinc oxide composite high flat cellulose powder. (Product 7) was obtained.
　得られた製品７について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１５μｍ、平均厚さが１.０μｍ、扁平度（平均粒径／平均厚さ）が１５の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 7 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 15 μm, the average thickness was 1.0 μm, and the flatness (average) The particle size / average thickness was 15 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　８
　　　水素添加レシチン処理微粒子酸化亜鉛複合高扁平セルロース粉体の
　　　製造（８）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、水素添加レシチン（レシノールＳ－１０　日光ケミカルズ社製）を０.７ｇ、微粒子酸化亜鉛（ＺｎＯ－６１０　住友大阪セメント社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、水素添加レシチン処理微粒子酸化亜鉛複合高扁平セルロース粉体（製品８）を得た。 Example 8
Production of hydrogenated lecithin-treated fine zinc oxide composite high flat cellulose powder (8):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of fine zinc oxide (ZnO-610 manufactured by Sumitomo Osaka Cement) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and hydrogenated lecithin-treated fine zinc oxide composite high flat cellulose powder. A body (product 8) was obtained.
　得られた製品８について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１５μｍ、平均厚さが１.２μｍ、扁平度（平均粒径／平均厚さ）が１２.５の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 8 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 15 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　９
　　　セラミド処理微粒子酸化亜鉛複合高扁平セルロース粉体の
　　　製造（９）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ、微粒子酸化亜鉛（ＺｎＯ－６１０　住友大阪セメント社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理微粒子酸化亜鉛複合高扁平セルロース粉体（製品９）を得た。 Example 9
Production of Ceramide-treated Fine Zinc Oxide Composite High Flat Cellulose Powder (9):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) and 28 g of fine particle zinc oxide (ZnO-610, Sumitomo Osaka Cement Co., Ltd.) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated fine zinc oxide composite high flat cellulose powder ( Product 9) was obtained.
　得られた製品９について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１５μｍ、平均厚さが１.２μｍ、扁平度（平均粒径／平均厚さ）が１２.５の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 9 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 15 μm, the average thickness was 1.2 μm, and the flatness (average) The particle size / average thickness was 12.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１０
　　　水素添加レシチン処理酸化チタン複合高扁平セルロース粉体の
　　　製造（１０）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（５５.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、水素添加レシチン（レシノールＳ－１０　日光ケミカルズ社製）を０.７ｇ、酸化チタン（ＴＩＰＡＱＵＥ　ＣＲ－５０　石原産業社製）（平均粒径　２５０ｎｍ）を１４ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、水素添加レシチン処理酸化チタン複合高扁平セルロース粉体（製品１０）を得た。 Example 10
Production of hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (10):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) (average particle size 250 nm) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration) grinding energy), and hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder. (Product 10) was obtained.
　得られた製品１０について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１８μｍ、平均厚さが２.２μｍ、扁平度（平均粒径／平均厚さ）が８.２の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 10 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 18 μm, the average thickness was 2.2 μm, and the flatness (average) The particle size / average thickness was 8.2. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１１
　　　水素添加レシチン処理酸化チタン複合高扁平セルロース粉体の
　　　製造（１１）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、水素添加レシチン（レシノールＳ－１０　日光ケミカルズ社製）を０.７ｇ、酸化チタン（ＴＩＰＡＱＵＥ　ＣＲ－５０　石原産業社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、水素添加レシチン処理酸化チタン複合高扁平セルロース粉体（製品１１）を得た。 Example 11
Production of hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder (11):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration) grinding energy), and hydrogenated lecithin-treated titanium oxide composite high flat cellulose powder. (Product 11) was obtained.
　得られた製品１１について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１７μｍ、平均厚さが１.５μｍ、扁平度（平均粒径／平均厚さ）が１１.３の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 11 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１２
　　　セラミド処理酸化チタン複合高扁平セルロース粉体の製造（１２）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（５５.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ、酸化チタン（ＴＩＰＡＱＵＥ　ＣＲ－５０　石原産業社製）を１４ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理酸化チタン複合高扁平セルロース粉体（製品１２）を得た。 Example 12
Production of ceramide-treated titanium oxide composite high flat cellulose powder (12):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (55.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying under reduced pressure at 40 ° C. is put together with alumina grinding balls into a sealable alumina grinding container (volume: 500 mL). Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries) and 14 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added. After that, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, ceramide-treated titanium oxide composite high flat cellulose powder (product) 12) was obtained.
　得られた製品１２について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１８μｍ、平均厚さが２.２μｍ、扁平度（平均粒径／平均厚さ）が８.２の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 For the obtained product 12, the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 18 μm, the average thickness was 2.2 μm, and the flatness (average) The particle size / average thickness was 8.2. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１３
　　　セラミド処理酸化チタン複合高扁平セルロース粉体の製造（１３）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ、酸化チタン（ＴＩＰＡＱＵＥ　ＣＲ－５０　石原産業社製）を２８ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理酸化チタン複合高扁平セルロース粉体（製品１３）を得た。 Example 13
Production of ceramide-treated titanium oxide composite high flat cellulose powder (13):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries) and 28 g of titanium oxide (TIPAQUE CR-50 manufactured by Ishihara Sangyo Co., Ltd.) were added. After that, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, ceramide-treated titanium oxide composite high flat cellulose powder (product) 13) was obtained.
　得られた製品１３について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１７μｍ、平均厚さが１.５μｍ、扁平度（平均粒径／平均厚さ）が１１.３の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 13 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１４
　　　セラミド処理酸化チタン・酸化鉄複合高扁平セルロース粉体の
　　　製造（１４）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末４１.３ｇ（５９％）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ（１％）、酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００　テイカ社製）（平均粒径　２７０ｎｍ）を２１ｇ（３０％）、赤酸化鉄（タロックス　Ｒ－５１６Ｐ　チタン工業社製）（平均粒径　短軸：８０ｎｍ、長軸：８００ｎｍ）を０.８７５ｇ（１.２５％）、黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ　チタン工業社製）（平均粒径　短軸：９０ｎｍ、長軸：９００ｎｍ）を６.１２５ｇ（８.７５％）添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理酸化チタン・酸化鉄複合高扁平セルロース粉体（製品１４）を得た。 Example 14
Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (14):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, 41.3 g (59%) of cellulose powder from which adsorbed moisture has been sufficiently removed to 0.1% or less by drying under reduced pressure at 40 ° C. is placed in an alumina crushing container (capacity 500 mL) in an alumina crushing ball. In addition, 0.7 g (1%) of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.), 21 g (30%) of titanium oxide (manufactured by TITANIX JR-800 Teika) (average particle size 270 nm), red 0.875 g (1.25%) of iron oxide (Tarox R-516P made by Titanium Industry Co., Ltd.) (average particle diameter minor axis: 80 nm, major axis: 800 nm), yellow iron oxide (Tarox synthetic iron oxide YP1200P made by Titanium Industry Co., Ltd. ) (Average particle diameter minor axis: 90 nm, major axis: 900 nm) was added in an amount of 6.125 g (8.75%). Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder. A body (product 14) was obtained.
　得られた製品１４について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１７μｍ、平均厚さが１.５μｍ、扁平度（平均粒径／平均厚さ）が１１.３の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 14 was measured for average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１５
　　　セラミド処理酸化チタン・酸化鉄複合高扁平セルロース粉体の
　　　製造（１５）：
　実施例１４と同様な方法により、精製木材パルプ由来セルロース粉末（Ｗ－４００Ｇ）５９％、セラミド（Ｃｅｒａｍｉｄｅ　II）を１％、酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００）を３８.２％、赤酸化鉄（タロックス　Ｒ－５１６Ｐ）を０.４５％および黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ）を１.３５％を用い、セラミド処理酸化チタン・酸化鉄複合高扁平セルロース粉体（製品１５）を得た。 Example 15
Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (15):
In the same manner as in Example 14, purified wood pulp-derived cellulose powder (W-400G) 59%, ceramide (Ceramide II) 1%, titanium oxide (TITANIX JR-800) 38.2%, red iron oxide ( A ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 15) was obtained using 0.45% of Tarox R-516P) and 1.35% of yellow iron oxide (Tarox synthetic iron oxide YP1200P).
　得られた製品１５について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１７μｍ、平均厚さが１.５μｍ、扁平度（平均粒径／平均厚さ）が１１.３の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 15 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１６
　　　ステアリン酸処理酸化チタン・酸化鉄複合高扁平セルロース粉体の
　　　製造（１６）：
　実施例１４と同様な方法により、精製木材パルプ由来セルロース粉末（Ｗ－４００Ｇ）５７％、セラミドに代えてステアリン酸を３％、酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００）を３８.２％、赤酸化鉄（タロックス　Ｒ－５１６Ｐ）を０.４５％および黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ）を１.３５％を用い、ステアリン酸処理酸化チタン・酸化鉄複合高扁平セルロース粉体（製品１６）を得た。 Example 16
Manufacture of stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (16):
In the same manner as in Example 14, 57% of purified wood pulp-derived cellulose powder (W-400G), 3% of stearic acid instead of ceramide, 38.2% of titanium oxide (TITANIX JR-800), red iron oxide (Tarox R-516P) 0.45% and yellow iron oxide (Tarox synthetic iron oxide YP1200P) 1.35% were used to obtain stearic acid-treated titanium oxide / iron oxide composite high flat cellulose powder (Product 16). It was.
　得られた製品１６について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１７μｍ、平均厚さが１.１μｍ、扁平度（平均粒径／平均厚さ）が１５．５の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 16 was measured for the average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 17 μm, the average thickness was 1.1 μm, and the flatness (average) The particle size / average thickness was 15.5. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１７
　　　セラミド処理酸化チタン・酸化鉄複合高扁平セルロース粉体の
　　　製造（１７）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（４１.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ、酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００　テイカ社製）を２５.９ｇ、赤酸化鉄（タロックス　Ｒ－５１６Ｐ　チタン工業社製）を０.５２５ｇ、黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ　チタン工業社製）を１.５７５ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理酸化チタン・酸化鉄複合高扁平セルロース粉体（製品１７）を得た。 Example 17
Production of Ceramide-treated Titanium Oxide / Iron Oxide Composite High Flat Cellulose Powder (17):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (41.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing container (capacity 500 mL) together with alumina crushing balls. In addition, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries), 25.9 g of titanium oxide (TITANIX JR-800 Teika), and 0 of red iron oxide (Tarox R-516P made by Titanium Industry Co., Ltd.) .525 g, 1.575 g of yellow iron oxide (Tarox synthetic iron oxide YP1200P manufactured by Titanium Industry Co., Ltd.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding is performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)), and ceramide-treated titanium oxide / iron oxide composite high flat cellulose powder. A body (product 17) was obtained.
　得られた製品１７について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１７μｍ、平均厚さが１.５μｍ、扁平度（平均粒径／平均厚さ）が１１.３の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained product 17 was measured for the average particle size, thickness and flatness in the same manner as in Example 1 (2). The average particle size was 17 μm, the average thickness was 1.5 μm, and the flatness (average) The particle size / average thickness was 11.3. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
比　較　例　１
　　　セラミド処理高扁平セルロース粉体／酸化チタン・酸化鉄混合物の
　　　製造（１）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（６３.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理扁平セルロース粉体を得た。次に、得られたセラミド処理高扁平セルロース粉体（６０ｇ）と、酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００　テイカ社製）３０ｇ、赤酸化鉄（タロックス　Ｒ－５１６Ｐ　チタン工業社製）１.２５ｇ、黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ　チタン工業社製）８.７５ｇをヘンシェルミキサー（三井三池社製）にて１０分間混合し、セラミド処理高扁平セルロース粉体／酸化チタン・酸化鉄混合物（比較製品１）を得た。 Comparative Example 1
Manufacture of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (1):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotation speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) to obtain a ceramide-treated flat cellulose powder. Next, the obtained ceramide-treated high flattened cellulose powder (60 g), 30 g of titanium oxide (manufactured by TITANIX JR-800 Teika), 1.25 g of red iron oxide (Tarox R-516P manufactured by Titanium Industry Co., Ltd.), yellow oxide Iron (Tarox synthetic iron oxide YP1200P manufactured by Titanium Industry Co., Ltd.) 8.75 g was mixed for 10 minutes with a Henschel mixer (Mitsui Miike Co., Ltd.), and ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (Comparative product 1) Got.
　得られた比較製品１について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１９μｍ、平均厚さが１.４μｍ、扁平度（平均粒径／平均厚さ）が１３.６の扁平なものであった。 About the obtained comparative product 1, the average particle diameter, thickness, and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.
比　較　例　２
　　　セラミド処理高扁平セルロース粉体／酸化チタン・酸化鉄混合物の
　　　製造（２）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（６３.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、セラミド（Ｃｅｒａｍｉｄｅ　II　和光純薬社製）を０.７ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、セラミド処理高扁平セルロース粉体を得た。次に、得られたセラミド処理扁平セルロース粉体（６０ｇ）と、酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００　テイカ社製）３７ｇ、赤酸化鉄（タロックス　Ｒ－５１６Ｐ　チタン工業社製）０.７５ｇ、黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ　チタン工業社製）２.２５ｇをヘンシェルミキサー（三井三池社製）にて１０分間混合し、セラミド処理高扁平セルロース粉体／酸化チタン・酸化鉄混合物（比較製品２）を得た。 Comparative Example 2
Manufacture of ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (2):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Furthermore, 0.7 g of ceramide (Ceramide II Wako Pure Chemical Industries, Ltd.) was added. Thereafter, using a planetary ball mill (Misho Industry Co., Ltd.) and grinding at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) for 40 minutes, a ceramide-treated high flat cellulose powder was obtained. Next, the obtained ceramide-treated flat cellulose powder (60 g), 37 g of titanium oxide (manufactured by TITANIX JR-800 Teika Co., Ltd.), 0.75 g of red iron oxide (manufactured by Tarox R-516P Titanium Industry Co., Ltd.), yellow iron oxide 2.25 g (Tarox synthetic iron oxide YP1200P made by Titanium Industry Co., Ltd.) was mixed for 10 minutes with a Henschel mixer (Mitsui Miike Co., Ltd.), and a ceramide-treated high flat cellulose powder / titanium oxide / iron oxide mixture (Comparative product 2) Obtained.
　得られた比較製品２について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１９μｍ、平均厚さが１.４μｍ、扁平度（平均粒径／平均厚さ）が１３.６の扁平なものであった。 The obtained comparative product 2 was measured for average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.
比　較　例　３
　　　ラウロイルリジン処理高扁平セルロース粉体／微粒子酸化チタン
　　　混合物の製造（３）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（６３.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、ラウロイルリジン（アミホープＬＬ　味の素社製）を０.７ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ラウロイルリジン処理高扁平セルロース粉体を得た。次に、得られたラウロイルリジン処理扁平セルロース粉体（６０ｇ）と、微粒子酸化チタン（ＴＴＯ－Ｓ－４　石原産業社製）（１２ｇ）をヘンシェルミキサー（三井三池社製）にて１０分間混合し、ラウロイルリジン処理高扁平セルロース粉体／微粒子酸化チタン混合物（比較製品３）を得た。 Comparative Example 3
Production of Lauroyllysine-treated High Flat Cellulose Powder / Fine Particle Titanium Oxide Mixture (3):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) to obtain a lauroyllysine-treated high flat cellulose powder. Next, the obtained lauroyllysine-treated flat cellulose powder (60 g) and fine particle titanium oxide (TTO-S-4 manufactured by Ishihara Sangyo Co., Ltd.) (12 g) were mixed with a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) for 10 minutes. A lauroyllysine-treated high flat cellulose powder / fine particle titanium oxide mixture (Comparative Product 3) was obtained.
　得られた比較製品３について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１９μｍ、平均厚さが１.４μｍ、扁平度（平均粒径／平均厚さ）が１３.６の扁平なものであった。 About the obtained comparative product 3, the average particle diameter, thickness, and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.
比　較　例　４
　　　ラウロイルリジン処理高扁平セルロース粉体／微粒子酸化亜鉛混合物
　　　の製造（４）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（６３.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、ラウロイルリジン（アミホープＬＬ　味の素社製）を０.７ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ラウロイルリジン処理高扁平セルロース粉体を得た。次に、得られたラウロイルリジン処理扁平セルロース粉体（６０ｇ）と、微粒子酸化亜鉛（ＺｎＯ－６１０　住友大阪セメント社製）（１２ｇ）をヘンシェルミキサー（三井三池社製）にて１０分間混合し、ラウロイルリジン処理高扁平セルロース粉体と微粒子酸化亜鉛の混合物（比較製品４）を得た。 Comparative Example 4
Production of Lauroyllysine-treated High Flat Cellulose Powder / Fine Particle Zinc Oxide Mixture (4):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of lauroyl lysine (Amihop LL Ajinomoto Co.) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding was performed for 40 minutes at a rotational speed of 200 rpm (pulverization energy of about 10 G (gravity acceleration)) to obtain a lauroyllysine-treated high flat cellulose powder. Next, the obtained lauroyllysine-treated flat cellulose powder (60 g) and fine particle zinc oxide (ZnO-610, manufactured by Sumitomo Osaka Cement Co., Ltd.) (12 g) were mixed with a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.) for 10 minutes. A mixture (comparative product 4) of lauroyllysine-treated high flat cellulose powder and fine zinc oxide was obtained.
　得られた比較製品４について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１９μｍ、平均厚さが１.４μｍ、扁平度（平均粒径／平均厚さ）が１３.６の扁平なものであった。 About the obtained comparative product 4, the average particle diameter, thickness, and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.
比　較　例　５
　　　水素添加レシチン処理高扁平セルロースの製造（５）：
　原料としては精製した木材パルプ由来のセルロース粉末（日本製紙ケミカル社：Ｗ－４００Ｇ）を用いた。まず、４０℃での減圧乾燥により吸着水分を０.１％以下まで十分に除去したセルロース粉末（６３.３ｇ）を、密閉可能なアルミナ製粉砕容器（容積５００ｍＬ）に、アルミナ製粉砕ボールとともに投入し、更に、水素添加レシチン（レシノールＳ－１０　日光ケミカルズ社製）を０.７ｇ添加した。その後、遊星型ボールミル（三庄インダストリー株式会社）を用い、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、水素添加レシチン処理高扁平セルロース粉体（比較製品５）を得た。 Comparative Example 5
Production of hydrogenated lecithin-treated high flattened cellulose (5):
As a raw material, purified wood pulp-derived cellulose powder (Nippon Paper Chemical Co., Ltd .: W-400G) was used. First, cellulose powder (63.3 g) from which adsorbed moisture has been sufficiently removed to less than 0.1% by drying at 40 ° C. under reduced pressure is charged into an alumina crushing vessel (capacity 500 mL) together with alumina crushing balls. Further, 0.7 g of hydrogenated lecithin (Resinol S-10 manufactured by Nikko Chemicals) was added. Then, using a planetary ball mill (Misho Industry Co., Ltd.), grinding for 40 minutes at a rotation speed of 200 rpm (about 10 G (gravity acceleration) grinding energy), hydrogenated lecithin treated high flat cellulose powder (comparative product) 5) was obtained.
　得られた比較製品５について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１９μｍ、平均厚さが１.４μｍ、扁平度（平均粒径／平均厚さ）が１３.６の扁平なものであった。 The obtained comparative product 5 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 19 μm, the average thickness was 1.4 μm, and the flatness ( The average particle diameter / average thickness was 13.6.
比　較　例　６
　　　酸化チタン・酸化鉄複合セルロース粉体（６）：
　６０質量％の精製木材パルプ由来セルロース粉末（Ｗ－４００Ｇ）を、遊星型ボールミル（三庄インダストリー株式会社）に取り、これに酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００）を３８.２％、赤酸化鉄（タロックス　Ｒ－５１６Ｐ）を０.４５％および黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ）を１.３５％を加え、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、酸化チタン・酸化鉄複合セルロース粉体（比較製品６）を得た。 Comparative Example 6
Titanium oxide / iron oxide composite cellulose powder (6):
60% by mass of refined wood pulp-derived cellulose powder (W-400G) was put in a planetary ball mill (Misho Industry Co., Ltd.), and 38.2% titanium oxide (TITANIX JR-800), red iron oxide ( Add 0.45% of Tarox R-516P) and 1.35% of yellow iron oxide (Tarox synthetic iron oxide YP1200P), and crush for 40 minutes at a rotation speed of 200 rpm (crushing energy of about 10 G (gravity acceleration)). Then, a titanium oxide / iron oxide composite cellulose powder (Comparative Product 6) was obtained.
　得られた比較製品６について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が１８μｍ、平均厚さが２．０μｍ、扁平度（平均粒径／平均厚さ）が９．０の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained comparative product 6 was measured for the average particle diameter, thickness and flatness in the same manner as in Example 1 (2). The average particle diameter was 18 μm, the average thickness was 2.0 μm, and the flatness ( The average particle size / average thickness was 9.0. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
比　較　例　７
　　　ポリシロキサン処理酸化チタン・酸化鉄複合セリサイト（７）：
　６０質量％のジメチルポリシロキサン３％処理セリサイト（ＳＡセリサイトＦＳＥ；三好化成社製）を、遊星型ボールミル（三庄インダストリー株式会社）に取り、これに酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００）を３８.２％、赤酸化鉄（タロックス　Ｒ－５１６Ｐ）を０.４５％および黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ）を１.３５％を加え、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ポリシロキサン処理酸化チタン・酸化鉄複合セリサイト（比較製品７）を得た。 Comparative Example 7
Polysiloxane-treated titanium oxide / iron oxide composite sericite (7):
60% by mass of dimethylpolysiloxane 3% -treated sericite (SA sericite FSE; manufactured by Miyoshi Kasei Co., Ltd.) is placed in a planetary ball mill (Misho Industry Co., Ltd.), and titanium oxide (TITANIX JR-800) is added to 38 0.2%, 0.45% red iron oxide (Tarox R-516P) and 1.35% yellow iron oxide (Tarox synthetic iron oxide YP1200P) were added, and the grinding energy was 200rpm (about 10G (gravity acceleration)) ) For 40 minutes to obtain polysiloxane-treated titanium oxide / iron oxide composite sericite (Comparative Product 7).
　得られた比較製品７について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が７．０μｍ、平均厚さが１．０μｍ、扁平度（平均粒径／平均厚さ）が７．０の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 For the obtained comparative product 7, the average particle diameter, thickness and flatness were measured in the same manner as in Example 1 (2). The average particle diameter was 7.0 μm, the average thickness was 1.0 μm, and the flatness was measured. The degree (average particle diameter / average thickness) was 7.0. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
比　較　例　８
　　　ポリシロキサン処理処理酸化チタン・酸化鉄複合タルク（８）：
　６０質量％のジメチルポリシロキサン２％処理タルク（ＳＡタルクＪＡ－６８Ｒ；三好化成社製）を、遊星型ボールミル（三庄インダストリー株式会社）に取り、これに酸化チタン（ＴＩＴＡＮＩＸ　ＪＲ－８００）を３８.２％、赤酸化鉄（タロックス　Ｒ－５１６Ｐ）を０.４５％および黄酸化鉄（タロックス合成酸化鉄ＹＰ１２００Ｐ）を１.３５％を加え、回転数２００ｒｐｍ（約１０Ｇ（重力加速度）の粉砕エネルギー）にて、４０分間粉砕を行ない、ポリシロキサン処理処理酸化チタン・酸化鉄複合タルク（比較製品８）を得た。 Comparative Example 8
Polysiloxane-treated titanium oxide / iron oxide composite talc (8):
60% by mass of dimethylpolysiloxane 2% treated talc (SA talc JA-68R; manufactured by Miyoshi Kasei Co., Ltd.) is placed on a planetary ball mill (Misho Industry Co., Ltd.), and titanium oxide (TITANIX JR-800) is added to 38 0.2%, 0.45% red iron oxide (Tarox R-516P) and 1.35% yellow iron oxide (Tarox synthetic iron oxide YP1200P) were added, and the grinding energy was 200rpm (about 10G (gravity acceleration)) ) For 40 minutes to obtain polysiloxane-treated titanium oxide / iron oxide composite talc (Comparative Product 8).
　得られた比較製品８について、実施例１（２）と同様にして、平均粒径、厚さおよび扁平度を測定したところ、平均粒径が７．０μｍ、平均厚さが０．７μｍ、扁平度（平均粒径／平均厚さ）が１０．０の扁平なものであった。また、複合化後の金属酸化物の粒径は複合化前の粒径とほぼ同等であった。 The obtained comparative product 8 was measured for the average particle diameter, thickness, and flatness in the same manner as in Example 1 (2). The average particle diameter was 7.0 μm, the average thickness was 0.7 μm, and the flatness was measured. The degree (average particle diameter / average thickness) was 10.0 flat. Further, the particle size of the metal oxide after composite formation was almost the same as that before composite formation.
実　施　例　１８
　　　ＵＶ遮断性試験（１）：
　実施例１、２で製造した微粒子酸化チタン複合化高扁平セルロース粉体（製品１、製品２）について、そのＵＶ遮断能を調べた。実験は、１ｍｇ／ｃｍ２になるように、各粉体０.０４ｇをトランスポアテープ（５ｃｍ×８ｃｍ）に均一に塗布し、３００－４５０ｎｍの領域のＵＶ遮断能をＳＰＦアナライザー（三洋貿易社製）を用いて測定した。なお、比較としては、比較製品３を用いた。この結果を表１に示す。 Example 18
UV blocking test (1):
The UV blocking ability of the finely divided titanium oxide composite high flat cellulose powder (Product 1 and Product 2) produced in Examples 1 and 2 was examined. In the experiment, 0.04 g of each powder was uniformly applied to a transpore tape (5 cm × 8 cm) so as to be 1 mg / cm 2, and the UV blocking ability in the region of 300 to 450 nm was measured with an SPF analyzer (manufactured by Sanyo Trading Co., Ltd.). ). For comparison, comparative product 3 was used. The results are shown in Table 1.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　表１に示したように、本発明の製品１及び製品２は、微粒子酸化チタンを混合した高扁平セルロース粉体（比較製品３）に比べ、ＳＰＦ値が約５倍以上高く、ＵＶ遮断能に優れている粉体であった。 As shown in Table 1, the products 1 and 2 of the present invention have an SPF value of about 5 times higher than that of the high flat cellulose powder mixed with fine particle titanium oxide (Comparative Product 3), and have a UV blocking ability. It was an excellent powder.
実　施　例　１９
　　　ＵＶ遮断性試験（２）：
　実施例６～９で製造した微粒子酸化亜鉛複合化高扁平セルロース粉体（製品６～９）について、ＵＶ遮断能を実施例１８と同様にして調べた。なお、比較としては、比較製品４を使用した。この結果を表２に示す。 Example 19
UV blocking test (2):
The UV blocking ability of the fine zinc oxide composite high flat cellulose powder (Products 6 to 9) produced in Examples 6 to 9 was examined in the same manner as in Example 18. For comparison, the comparative product 4 was used. The results are shown in Table 2.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
　表２に示したように、本発明の製品６は、微粒子酸化亜鉛を混合した高扁平セルロース粉体（比較製品４）に比べ、ＳＰＦ値が約２倍以上高く、また、製品７～９は約３倍以上高く、本発明の粉体はＵＶ遮断能に優れている粉体であった。 As shown in Table 2, the product 6 of the present invention has an SPF value that is about twice or more higher than that of the highly flat cellulose powder mixed with fine zinc oxide (Comparative Product 4). About 3 times higher, the powder of the present invention was excellent in UV blocking ability.
実　施　例　２０
　　　色変化性試験：
　実施例１５および１６並びに比較例６ないし８で調製した粉体について、その色変化性を試験した。 Example 20
Color change test:
The powders prepared in Examples 15 and 16 and Comparative Examples 6 to 8 were tested for color change.
　まず各粉体を、同じ重量の油分（トリ２－エチルヘキサン酸グリセリル）と、へらで十分に混合し、被験試料を調製した。この被験試料と、製造された粉体自体を、ガラスセルに充填した後、その色値（ａ値；赤み／ｂ値；黄み）を、分光色差計ＳＥ－２０００（日本電飾工業社製）で、それぞれ測定した。 First, each powder was thoroughly mixed with the same weight of oil (glyceryl tri-2-ethylhexanoate) with a spatula to prepare a test sample. After filling this test sample and the produced powder itself into a glass cell, the color value (a value; redness / b value; yellowness) is measured with a spectral color difference meter SE-2000 (manufactured by Nippon Denshoku Kogyo Co., Ltd.). ) Respectively.
　これらの色値のうち、顔料自体のａ値（ａ１）およびｂ値（ｂ１）と、油分と混合した顔料のａ値（ａ２）およびｂ値（ｂ２）のそれぞれの差（ΔａおよびΔｂ）を求め、更にこの値から、下式で全体の色変化性を求めた。この色変化性を元に、下記基準により色変化性を評価した。この結果を表３に示す。 Among these color values, the difference (Δa and Δb) between the a value (a1) and b value (b1) of the pigment itself and the a value (a2) and b value (b2) of the pigment mixed with the oil component, respectively. Further, from this value, the whole color change property was obtained by the following equation. Based on this color change property, the color change property was evaluated according to the following criteria. The results are shown in Table 3.
　　　　色変化性＝√（（Δａ）２＋（Δｂ）２）
　　　　　　　　　但し、Δａは、ａ１とａ２の差を意味し、Δｂはｂ１と
　　　　　　　　　ｂ２の差を意味する。 Color changeability = √ ((Δa) 2 + (Δb) 2 )
However, Δa means the difference between a1 and a2, and Δb means the difference between b1 and b2.
　（　評価基準　）
　　　　色変化性　　　　　　　　：　　評　価
　　　　　０以上１.５以下　　　　:　　　◎
　　　　　１.５を越え２.０以下　：　　　○
　　　　　２.０を越え２.５以下　：　　　△
　　　　　２.５を越える～　　　　：　　　× ( Evaluation criteria )
Color change: Evaluation 0 or more and 1.5 or less: ◎
More than 1.5 and less than 2.0: ○
Over 2.0 and under 2.5: △
Over 2.5 ~: ×
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
　表３に示したように、本発明の製品１５及び製品１６は油分と混合しても色の変化が小さく優れたものであった。それに比べ、酸化チタン及び酸化鉄の混合量が同じであっても、粉砕助剤を用いていない比較製品６、ジメチルポリシロキサン処理セリサイトが母粉体である比較製品７、ジメチルポリシロキサン処理タルクが母粉体である比較製品８は、油分と混合した際に色の変化が大きく劣るものであった。 As shown in Table 3, the product 15 and the product 16 of the present invention were excellent with little color change even when mixed with oil. In contrast, even if the mixing amount of titanium oxide and iron oxide is the same, comparative product 6 without using a grinding aid, comparative product 7 in which dimethylpolysiloxane-treated sericite is the base powder, dimethylpolysiloxane-treated talc Comparative product 8, which is a mother powder, was greatly inferior in color change when mixed with oil.
実　施　例　２１
　　　パウダーファンデーション（１）：
　実施例１から５で製造した微粒子酸化チタン複合化高扁平セルロース粉体（製品１～５）を用い、表４の処方および下記方法で本発明化粧料１から５のパウダーファンデーションを調製した。このパウダーファンデーションについて、下記方法でＵＶ遮断能、ＳＰＦ値、化粧膜の均一性、自然な仕上がり（粉白さのなさ）、化粧持ち、安定性（凝集物の有無）、および使用感（塗布時の滑らかさ）を調べた。なお、比較として、微粒子酸化チタン被覆マイカ（マイカ５８．５％、酸化チタン４０％、酸化鉄１．５％）（ＳＰＳ－ＬＴＦ　テイカ社製）を利用したもの（比較化粧料１）および高扁平セルロース粉体と微粒子酸化チタンの混合物（比較製品３）を使用したもの（比較化粧料２）を用いた。この結果も表４に示す。 Example 21
Powder foundation (1):
Using the finely divided titanium oxide composite high flattened cellulose powders (Products 1 to 5) produced in Examples 1 to 5, powder foundations of the cosmetics 1 to 5 of the present invention were prepared by the formulation shown in Table 4 and the following method. About this powder foundation, UV blocking ability, SPF value, uniformity of makeup film, natural finish (no whitening), makeup lasting, stability (presence of aggregates), and feeling of use (when applying) Smoothness). As a comparison, fine titanium oxide-coated mica (mica 58.5%, titanium oxide 40%, iron oxide 1.5%) (manufactured by SPS-LTF Teica) (comparative cosmetic 1) and high flatness A mixture (comparative cosmetic 2) using a mixture of cellulose powder and fine particle titanium oxide (Comparative Product 3) was used. The results are also shown in Table 4.
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
　（　製造方法　）
　成分１～１８をヘンシェルミキサーにて１０分混合後、成分１９～２３を添加し、５分攪拌する。その後、アトマイザー（１ＨＰ　スクリーン径１.５ｍｍφ）にて粉砕し、樹脂皿に充填し、パウダーファンデーションを得る。 ( Production method )
Ingredients 1-18 are mixed in a Henschel mixer for 10 minutes, then ingredients 19-23 are added and stirred for 5 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.
　（　試験方法　）
　　ＵＶ遮断能およびＳＰＦ値：
　本発明化粧料１～５、及び比較化粧料１、２で製造したパウダーファンデーションについて、そのＵＶ遮断能を調べた。実験は、１ｍｇ／ｃｍ２になるように、各粉体０.０４ｇをトランスポアテープ（５ｃｍ×８ｃｍ）に均一に塗布し、３００－４５０ｎｍの領域のＵＶ遮断能を、ＳＰＦアナライザー（三洋貿易社製）を用いて測定した。尚、評価は、以下の判定にて実施した。 ( Test method )
UV blocking ability and SPF value:
The UV blocking ability of the powder foundations produced with the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2 was examined. In the experiment, 0.04 g of each powder was uniformly applied to a transpore tape (5 cm × 8 cm) so as to be 1 mg / cm 2, and the UV blocking ability in the region of 300 to 450 nm was measured with an SPF analyzer (Sanyo Trading Co., Ltd.). ). In addition, evaluation was implemented by the following determination.
　　評　価　　　内　　　容
　　　◎　：　ＳＰＦが２５以上である。
　　　○　：　ＳＰＦが２０以上、２５未満である。
　　　△　：　ＳＰＦが１５以上、２０未満である。
　　　×　：　ＳＰＦが１５未満である。 Evaluation content A: SPF is 25 or more.
○: SPF is 20 or more and less than 25.
Δ: SPF is 15 or more and less than 20.
X: SPF is less than 15.
　　「化粧膜の均一性」、「自然な仕上がり（粉白さのなさ）」、「化粧持
　　　ち（付着性及び色変化のなさ）」および「使用感」：
　化粧品評価専門パネル２０名に本発明化粧料１～５及び比較化粧料１、２のパウダーファンデーションを使用してもらい、「化粧膜の均一性」、「自然な仕上がり（粉白さのなさ）」、「化粧持ち（付着性及び色変化のなさ）」および「使用感」について各自が以下の評価基準に従って７段階評価し、サンプル毎に評点を付した。次いで、全パネルの評点の平均点から、以下の判定基準に従って各製品を判定した。なお、「使用感」は、塗布時のなめらかさで評価した。 “Makeup uniformity”, “Natural finish (no whitening)”, “Make-up (no adhesion and no color change)” and “Usage”:
Twenty panelists specializing in cosmetics evaluation use the powder foundations of the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2, and “uniformity of the cosmetic film” and “natural finish (no whitening)” Each of the samples was evaluated on a 7-point scale according to the following evaluation criteria for “make-up holding (no adhesion and no color change)” and “use feeling”, and a score was assigned to each sample. Next, each product was determined from the average score of all panels according to the following criteria. The “use feeling” was evaluated by the smoothness at the time of application.
　評価基準；
　　（評　価）　：　　（　内　容　）
　　　　６　　　：　　非常に良い
　　　　５　　　：　　良い
　　　　４　　　：　　やや良い
　　　　３　　　：　　普通
　　　　２　　　：　　やや悪い
　　　　１　　　：　　悪い
　　　　０　　　：　　非常に悪い Evaluation criteria;
(Evaluation): (Contents)
6: Very good 5: Good 4: Somewhat good 3: Normal 2: Somewhat bad 1: Bad 0: Very bad
　判定基準；
（　評点の平均点　）　　　　　：　　（判定）
　　５．０以上　　　　　　　　：　◎（非常に良好）
　　３．５以上５．０未満　　　：　○（良好）
　　１．５以上３．５未満　　　：　△（やや不良）
　　１．５未満　　　　　　　　：　×（不良） Judgment criteria;
(Average score): (Judgment)
5.0 or more: ◎ (very good)
3.5 or more and less than 5.0: ○ (good)
1.5 or more and less than 3.5: △ (somewhat poor)
Less than 1.5: × (defect)
　　安定性（凝集物の有無）：
　安定性は、凝集物の有無で評価した。樹脂皿に成型した本発明化粧料１～５及び比較化粧料１、２のパウダーファンデーションについて、化粧用スポンジを用いて、表面を２０回塗擦後の表面状態を目視にて観察した。尚、評価は、以下の判定にて実施した。 Stability (with or without aggregates):
Stability was evaluated by the presence or absence of aggregates. For the powder foundations of the cosmetics 1 to 5 of the present invention and the comparative cosmetics 1 and 2 molded on a resin dish, the surface state after 20 times of surface coating was visually observed using a cosmetic sponge. In addition, evaluation was implemented by the following determination.
　　評　価　　　　内　　容
　　　◎　：　凝集物が観察されない。
　　　○　：　凝集物が観察されるが、その量は少ない。
　　　△　：　凝集物が観察され、その量は多い。
　　　×　：　大きな凝集物が観察され、その量は多い。 Evaluation content A: Aggregates are not observed.
○: Aggregates are observed, but the amount is small.
Δ: Agglomerates are observed and the amount is large.
X: Large aggregates are observed and the amount is large.
　表４に示したように、本発明化粧料１～５のパウダーファンデーションはＳＰＦ値が高く、ＵＶ遮断能に優れ、化粧膜の均一性、自然な仕上がり（粉白さのなさ）、化粧持ち（付着性及び色変化のなさ）、安定性（凝集物の有無）、使用感（塗布時の滑らかさ）の全ての項目に優れるパウダーファンデーションであった。 As shown in Table 4, the powder foundations of the cosmetics 1 to 5 of the present invention have a high SPF value, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), long-lasting makeup ( The powder foundation was excellent in all the items of adhesion and no color change), stability (presence / absence of aggregates), and feeling of use (smoothness during application).
　それに対して、本発明化粧料１の製品１を従来の微粒子酸化チタン複合マイカに代えた比較化粧料１のパウダーファンデーションは粉体の凝集が見られ、化粧膜の均一性や自然な仕上がり等が劣るものであった。また、本発明化粧料１の製品１を比較製品３に代えた比較化粧料２のパウダーファンデーションはＳＰＦ値が低く、ＵＶ遮断能が劣り、使用感（塗布時の滑らかさ）等、全ての項目が劣るものであった。 On the other hand, the powder foundation of the comparative cosmetic 1 in which the product 1 of the cosmetic 1 of the present invention is replaced with the conventional fine particle titanium oxide composite mica shows agglomeration of the powder, and the uniformity of the cosmetic film, the natural finish, etc. It was inferior. Moreover, the powder foundation of the comparative cosmetic 2 in which the product 1 of the cosmetic 1 of the present invention is replaced with the comparative product 3 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application). Was inferior.
実　施　例　２２
　　　パウダーファンデーション（２）：
　実施例６から９で製造した微粒子酸化亜鉛複合化高扁平セルロース粉体を用い、表５の処方および下記方法で本発明化粧料６から９のパウダーファンデーションを調製した。このパウダーファンデーションについて、実施例２１と同様にしてＵＶ遮断能、ＳＰＦ値、化粧膜の均一性、自然な仕上がり（粉白さのなさ）、化粧持ち、使用感、および安定性を調べた。なお、比較として、微粒子酸化亜鉛被覆マイカ／硫酸バリウム複合体（マイカ４０％、酸化亜鉛５０％、硫酸バリウム１０％）（ＲＯＮＡＦＬＡＩＲ　ＳＨＡＤＥＬＥＡＦ　Ａ　メルク社製）を利用したもの（比較化粧料３）および高扁平セルロース粉体と微粒子酸化亜鉛の混合物（比較製品４）を利用したもの（比較化粧料４）を用いた。この結果も表５に示す。 Example 22
Powder foundation (2):
Using the fine zinc oxide composite high flat cellulose powder produced in Examples 6 to 9, powder foundations of the cosmetics 6 to 9 of the present invention were prepared according to the formulation shown in Table 5 and the following method. About this powder foundation, it carried out similarly to Example 21, and investigated UV blocking ability, SPF value, the uniformity of a cosmetic film, the natural finish (no powder whiteness), makeup lasting, usability, and stability. For comparison, a product using a zinc oxide-coated mica / barium sulfate composite (mica 40%, zinc oxide 50%, barium sulfate 10%) (manufactured by RONAFAIR SHADELEAF A Merck) (comparative cosmetic 3) and high A product (comparative cosmetic 4) using a mixture of flat cellulose powder and fine zinc oxide (Comparative product 4) was used. The results are also shown in Table 5.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
　（　製造方法　）
　成分１～１７をヘンシェルミキサーにて１０分混合後、成分１８～２２を添加し、５分攪拌する。その後、アトマイザー（１ＨＰ　スクリーン径１.５ｍｍφ）にて粉砕し、樹脂皿に充填し、パウダーファンデーションを得る。 ( Production method )
Ingredients 1-17 are mixed in a Henschel mixer for 10 minutes, then ingredients 18-22 are added and stirred for 5 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.
　表５に示したように、本発明化粧料６～９のパウダーファンデーションはＳＰＦ値が高く、ＵＶ遮断能に優れ、化粧膜の均一性、自然な仕上がり（粉白さのなさ）、化粧持ち、安定性（凝集物の有無）、使用感（塗布時の滑らかさ）の全ての項目に優れるパウダーファンデーションであった。 As shown in Table 5, the powder foundation of the cosmetics 6 to 9 of the present invention has a high SPF value, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), long-lasting makeup, The powder foundation was excellent in all items of stability (presence / absence of aggregates) and feeling of use (smoothness during application).
　それに対して、本発明化粧料６の製品６を微粒子酸化亜鉛被覆マイカ／硫酸バリウム複合粉体に代えた比較化粧料３のパウダーファンデーションは粉体の凝集が見られ、化粧膜の均一性や自然な仕上がり等が劣るものであった。また、本発明化粧料６の製品６を比較製品４に代えた比較化粧料４のパウダーファンデーションはＳＰＦ値が低く、ＵＶ遮断能が劣り、使用感（塗布時の滑らかさ）等、全ての項目が劣るものであった。 On the other hand, the powder foundation of the comparative cosmetic 3 in which the product 6 of the cosmetic 6 of the present invention is replaced with the fine particle zinc oxide-coated mica / barium sulfate composite powder shows agglomeration of the powder, uniformity of the cosmetic film and natural The finish was inferior. In addition, the powder foundation of the comparative cosmetic 4 in which the product 6 of the cosmetic 6 of the present invention is replaced with the comparative product 4 has a low SPF value, inferior UV blocking ability, and a feeling of use (smoothness during application). Was inferior.
実　施　例　２３
　　　パウダーファンデーション（３）：
　実施例１０から１３で製造した酸化チタン複合化高扁平セルロース粉体（製品１０～１３）を用い、表６の処方および下記方法で本発明化粧料１０から１３のパウダーファンデーションを調製した。このパウダーファンデーションについて、下記方法で隠蔽性を、また実施例２１と同様にして化粧膜の均一性、化粧持ちおよび使用感を調べた。なお、比較として、高扁平セルロース粉体と酸化チタンを別個に配合したもの（比較化粧料５、６）を用いた。この結果も表６に示す。 Example 23
Powder foundation (3):
Using the titanium oxide composite high flattened cellulose powders (Products 10 to 13) produced in Examples 10 to 13, powder foundations of the cosmetics 10 to 13 of the present invention were prepared by the formulation shown in Table 6 and the following method. The powder foundation was examined for concealment by the following method, and in the same manner as in Example 21, the uniformity of the cosmetic film, the cosmetic durability and the feeling of use were examined. For comparison, high-flat cellulose powder and titanium oxide (comparative cosmetics 5 and 6) were used separately. The results are also shown in Table 6.
Figure JPOXMLDOC01-appb-T000006
Figure JPOXMLDOC01-appb-T000006
　（　製造方法　）
　成分１～１６をヘンシェルミキサーにて１０分混合後、成分１７～１９を添加し、２分攪拌する。その後、アトマイザー（１ＨＰ　スクリーン径１.５ｍｍφ）にて粉砕し、樹脂皿に充填し、パウダーファンデーションを得る。 ( Production method )
Ingredients 1-16 are mixed in a Henschel mixer for 10 minutes, then ingredients 17-19 are added and stirred for 2 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.
　（　試験方法　）
　　隠蔽性：
化粧品評価専門パネル２０名に本発明化粧料１０～１３及び比較化粧料５、６のパウダーファンデーションを使用してもらい、「隠蔽性」について各自が以下の評価基準に従って７段階評価し、サンプル毎に評点を付した。次いで、全パネルの評点の平均点から、以下の判定基準に従って各製品を判定した。 ( Test method )
Concealment:
20 panelists specializing in cosmetics evaluation use the powder foundations of the present cosmetics 10 to 13 and comparative cosmetics 5 and 6, and each of them evaluates the “concealment” in 7 levels according to the following evaluation criteria. A rating was given. Next, each product was determined from the average score of all panels according to the following criteria.
　評価基準；
　（　評　価　）：　　（　内　容　）
　　　　６　　　：　　非常に良い
　　　　５　　　：　　良い
　　　　４　　　：　　やや良い
　　　　３　　　：　　普通
　　　　２　　　：　　やや悪い
　　　　１　　　：　　悪い
　　　　０　　　：　　非常に悪い Evaluation criteria;
(Evaluation): (Contents)
6: Very good 5: Good 4: Somewhat good 3: Normal 2: Somewhat bad 1: Bad 0: Very bad
　判定基準；
　（　評点の平均点　）　　　　　：　（　判　定　）
　　　５．０以上　　　　　　　　：　◎（非常に良好）
　　　３．５以上５．０未満　　　：　○（良好）
　　　１．５以上３．５未満　　　：　△（やや不良）
　　　１．５未満　　　　　　　　：　×（不良） Judgment criteria;
(Average score): (judgment)
5.0 or more: ◎ (very good)
3.5 or more and less than 5.0: ○ (good)
1.5 or more and less than 3.5: △ (somewhat poor)
Less than 1.5: × (defect)
　表６に示したように本発明化粧料１０～１３のパウダーファンデーションは、化粧膜の均一性、隠蔽性、化粧持ち、使用感（塗布時の滑らかさ）の全ての項目に優れるパウダーファンデーションであった。 As shown in Table 6, the powder foundation of the cosmetics 10 to 13 of the present invention is a powder foundation that is excellent in all items of uniformity of the cosmetic film, concealment, makeup lasting, and feeling of use (smoothness during application). It was.
　それに対して、本発明化粧料１０とほぼ同じ質量の酸化チタンを処理をせずに他成分と混合配合した比較化粧料５は、酸化チタンの分散が悪く、化粧持ちが悪く、隠蔽性や使用感（塗布時の滑らかさ）も劣るものであった。また、酸化チタンを倍量配合した比較化粧料６では隠蔽性は出るものの、使用感（塗布時の滑らかさ）や化粧膜の均一性、化粧持ちが悪いものであった。 On the other hand, the comparative cosmetic 5 in which the titanium oxide having almost the same mass as that of the cosmetic 10 of the present invention is mixed and mixed with other components without treatment is poor in dispersion of titanium oxide, has poor makeup, and has concealment and use. The feeling (smoothness during application) was also inferior. Moreover, although the comparative cosmetic 6 containing double amount of titanium oxide has a concealing property, the feeling of use (smoothness at the time of application), the uniformity of the cosmetic film, and the longevity of the makeup are poor.
実　施　例　２４
　　　パウダーファンデーション（４）：
　実施例１４から１５で製造した酸化チタン・酸化鉄複合化高扁平セルロース粉体（製品１４、１５）を用い、表７の処方および下記方法で本発明化粧料１４および１５のパウダーファンデーションを調製した。このパウダーファンデーションについて、下記方法で発色性を、また実施例２１と同様にして化粧膜の均一性、化粧持ちおよび使用感を調べた。 Example 24
Powder foundation (4):
Using the titanium oxide / iron oxide composite high flattened cellulose powder (Products 14 and 15) produced in Examples 14 to 15, the powder foundations of the cosmetics 14 and 15 of the present invention were prepared by the formulation shown in Table 7 and the following method. . The powder foundation was examined for color development by the following method, and in the same manner as in Example 21, the uniformity of the cosmetic film, the cosmetic durability and the feeling of use were examined.
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000007
　（　製造方法　）
　成分１～１３をヘンシェルミキサーにて１０分混合後、成分１４～１６を添加し、３分攪拌する。その後、アトマイザー（１ＨＰ　スクリーン径１.５ｍｍφ）にて粉砕し、樹脂皿に充填し、パウダーファンデーションを得る。 ( Production method )
Ingredients 1-13 are mixed in a Henschel mixer for 10 minutes, then ingredients 14-16 are added and stirred for 3 minutes. Then, it grind | pulverizes with an atomizer (1HP screen diameter 1.5mmphi), and it fills with a resin dish, and obtains a powder foundation.
　（　試験方法　）
　　発色性：
　化粧品評価専門パネル２０名に本発明化粧料１４～１５及び比較化粧料７、８のパウダーファンデーションを使用してもらい、その「発色性」について各自が以下の評価基準に従って７段階評価し、サンプル毎に評点を付した。次いで、全パネルの評点の平均点から、以下の判定基準に従って各製品を判定した。 ( Test method )
Color development:
20 panelists specializing in cosmetics evaluation use the powder foundations of the present cosmetics 14 to 15 and comparative cosmetics 7 and 8, and each of them evaluates their “color development” in 7 stages according to the following evaluation criteria. Was given a score. Next, each product was determined from the average score of all panels according to the following criteria.
　　　評価基準；
　（　評　価　）：　　（　内　容　）
　　　　６　　　：　　非常に良い
　　　　５　　　：　　良い
　　　　４　　　：　　やや良い
　　　　３　　　：　　普通
　　　　２　　　：　　やや悪い
　　　　１　　　：　　悪い
　　　　０　　　：　　非常に悪い Evaluation criteria;
(Evaluation): (Contents)
6: Very good 5: Good 4: Somewhat good 3: Normal 2: Somewhat bad 1: Bad 0: Very bad
　判定基準；
　（　評点の平均点　）　　　　　：　（　判　定　）
　　　５．０以上　　　　　　　　：　◎（非常に良好）
　　　３．５以上５．０未満　　　：　○（良好）
　　　１．５以上３．５未満　　　：　△（やや不良）
　　　１．５未満　　　　　　　　：　×（不良） Judgment criteria;
(Average score): (judgment)
5.0 or more: ◎ (very good)
3.5 or more and less than 5.0: ○ (good)
1.5 or more and less than 3.5: △ (somewhat poor)
Less than 1.5: × (defect)
　表７に示したように本発明化粧料１４及び１５のパウダーファンデーションは、化粧膜の均一性、隠蔽性、化粧持ち、使用感（塗布時の滑らかさ）の全ての項目に優れるパウダーファンデーションであった。 As shown in Table 7, the powder foundations of the cosmetics 14 and 15 of the present invention are powder foundations that are excellent in all items of uniformity of the cosmetic film, concealment, makeup lasting, and feeling of use (smoothness during application). It was.
　それに対して、酸化チタンや酸化鉄をセルロース粉体と混合処理した混合物を配合した比較化粧料７及び８は発色性や化粧持ちが特に悪いものであった。 On the other hand, comparative cosmetics 7 and 8 containing a mixture of titanium oxide or iron oxide mixed with cellulose powder had particularly poor color development and long lasting makeup.
実　施　例　２５
　　　パウダーファンデーション（５）：
　実施例７で製造した微粒子酸化亜鉛複合化高扁平セルロース粉体（製品７）を用い、表８の処方および下記方法で本発明化粧料１６のパウダーファンデーションを調製した。このパウダーファンデーションについて、下記方法でＳＰＦ値を、また実施例２１と同様にしてＵＶ遮断能、化粧膜の均一性、自然な仕上がり（粉白さのなさ）、化粧持ち、安定性（凝集物の有無）、使用感（塗布時の滑らかさ）を調べた。なお、比較としては、比較例４の扁平セルロース粉末と微粒子酸化亜鉛混合物を使用した化粧料（比較化粧料９）用いた。この結果を表８に示す。 Example 25
Powder foundation (5):
Using the fine zinc oxide composite high flat cellulose powder (Product 7) produced in Example 7, a powder foundation of the cosmetic 16 of the present invention was prepared according to the formulation shown in Table 8 and the following method. For this powder foundation, the SPF value was determined by the following method, and in the same manner as in Example 21, UV blocking ability, uniformity of the cosmetic film, natural finish (no whitening), makeup retention, stability (of aggregates) Existence) and usability (smoothness during application) were examined. For comparison, a cosmetic (comparative cosmetic 9) using the flat cellulose powder of Comparative Example 4 and a fine particle zinc oxide mixture was used. The results are shown in Table 8.
（　製造方法　）
　　Ａ：成分１～１２をヘンシェルミキサーにて１０分混合する。
　　Ｂ：Ａに成分１３～１８を添加し、４分混合する。
　　Ｃ：Ｂをアトマイザー（１ＨＰ　スクリーン径１.５ｍｍφ）にて粉砕す
　　　　る。
　　Ｄ：軽質流動パラフィン６０部とＣ１００部を混合し、樹脂皿に充填成
　　　　型後、７０℃で乾燥させパウダーファンデーションを得る。 ( Production method )
A: Components 1 to 12 are mixed with a Henschel mixer for 10 minutes.
B: Components 13 to 18 are added to A and mixed for 4 minutes.
C: B is pulverized with an atomizer (1HP screen diameter 1.5 mmφ).
D: 60 parts of light liquid paraffin and 100 parts of C are mixed, filled in a resin dish, dried at 70 ° C. to obtain a powder foundation.
　（　実測ＳＰＦ値　）
　日本化粧品工業連合会の定める「ＳＰＦ測定法基準（２００７年改訂版）」を基準とした、以下の方法により評価した。 (Measured SPF value)
Evaluation was made by the following method based on “SPF measurement method standard (2007 revised version)” established by the Japan Cosmetic Industry Association.
　まず、被験者を、ＦｉｔｚｐａｔｒｉｃｋのスキンタイプＩ、II、IIIに該当する１８歳以上６０歳以下の健康な男女から１０名選択した（ただし、問診を行い、光線過敏症を有する人や、皮膚の光感受性に関与するような薬物（抗炎症剤、降圧剤など）を服用する人を除いた）。また、被験部位としては、被験者の背部とし、色素沈着や母斑などがなく、ほぼ均一な皮膚色をしている部位を選択した。この被験部位の５０ｃｍ２に、被験試料を塗布した。塗布量は、２.００ｍｇ／ｃｍ２±２.５％／ｃｍ２とした。 First, 10 subjects were selected from healthy men and women aged 18 to 60 who fall under Fitzpatrick skin types I, II, and III (however, they were interviewed and those with photosensitivity or light on the skin) (Except for those who take drugs related to sensitivity (such as anti-inflammatory drugs, antihypertensive drugs)). Moreover, as a test site | part, the site | part which is a test subject's back, and there is no pigmentation, a nevus, etc. and the skin color was substantially uniform was selected. A test sample was applied to 50 cm 2 of this test site. The coating amount was 2.00 mg / cm 2 ± 2.5% / cm 2 .
　上記、被験者の試験試料塗布部位に、キセノンアークソーラーシュミレーター（ＳＯＬＡＲ　ＬＩＧＨＴ社製）を光源として用い、紫外線を照射した。このキセノンアークシュミレーターは、波長２９０～４００ｎｍのＵＶ－ＢおよびＵＶ－Ａ領域において、太陽光に近似した連続スペクトルを有するものである。また、波長２９０ｎｍ以下の紫外線は、フィルターを用い、可能な限り除去した。 The test sample application site of the subject was irradiated with ultraviolet rays using a xenon arc solar simulator (manufactured by SOLAR LIGHT) as a light source. This xenon arc simulator has a continuous spectrum similar to that of sunlight in the UV-B and UV-A regions with wavelengths of 290 to 400 nm. Further, ultraviolet rays having a wavelength of 290 nm or less were removed as much as possible using a filter.
　紫外線を照射してから１６～２４時間後に、十分に明るい部屋で、紫外線被照射部位の紅斑の発生を調べた。被照射部位の２／３以上の部位に、境界が明瞭な、僅かな紅斑を最初に惹起する最小の紫外線照射量を、最小紅斑量（ＭＥＤ）とした。被験試料塗布部と無塗布部でのＭＥＤをそれぞれ用い、下式により各被験者のＳＰＦ値を求め、これを算術平均して実測ＳＰＦ値とした。 16 to 24 hours after irradiation with ultraviolet rays, the occurrence of erythema at the site irradiated with ultraviolet rays was examined in a sufficiently bright room. The minimum amount of ultraviolet irradiation that initially causes slight erythema with a clear boundary at 2/3 or more of the irradiated region was defined as the minimum erythema dose (MED). Using the MED at the test sample application part and the non-application part, respectively, the SPF value of each subject was determined by the following formula, and this was arithmetically averaged to obtain the measured SPF value.
　　　　ＳＰＦ値　＝　ＭＥＤ（試料塗布部）／ＭＥＤ（試料無塗布部） SPF value = MED (sample application part) / MED (sample non-application part)
Figure JPOXMLDOC01-appb-T000008
Figure JPOXMLDOC01-appb-T000008
　表８に示したように、本発明化粧料１６のパウダーファンデーションは、比較化粧料９に比べＳＰＦ実測値が高くなり、ＵＶ遮断能に優れ、化粧膜の均一性、自然な仕上がり（粉白さのなさ）、化粧持ち（付着性及び色変化のなさ）、安定性（凝集物の有無）、使用感（塗布時の滑らかさ）の全ての項目に優れるパウダーファンデーションであった。 As shown in Table 8, the powder foundation of the cosmetic 16 of the present invention has a higher SPF measured value than the comparative cosmetic 9, excellent UV blocking ability, uniformity of the cosmetic film, natural finish (powder whiteness) No powder), makeup lasting (no adhesion and no color change), stability (presence of agglomerates), and feeling of use (smoothness during application) were excellent powder foundations.
　それに対して、本発明化粧料１６の製品７をラウロイルリジン処理高扁平セルロース粉体／微粒子酸化亜鉛混合物に代えた比較化粧料９のパウダーファンデーションはＳＰＦ実測値及びＵＶ遮断能がやや低く、さらに、使用感（塗布時の滑らかさ）等、全ての項目が劣るものであった。 On the other hand, the powder foundation of the comparative cosmetic 9 in which the product 7 of the cosmetic 16 of the present invention is replaced with a lauroyl lysine-treated high flattened cellulose powder / particulate zinc oxide mixture has a slightly low SPF measured value and UV blocking ability, All items, such as a feeling of use (smoothness at the time of application | coating), were inferior.
実　施　例　２６
　　　パウダーファンデーション（６）
　実施例１４で調製した製品１４および実施例１５で調製した製品１５の顔料を用い、下記表９に記載の組成により、下記方法でパウダーファンデーションを製造した（処方１～３）。比較としては、特段処理をしない酸化鉄を用いたものを使用した（比較処方）。なお、本実施例での各処方での酸化鉄の総量は、組成１が比較処方と同量（１００％）であり、組成２および３は、比較処方の８０％である。 Example 26
Powder foundation (6)
Using the pigments of the product 14 prepared in Example 14 and the product 15 prepared in Example 15, powder foundations were prepared by the following method according to the composition described in Table 9 below (Formulations 1 to 3). As a comparison, the one using iron oxide not subjected to special treatment was used (comparison prescription). In addition, as for the total amount of iron oxide in each prescription in a present Example, the composition 1 is the same amount (100%) as a comparison prescription, and the compositions 2 and 3 are 80% of a comparison prescription.
Figure JPOXMLDOC01-appb-T000009
Figure JPOXMLDOC01-appb-T000009
　＜　製造方法　＞
　Ａ：　成分１～１３を、ヘンシェルミキサーにて１０分間混合する。
　Ｂ：　Ａに成分１４～２０を添加し、５分間混合する。
　Ｃ：　Ｂをアトマイザー（１ＨＰ　スクリーン径１.５ｍｍφ）にて粉砕す
　　　　る。
　Ｄ：　軽質流動パラフィン６０部と、Ｃ１００部を混合し、樹脂皿に充填
　　　　成型後、７０℃で乾燥させ、パウダーファンデーションを得る。 <Manufacturing method>
A: Components 1 to 13 are mixed with a Henschel mixer for 10 minutes.
B: Add components 14 to 20 to A and mix for 5 minutes.
C: B is pulverized with an atomizer (1HP screen diameter 1.5 mmφ).
D: 60 parts of light liquid paraffin and 100 parts of C are mixed, filled in a resin dish, molded and dried at 70 ° C. to obtain a powder foundation.
　得られた各組成について、「発色性」、「化粧持ち（色沈みのなさ）」、「化粧持ち（付着性）」を調べた。化粧持ち（付着性）については、実施例２１と同様にして調べた。また、「発色性」については、上記製造方法により成型された状態の各パウダーファンデーションを、「化粧持ち（色沈みのなさ）」については、各パウダーファンデーションを上腕内側部上に塗布したものを、それぞれの外観色について、分光色差計ＳＥ－２０００（日本電飾工業社製）を用い、ａおよびｂ、あるいはＬ、ａおよびｂを測定し、下記のように計算することで評価した。この結果は表１０に示す。 For each of the obtained compositions, “color development”, “long-lasting makeup (no color sink)”, and “long-lasting makeup (adhesion)” were examined. The makeup holding (adhesiveness) was examined in the same manner as in Example 21. In addition, for “color development”, each powder foundation in a state molded by the above manufacturing method, and for “makeup (no color sink)”, each powder foundation applied on the inner side of the upper arm, Each appearance color was evaluated by measuring a and b or L, a and b using a spectral color difference meter SE-2000 (manufactured by Nippon Denshoku Kogyo Co., Ltd.) and calculating as follows. The results are shown in Table 10.
　　発　色　性：
　各処方について、測定したそれぞれのａおよびｂの値を、比較処方のａおよびｂの値（ａｓおよびｂｓ）と比較し、その差（ΔａおよびΔｂ）を求めた。このΔａおよびΔｂを、２乗して加えた後、その値を平方根で開き、その値を「発色性」の評価値とした。この評価値については、１以上が◎、０.５以上１未満を○、０.２５以上０.５未満を△、０.２５未満を×として評価した。 Color development:
For each formulation, the measured a and b values were compared to the comparative formulation a and b values (as and bs) to determine the difference (Δa and Δb). After Δa and Δb were squared and added, the value was opened with a square root, and the value was used as an evaluation value of “color development”. For this evaluation value, 1 or more was evaluated as ◎, 0.5 or more and less than 1 as ◯, 0.25 or more and less than 0.5 as Δ, and less than 0.25 as ×.
　　化粧持ち（色沈みのなさ）：
　塗布直後および塗布２時間後に、本発明処方および比較処方の外観の、Ｌ、ａおよびｂの値を求めた。各処方での塗布直後および塗布２時間後の測定値の差（ΔＬ０－２、Δａ０－２およびΔｂ０－２）をそれぞれ２乗し、これらを足し合わせた後に、平方根で開いた。この値を「化粧持ち（色沈みのなさ）」の評価値とした。この評価値については、０以上１以下が◎、１を超え１.５以下を○、１.５を超え２以下を△、２を超えたものを×として評価した。 Makeup (no color sink):
Immediately after application and 2 hours after application, the values of L, a, and b of the appearances of the present invention and comparative formulations were determined. The difference between the measured values immediately after application in each formulation and 2 hours after application (ΔL 0-2 , Δa 0-2 and Δb 0-2 ) was squared, and after adding them, the square root was opened. This value was used as an evaluation value for “long makeup (no color sinking)”. With respect to this evaluation value, 0 or more and 1 or less were evaluated as ◎, 1 and 1.5 or less were evaluated as ◯, 1.5 or more and 2 or less as Δ, and 2 or more as x.
Figure JPOXMLDOC01-appb-T000010
Figure JPOXMLDOC01-appb-T000010
　表１０に示したように、実施例１４の製品１４を用いて、処方全体中に、比較処方と同質量の酸化鉄を配合した処方１は、比較処方に比べ、発色性が高まり、塗布２時間後の色沈みが小さく、付着性に優れるものであった。また、処方１から酸化鉄の配合量を減らして、酸化鉄の配合量を比較処方の８０％にした処方２は、酸化鉄の配合量が比較処方より少ないにもかかわらず、比較処方よりも発色性に優れ、他の項目も優れていた。実施例１５の製品１５を使用し、処方２同様に酸化鉄の配合量を比較処方の８０％にした処方３も、発色性が良好であり、他の項目も優れていた。 As shown in Table 10, the formulation 1 in which the same amount of iron oxide as the comparative formulation was blended in the overall formulation using the product 14 of Example 14 was higher in color development than the comparative formulation, and the application 2 The color settling after time was small and the adhesion was excellent. In addition, Formula 2 in which the compounding amount of iron oxide is reduced from Formula 1 and the compounding amount of iron oxide is 80% of the comparative formulation is less than that of the comparative formulation, although the compounding amount of iron oxide is smaller than that of the comparative formulation. Excellent color development and other items were also excellent. The formulation 3 using the product 15 of Example 15 and having the compounding amount of iron oxide 80% of the comparative formulation as in the formulation 2 also had good color development and other items.
実　施　例　２７
　　　二層ローション：
　以下に示す組成の二層ローションを下記の方法により製造した。 Example 27
Double layer lotion:
A two-layer lotion having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000011
Figure JPOXMLDOC01-appb-I000011
　　（　製　法　）
　（１）成分１～３を混合する。
　（２）（１）に成分４～９を添加、均一に攪拌し、二層ローションを
　　　　得た。 (Production method)
(1) Components 1 to 3 are mixed.
(2) Components 4 to 9 were added to (1) and stirred uniformly to obtain a two-layer lotion.
　得られた二層ローションは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性に優れた二層ローションであった。 The obtained two-layer lotion was excellent in powder dispersibility, a smooth feeling in use, and a two-layer lotion excellent in the uniformity of the decorative film.
実　施　例　２８
　　　乳　　液　：
　以下に示す組成の乳液を下記の方法により製造した。 Example 28
Milk liquid:
An emulsion having the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000012
Figure JPOXMLDOC01-appb-I000012
　　（　製　法　）
　（１）成分１～７を８０℃にて均一に混合する。
　（２）成分８～１４を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）を攪拌しながら冷却し、成分１５を添加後均一混合し、
　　　　乳液を得た。 (Production method)
(1) Components 1 to 7 are uniformly mixed at 80 ° C.
(2) Components 8 to 14 are mixed uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) Cool (3) while stirring, add component 15 and mix uniformly;
An emulsion was obtained.
　得られた乳液は、乳化安定性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能に優れた乳液であった。 The obtained emulsion was excellent in emulsification stability, smooth use feeling, uniformity of decorative film, and excellent UV blocking ability.
実　施　例　２９
　　　クリーム：
　以下に示す組成のクリームを下記の方法により製造した。 Example 29
cream:
A cream having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000013
Figure JPOXMLDOC01-appb-I000013
　　（　製　法　）
　（１）成分１～７を８０℃にて均一に混合する。
　（２）成分８～１３を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）を攪拌しながら冷却し、クリームを得た。 (Production method)
(1) Components 1 to 7 are uniformly mixed at 80 ° C.
(2) Components 8 to 13 are mixed uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) (3) was cooled with stirring to obtain a cream.
　得られたクリームは乳化安定性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能に優れたクリームであった。 The obtained cream was excellent in emulsification stability, smooth use feeling, uniformity of cosmetic film, and excellent UV blocking ability.
実　施　例　３０
　　　美　容　液　：
　以下に示す組成の美容液を下記の方法により製造した。 Example 30
Beauty liquid:
A serum having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000014
Figure JPOXMLDOC01-appb-I000014
　　（　製　法　）
　（１）成分１～１０を常温にて混合溶解し、攪拌しながら美容液を得た。 (Production method)
(1) Components 1 to 10 were mixed and dissolved at room temperature, and a cosmetic liquid was obtained while stirring.
　得られた美容液は安定性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能に優れた美容液であった。 The obtained essence was excellent in stability, smooth sensation of use, uniformity of cosmetic film, and essence excellent in UV blocking ability.
実　施　例　３１
　　　パ　ッ　ク　：
　以下に示す組成のパックを下記の方法により製造した。 Example 31
Pack:
A pack having the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000015
Figure JPOXMLDOC01-appb-I000015
　　（　製　法　）
　（１）成分１～４を８０℃にて均一に混合する。
　（２）成分５～１２を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）を攪拌しながら冷却し、パックを得た。 (Production method)
(1) Components 1 to 4 are uniformly mixed at 80 ° C.
(2) Mix components 5 to 12 uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) (3) was cooled with stirring to obtain a pack.
　得られたパックは乳化安定性に優れ、滑らかな使用感、化粧膜の均一性に優れたパックであった。 The obtained pack was excellent in emulsification stability, smooth in feeling of use, and excellent in uniformity of the decorative film.
実　施　例　３２
　　　洗　顔　料　：
　以下に示す組成の洗顔料を下記の方法により製造した。 Example 32
Facial wash :
A face wash having the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000016
Figure JPOXMLDOC01-appb-I000016
　　（　製　法　）
　（１）成分１～７を８０℃にて均一に混合する。
　（２）成分８～１１を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、中和する。
　（４）（３）に成分１２を添加し、均一に混合する。
　（５）（４）を攪拌しながら冷却し、洗顔料を得た。 (Production method)
(1) Components 1 to 7 are uniformly mixed at 80 ° C.
(2) Components 8 to 11 are mixed uniformly at 80 ° C.
(3) Add (2) to (1) and neutralize.
(4) Add component 12 to (3) and mix uniformly.
(5) (4) was cooled while stirring to obtain a face wash.
　得られた洗顔料は滑らかな使用感に優れた洗顔料であった。 The obtained facial cleanser was an excellent facial cleanser.
実　施　例　３３
　　　クレンジングクリーム：
　以下に示す組成のクレンジングクリームを下記の方法により製造した。 Example 33
Cleansing cream:
A cleansing cream having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000017
Figure JPOXMLDOC01-appb-I000017
　　（　製　法　）
　（１）成分１～８を８０℃にて均一に混合する。
　（２）成分９～１４を８０℃にて均一に混合する。
　（３）（２）に（１）を添加し、乳化する。
　（４）（３）を攪拌しながら冷却し、クレンジングクリームを得た。 (Production method)
(1) Components 1 to 8 are uniformly mixed at 80 ° C.
(2) Components 9 to 14 are uniformly mixed at 80 ° C.
(3) Add (1) to (2) and emulsify.
(4) Cooling with stirring (3) gave a cleansing cream.
　得られたクレンジングクリームは乳化安定性に優れ、滑らかな使用感に優れたクレンジングクリームであった。 The obtained cleansing cream was excellent in emulsification stability and excellent in smooth use feeling.
実　施　例　３４
　　　ヘアワックス：
　以下に示す組成のヘアワックスを下記の方法により製造した。 Example 34
Hair wax:
A hair wax having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000018
Figure JPOXMLDOC01-appb-I000018
　　（　製　法　）
　（１）成分１～３を８０℃にて均一に混合する。
　（２）成分４～８を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）に成分９～１６を添加後、攪拌しながら冷却し、
　　　　ヘアワックスを得た。 (Production method)
(1) Components 1 to 3 are uniformly mixed at 80 ° C.
(2) Components 4 to 8 are uniformly mixed at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) After adding components 9 to 16 to (3), cool with stirring,
A hair wax was obtained.
　得られたヘアワックスは乳化安定性、整髪性に優れ、滑らかな使用感、ＵＶ遮断能に優れたヘアワックスであった。 The obtained hair wax was excellent in emulsification stability and hair styling property, and was a hair wax excellent in smooth use feeling and UV blocking ability.
実　施　例　３５
　　　油性アイライナー：
　以下に示す組成の油性アイライナーを下記の方法により製造した。 Example 35
Oily eyeliner:
An oily eyeliner having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000019
Figure JPOXMLDOC01-appb-I000019
　　（　製　法　）
　（１）成分１～４を１００℃に加温し、均一混合する。
　（２）成分５～９を８０℃に加温し、均一混合する。
　（３）（１）に（２）を添加し、均一に混合する。
　（４）（３）をローラーにて処理し、油性アイライナーを得た。 (Production method)
(1) Ingredients 1 to 4 are heated to 100 ° C. and mixed uniformly.
(2) Ingredients 5 to 9 are heated to 80 ° C. and mixed uniformly.
(3) Add (2) to (1) and mix uniformly.
(4) (3) was processed with a roller to obtain an oily eyeliner.
　得られた油性アイライナーは滑らかな使用感、化粧膜の均一性、化粧持続効果に優れた油性アイライナーであった。 The obtained oily eyeliner was an oily eyeliner excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.
実　施　例　３６
　　　水性アイライナー：
　以下に示す組成の水性アイライナーを下記の方法により製造した。 Example 36
Aqueous eyeliner:
An aqueous eyeliner having the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000020
Figure JPOXMLDOC01-appb-I000020
　　（　製　法　）
　（１）成分１～５をローラーにて均一に分散する。
　（２）成分６～１０を均一に混合する。
　（３）（２）に（１）を添加、均一に混合し、水性アイライナーを得た。 (Production method)
(1) Components 1 to 5 are uniformly dispersed with a roller.
(2) Components 6 to 10 are mixed uniformly.
(3) (1) was added to (2) and mixed uniformly to obtain an aqueous eyeliner.
　得られた水性アイライナーは滑らかな使用感、化粧膜の均一性、化粧持続効果に優れた水性アイライナーであった。 The obtained water-based eyeliner was a water-based eyeliner excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.
実　施　例　３７
　　　アイブロウ：
　以下に示す組成のアイブロウを下記の方法により製造した。 Example 37
Eyebrow:
An eyebrow having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000021
Figure JPOXMLDOC01-appb-I000021
　　（　製　法　）
　（１）成分１～４を均一に混合する。
　（２）成分５～１０をローラーにて処理する。
　（３）（１）に（２）、成分１１、１２を添加後、均一に混合し、
　　　　アイブロウを得た。 (Production method)
(1) Components 1 to 4 are mixed uniformly.
(2) Components 5 to 10 are treated with a roller.
(3) After adding (2), components 11 and 12 to (1), mix uniformly,
I got an eyebrow.
　得られたアイブロウは滑らかな使用感、化粧膜の均一性、化粧持続効果に優れたアイブロウであった。 The obtained eyebrow was an eyebrow excellent in smooth use feeling, uniformity of the makeup film, and makeup lasting effect.
実　施　例　３８
　　　Ｏ／Ｗ型マスカラ：
　以下に示す組成のＯ／Ｗ型マスカラを下記の方法により製造した。 Example 38
O / W type mascara:
An O / W type mascara having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000022
Figure JPOXMLDOC01-appb-I000022
　　（　製　法　）
　（１）成分１～８を８０℃にて均一に混合し、ローラー処理する。
　（２）成分９～１４を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）を冷却し、マスカラ（Ｏ／Ｗ）を得た。 (Production method)
(1) Components 1 to 8 are uniformly mixed at 80 ° C. and subjected to a roller treatment.
(2) Components 9 to 14 are uniformly mixed at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) (3) was cooled to obtain mascara (O / W).
　得られたＯ／Ｗ型マスカラは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、化粧持続効果に優れたＯ／Ｗ型マスカラであった。 The obtained O / W type mascara was excellent in powder dispersibility, and was an O / W type mascara excellent in smooth feeling of use, uniformity of the cosmetic film, and makeup lasting effect.
実　施　例　３９
　　　非水系マスカラ：
　以下に示す組成の非水系マスカラを下記の方法により製造した。 Example 39
Non-aqueous mascara:
A non-aqueous mascara having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000023
Figure JPOXMLDOC01-appb-I000023
　　（　製　法　）
　（１）成分１～５を１１０℃に加温する。
　（２）（１）に成分６～９を添加混合する。
　（３）（２）に成分１０～１３を添加混合する。
　（４）（３）をローラーにて処理し、非水系マスカラを得た。 (Production method)
(1) Ingredients 1 to 5 are heated to 110 ° C.
(2) Add components 6 to 9 to (1) and mix.
(3) Add components 10 to 13 to (2) and mix.
(4) (3) was processed with a roller to obtain a non-aqueous mascara.
　得られた非水系マスカラは滑らかな使用感、化粧膜の均一性、化粧持続効果に優れた非水系マスカラであった。 The obtained non-aqueous mascara was a non-aqueous mascara excellent in smooth use feeling, uniformity of the cosmetic film, and a makeup lasting effect.
実　施　例　４０
　　　スティック状口紅：
　以下に示す組成のスティック状口紅を下記の方法により製造した。 Example 40
Sticky lipstick:
A stick-shaped lipstick having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000024
Figure JPOXMLDOC01-appb-I000024
　　（　製　法　）
　（１）成分１～７を１００℃にて均一に溶解混合する。
　（２）（１）に成分８～１３を添加し、均一に混合する。
　（３）（２）を容器に流し込み、冷却してスティック状口紅を得た。 (Production method)
(1) Components 1 to 7 are uniformly dissolved and mixed at 100 ° C.
(2) Add components 8 to 13 to (1) and mix uniformly.
(3) (2) was poured into a container and cooled to obtain a stick-shaped lipstick.
　得られたスティック状口紅は滑らかな使用感、化粧膜の均一性、化粧持続効果に優れた口紅であった。 The obtained stick-shaped lipstick was a lipstick with a smooth feeling of use, uniformity of the cosmetic film, and excellent makeup lasting effect.
実　施　例　４１
　　　リキッドルージュ：
　以下に示す組成のリキッドルージュを下記の方法により製造した。 Example 41
Liquid Rouge:
A liquid rouge having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000025
Figure JPOXMLDOC01-appb-I000025
　　（　製　法　）
　（１）成分１～５を１００℃にて均一に溶解混合する。
　（２）（１）に成分６～１２を添加し、均一に混合する。
　（３）（２）を容器に流し込み、冷却してリキッドルージュを得た。 (Production method)
(1) Components 1 to 5 are uniformly dissolved and mixed at 100 ° C.
(2) Add components 6 to 12 to (1) and mix uniformly.
(3) (2) was poured into a container and cooled to obtain a liquid rouge.
　得られたリキッドルージュは滑らかな使用感、化粧膜の均一性、化粧持続効果に優れたリキッドルージュであった。 The obtained liquid rouge was a liquid rouge excellent in smooth feeling of use, uniformity of the makeup film, and makeup lasting effect.
実　施　例　４２
　　　Ｏ／Ｗ型ファンデーション：
　以下に示す組成のＯ／Ｗ型ファンデーションを下記の方法により製造した。 Example 42
O / W type foundation:
An O / W type foundation having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000026
Figure JPOXMLDOC01-appb-I000026
　　（　製　法　）
　（１）成分１～８をローラーにて均一に分散する。
　（２）成分９～１２を均一に混合する。
　（３）（２）に（１）を添加し、均一に混合する。
　（４）成分１３～１９を８０℃にて混合溶解する。
　（５）（３）に（４）を８０℃にて添加し、乳化する。
　（６）（５）を冷却し、成分２０を添加し、Ｏ／Ｗ型ファンデーションを
　　　　得た。 (Production method)
(1) Components 1 to 8 are uniformly dispersed with a roller.
(2) Mix components 9 to 12 uniformly.
(3) Add (1) to (2) and mix uniformly.
(4) Components 13 to 19 are mixed and dissolved at 80 ° C.
(5) Add (4) to (3) at 80 ° C. and emulsify.
(6) (5) was cooled, component 20 was added, and an O / W type foundation was obtained.
　得られたＯ／Ｗ型ファンデーションは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、隠蔽性、ＵＶ遮断能、化粧持続効果に優れたＯ／Ｗ型ファンデーションであった。 The obtained O / W type foundation was excellent in powder dispersibility, and was an O / W type foundation excellent in smooth use feeling, uniformity of cosmetic film, hiding property, UV blocking ability, and makeup lasting effect.
実　施　例　４３
　　　Ｗ／Ｏ型ファンデーション：
　以下に示す組成のＷ／Ｏ型ファンデーションを下記の方法により製造した。 Example 43
W / O type foundation:
A W / O type foundation having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000027
Figure JPOXMLDOC01-appb-I000027
　　（　製　法　）
　（１）成分１～３を均一に混合する。
　（２）成分４～１１をローラーにて均一に分散する。
　（３）（１）に（２）を添加し、均一混合する。
　（４）（３）に成分１２～１５を添加、乳化し、Ｗ／Ｏ型ファンデーショ
　　　　ンを得た。 (Production method)
(1) Components 1 to 3 are mixed uniformly.
(2) Components 4 to 11 are uniformly dispersed with a roller.
(3) Add (2) to (1) and mix uniformly.
(4) Components 12 to 15 were added to (3) and emulsified to obtain a W / O type foundation.
　得られたＷ／Ｏ型ファンデーションは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、隠蔽性、ＵＶ遮断能、化粧持続効果に優れたＷ／Ｏ型ファンデーションであった。 The obtained W / O-type foundation was excellent in powder dispersibility, and was a W / O-type foundation excellent in smooth feeling of use, cosmetic film uniformity, hiding properties, UV blocking ability, and makeup lasting effect.
実　施　例　４４
　　　Ｏ／Ｗ型アイカラー：
　以下に示す組成のＯ／Ｗ型アイカラーを下記の方法により製造した。 Example 44
O / W eye color:
An O / W eye color having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000028
Figure JPOXMLDOC01-appb-I000028
　　（　製　法　）
　（１）成分１～５を８０℃にて均一に混合する。
　（２）（１）に成分６～８を添加し、乳化する。
　（３）成分９～１４をローラーにて均一に分散する。
　（４）（２）に（３）、成分１５を添加し、Ｏ／Ｗ型アイカラーを得た。 (Production method)
(1) Components 1 to 5 are uniformly mixed at 80 ° C.
(2) Add components 6 to 8 to (1) and emulsify.
(3) Components 9 to 14 are uniformly dispersed with a roller.
(4) (3) and Component 15 were added to (2) to obtain an O / W type eye color.
　得られたＯ／Ｗ型アイカラーは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、発色性、化粧持続効果に優れたＯ／Ｗ型アイカラーであった。 The obtained O / W type eye color was excellent in powder dispersibility, and was an O / W type eye color excellent in smooth feeling of use, uniformity of the cosmetic film, color developability, and makeup lasting effect.
実　施　例　４５
　　　油性固型ファンデーション：
　以下に示す組成の油性固型ファンデーションを下記の方法により製造した。 Example 45
Oil solid foundation:
An oily solid foundation having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000029
Figure JPOXMLDOC01-appb-I000029
　　（　製　法　）
　（１）成分７～１３を９０℃にて加熱溶解する。
　（２）（１）に成分１～６を添加し、ローラーにて均一に分散する。
　（３）（２）に成分１４を添加し、８０℃にて溶解後、金皿に充填し、
　　　　油性固型ファンデーションを得た。 (Production method)
(1) Components 7 to 13 are dissolved by heating at 90 ° C.
(2) Add components 1 to 6 to (1) and uniformly disperse with a roller.
(3) Add component 14 to (2) and dissolve at 80 ° C., then fill into a metal pan,
An oily solid foundation was obtained.
　得られた油性固型ファンデーションは粉体分散性に優れ、滑らかな使用感で、化粧膜の均一性、ＵＶ遮断能、化粧持続効果にも優れた油性固型ファンデーションであった。 The obtained oil-based solid foundation was excellent in powder dispersibility, had a smooth feeling of use, and was excellent in the uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.
実　施　例　４６
　　　スティック状コンシーラー：
　以下に示す組成のスティック状コンシーラーを下記の方法により製造した。 Example 46
Stick concealer:
A stick concealer having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000030
Figure JPOXMLDOC01-appb-I000030
　　（　製　法　）
　（１）成分１～５を９０℃にて加熱溶解する。
　（２）（１）に成分６～１２を添加し、ローラーにて均一に分散する。
　（３）（２）に成分１３を添加し、８０℃にて溶解後、容器に充填し、
　　　　スティック状コンシーラーを得た。 (Production method)
(1) Components 1 to 5 are dissolved by heating at 90 ° C.
(2) Add components 6 to 12 to (1) and uniformly disperse with a roller.
(3) Add component 13 to (2) and dissolve at 80 ° C.
A stick-like concealer was obtained.
　得られたスティック状コンシーラーは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、隠蔽性、ＵＶ遮断能、化粧持続効果に優れたスティック状コンシーラーであった。 The obtained stick-like concealer was excellent in powder dispersibility, and was a stick-like concealer excellent in smooth feeling of use, makeup film uniformity, hiding property, UV blocking ability, and makeup lasting effect.
実　施　例　４７
　　　ボディミルク：
　以下に示す組成のボディミルクを下記の方法により製造した。 Example 47
Body milk:
Body milk having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000031
Figure JPOXMLDOC01-appb-I000031
　　（　製　法　）
　（１）成分１～７を８０℃にて均一に溶解する。
　（２）成分８～１６を８０℃にて均一に溶解する。
　（３）（２）に（１）を添加し、乳化する。
　（４）（３）に成分１７を添加、均一混合後、攪拌冷却し、
　　　　ボディミルクを得た。 (Production method)
(1) Components 1 to 7 are uniformly dissolved at 80 ° C.
(2) Components 8 to 16 are uniformly dissolved at 80 ° C.
(3) Add (1) to (2) and emulsify.
(4) Add component 17 to (3), stir and cool after uniform mixing,
Got body milk.
　得られたボディミルクは乳化安定性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能、化粧持続効果に優れたボディミルクであった。 The obtained body milk was excellent in emulsification stability, and was excellent in smooth use feeling, uniformity of cosmetic film, UV blocking ability, and makeup lasting effect.
実　施　例　４８
　　　コンディショナー：
　以下に示す組成のコンディショナーを下記の方法により製造した。 Example 48
conditioner:
A conditioner having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000032
Figure JPOXMLDOC01-appb-I000032
　　（　製　法　）
　（１）成分１～５を８０℃にて均一に混合する。
　（２）成分６～９を８０℃にて均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）に成分１０を添加、均一混合後、攪拌冷却し、
　　　　コンディショナーを得た。 (Production method)
(1) Components 1 to 5 are uniformly mixed at 80 ° C.
(2) Mix components 6 to 9 uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) Add component 10 to (3), stir and cool after uniform mixing,
I got a conditioner.
　得られたコンディショナーは乳化安定性に優れ、滑らかな使用感に優れたコンディショナーであった。 The obtained conditioner was excellent in emulsification stability and excellent in smooth use feeling.
実　施　例　４９
　　　ヘアパック：
　以下に示す組成のヘアパックを下記の方法により製造した。 Example 49
Hair pack:
A hair pack having the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000033
Figure JPOXMLDOC01-appb-I000033
　　（　製　法　）
　（１）成分１～６を８０℃にて均一に混合する。
　（２）成分７～９を８０℃に均一に混合する。
　（３）（１）に（２）を添加し、乳化する。
　（４）（３）に成分１０を添加、均一混合後、攪拌冷却し、
　　　　ヘアパックを得た。 (Production method)
(1) Components 1 to 6 are mixed uniformly at 80 ° C.
(2) Mix components 7 to 9 uniformly at 80 ° C.
(3) Add (2) to (1) and emulsify.
(4) Add component 10 to (3), stir and cool after uniform mixing,
I got a hair pack.
　得られたヘアパックは乳化安定性に優れ、滑らかな使用感に優れたヘアパックであった。 The obtained hair pack was excellent in emulsification stability and was excellent in smooth usability.
実　施　例　５０
　　　Ｗ／Ｏ型日焼け止め料：
　以下に示す組成の日焼け止め料を下記の方法により製造した。 Example 50
W / O sunscreen:
A sunscreen with the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000034
Figure JPOXMLDOC01-appb-I000034
　　（　製　法　）
　（１）成分１～５をローラーにて均一に分散する。
　（２）（１）に成分６～９を添加し、均一に混合する。
　（３）（２）に成分１０～１４を添加、乳化し、Ｗ／Ｏ型日焼け止め料を
　　　　得た。 (Production method)
(1) Components 1 to 5 are uniformly dispersed with a roller.
(2) Add components 6 to 9 to (1) and mix uniformly.
(3) Components 10 to 14 were added to (2) and emulsified to obtain a W / O type sunscreen.
　得られたＷ／Ｏ型日焼け止め料は粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能、化粧持続効果に優れた日焼け止め料であった。 The obtained W / O type sunscreen was excellent in powder dispersibility, and was excellent in smooth use feeling, uniformity of cosmetic film, UV blocking ability, and makeup lasting effect.
実　施　例　５１
　　　マニキュア：
　以下に示す組成のマニキュアを下記の方法により製造した。 Example 51
Manicure:
A nail polish having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000035
Figure JPOXMLDOC01-appb-I000035
　　（　製　法　）
　（１）成分１～９を均一に混合し、マニキュアを得た。 (Production method)
(1) Components 1 to 9 were mixed uniformly to obtain nail polish.
　得られたマニキュアは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、化粧持続効果に優れたマニキュアであった。 The obtained nail polish was excellent in powder dispersibility, smooth maneuverability, uniformity of the cosmetic film, and excellent makeup lasting effect.
実　施　例　５２
　　　化粧下地：
　以下に示す組成の化粧下地を下記の方法により製造した。 Example 52
Makeup base:
A makeup base having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000036
Figure JPOXMLDOC01-appb-I000036
　　（　製　法　）
　（１）成分１～４を８０℃にて均一に溶解する。
　（２）成分５～１２を８０℃にて均一に溶解する。
　（３）（２）に（１）を添加し、乳化する。
　（４）（３）に成分１３～１４を添加混合、冷却し、化粧下地を得た。 (Production method)
(1) Components 1 to 4 are uniformly dissolved at 80 ° C.
(2) Components 5 to 12 are uniformly dissolved at 80 ° C.
(3) Add (1) to (2) and emulsify.
(4) Components 13 to 14 were added to (3), mixed and cooled to obtain a makeup base.
　得られた化粧下地は乳化安定性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能、化粧持続効果に優れた下地であった。 The obtained makeup base was excellent in emulsification stability, and was excellent in smooth use feeling, uniformity of makeup film, UV blocking ability, and makeup lasting effect.
実　施　例　５３
　　　白　　粉　：
　以下に示す組成の白粉を下記の方法により製造した。 Example 53
White powder:
White powder having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000037
Figure JPOXMLDOC01-appb-I000037
　　（　製　法　）
　（１）成分１～５、成分８～１０を均一に混合する。
　（２）（１）に成分６、７を添加し、均一に混合する。
　（３）（２）をパルベライザーで粉砕し、白粉を得た。 (Production method)
(1) Components 1 to 5 and components 8 to 10 are mixed uniformly.
(2) Add components 6 and 7 to (1) and mix uniformly.
(3) (2) was pulverized with a pulverizer to obtain white powder.
　得られた白粉は粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能、化粧持続効果に優れた白粉であった。 The obtained white powder was excellent in powder dispersibility, and was excellent in smooth use feeling, uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.
実　施　例　５４
　　　固形粉末型ファンデーション：
　以下に示す組成の固形粉末型ファンデーションを下記の方法により製造した。 Example 54
Solid powder foundation:
A solid powder type foundation having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000038
Figure JPOXMLDOC01-appb-I000038
　　（　製　法　）
　（１）成分１～７、成分１１～１３を均一に混合する。
　（２）（１）に成分８～１０を添加し、均一に混合する。
　（３）（２）をパルベライザーで粉砕する。
　（４）（３）を金皿に充填し、固形粉末型ファンデーションを得た。 (Production method)
(1) Components 1 to 7 and components 11 to 13 are mixed uniformly.
(2) Add components 8 to 10 to (1) and mix uniformly.
(3) Grind (2) with a pulverizer.
(4) A metal pan was filled with (3) to obtain a solid powder type foundation.
　得られた固形粉末型ファンデーションは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能、化粧持続効果に優れたファンデーションであった。 The obtained solid powder type foundation was excellent in powder dispersibility, and had a smooth feeling in use, uniformity of a cosmetic film, UV blocking ability, and a makeup lasting effect.
実　施　例　５５
　　　固形粉末型チーク：
　以下に示す組成の固形粉末型チークを下記の方法により製造した。 Example 55
Solid powder type teak:
A solid powder type cheek having the composition shown below was produced by the following method.
Figure JPOXMLDOC01-appb-I000039
Figure JPOXMLDOC01-appb-I000039
　　（　製　法　）
　（１）成分１～４、成分７～９を均一に混合する。
　（２）（１）に成分５、６を添加し、均一に混合する。
　（３）（２）をパルベライザーで粉砕する。
　（４）（３）を金皿に充填し、固形粉末型チークを得た。 (Production method)
(1) Components 1 to 4 and components 7 to 9 are mixed uniformly.
(2) Add components 5 and 6 to (1) and mix uniformly.
(3) Grind (2) with a pulverizer.
(4) (3) was filled in a metal pan to obtain a solid powder type teak.
　得られた固形粉末型チークは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、ＵＶ遮断能、化粧持続効果に優れたチークであった。 The obtained solid powder type cheek was excellent in powder dispersibility, excellent in smooth use feeling, uniformity of the cosmetic film, UV blocking ability, and makeup lasting effect.
実　施　例　５６
　　　固形粉末型アイシャドウ：
　以下に示す組成の固形粉末型アイシャドウを下記の方法により製造した。 Example 56
Solid powder eyeshadow:
A solid powder eye shadow having the following composition was produced by the following method.
Figure JPOXMLDOC01-appb-I000040
Figure JPOXMLDOC01-appb-I000040
　　（　製　法　）
　（１）成分１～６、成分１０～１２を均一に混合する。
　（２）（１）に成分７～９を添加し、均一に混合する。
　（３）（２）をパルベライザーで粉砕する。
　（４）（３）を金皿に充填し、固形粉末型ファンデーションを得た。 (Production method)
(1) Components 1 to 6 and components 10 to 12 are mixed uniformly.
(2) Add components 7 to 9 to (1) and mix uniformly.
(3) Grind (2) with a pulverizer.
(4) A metal pan was filled with (3) to obtain a solid powder type foundation.
　得られた固形粉末型アイシャドウは粉体分散性に優れ、滑らかな使用感、化粧膜の均一性、発色性、化粧持続効果に優れたファンデーションであった。 The obtained solid powder type eye shadow was excellent in powder dispersibility, and had a smooth feeling in use, a makeup film uniformity, color development, and a makeup lasting effect.
　本発明の金属酸化物複合化高扁平セルロース粉体は、基材のセルロース自体が有機物であり、しかも扁平であるとともに、その表面が極めて微細な金属酸化物粒子で複合化されているため、従来の扁平な無機物であるタルクやセリサイトを金属酸化物で複合化した粉体と比べ、付着性が高く、優れた使用感があるとともに、金属酸化物によるＵＶ遮断能や、発色力も優れたものである。 In the metal oxide composite high flat cellulose powder of the present invention, since the base cellulose itself is an organic substance and is flat, the surface thereof is composited with extremely fine metal oxide particles. Compared with powders made by combining talc and sericite, which are flat inorganic materials, with metal oxides, they have higher adhesion, excellent usability, and excellent UV blocking ability and coloring ability due to metal oxides It is.
　従って、本発明の金属酸化物複合化高扁平セルロース粉体は、多くの化粧料に利用できるが、特にその効果が発現しやすい化粧料としては、パウダーファンデーション、アイシャドウ、ほほ紅、粉白粉等の粉体成分と油性成分とを含有する化粧料を挙げることができる。これらの化粧料の中でもプレス充填された化粧料が好ましく、特にパウダーファンデーションおよびアイシャドウが好ましい。本発明の化粧料をパウダーファンデーションおよびアイシャドウとした場合には、粉っぽさが無く、ウェット感、肌への付着力がよく、その結果、肌と自然に馴染み、ムラ、ヨレ、色のくすみ、浮きなどの無い、化粧持ちの良いものとなる。 Accordingly, the metal oxide-complexed high flat cellulose powder of the present invention can be used in many cosmetics. Particularly, cosmetics that easily exhibit the effect include powder foundation, eye shadow, blusher, powdered white powder, etc. And cosmetics containing the powder component and the oil component. Among these cosmetics, press-filled cosmetics are preferable, and powder foundations and eye shadows are particularly preferable. When the cosmetic of the present invention is a powder foundation and eye shadow, there is no powderiness, good wet feeling, good adhesion to the skin, and as a result, it blends naturally with the skin, unevenness, twist, color It will have good makeup without dullness or float.

Claims (20)

  1. 　セルロース系物質と、粉砕助剤と、金属酸化物とを機械的に粉砕処理することにより得られる金属酸化物複合化高扁平セルロース粉体。 Metal oxide composite high flat cellulose powder obtained by mechanically pulverizing a cellulosic material, a pulverization aid, and a metal oxide.
  2. 　平均粒径が１～５０μｍ、平均厚さが０.１～１０μｍ、かつ扁平度が４～２００である請求項１記載の金属酸化物複合化高扁平セルロース粉体。 2. The metal oxide composite high flat cellulose powder according to claim 1, having an average particle diameter of 1 to 50 μm, an average thickness of 0.1 to 10 μm, and a flatness of 4 to 200.
  3. 　全体中の金属酸化物の量が５～５０質量％である請求項１または２記載の金属酸化物複合化高扁平セルロース粉体。 3. The metal oxide composite high flat cellulose powder according to claim 1, wherein the amount of the metal oxide in the whole is 5 to 50% by mass.
  4. 　全体中の粉砕助剤の量が０.５～５質量％である請求項１ないし３のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 4. The metal oxide composite high flattened cellulose powder according to claim 1, wherein the amount of the grinding aid in the whole is 0.5 to 5% by mass.
  5. 　機械的な粉砕処理を遊星型ボールミルで行う請求項１ないし４のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 The metal oxide composite high flat cellulose powder according to any one of claims 1 to 4, wherein the mechanical pulverization is performed by a planetary ball mill.
  6. 　セルロース系物質が、木材を起源とする繊維状もしくは粉末状の木粉または木材パルプ、綿花を起源とする繊維状もしくは粉末状の木綿またはリンター繊維並びにそれらを精製した繊維状または粉末状のものからなる群から選ばれるセルロース系物質である請求項１ないし５のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 Cellulosic material from fibrous or powdered wood flour or wood pulp originating from wood, fibrous or powdered cotton or linter fiber originating from cotton and refined fibers or powders The metal oxide composite high flat cellulose powder according to any one of claims 1 to 5, which is a cellulosic material selected from the group consisting of:
  7. 　粉砕助剤が、両親媒性物質、アミノ酸類および脂肪酸類よりなる群より選ばれるものである請求項１ないし６のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 The metal oxide composite high flattened cellulose powder according to any one of claims 1 to 6, wherein the grinding aid is selected from the group consisting of an amphiphile, amino acids and fatty acids.
  8. 　両親媒性物質が、リン脂質、セラミド、コレステロールもしくはその誘導体およびフィトステロールもしくはその誘導体からなる群から選ばれるものである請求項７記載の金属酸化物複合化高扁平セルロース粉体。 The metal oxide composite high flat cellulose powder according to claim 7, wherein the amphiphilic substance is selected from the group consisting of phospholipid, ceramide, cholesterol or a derivative thereof and phytosterol or a derivative thereof.
  9. 　アミノ酸類が、Ｎ－アシルアミノ酸、テアニンからなる群から選ばれるものである請求項７記載の金属酸化物複合化高扁平セルロース粉体。 The metal oxide composite high flat cellulose powder according to claim 7, wherein the amino acids are selected from the group consisting of N-acylamino acids and theanine.
  10. 　脂肪酸類が、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸およびその塩からなる群から選ばれるものである請求項７記載の金属酸化物複合化高扁平セルロース粉体。 The metal oxide composite high flattened cellulose powder according to claim 7, wherein the fatty acids are selected from the group consisting of lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid and salts thereof.
  11. 　金属酸化物が、酸化鉄、酸化チタンおよび酸化亜鉛よりなる群から選ばれる化合物である請求項１ないし１０のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 The metal oxide composite high flat cellulose powder according to any one of claims 1 to 10, wherein the metal oxide is a compound selected from the group consisting of iron oxide, titanium oxide and zinc oxide.
  12. 　複合化された金属酸化物の平均粒径が、１０～１００ｎｍである請求項１ないし１１のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 12. The metal oxide composite high flat cellulose powder according to claim 1, wherein the composite metal oxide has an average particle size of 10 to 100 nm.
  13. 　複合化された金属酸化物の平均粒径が、１００ｎｍを超え１０００ｎｍ以下である請求項１ないし１１のいずれかに記載の金属酸化物複合化高扁平セルロース粉体。 12. The metal oxide composite high flat cellulose powder according to claim 1, wherein the composite metal oxide has an average particle size of more than 100 nm and 1000 nm or less.
  14. 　請求項１ないし１３のいずれかに記載の金属酸化物複合化高扁平セルロース粉体を含有する化粧料。 Cosmetics containing the metal oxide composite high flattened cellulose powder according to any one of claims 1 to 13.
  15. 　粉体化粧料である請求項１４に記載の化粧料。 15. The cosmetic according to claim 14, which is a powder cosmetic.
  16. 　ファンデーション、アイシャドウ、ほほ紅、粉白粉、日焼け止め料または化粧下地である請求項１４または１５に記載の化粧料。 The cosmetic according to claim 14 or 15, which is a foundation, eye shadow, cheek red, powdered white powder, sunscreen or makeup base.
  17. 　セルロース系物質に、粉砕助剤および金属酸化物を添加して混合物とし、この混合物を機械的に粉砕処理することを特徴とする金属酸化物複合化高扁平セルロース粉体の製造方法。 A method for producing a metal oxide composite high flattened cellulose powder comprising adding a grinding aid and a metal oxide to a cellulosic material to form a mixture, and mechanically grinding the mixture.
  18. 　金属酸化物の添加量が、全体中５～５０質量％である請求項１７記載の金属酸化物複合化高扁平セルロース粉体の製造方法。 The method for producing a metal oxide composite high flat cellulose powder according to claim 17, wherein the addition amount of the metal oxide is 5 to 50% by mass in the whole.
  19. 　粉砕助剤の添加量が、全体中０.５～５質量％である請求項１７または１８記載の金属酸化物複合化高扁平セルロース粉体の製造方法。 The method for producing a metal oxide composite high flattened cellulose powder according to claim 17 or 18, wherein the addition amount of the grinding aid is 0.5 to 5% by mass in the whole.
  20. 　機械的な粉砕処理を、遊星型ボールミルで行う請求項１７ないし１９のいずれかに記載の金属酸化物複合化高扁平セルロース粉体の製造方法。
          The method for producing a metal oxide composite high flat cellulose powder according to any one of claims 17 to 19, wherein the mechanical pulverization is performed by a planetary ball mill.
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CN103442685B (en) 2016-03-09
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JPWO2012133018A1 (en) 2014-07-28
JP6069189B2 (en) 2017-02-01
KR101600058B1 (en) 2016-03-04
TW201302228A (en) 2013-01-16
CN103442685A (en) 2013-12-11
KR20140036158A (en) 2014-03-25

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