WO2014102862A1 - 表面処理粉体及びこれを配合した化粧料 - Google Patents
表面処理粉体及びこれを配合した化粧料 Download PDFInfo
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- WO2014102862A1 WO2014102862A1 PCT/JP2012/008345 JP2012008345W WO2014102862A1 WO 2014102862 A1 WO2014102862 A1 WO 2014102862A1 JP 2012008345 W JP2012008345 W JP 2012008345W WO 2014102862 A1 WO2014102862 A1 WO 2014102862A1
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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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
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
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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
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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- 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
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- 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
- A61Q1/04—Preparations containing skin colorants, e.g. pigments for lips
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- 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
- A61Q1/04—Preparations containing skin colorants, e.g. pigments for lips
- A61Q1/06—Lipsticks
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- 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
- A61Q1/10—Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
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- 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
- A61Q1/12—Face or body powders for grooming, adorning or absorbing
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/002—Aftershave preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/007—Preparations for dry skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q3/00—Manicure or pedicure preparations
- A61Q3/02—Nail coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/12—Preparations containing hair conditioners
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- 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
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
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- 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
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/614—By macromolecular compounds
Definitions
- the present invention relates to a cosmetic powder obtained by surface-treating a cosmetic powder with a silicone gel and a cosmetic containing the same.
- the cosmetic treatment powder of the present invention has good water repellency, is smooth and light and moist, and has excellent adhesion to the skin. In addition to excellent properties, the aging stability of cosmetics is good.
- sunscreen cosmetics such as foundations, eye shadows, and mascara are required to have water repellency to sweat in order to prevent the makeup from collapsing due to sweat.
- sunscreen cosmetics contain fine particles of zinc oxide, titanium dioxide, cerium oxide, and iron oxide as UV protection agents to protect against ultraviolet rays, but they provide water repellency and water resistance as sunscreen cosmetics.
- powders surface-treated with a silicone compound, fatty acid, amino acid or the like are blended in order to improve usability and adhesion to the skin.
- hexagonal boron nitride, lauroyl lysine, plate-like barium sulfate, hekakai talc, synthetic mica by wet pulverization, plate-like PMMA, plate-like cellulose and the like have been developed. Even if these known surface treatments are applied to these powders, compatibility between usability and adhesion to the skin is still not satisfactory.
- Other feel improvers that are added and contained in addition to the powder include partially crosslinked organopolysiloxanes obtained by the addition reaction of dimethicone having Si—H groups, represented by KSG-15 (manufactured by Shin-Etsu Chemical Co., Ltd.) and vinyl dimethicone.
- Patent Documents 4, 5, and 6) are silicone gels or silicone elastomers, and are gel compositions by mixing with low viscosity silicone oil or low molecular oil.
- the surface-treated powder is coated with a silicone elastomer in order to obtain a soft feel powder with the surface of scaly inorganic particles having good adhesion to the skin covered with a resin, or a silicone elastomer with a good sliding feeling.
- a powder is disclosed.
- Patent Documents 7, 8, 9, 10 Silicone elastomer-coated powders not only have sufficient water repellency, but also have strong agglomeration, causing aggregation when coated on powder particles, Many unprocessed parts occur. As a result, it has an unfavorable feeling of use and has a disadvantage of poor adhesion to the skin.
- An object of the present invention is to provide a powder for cosmetics which is smooth and light and has a moist feeling, and has excellent adhesion to the skin, a method for producing the same, and a cosmetic containing the same.
- the present inventors have surface-treated cosmetic powder with a silicone gel, so that the water repellency is good, and a smooth and light feel can be expressed. It is possible to provide a powder having a good feeling of use and excellent adhesion to the skin, and the cosmetics containing this powder have excellent feeling of use, makeup effect and makeup sustainability, and stability of the cosmetics over time. Has been found to be favorable, and has led to the present invention.
- the present invention relates to a cosmetic powder surface-treated with a silicone gel.
- the following can be mentioned as a preferable aspect of the powder for cosmetics surface-treated with the silicone gel according to the present invention.
- R 1 is a hydrolyzable group, a hydroxyl group, an amino group, an acetoxy group, an alkoxy group, a hydrogen atom
- R 2 is an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms
- L is 3 ⁇ 10,000.
- R 3 is a group selected from a monovalent hydrocarbon group having 1 to 20 carbon atoms, an amino group, an aminoethyl group, a mercapto group, an isocyanate, and a phenyl group
- R 4 is a monovalent group having 0 to 3 carbon atoms.
- a lower alkyl group a group selected from phenyl groups, X is a hydroxyl group or an alkoxy group, and n is 0 or 1.
- R 5 is a hydrolyzable group or an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms, and the hydrolyzable group is a hydroxyl group, an amino group, an acetoxy group, an alkoxy group, a hydrogen atom, And n is 3 to 1,000, and has at least three hydrolyzable groups in one molecule.
- the silicone gel has a strain rate of 17% at 25 ° C., a complex elastic modulus of 3,000 to 100,000 Pa measured by dynamic viscoelasticity at a shear frequency of 4 Hz, and a loss coefficient tan ⁇ of 1.0 to 2.5.
- a water emulsion obtained by mechanically emulsifying the dimethiconol having the dimethylsiloxane unit L number of 3 to 1,000 in the formula (1) as a starting material for surface treatment is described in (iv) Powder for cosmetics.
- a water emulsion obtained by emulsion polymerization of the dimethiconol having the dimethylsiloxane unit L number of 3 to 1,000 in the formula (1) is used as a starting material for surface treatment. Powder for cosmetics.
- the powder for cosmetics of the present invention has good water repellency, can express a smooth and light touch, has a moist feeling unique to silicone gel, and has excellent adhesion to the skin.
- the blended cosmetic can provide a cosmetic that is excellent in feeling of use, makeup effect, and makeup sustainability, and has good stability over time.
- Cosmetic powder surface-treated with a silicone gel is a powder surface-treated with a silicone gel, preferably with a dimethiconol water emulsion as a starting material. It is a surface-treated powder obtained by treatment.
- the surface-treated powder of the present invention is a cosmetic powder blended in a cosmetic.
- the powder for cosmetics may be any of generally used inorganic powder, organic powder, inorganic / inorganic composite powder, inorganic / organic composite powder, or organic / organic composite powder. Two or more kinds can be used in combination as appropriate, and powders having a safety to the human body and the skin and substantially usable for cosmetics and those having a particle size in the entire range can be applied. Further, as long as the geometrical form is usually used for cosmetics, it may be any shape such as spherical, hemispherical, star-shaped, polyhedral, spindle-shaped, needle-shaped, plate-shaped, etc. Either porous or porous may be used.
- the average particle diameter is preferably in the range of 0.01 to 500 ⁇ m, more preferably 0.1 to 100 ⁇ m.
- the average particle diameter is measured by selecting appropriately according to the principle of a microscope method, a light scattering method, a laser diffraction method, a liquid phase precipitation method, an electric resistance method, etc. according to each shape of the powder particles.
- Inorganic powders include sericite, natural mica, calcined mica, synthetic mica, synthetic sericite, alumina, mica, talc, kaolin, bentonite, smectite, montmorillonite, hectorite, zeolite, calcium carbonate, magnesium carbonate, silicic anhydride , Magnesium silicate, aluminum silicate, aluminum magnesium silicate, calcium silicate, barium silicate, strontium silicate salt, calcium phosphate, magnesium oxide, barium sulfate, magnesium metasilicate aluminate, iron oxide, chromium oxide, titanium oxide, Zinc oxide, cerium oxide, aluminum oxide, magnesium oxide, chromium hydroxide, bitumen, ultramarine, calcium carbonate, magnesium carbonate, calcium phosphate, aluminum hydroxide, barium sulfate, magnesium sulfate Um, silicon carbide, metal tungstate, magnesium aluminate, magnesium metasilicate aluminate, chlorohydroxyalum
- powders may be used alone or in combination.
- powder Excel Mica JP-2, Excel Pearl: Miyoshi Kasei Co., Ltd.
- aluminum hydroxide is combined on the mica particle surface or pearl particle surface, or hydroxyapatite and zinc oxide are combined and immobilized on the sericite particle surface.
- Powder powder with silica beads composited on the surface of mica particles
- SXI-5 Miyoshi Kasei Co., Ltd.
- titanium oxide and fine titanium oxide composites on the surface of mica and talc particles Powder TMC series and TTC series: Miyoshi Kasei Co., Ltd.
- Organic powders include polyamide, polyacrylic acid / acrylic ester, polyester, polyethylene, polypropylene, polystyrene, styrene / acrylic acid copolymer, divinylbenzene / styrene copolymer, polyurethane, vinyl resin, urea resin, melamine resin , Benzoguanamine, polymethylbenzoguanamine, polyethylene terephthalate, polymethyl methacrylate such as polymethyl methacrylate, cellulose, silk, phenol resin, epoxy resin, polycarbonate, silicone resin powder, silicone rubber powder, Teflon (registered trademark) powder, etc.
- Powder such as powder, zinc stearate, aluminum stearate, calcium stearate, magnesium stearate, zinc myristate, magnesium myristate,
- metal soaps such as zinc tilphosphate, calcium cetyl phosphate, and sodium zinc cetyl phosphate, lauroyl lysine, alkyl phosphate, chitin, chitosan, polysaccharide powder, protein powder, carbon black, and organic dyes.
- the powder to be surface-treated in the present invention has, for example, aluminum, calcium, magnesium, cerium, silicon, zirconium, titanium, zinc, iron, cobalt, in order to improve the affinity with the surface treatment agent and the fixing property. It may be coated with at least one oxide or hydrated oxide of manganese, nickel and tin.
- the silicone gel as referred to in the present invention is obtained from a curable liquid silicone composition, and the curing is based on an addition reaction and on the condensation reaction.
- the addition reaction include an organopolysiloxane having at least two monovalent olefinically unsaturated groups in one molecule and an organohydrogenpolysiloxane having at least three hydrogen atoms bonded to silicon atoms in one molecule.
- a silicone gel obtained by addition reaction with a platinum-based catalyst may be mentioned.
- a liquid silicone comprising an organopolysiloxane having at least two hydroxyl groups bonded to silicon atoms in one molecule and an organohydrogenpolysiloxane having at least three hydrogen atoms bonded to silicon atoms in one molecule
- examples thereof include a silicone gel obtained by condensation polymerization of the composition in the presence of a condensation catalyst.
- a preferred method of obtaining the silicone gel of the present invention is by a condensation reaction.
- a silane coupling agent having two or more hydrolyzable groups in one molecule of the following formula (2) as a cross-linking agent and a both-end reactive diorganopolysiloxane represented by the following formula (1) is a polymer having a fine three-dimensional crosslinked structure of diorganopolysiloxane obtained by hydrolysis and condensation reaction with an organopolysiloxane containing at least one of the reactive organopolysiloxanes of the following formula (3).
- R 1 is a hydrolyzable group, a hydroxyl group, an amino group, an acetoxy group, an alkoxy group, a hydrogen atom
- R 2 is an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms
- L is 3 ⁇ 10,000.
- R 3 is a group selected from a monovalent hydrocarbon group having 1 to 20 carbon atoms, an amino group, an aminoethyl group, a mercapto group, an isocyanate, and a phenyl group
- R 4 is a monovalent group having 0 to 3 carbon atoms.
- a lower alkyl group a group selected from phenyl groups, X is a hydroxyl group or an alkoxy group, and n is 0 or 1.
- R 5 is a hydrolyzable group or an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms. Examples of the hydrolyzable group include a hydroxyl group, an amino group, an acetoxy group, an alkoxy group, hydrogen Any of the atoms, n is 3 to 1,000, and has at least three hydrolyzable groups in one molecule.
- R 2 in the formula for example, methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group, heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tetradecyl group Group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, nonadecyl group, eicosyl group, henicosyl group, docosyl group, tricosyl group, tetrasil group, triacotyl group and other alkyl groups; cyclobutyl group, cyclopentyl group, cyclohexyl group, cycloheptyl A cycloalkyl group such as a group; an aryl group such as a phenyl group, a tolyl group
- silicone gels that are surface-treated on cosmetic powders are not elastic solids but can take the form of particles.
- the powder particle surface may be surface-treated in any shape.
- the surface treatment referred to in the present invention refers to a state in which silicone gel is attached or coated on the surface of the powder particles.
- the density and shape attached to the surface of the powder particles are not particularly limited in the case where the effect achieved by the present invention is exhibited.
- the particulate silicone gel adheres sparsely to the powder particle surface
- the particulate silicone gel adheres to the powder particle surface without gaps
- the silicone gel having no particle shape adheres sparsely to the powder particle surface
- the silicone gel may be in the form of a film and the powder particle surface may be coated and adhered without any gap, or a combination of these may be used.
- One type of suitable silicone microcrosslinking reaction system for obtaining a silicone gel according to the present invention is, for example, between a silanol ( ⁇ Si—OH) group and a silicon hydride ( ⁇ Si—H) group.
- this microcrosslinking reaction system is a reaction between a siloxane polymer having a silanol group and a crosslinkable compound having a hydrolyzable group directly bonded to a silicon atom.
- Another example of this reaction system is a reaction between a siloxane polymer having a hydrolyzable or condensable group directly bonded to a silicon atom and a crosslinkable compound having a silanol group.
- Yet another example of this curing system is the reaction between two siloxane polymers having hydrolyzable or condensable groups directly attached to silicon atoms.
- siloxane polymers having hydrolyzable or condensable groups directly bonded to silicon atoms and siloxanes having active hydrogen atoms, ie hydroxyl groups, ureido groups, mercapto groups or amino groups. Reaction between polymers.
- micro-crosslinking reaction system in the present invention are hydroxysilyl group ( ⁇ SiOH) and ethoxysilyl group ( ⁇ SiOCH 2 CH 3 ), hydroxysilyl group ( ⁇ SiOH) and methoxysilyl group ( ⁇ SiOCH 3 ), hydroxy
- This is a condensation reaction between a silyl group ( ⁇ SiOH) and a hydrosilyl group ( ⁇ SiH).
- Examples of the both-end reactive diorganopolysiloxane of the above formula (1) include both-end hydroxysilyl group modification, methoxy modification, ethoxy modification, amino modification, and both-end hydroxysilyl group-modified silicone.
- Generally available are X-21-5849, X-21-5841, KF-9701A (Shin-Etsu Chemical Co., Ltd.), FINISH WS 62M, CT601M, CT5000M, CT6000M (Asahi Kasei Wacker Silicone) or more.
- Examples include silyl group-modified silicone, KF8010, X-22-161A, KF8008 (Shin-Etsu Chemical Co., Ltd.) and more, both-end amino-modified silicone.
- the both-end-reactive diorganopolysiloxane of the present invention is preferably a both-end hydroxysilyl group-modified silicone (dimethiconol) that generates water as a by-product after hydrolysis / condensation reaction.
- silane coupling agent of the above formula (2) examples include dimethyldimethoxysilane, methyltrimethoxysilane, dimethyldiethoxysilane, methyltriethoxysilane, diphenyldiethoxysilane, phenyltriethoxysilane, and 3-glycidoxypropyl.
- Examples of the reactive organopolysiloxane having at least three hydrolyzable groups in one molecule of the above formula (3) include ⁇ -trihydroxydimethylpolysiloxane, ⁇ -trialkoxypolydimethylsiloxane, ⁇ , ⁇ -di Examples include alkoxypolydimethylsiloxane, ⁇ , ⁇ -hexaalkoxypolydimethylsiloxane, dimethylhydrogenpolysiloxane, triethoxysilylethylpolydimethylsiloxyethyl dimethicone, triethoxysilylethylpolydimethylsiloxyethylhexyl dimethicone, and the like. It is not limited, and two or more kinds can be mixed and used according to the purpose.
- the most preferred micro-crosslinking reaction system is a reaction in which the both-end reactive diorganopolysiloxane of the formula (1) is in the form of a water suspension or water emulsion with the crosslinking agent as a starting material. It is a silicone gel.
- the method for preparing a water emulsion of the both-end reactive diorganopolysiloxane of the formula (1) include a method of emulsion polymerization using a low-molecular cyclic siloxane as a starting material, and an oily both-end reactive diorganopolysiloxane and an interface.
- a method of mechanically emulsifying a system containing at least an activator and water with an emulsification mixer is exemplified.
- Any type of mixing device may be used to carry out the emulsification process. That is, batch mixers, planetary mixers, continuous mixers such as single or multi-screw extruders, dynamic or static mixers, colloid mills, homogenizers and sonolators, or combinations thereof are used. .
- an emulsion can be produced by a known method, for example, when an aqueous emulsion of a bi-terminal reactive diorganopolysiloxane is obtained by mechanical emulsification, the viscosity of the diorganosiloxane is limited.
- the number of diorganosiloxane units is preferably in the range of 3 to 1,000.
- it can obtain by mixing and emulsifying both terminal reactive diorganopolysiloxane, surfactant, and water.
- the molecular weight of the obtained organopolysiloxane can be known by measuring the PS converted Mw by GPC of the component after evaporation of the water of the emulsion and volatilization.
- low molecular cyclic siloxane a small amount of a crosslinking agent, a surfactant and water are added for emulsification, then an acid is added to cause a polymerization reaction, and then an alkali is added for neutralization. It is also possible to obtain a water emulsion of a partially slightly crosslinked organopolysiloxane silicone containing hydroxyl groups bonded to silicon atoms at both ends.
- the surfactant used for emulsifying the water emulsion of the both-end reactive diorganopolysiloxane is not particularly limited.
- Anionic surfactant alkyltrimethylammonium salt, dialkyldimethylammonium salt, polyoxyethylenealkyldimethylammonium salt, dipolyoxyethylenealkylmethylammonium Cationic surfactants such as nium salts, tripolyoxyethylene alkylammonium salts, alkylbenzyldimethylammonium salts, alkylpyridium salts, monoalkylamine salts, dialkylamine salts, trialkylamine salts, monoalkylamidoamine salts, and cationized cellulose
- An amphoteric surfactant such as alkyldimethylamine oxide, alkyldimethylcarboxybetaine, alkylamidopropyldimethylcarboxybetaine, alkylhydroxysulfobetaine, alkylcarboxymethylhydroxyethylimidazolinium betaine; These surfactants can be used individually by 1 type or in combination of 2 or more types as appropriate.
- Preferred surfactants are those that have low irritation to the skin and that are not regulated substances such as the PRTR method (Pollutant Release and Transfer Register).
- PRTR method Policy Release and Transfer Register
- silicone lauroyl glutamic acid, myristoyl glutamic acid, lauroyl aspartic acid, myristoyl aspartic acid, lauroyl alanine, lauroyl methyl taurine, Na and K salts such as myristoyl methyl taurine, etc. are exemplified, and one or more kinds can be blended. .
- the surfactant contained in the water emulsion is used to impart water repellency to the surface-treated powder and in the powder. It is preferable that the amount is as small as possible in terms of residual due to adsorption to the surface, etc.
- the blending weight ratio (B) / (A) ⁇ 100 of the reactive polyorganosiloxane (A) at both ends and the amount of surfactant (B) is 6 Preferably it is less than 0.0. If it is 6.0 or more, the water repellency of the surface-treated powder may be lowered or a light touch may not be obtained.
- the compounding ratio of the both-end reactive diorganopolysiloxane and the crosslinking agent and the number of reactive groups are determined by whether or not a silicone gel can be obtained by a microcrosslinking reaction. Generally, when the sum of the number of reactive groups in the reactive diorganopolysiloxane and the number of reactive groups in the crosslinking agent is at least 5, a silicone elastomer-like structure is formed by the crosslinking reaction. If the molecular weights of the both-end reactive diorganopolysiloxane and the crosslinking agent are both small, the resulting silicone polymer becomes a solid elastic body.
- the ratio of siloxane to crosslinking agent can be obtained in a blending range of about 100 / 0.1 to 100/35 (wt%).
- the amount of the crosslinking agent is less than 0.1 wt%, the silicone oil or gum has a viscosity, and when it exceeds 35 wt%, the silicone elastomer has elasticity and the water repellency of the surface-treated powder decreases.
- Preferred suitable catalysts include acidic or alkaline materials.
- the acidic substance is not particularly limited.
- organic acids such as lactic acid, citric acid, malic acid, succinic acid, hydrochloric acid, sulfuric acid, phosphoric acid, aluminum chloride, zinc chloride, magnesium chloride, polyaluminum chloride, aluminum sulfate, zinc sulfate Etc. can be used.
- the alkaline substance is not particularly limited, and examples thereof include alkali metal hydroxides such as potassium hydroxide, sodium hydroxide and lithium hydroxide; alkaline earth metal hydroxides such as calcium hydroxide, magnesium hydroxide and barium hydroxide; Alkali metal carbonates such as potassium carbonate and sodium carbonate; ammonia, triethanolamine and the like can be used.
- the silicone gel should just be a compound which has silicone which does not have rubber elasticity as a main component.
- dimethylpolysiloxane if the number of units of linear siloxane is small, that is, if the molecular weight is small, it is volatile. As the molecular weight increases, it becomes liquid, viscous liquid, or gum.
- a molecular cross-linking agent to a dimethylpolysiloxane chain having a linear molecular structure, the properties change to a gel, elastic body, or resinous material due to an increase in the amount added.
- the amount of the silicone gel that is a coating agent used for the surface treatment in the present invention varies depending on the type of powder used and the coating method, and is not particularly limited, but the ratio of the powder to the silicone gel that is the surface treatment agent is the mass.
- the ratio of powder: silicone gel is preferably 99.99: 0.01 to 70:30 and particularly preferably 99: 1 to 90:10. If it is this range, the powder for cosmetics which is moist by the smooth and light touch of this invention, and was excellent in the adhesiveness to skin is obtained.
- the silicone gel referred to in the present invention is a polymer having a fine three-dimensional crosslinked structure of diorganopolysiloxane which does not have rubber elasticity, that is, rubber hardness.
- a durometer measurement method defined in ISO7619-1 as a method for measuring rubber hardness.
- This measurement method includes a durometer type AO measurement method capable of measuring the soft rubber hardness, but the preferable measurement value of the silicone gel of the present invention is less than 10, more preferably less than 5, and still more preferably 0.
- the rheological properties of the silicone gel are as follows: the dynamic viscoelasticity is measured at a strain rate of 17% at 25 ° C., the complex elastic modulus at a shear frequency of 4 Hz is 3,000 to 100,000 Pa, and the loss coefficient tan ⁇ is 1.0 to A silicone gel that is 2.5 is applied. More preferably, the complex elastic modulus is 10,000 to 100,000 Pa, and the loss coefficient (loss elastic modulus G ′′ / storage elastic modulus G ′) tan ⁇ is 1.0 to 2.0.
- the viscosity is less than 1,000 Pa
- the properties of the silicone oil are exhibited and the feeling of use of the present invention is not obtained
- the complex elastic modulus is greater than 100,000
- the properties of the elastic body are exhibited and the water repellency and the adhesion to the skin tend to be reduced.
- the loss coefficient tan ⁇ is less than 1.0
- the shear frequency of 4 Hz is a range of a general physical operation speed for humans, and approximates the speed when applying cosmetics to the skin. It depends on the reason.
- the rheological properties of the silicone gel of the invention can be measured as follows.
- Dynamic viscoelasticity measuring device Rheosol-G3000 (manufactured by UBM) Measurement jig: Parallel plate with a diameter of 20 mm Measurement frequency: 4 Hz Measurement temperature: 25 ⁇ 1.0 ° C Measurement strain setting: The strain rate is set to 17%, and the measurement is performed in the automatic measurement mode. Measurement sample thickness (gap): 1.0 mm
- the sample preparation method for rubber hardness measurement and dynamic viscoelasticity measurement of silicone gel is to emulsify both end-reactive diorganopolysiloxane with ion-exchanged water with a surfactant, and then add a crosslinking agent to make the pH basic. Thereafter, it can be obtained as a residue obtained by volatilizing water by heating.
- the method for producing a cosmetic powder surface-treated with a silicone gel in the present invention may be performed by simply mixing the cosmetic powder and the silicone gel with a mixer or the like. Is possible.
- silicone gel is preferably mixed with an organic solvent having a low surface tension from the viewpoint of water repellency, feeling of use, and adhesion to the skin.
- a preferred method for producing a silicone gel-treated powder is to deposit the silicone gel on the powder particle surface in the presence of cosmetic powder by an in-situ method, and then heat the silicone gel to adhere to the particle surface.
- a silicone gel is fixed by the in-situ method using a water emulsion of a both-end reactive organopolysiloxane as a starting material.
- This method increases the adhesion of the silicone gel to the surface of the powder particles and the uniformity of the coating, makes it possible to give a better light feeling with good water repellency and better silicone gel cosmetics with better adhesion to the skin Powder can be obtained.
- the cosmetic powder surface-treated with the silicone gel is prepared by mixing the water-soluble solvent and the cosmetic powder in either the capillary or slurry state, and in the presence of the cosmetic powder. After hydrolyzing and condensing at least partly in the step of adding the both-end reactive diorganopolysiloxane of (1) and the compound of (2) or (3) separately or simultaneously
- the surface treatment powder is obtained by heating the product temperature at 100 to 180 ° C. for 3 hours or more.
- the water-soluble component is preferably 3 to 1500 parts by weight and more preferably 10 to 800 parts by weight with respect to 100 parts by weight of the cosmetic powder. .
- the amount is less than 3 parts by mass, the capillary region is not reached, and the powder is agglomerated, and the powder particles are agglomerated, resulting in poor usability.
- the amount exceeds 1500 parts by mass, the productivity of the surface-treated powder is deteriorated and the production cost is increased, which is not preferable.
- the mixed state of powder and liquid as referred to in the present invention refers to a solid, liquid and gas filling form: (a) a dry state where the solid phase and the gas phase are continuous and there is almost no liquid phase; (b) Pendular state where the solid phase and the gas phase are continuous and the liquid phase is discontinuous, (c) The solid phase, the funicular state where the gas phase and the liquid phase are continuous, (d) The solid phase is discontinuous Capillary state where liquid is continuous but not flowing, (e) Slurry state where solid phase is discontinuous and liquid is continuously flowing, mixing in (d) and (e) states Alternatively, it is preferable to carry out the hydrolysis / condensation reaction while kneading and stirring.
- the water-soluble solvent any of water, ethanol, isopropyl alcohol (IPA), and a mixed solvent thereof is used.
- the water-soluble solvent is preferably water, but ethanol or IPA can be used as a washing solvent when removing a compound, a surfactant or the like by-produced in the reaction process.
- a powder for cosmetics, a water-soluble solvent and a bi-terminal reactive diorganopolysiloxane are well kneaded with a kneader, and then a crosslinking agent is gradually added while kneading.
- An acidic substance or an alkaline substance is added as a reaction catalyst and further kneaded for a certain time.
- the kneaded product is taken out and heated at a temperature of 100 to 180 ° C. with a hot air dryer at a set temperature for 3 hours or longer, then cooled and pulverized to obtain a silicone gel surface-treated powder.
- the dimethiconol at this time may be in the form of an oil or a water emulsion, but the use of a water emulsion is preferred from the viewpoint of water repellency.
- a manufacturing method in a slurry state for example, cosmetic powder is put into a water-soluble solvent and dispersed with a stirrer. After stirring, a water emulsion of reactive diorganopolysiloxane at both ends is gradually added, and then homogenized. Then, a cross-linking agent is added gradually to maintain stirring, and an acidic substance or alkaline substance is added as a reaction catalyst as necessary. And stir for a certain time. As the condensation reaction proceeds, the slurry liquid thickens, so stirring is performed for a certain period of time.
- the cake which has been drained by filtration or centrifuge and washed as necessary, and then drained, is heated at a temperature of 100 to 180 ° C in a hot air dryer at a set temperature for 3 hours or more, then cooled and ground.
- a silicone gel surface-treated powder is heated by heating under normal pressure or reduced pressure.
- the dispersion is allowed to stand under heating to remove moisture, and the dispersion is heated. Examples thereof include a method of removing moisture while stirring and flowing, a method of spraying and dispersing a dispersion in a hot air stream like a flash dryer and a spray dryer, a method of using a fluidized heat medium, and the like.
- the addition order of the both-end reactive diorganopolysiloxane, the crosslinking agent, and the reaction catalyst may be processed in a step that maximizes the effect of the present invention depending on the type of powder, It may be added in portions or simultaneously.
- the kneading and stirring in the above production method is preferably strong kneading and stirring because it enables uniform surface treatment to the powder particles, and examples thereof include a kneader, a biaxial kneader, a disper mixer, and a homomixer.
- the temperature during the surface treatment is preferably 5 to 60 ° C., more preferably 15 to 30 ° C. If the temperature is lower than 5 ° C, the hydrolysis / condensation reaction is difficult to proceed, and the intended effect cannot be obtained. If the temperature is higher than 60 ° C, the obtained particles cause strong aggregation and deteriorate the feeling of use.
- the powder after drying may be crushed or classified by a pulverizer such as a pin mill, a hammer mill, a jet mill, or a ball mill depending on the aggregation state of the powder particles.
- a pulverizer such as a pin mill, a hammer mill, a jet mill, or a ball mill depending on the aggregation state of the powder particles.
- the silicone gel cosmetic powder of the present invention can be used in various cosmetics, such as skin care products, makeup products, hair products, It is suitably used for cosmetics such as antiperspirant products and UV protection products, especially for skin and hair.
- the blending ratio of the composite particles is not particularly limited, and is appropriately selected in the range of 0.1 to 100.0% by mass with respect to the entire cosmetic according to each preparation.
- the cosmetic can contain various components used in ordinary cosmetics within a range not impairing the effects of the present invention.
- Ingredients include, for example, oils, powders, surfactants, water-soluble or water-swellable polymer compounds, UV absorbers, moisturizers, oil-soluble gelling agents, antibacterial preservatives, salts, antioxidants, and skin beautifying ingredients. (Whitening agents, cell activators, rough skin improvers, blood circulation promoters, skin astringents, antiseborrheic agents, etc.), vitamins, amino acids, antiperspirants, alcohol, film formers, anti-inflammatory agents, cooling agents, Nucleic acids, hormones, inclusion compounds, pH adjusters, chelating agents, and other additives may be included. These can be used individually by 1 type or in combination of 2 or more types.
- the oil agent that can be blended in the cosmetic of the present invention may be solid, semi-solid, or liquid.
- natural animal and vegetable oils and fats and semi-synthetic oils, hydrocarbon oils, higher alcohols, ester oils, silicone oils. , And fluorine-based oils can be used.
- natural animal and plant oils and semi-synthetic fats and oils include avocado oil, linseed oil, almond oil, ibotarou, eno oil, olive oil, cocoa butter, kapok wax, kaya oil, carnauba wax, liver oil, candelilla wax, and refined canned oil.
- Delilah wax beef tallow, beef tallow, beef bone fat, hydrogenated beef tallow, kyounin oil, whale wax, hydrogenated oil, wheat germ oil, sesame oil, rice germ oil, rice bran oil, sugar cane wax, sasanqua oil, safflower oil, shea butter oil , Cinnamon oil, cinnamon oil, jojoballow, squalane, squalene, shellac wax, turtle oil, soybean oil, tea seed oil, camellia oil, evening primrose oil, corn oil, lard oil, rapeseed oil, Japanese kiri oil, nukarou, germ oil, Horse fat, persic oil, palm oil, palm kernel oil, castor oil, hydrogenated castor oil, castor oil fatty acid methyl ester, sunflower Oil, Grape oil, Bayberry wax, Jojoba oil, Macadamia nut oil, Beeswax, Mink oil, Meadow foam oil, Cottonseed oil, Cotton wax, Owl, Owl kernel oil, Montan wax, Palm
- hydrocarbon oil examples include linear, branched, and volatile hydrocarbon oils. Specifically, ozokerite, ⁇ -olefin oligomer, light isoparaffin, isododecane, isohexadecane, light liquid isoparaffin, squalane.
- Examples include cholesterol, phytosterol, polyoxyethylene cholesterol ether, monostearyl glycerin ether (batyl alcohol), monooleyl glyceryl ether (ceracyl alcohol), and the like.
- Ester oils include diisobutyl adipate, 2-hexyldecyl adipate, di-2-heptylundecyl adipate, N-alkyl glycol monoisostearate, isocetyl isostearate, trimethylolpropane triisostearate, di-2-ethyl Ethylene glycol hexanoate, cetyl 2-ethylhexanoate, trimethylolpropane tri-2-ethylhexanoate, pentaerythritol tetra-2-ethylhexanoate, cetyl octanoate, octyldodecyl gum ester, oleyl oleate, octyldodecyl oleate Decyl oleate, neopentyl glycol dioctanoate, neopentyl glycol dicaprate, trieth
- Silicone oils include dimethylpolysiloxane, tristrimethylsiloxymethylsilane, caprylylmethicone, phenyltrimethicone, tetrakistrimethylsiloxysilane, methylphenylpolysiloxane, methylhexylpolysiloxane, methylhydrogenpolysiloxane, dimethylsiloxane / methylphenylsiloxane Low to high viscosity linear or branched organopolysiloxanes such as copolymers, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, tetramethyltetrahydrogencyclotetrasiloxane, tetramethyl Cyclic organopolysiloxanes such as tetraphenylcyclotetrasiloxane, amino-modified organopoly
- Fluorine-based oils include perfluoropolyether, perfluorodecalin, perfluorooctane and the like.
- the blending amount of the oil is appropriately selected from the range of 1 to 90% by mass of the entire cosmetic depending on the dosage form.
- Examples of the powder include inorganic particles, organic particles, inorganic / organic composite powders, and silicone resin particles.
- the inorganic particles, resin particles, and inorganic / organic composite powder are the same as the inorganic particles, resin particles, and inorganic / organic composite powder used in the present invention.
- the silicone resin particles include silicone elastomer particles, polymethylsilsesquioxane particles, and particles formed by coating the surface of the silicone elastomer particles with polymethylsilsesquioxane. These powders can be used in which the particle surface is further treated with a silylating agent, silicone oil, silicone resin, waxes, paraffins, organic fluorine compounds, acylated amino acids, lecithin, ester oil and the like.
- surfactant examples include nonionic, anionic, cationic and amphoteric active agents, and the same surfactants as those used in the production of the composite particles of the present invention described above are exemplified.
- these surfactants linear or branched polyoxyethylene-modified organopolysiloxane, linear or branched polyoxyethylene polyoxypropylene-modified organopolysiloxane, linear or branched polyoxyethylene / alkyl co-modified organo Polysiloxane, linear or branched polyoxyethylene polyoxypropylene / alkyl co-modified organopolysiloxane, linear or branched polyglycerin-modified organopolysiloxane, linear or branched polyglycerin / alkyl co-modified organopolysiloxane It is preferable.
- the content of hydrophilic polyoxyethylene group, polyoxyethylene polyoxypropylene group or polyglycerin residue preferably accounts for 10 to 70% by mass in the molecule.
- the blending amount is preferably from 0.1 to 20% by weight, more preferably from 0.2 to 10% by weight, based on the total cosmetic.
- the HLB of the surfactant is not limited, but is preferably 2 to 14.5.
- water-soluble or water-swellable polymer compound examples include gum arabic, tragacanth, galactan, carob gum, guar gum, caraya gum, carrageenan, pectin, agar, quince seed (malmello), starch (rice, corn, potato, wheat, etc.), algae Plant-based polymer compounds such as colloids, tant gum, locust bean gum; microbial polymer compounds such as xanthan gum, dextran, succinoglucan, pullulan; animal-based polymer compounds such as collagen, casein, albumin, gelatin; carboxymethyl starch , Starch-based polymer compounds such as methylhydroxypropyl starch; methylcellulose, ethylcellulose, methylhydroxypropylcellulose, carboxymethylcellulose, hydroxymethylcellulose, Cellulose polymer compounds such as droxypropyl cellulose, nitrocellulose, sodium cellulose sulfate, sodium carboxymethyl cellulose, crystalline cellulose, cellulose powder; alginic acid polymer
- High molecular compounds polyethyleneimine, other synthetic water-soluble high molecular compounds such as cationic polymers, bentonite, aluminum silicate Magnesium, montmorillonite, beidellite, nontronite, saponite, hectorite, and inorganic-based water-soluble polymer compound such as silicic anhydride.
- These water-soluble polymer compounds also include film forming agents such as polyvinyl alcohol and polyvinyl pyrrolidone.
- the blending amount is preferably in the range of 0.1 to 25% by mass of the entire cosmetic.
- UV absorbers examples include benzoic acid UV absorbers such as paraaminobenzoic acid; anthranilic acid UV absorbers such as methyl anthranilate; salicylic acid UV absorbers such as methyl salicylate, octyl salicylate and trimethylcyclohexyl salicylate; Cinnamic acid UV absorbers such as octyl cinnamate; Benzophenone UV absorbers such as 2,4-dihydroxybenzophenone; Urocanic acid UV absorbers such as ethyl urocanate; 4-t-butyl-4'-methoxy- Dibenzoylmethane-based ultraviolet absorbers such as dibenzoylmethane; phenylbenzimidazolesulfonic acid, triazine derivatives, etc.
- benzoic acid UV absorbers such as paraaminobenzoic acid
- anthranilic acid UV absorbers such as methyl anthranilate
- salicylic acid UV absorbers such as
- ultraviolet absorbing and scattering agents include fine particle titanium oxide, fine particle iron-containing titanium oxide, fine particle zinc oxide, fine particle cerium oxide, Fine particles Of iron and complexes thereof and the like, particles that absorb scattering ultraviolet light and the like, it can also be used dispersions of particles that absorb scattering these ultraviolet dispersed in advance oil.
- Moisturizers include glycerin, sorbitol, propylene glycol, dipropylene glycol, 1,3-butylene glycol, pentylene glycol, glucose, xylitol, maltitol, polyethylene glycol, hyaluronic acid, chondroitin sulfate, pyrrolidone carboxylate, polyoxy Examples include ethylene methyl glucoside, polyoxypropylene methyl glucoside, egg yolk lecithin, soybean lecithin, phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidylinositol, sphingophospholipid and the like.
- oil-soluble gelling agents include metal soaps such as aluminum stearate, magnesium stearate, zinc myristate; amino acids such as N-lauroyl-L-glutamic acid dibutylamide and N-2-ethylhexanoyl-L-glutamic acid dibutylamide Derivatives; dextrin fatty acid esters such as dextrin palmitic acid ester, dextrin stearic acid ester, dextrin 2-ethylhexanoic acid palmitic acid ester; sucrose fatty acid esters such as sucrose palmitic acid ester and sucrose stearic acid ester; fructooligosaccharide stearic acid ester Fructooligosaccharide fatty acid esters such as fructooligosaccharide 2-ethylhexanoate; and sorbitol such as monobenzylidene sorbitol and dibenzylidene sorbitol Jiriden derivatives
- paraoxybenzoic acid alkyl ester benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, phenoxyethanol, etc.
- benzoic acid salicylic acid, carboxylic acid, sorbic acid, paraoxybenzoic acid alkyl ester, Parachlorometacresol, hexachlorophene, benzalkonium chloride, chlorhexidine chloride, trichlorocarbanilide, photosensitizer, phenoxyethanol and the like
- benzoic acid salicylic acid, carboxylic acid, sorbic acid, paraoxybenzoic acid alkyl ester, Parachlorometacresol, hexachlorophene, benzalkonium chloride, chlorhexidine chloride, trichlorocarbanilide, photosensitizer, phenoxyethanol and the like
- Salts include inorganic salts, organic acid salts, amine salts and amino acid salts.
- inorganic salts include sodium salts, potassium salts, magnesium salts, calcium salts, aluminum salts, zirconium salts, zinc salts, and the like of inorganic acids such as hydrochloric acid, sulfuric acid, carbonic acid, and nitric acid; Salts of organic acids such as dehydroacetic acid, citric acid, malic acid, succinic acid, ascorbic acid and stearic acid; amine salts and amino acid salts include, for example, salts of amines such as triethanolamine, and amino acids such as glutamic acid And the like.
- a salt such as hyaluronic acid or chondroitin sulfate, an aluminum zirconium glycine complex, or the like, or an acid-alkali neutralized salt used in a cosmetic formulation can also be used.
- antioxidant examples include tocopherol, pt-butylphenol, butylhydroxyanisole, dibutylhydroxytoluene, phytic acid, and the like.
- pH adjuster examples include lactic acid, citric acid, glycolic acid, succinic acid, tartaric acid, dl- Malic acid, potassium carbonate, sodium hydrogen carbonate, ammonium hydrogen carbonate and the like can be mentioned.
- the chelating agent examples include alanine, sodium edetate, sodium polyphosphate, sodium metaphosphate, phosphoric acid and the like.
- Anti-inflammatory agents such as menthol and camphor include allantoin, glycyrrhizic acid and its salts, glycyrrhetinic acid and stearyl glycyrrhetinate, tranexamic acid, azulene and the like.
- whitening agents such as placenta extract, arbutin, glutathione, and yukinoshita extract
- cell activating agents such as royal jelly, photosensitizer, cholesterol derivative, and calf blood extract
- rough skin ameliorating agent Nicotinic acid benzyl ester, nicotinic acid ⁇ -butoxyethyl ester, capsaicin, zingerone, cantalis tincture, ictamol, caffeine, tannic acid, ⁇ -borneol, tocopherol nicotinate, inositol hexanicotinate, cyclandrate, cinnarizine, trazoline
- blood circulation promoters such as acetylcholine, verapamil, cephalanthin, and ⁇ -oryzanol
- skin astringents such as zinc oxide and tannic acid
- antiseborrheic agents such as sulfur and thianthol.
- Vitamins such as vitamin A oil, retinol, retinol acetate, retinol palmitate, etc .; vitamin B2 such as riboflavin, riboflavin butyrate, flavin adenine nucleotide, pyridoxine hydrochloride, pyridoxine dioctanoate, pyridoxine tripalmi Vitamin B6 such as tate, vitamin B12 and its derivatives, vitamin B15 such as vitamin B15 and its derivatives; L-ascorbic acid, L-ascorbic acid dipalmitate, L-ascorbic acid-2-sodium sulfate, L- Vitamin Cs such as ascorbic acid phosphate diester dipotassium; Vitamin Ds such as ergocalciferol and cholecalciferol; ⁇ -tocopherol, ⁇ -tocopherol, ⁇ -tocopherol, dl- ⁇ -tocopherol acetate, ni Vitamin E such as
- Amino acids include glycine, valine, leucine, isoleucine, serine, threonine, phenylalanine, arginine, lysine, aspartic acid, glutamic acid, cystine, cysteine, methionine, tryptophan, etc.
- Nucleic acids include deoxyribonucleic acid, etc. as hormones Include estradiol, etenyl estradiol, and the like.
- antiperspirant examples include aluminum chlorohydrate, aluminum chloride, aluminum sesquichlorohydrate, zirconyl hydroxychloride, aluminum zirconium hydroxychloride, aluminum zirconium glycine complex and the like.
- the cosmetic of the present invention may be in the form of powder, oily, water-in-oil emulsion, oil-in-water emulsion, non-water emulsion, multi-emulsion such as W / O / W and O / W / O, Further, it may be liquid, emulsion, cream, solid, paste, gel, powder, press, multilayer, mousse, spray, stick, pencil, and the like.
- cosmetics include skin lotions, milky lotions, creams, cleansings, packs, oil liquids, massages, essences, beauty oils, cleaning agents, deodorants, hand creams, lip balms, wrinkle masks and other skin care cosmetics.
- Makeup makeup base, concealer, white powder, powder foundation, liquid foundation, cream foundation, oil foundation, blusher, eyeshadow, mascara, eyeliner, eyebrow, lipstick, makeup cosmetics, shampoo, rinse, treatment, set agent UV protection cosmetics such as hair cosmetics such as antiperspirants, sunscreen oils, sunscreen emulsions, and sunscreen creams.
- Various forms can be selected.
- Dimethiconol oil ( ⁇ , ⁇ -dihydroxypolydimethylsiloxane) having a viscosity of 30 mPa ⁇ s was prepared as a reactive diorganopolysiloxane at both ends.
- a water emulsion of dimethiconol was prepared by the following method.
- Dimethiconol (500 g) having a viscosity of 30 mPa ⁇ s was charged into a 2 liter polyethylene beaker, and 22.5 g of sodium lauroylmethyltaurine and 50 g of ion-exchanged water were gradually added dropwise with stirring at 5,000 rpm with a homomixer. I let you. After thickening, the stirring speed was increased to 7,000 rpm and stirring was continued for 15 minutes, and 450 g of ion-exchanged water was added for dilution.
- Dimethiconol (500 g) having a viscosity of 30 mPa ⁇ s was charged into a 2 liter polyethylene beaker, and 22.5 g of sodium lauroylmethyltaurine and 50 g of ion-exchanged water were gradually added dropwise with stirring at 5,000 rpm with a homomixer. I let you. After thickening, the stirring speed was increased to 7,000 rpm and stirring was continued for 15 minutes, and 450 g of ion-exchanged water was added for dilution.
- a water emulsion of high molecular weight dimethiconol was obtained by emulsifying and dispersing once at 50 MPa with a desktop pressure homogenizer (manufactured by APV Gorin). Subsequently, 10% sodium carbonate was added to adjust to pH 7 to obtain a water emulsion. This water emulsion was dried at 105 ° C. for 3 hours, and the molecular weight in terms of PS converted by GPC was determined for the solid content from which water was volatilized and removed. The solid content was 46.5%.
- the pH was adjusted to 10.5 with a 1N-NaOH aqueous solution and stirred for 15 minutes, then transferred to an aluminum dish, and water was volatilized at 105 ° C./24 h to obtain a silicone reactant.
- the both-end reactive diorganopolysiloxane is a water emulsion
- the water amount is set to 100 g in ion-exchanged water and the same operation as described above is performed.
- the weight blending ratio (A) / (B) between the both-end reactive diorganopolysiloxane (A) and the crosslinking agent (B) was set to 100/10, 7/1, or 3/1.
- test surface is prepared by flattening the surface so that the silicone reaction product comes out slightly from the surface in a styrene square case (vertical 36 ⁇ width 36 ⁇ height 14 mm).
- the durometer pressure plate is placed at a position 20 mm above the test surface, and the pressure plate is pressed against the test piece while the test surface surface and the pressure plate are maintained in parallel, and the scale of the needle is read. This operation was repeated 5 times and the average value was taken as the measured value. In addition, it was set as NA (Not Applicable) when the needle did not move by measurement.
- the soft paste was taken out and dried at 120 ° C. for 16 hours with a dryer. At this time, when the product temperature was recorded by inserting a temperature sensor into the paste, the product temperature was heated at 115 ° C. or more for 5 hours. The dried cake was pulverized with a pulverizer to obtain a 3% silicone gel surface-treated talc.
- the mixture was stirred at 3000 rpm for 30 minutes. After filtration with a centrifugal dehydrator and washing with 7 L of water, the dehydrated cake was dried with a dryer at 120 ° C. for 16 hours. At this time, when the product temperature was recorded by inserting a temperature sensor into the cake, the product temperature was heated above 115 ° C. for 7 hours. The dried cake was pulverized with a pulverizer to obtain 5% silicone gel surface-treated sericite.
- the product temperature was recorded by inserting a temperature sensor into the paste, the product temperature was heated above 135 ° C. for 8 hours.
- the dried cake was pulverized with a pulverizer to obtain a silicone gel 5% surface-treated synthetic mica.
- 97 g of a dimethiconol water emulsion (Production Example 2) was added to keep the pH at 10.3 or more and stirred at 3000 rpm for 30 minutes. After filtration with a centrifugal dehydrator and washing with 7 L of water, the dehydrated cake was dried with a dryer at 120 ° C. for 16 hours. At this time, when the product temperature was recorded by inserting a temperature sensor into the cake, the product temperature was heated above 115 ° C. for 5 hours. The dried cake was pulverized with a pulverizer to obtain a 5% silicone gel surface-treated titanium oxide.
- talc FK300S manufactured by Yamaguchi Mica Industry Co., Ltd.
- the sericite of Example 2 was converted to Timiron Super of mica titanium.
- Red manufactured by Merck & Co., Inc.
- a silicone gel 5% surface-treated Timilon Super Red was obtained in the same manner.
- the titanium oxide of Example 4 was changed to yellow iron oxide yellow LL-100P (manufactured by Titanium Industry Co., Ltd.) to obtain a silicone gel 5% surface-treated yellow LL-100P in the same manner.
- the titanium oxide of Example 4 was changed to yellow iron oxide red R-516PS (manufactured by Titanium Industry Co., Ltd.) to obtain a silicone gel 5% surface-treated red R-516PS in the same manner.
- the titanium oxide of Example 4 was changed to yellow iron oxide black BL-100P (manufactured by Titanium Industry Co., Ltd.) to obtain a 5% silicone gel surface-treated black BL-100P in the same manner.
- the talc of Example 1 was changed to cross-linked spherical polymethyl methacrylate (trade name: Ganzpearl GMX-0810, manufactured by Ganz Kasei), and a 3% silicone gel surface-treated polymethyl methacrylate was obtained in the same manner.
- TTO-S-3 fine particle titanium oxide
- AM-40 Disper mixer
- the product temperature was recorded by inserting a temperature sensor into the cake, the product temperature was heated at 115 ° C. or more for 6 hours.
- the dried cake was pulverized with a JET mill to obtain 7% silicone gel surface-treated fine particle titanium oxide.
- composition No. Surface treatment powder with silicone gel No. 6 The same amount of surface was used in the same production method as in each Example, except that the surface treatment agent used in Examples 1 to 11 was replaced with dimethiconol water emulsion and KBE-13 in Production Example 1. Each surface-treated powder was obtained by treatment.
- Table 4 shows the evaluation results of the surface-treated powders of Examples and Comparative Examples.
- the cosmetic powder according to the present invention was proved to be superior in water repellency, smooth lightness, moist feeling, and adhesion to the skin as compared with the comparative powder.
- the surface-treated powders of Examples and Comparative Examples were blended and evaluated in a cosmetic preparation formulation.
- about each obtained formulation about 50 women's professional panelists about smoothness and lightness at the time of application, moist feeling, feeling of use such as elongation, adhesion to the skin, finish finish uniformity, makeup sustainability, Evaluation was performed according to the evaluation criteria shown in Table 5. The results were determined according to the following criteria based on the average score of 50 people.
- Example 12 and Comparative Example 12 Powder foundation (solid powder) (Production method)
- Example 12 uses Examples 1, 2, 4, 7, 8, 9 and Comparative Example 12 uses Comparative Examples 1, 2, 4, 7, 8, 9 .
- the results are shown in Table 8.
- the powder foundation in which the powder for cosmetics of the present invention is blended was a cosmetic having excellent usability and adhesion, uniform finish, and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- Example 13 and Comparative Example 13 Emulsification foundation (Production method) A: Components 1 to 4 were heated and mixed, and components 5 to 7 were added to make uniform. B: Components 8 to 9 and 11 were dissolved. C: Under stirring, B was gradually added to A to emulsify, and after cooling, component 10 was added to obtain a foundation.
- Example 13 used Examples 3, 4 and 7 and Comparative Example 13 used Comparative Examples 3, 4 and 7.
- the results are shown in Table 10.
- the emulsified foundation blended with the powder for cosmetics of the present invention was a cosmetic that was excellent in feeling of use and adhesion, had a uniform finish, and had excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- the emulsified preparation was also excellent in stability over time.
- Example 14 and Comparative Example 14 Face powder (powdered) (Production method)
- Example 14 used Examples 3, 6, and 10, and Comparative Example 14 used Comparative Examples 3, 6, and 10.
- the results are shown in Table 12.
- the face powder blended with the cosmetic powder of the present invention was a cosmetic excellent in use feeling and adhesion, having a uniform finish and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- Example 15 and Comparative Example 15 Eyeshadow (Production method) A: Components 1 to 4 were mixed, and components 5 to 8 were added and dispersed uniformly. B: Components 9 to 11 and 13 were uniformly dissolved. C: While stirring, B was gradually added to A to emulsify, and component 12 was added to obtain an eye shadow.
- Example 15 used Examples 3, 4 and 6 and Comparative Example 15 used Comparative Examples 3, 4 and 6.
- the results are shown in Table 14.
- the eye shadow blended with the cosmetic powder of the present invention was a cosmetic with excellent usability and adhesion, uniform finish and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- Example 16 and Comparative Example 16 Mascara (Production method) Components 1 to 12 are heated and mixed and dispersed, and then a mixture of components 13 to 14 is added and emulsified, and filled into a container.
- Example 16 was the same as that of Example 9, and Comparative Example 16 was that of Comparative Example 9.
- the results are shown in Table 16.
- the mascara blended with the cosmetic powder of the present invention was a cosmetic with excellent feeling of use and adhesion, uniform finish, and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- Step 1 Components 1 to 11 are mixed and dispersed.
- Step 2 A mixture of components 12 to 15 is added to the composition obtained in Step 1 and emulsified at room temperature.
- Example 17 used Examples 1 and 3 and Comparative Example 17 used Comparative Examples 1 and 3.
- the results are shown in Table 18.
- the base cream blended with the powder for cosmetics of the present invention was a cosmetic with excellent feeling of use and adhesion, uniform finish and excellent makeup sustainability. In addition, this preparation was excellent in stability over time.
- Example 18 and Comparative Example 18 Lipstick (Production method) A: Components 1 to 6 and a part of components 7 were mixed by heating and dissolved. B: The remainder of components 8 to 10 and 7 were mixed uniformly and added to A to make it uniform. C: Component 11 was added to B to obtain a lipstick.
- Example 18 used Examples 6 and 8, and Comparative Example 18 used Comparative Examples 6 and 8.
- the results are shown in Table 20.
- the lipstick blended with the powder for cosmetics of the present invention was a cosmetic with excellent feeling of use and adhesion, uniform finish and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- This formulation was also excellent in stability over time.
- Example 19 and Comparative Example 19 Eyeliner (Production method) A: Components 1 to 4 were mixed, and components 5 and 6 were added and mixed and dispersed uniformly. B: Components 7 to 10 were mixed. C: B was gradually added to A and emulsified to obtain an eyeliner.
- Example 19 used Examples 3 and 9, and Comparative Example 19 used Comparative Examples 3 and 9.
- the results are shown in Table 22.
- the eyeliner blended with the powder for cosmetics of the present invention was a cosmetic with excellent feeling of use and adhesion, uniform finish and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- the emulsified preparation was also excellent in stability over time.
- Example 20 and Comparative Example 20 Liquid emulsion foundation (Production method) A: Components 1 to 9 were heated and mixed, and components 10 to 12 were added to make uniform. B: Components 13 to 14 and 16 were dissolved by heating. C: While stirring, B was gradually added to A to emulsify, and after cooling, component 15 was added to obtain a liquid emulsion foundation.
- Example 20 used Examples 1 and 3 and Comparative Example 20 used Comparative Examples 1 and 3.
- the results are shown in Table 24.
- the liquid emulsification foundation blended with the powder for cosmetics of the present invention was a cosmetic excellent in use feeling and adhesion, having a uniform finish, and excellent in makeup sustainability.
- the color dullness was less than that of the comparative example.
- the emulsified preparation was also excellent in stability over time.
- Example 21 and Comparative Example 21 Oily solid foundation (Production method) A: Components 1 to 6 were heated and mixed. B: Components 7 to 15 were uniformly mixed and added to A and kneaded to be uniform. Thereafter, re-dissolution and deaeration were performed, and the product was obtained by filling into a special container.
- Example 21 uses Examples 1, 2, 5, 7, 8, 9 and Comparative Example 21 uses Comparative Examples 1, 2, 5, 7, 8, 9 .
- the results are shown in Table 26.
- the oily solid foundation in which the powder for cosmetics of the present invention is blended is a cosmetic excellent in use feeling and adhesion, having a uniform finish and excellent makeup sustainability.
- the color dullness was less than that of the comparative example.
- Example 22 and Comparative Example 22 Stick concealer (Production method) After the oil component was dissolved, the powder component was mixed and further mixed using a roller, then re-dissolved and degassed, filled in a mold, taken out after cooling, and placed in a container to obtain a product.
- Example 22 used Examples 1, 2, 4, 7, 8, 9 and Comparative Example 22 used Comparative Examples 1, 2, 4, 7, 8, 9 .
- the results are shown in Table 28.
- the stick-like concealer in which the cosmetic powder of the present invention was blended was a cosmetic excellent in use feeling and adhesion, having a uniform finish, and excellent in makeup sustainability.
- Example 23 and Comparative Example 23 Water-in-oil cream (Production method) A: Components 1 to 5 were mixed, and components 6 and 7 were added and mixed uniformly. B: Components 8 to 9 and 11 were mixed and dissolved. C: Under stirring, B was gradually added to A to emulsify, and then component 10 was added to obtain a cream. In addition, in the said table
- the results are shown in Table 30.
- the water-in-oil cream blended with the cosmetic powder of the present invention was a cosmetic that was excellent in feeling of use and adhesion, had a uniform finish, and had excellent makeup sustainability. In addition, the stability over time was excellent.
- Example 24 and Comparative Example 24 Oil-in-water cream (Production method) A: Components 4 to 10 were mixed. B: Components 1 to 3 were mixed, added to A and emulsified with stirring. In addition, in the said table
- the results are shown in Table 32.
- the oil-in-water cream blended with the cosmetic powder of the present invention was a cosmetic that was excellent in feeling of use and adhesion, had a uniform finish, and had excellent makeup sustainability. In addition, the stability over time was excellent.
- Example 25 and Comparative Example 25 Sunscreen emulsion (Production method) A: Components 1 to 6 were heated and mixed, and components 7 and 8 were uniformly dispersed. B: Components 9 to 11 and 13 were mixed by heating. C: While stirring, B was gradually added to A to emulsify, and after cooling, component 12 was added to obtain a sunscreen emulsion.
- Example 25 used Examples 6 and 11, and Comparative Example 25 used Comparative Examples 6 and 11.
- the sunscreen emulsion containing the powder for cosmetics of the present invention was a cosmetic that was excellent in feeling of use and adhesion, had a uniform finish, and had excellent makeup sustainability. In addition, the stability over time was excellent.
- Example 26 and Comparative Example 26 Suncut Cream (Production method) A: Component 2 was added to part of component 1 to make it uniform, and component 8 was added and dispersed with a bead mill. B: The remainder of component 1 and 3-7 were mixed to make uniform. C: Components 9 to 11 and 13 were mixed and dissolved. D: C was added to B and emulsified to disperse A, and further component 12 was added to obtain a sun cut cream.
- Example 26 used Examples 10 and 11, and Comparative Example 26 used Comparative Examples 10 and 11.
- the sun cut cream formulated with the powder for cosmetics of the present invention was a cosmetic that was excellent in feeling of use and adhesion, had a uniform finish, and had excellent makeup sustainability. In addition, the stability over time was excellent.
- Example 27 and Comparative Example 27 Nail enamel (Production method) A: Components 7 to 9 are mixed, and components 4 to 6 are added thereto and mixed uniformly. B: Components 1 to 3 are added to A and mixed. C: Component 10 was added to B and mixed to obtain a nail enamel.
- Example 27 was the same as that of Example 6, and Comparative Example 27 was the same as that of Comparative Example 6.
- the results are shown in Table 38.
- the nail enamel blended with the powder for cosmetics of the present invention was a cosmetic with excellent use feeling and adhesion, uniform finish and excellent makeup sustainability.
- Example 28 and Comparative Example 28 Moisturizing cream (Manufacturing procedure) Step 1 Components 1 to 7 and components 10 to 11 are mixed uniformly, and components 8 to 9 are added and dispersed uniformly. Step 2 Add ingredients 12 to 15 and ingredient 17 and dissolve. Step 3 The composition obtained in Step 2 is gradually added to the composition obtained in Step 1 to emulsify and cool. Step 4 Add component 16 to the composition obtained in step 3 and stir and mix.
- Example 28 used the one of Example 10
- Comparative Example 28 used the one of Comparative Example 10.
- the moisturizing cream blended with the powder for cosmetics of the present invention was a cosmetic with excellent usability and adhesion, uniform finish and excellent makeup sustainability.
- Example 29 and Comparative Example 29 After Shave Cream (Production method) A: Components 1 to 5 and components 11 to 12 are heated and mixed. B: Components 6 to 10 are heated and mixed. C: The composition obtained in Step 2 is gradually added to the composition obtained in Step 1 and emulsified.
- Example 29 was the same as that of Example 10, and Comparative Example 29 was the same as that of Comparative Example 10.
- Example 30 and Comparative Example 30 Lip gloss (Production method) Ingredients 1 to 6 are heated and mixed, filled into a container, and then cooled.
- Example 30 was the same as that of Example 6, and Comparative Example 30 was that of Comparative Example 6.
- the lip gloss blended with the powder for cosmetics of the present invention was a cosmetic with excellent usability and adhesion, uniform finish and excellent makeup sustainability.
- Example 31 and Comparative Example 31 Shampoo (Production method) A: Ingredients 1 to 4 are heated and mixed and dissolved. B: Components 5 to 8 are added to the composition obtained in step 1. C: Cool the composition obtained in step 2 and add ingredients 9-12. In addition, If necessary, component 13 is added to adjust the pH.
- Example 31 was the same as that of Example 10, and Comparative Example 31 was the same as that of Comparative Example 10.
- the results are shown in Table 46.
- the shampoo containing the cosmetic powder of the present invention was excellent in the feeling of use.
- Example 32 and Comparative Example 32 Conditioner (Production method) A: Ingredients 1 to 6 are heated and mixed and dissolved. B: Ingredients 7 to 8 are heated and mixed and dissolved. C: The composition obtained in Step 2 is added to the composition obtained in Step 1 and emulsified. D: Cool the composition obtained in step 3 and add components 9 and 10. In addition, the component 11 is added as needed.
- Example 32 was the same as that of Example 10, and Comparative Example 32 was the same as that of Comparative Example 10.
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Abstract
Description
[1]シリコーンゲルで表面処理した化粧料用粉体。
[2]上記シリコーンゲルで表面処理した化粧料用粉体の製造方法。
[3]上記シリコーンゲルで表面処理した化粧料用粉体を含有する化粧料。
に関する。
本発明に係る上記シリコーンゲルで表面処理した化粧料用粉体の好ましい態様としては、以下のものを挙げることができる。
(i)前記粉体が、無機粉体、有機粉体又はこれらの複合粉体である[1]に記載の化粧料用粉体。
(ii)前記シリコーンゲルが下記式(1)で示される両末端反応性ジオルガノポリシロキサンと架橋剤としての下記式(2)の1分子中に2つ以上の加水分解性基を有するシランカップリング剤または下記式(3)の反応性オルガノポリシロキサンのいずれかを少なくとも含有するオルガノポリシロキサンとを加水分解・縮合反応させた[1]または(i)に記載のシリコーンゲルで表面処理した化粧料用粉体。
(iv)前記式(1)のジオルガノポリシロキサンがジメチコノールである[1]及び(i)~(iii)のいずれかに記載の化粧料用粉体。
(v)前記式(1)のジメチルシロキサン単位L数が3~1,000である前記ジメチコノールを機械乳化して得られた水エマルジョンを表面処理をするための出発原料とした(iv)に記載の化粧料用粉体。
(vi)前記式(1)のジメチルシロキサン単位L数が3~1、000である前記ジメチコノールを乳化重合して得られた水エマルジョンを表面処理をするための出発原料とした(iv)に記載の化粧料用粉体。
(vii)オクタメチルシクロテトラシロキサンを出発原料として乳化重合により得られたジメチコノールの水エマルジョンを表面処理をするための出発原料とした(vi)に記載の化粧料用粉体。
(ix)前記ジメチコノールの水エマルジョン中のジメチコノール重量(A)と界面活性剤量(B)との配合重量比(B)/(A)×100が6.0未満である(v)~(viii)のいずれかに記載の化粧料用粉体。
(x)前記式(2)のシランカップリング剤の有機基R3が、アミノ基またはフェニル基のいずれかである[1]及び(i)~(ix)のいずれかに記載の化粧料用粉体。
(xi)前記シリコーンゲルと化粧料用粉体との重量比が100/0.1~100/25.0である[1]及び(i)~(x)のいずれかに記載の化粧料用粉体。
(xii)水溶性溶媒と化粧料用粉体の混合状態が、キャピラリーかスラリーのいずれかの状態にて、化粧料用粉体の存在下に前記(1)の両末端反応性ジオルガノポリシロキサンと前記(2)のシランカップリング剤または前記(3)のオルガノポリシロキサンを、別々に添加、または同時に添加する工程にて少なくとも一部を加水分解・縮合反応させる工程により得られた[1]及び(i)~(xi)のいずれかに記載の化粧料用粉体。
(xiii)[1]及び(i)~(xii)のいずれかに記載のシリコーンゲルで表面処理した化粧料用粉体を0.1重量%以上含有する化粧料。
本発明の化粧料用粉体は、シリコーンゲルで表面処理した粉体で、好適にはジメチコノールの水エマルジョンを出発原料として、シリコーンゲルを表面処理してなる表面処理粉体である。
本発明の表面処理粉体は、化粧料に配合される化粧料用粉体である。化粧料用粉体は、一般に用いられている無機粉体、有機粉体又は無機/無機複合粉体、無機/有機複合粉体、有機/有機複合粉体のいずれでもよく、1種単独で又は2種以上を適宜組み合わせて用いることができ、人体や肌への安全性を有し化粧料に実質的に使用可能な粉体及び全範囲の粒子径のものが適用できる。また、その幾何学的態様が、通常化粧料に用いられるものであれば、球状、半球状、星型状、多面体状、紡錘状、針状、板状等いずれの形状でもよく、また、無孔質、多孔質のいずれでもよい。
本発明のシリコーンゲルを得る好ましい方法は縮合反応によるものである。好ましい態様としては、下記式(1)で示される両末端反応性ジオルガノポリシロキサンと架橋剤としての下記式(2)の1分子中に2つ以上の加水分解性基を有するシランカップリング剤または下記式(3)の反応性オルガノポリシロキサンのいずれかを少なくとも含有するオルガノポリシロキサンとを加水分解・縮合反応させたジオルガノポリシロキサンの微3次元架橋構造を有する重合物である。
の間の縮合反応、水素化ケイ素と加水分解又は縮合可能な基の間の縮合反応、並びに同じ又は異なる化学種の2個の加水分解又は縮合可能な基同士間の縮合反応を伴う。
本発明において、シリコーンゲルは、ゴム弾性を有しないシリコーンを主成分とする化合物であればよい。一般にジメチルポリシロキサンの場合、リニアなシロキサンのユニット数が少ないと、つまり分子量が小さいと揮発性であり、分子量が大きくなるに従い液状、粘ちょう液体、ガム状となる。リニアな分子構造を有するジメチルポリシロキサン鎖に分子架橋剤が添加されることでその添加量の増加によりゲル状、弾性体、樹脂状物へと性状が変化する。
動的粘弾性測定装置:Rheosol-G3000(UBM社製)
測定治具:直径20mmのパラレルプレート
測定周波数:4Hz
測定温度:25±1.0℃
測定歪の設定:歪み率17%に設定し、自動測定モードにて測定を行う。
測定試料厚み(ギャップ):1.0mm
本発明におけるシリコーンゲルで表面処理した化粧料用粉体の製法は、化粧料用粉体とシリコーンゲルをミキサー等で単純混合して処理することも可能である。シリコーンゲルは粉体粒子同士を強固に凝集させるため、表面張力の低い有機溶媒を併用して混合処理をしたほうが撥水性や使用感、肌への密着性の観点で好ましいが、本発明のより好ましいシリコーンゲル処理粉体の製法としては、in-situ法にて化粧料用粉体の存在下でシリコーンゲルを粉体粒子表面に析出させた後、加熱することで粒子表面にシリコーンゲルを固着する方法で得ることができる。より好ましい製法としては、両末端反応性オルガノポリシロキサンの水エマルジョンを出発原料として前記in-situ法にてシリコーンゲルを固着する方法がある。この製法により粉体粒子表面へのシリコーンゲルの付着や被覆の均一性が高まり、撥水性が良くより良好な軽い使用感を付与することが可能となり肌への密着性により優れたシリコーンゲル化粧料用粉体を得ることができる。
本発明のシリコーンゲル化粧料用粉体は、各種の化粧料に使用することができ、例えば、スキンケア製品、メークアップ製品、頭髪製品、制汗剤製品、紫外線防御製品等の、特に皮膚や毛髪に外用される化粧料に好適に使用される。該複合粒子の配合割合は特に限定はなく、各製剤にあわせて、化粧料全体に対して0.1~100.0質量%の範囲で適宜選定される。該化粧料は、通常の化粧料に使用される種々の成分を本発明の効果を損なわない範囲で配合することができる。成分としては、例えば油剤、粉体、界面活性剤、水溶性又は水膨潤性高分子化合物、紫外線吸収剤、保湿剤、油溶性ゲル化剤、抗菌防腐剤、塩類、酸化防止剤、美肌用成分(美白剤、細胞賦活剤、肌荒れ改善剤、血行促進剤、皮膚収斂剤、抗脂漏剤等)、ビタミン類、アミノ酸類、制汗剤、アルコール、皮膜形成剤、抗炎症剤、清涼剤、核酸、ホルモン、包接化合物、pH調整剤、キレート剤、その他の添加剤を含んでよい。これらは1種単独で又は2種以上を適宜組み合わせて用いることができる。
前記の粘度が30mPa・sのジメチコノール500gを容量2リットルのポリエチレンビーカーに仕込み、ラウロイルメチルタウリンナトリウム22.5gおよびイオン交換水50gをホモミキサーで5,000rpmで攪拌しながら徐々に滴下して転相させた。増粘させた後、攪拌速度を7,000rpmに上げて15分間攪拌し、イオン交換水を450g加えて希釈した。次いで、卓上加圧ホモジナイザー(APVゴーリン製)で70MPaにて1回乳化分散してエマルジョンを得た。この水エマルジョンを105℃で3時間乾燥して水を揮発除去した固形分についてGPCによるPS換算の分子量を求めたところ6,000であった。固形分は51.0%であった。
前記の粘度が30mPa・sのジメチコノール500gを容量2リットルのポリエチレンビーカーに仕込み、ラウロイルメチルタウリンナトリウム22.5gおよびイオン交換水50gをホモミキサーで5,000rpmで攪拌しながら徐々に滴下して転相させた。増粘させた後、攪拌速度を7,000rpmに上げて15分間攪拌し、イオン交換水を450g加えて希釈した。次いで、卓上加圧ホモジナイザー(APVゴーリン製)で70MPaにて1回乳化分散してエマルジョンを得た。得られたエマルジョンを縮重合触媒であるクエン酸4.5gを投入、攪拌した後、10時間縮重合反応を行った。次いで10%炭酸ナトリウムを加えてpH7に調整して水エマルジョンを得た。この水エマルジョンを105℃で3時間乾燥して水を揮発除去した固形分についてGPCによるPS換算の分子量を求めたところ150,000であった。固形分は49.5%であった。
容量2リットルのポリエチレンビーカーにオクタメチルシクロテトラシロキサン450gとイオン交換水500g、ラウロイルメチルタウリンナトリウム6.75gを仕込みホモミキサー撹拌2,000rpmにより予備混合した後、クエン酸4gを添加して70℃に昇温してホモミキサー5,000rpmにより24時間乳化重合した。卓上加圧ホモジナイザー(APVゴーリン製)で50MPaにて1回乳化分散することにより高分子量のジメチコノールの水エマルジョンを得た。次いで10%炭酸ナトリウムを加えてpH7に調整して水エマルジョンを得た。この水エマルジョンを105℃で3時間乾燥して水を揮発除去した固形分についてGPCによるPS換算の分子量を求めたところ10,000であった。固形分は46.5%であった。
(シリコーン微架橋反応物の調製)
PP製300ml容器にイオン交換水100gにラウロイルメチルタウリンナトリウム0.1gを溶解後、両末端反応性ジオルガノポリシロキサンオイル(A)10gをホモミキサー6000rpm攪拌下に徐添する。10min攪拌を維持して常温にて乳化して水エマルジョンを得た。このエマルジョンをスターラーで攪拌下に架橋剤(B)25wt%IPA溶液を添加する。次いで必要に応じて1N-NaOH水溶液にてpHを10.5に調整して15min攪拌した後アルミ皿に移し、105℃/24hにて水を揮発してシリコーン反応物を得た。両末端反応性ジオルガノポリシロキサンが水エマルジョンの場合は、固形分が10gとなる量の水エマルジョンを投入後イオン交換水にて水分量を100gとして以下前記同様の操作をする。両末端反応性ジオルガノポリシロキサン(A)と架橋剤(B)との重量配合比(A)/(B)は、100/10、7/1、3/1のいずれかとした。
スチロール角型ケース(タテ36×ヨコ36×高さ14mm)にシリコーン反応物を面より僅かに出るように仕込み表面を平たんにして試験面とする。デュロメーターの加圧板を試験面上20mm位置に置き試験面表面と加圧板が平行になるように維持された状態で加圧板を試験片に押し当てて針の目盛りを読み取る。この操作を5回行い平均値を測定値とした。なお、測定により針が動かなかった場合はNA(Not Applicable)とした。
(動的粘弾性測定による複素弾性率とtanδの測定条件)
下記に示す条件によりG’(貯蔵弾性率)およびG”(損失弾性率)を求め複素弾性率とtanδを求めた。
・測定治具:直径20mmのパラレルプレート
・測定周波数:4Hz
・測定温度:25±1.0℃
・測定歪の設定:歪み率17%に設定し、自動測定モードにて測定
・測定試料厚み(ギャップ):1.0mm
[実施例1](ジメチコノール/架橋剤比=100/10wt%)
タルクJA-13R(浅田製粉株式会社製)1kgを万能混合機に仕込み水550gとIPA/粘度が30mPa・sのジメチコノール=60g/35gの混合液を投入して15分間混合攪拌して粉体粒子が軟ペースト状(キャピラリー状態)とした。架橋剤として5質量%KBE-903水溶液を70g添加してさらに15分間混合攪拌した。軟ペーストを取り出し乾燥機にて120℃にて16時間乾燥した。この時ペースト中に温度センサーを挿入しての品温を記録したところ品温は115℃以上で5時間加熱されていた。乾燥したケーキをパルベライザーで粉砕してシリコーンゲル3%表面処理タルクを得た。
容量20リットルのPE製容器に水7LとセリサイトFSE(三信鉱工株式会社製)1kgを仕込みディスパーミキサー(プライムミクス社;AM-40)にて2000rpmで5分間分散(スラリー状態)した。ジメチコノールの水エマルジョン(製造例3)103gを添加して2500rpmにて5分間攪拌した。次いで、架橋剤として5質量%KBE-903水溶液を96g添加した。1N-NaOH水溶液にてpHを10.3に調整した後、3000rpmにて30分間攪拌反応させた。遠心脱水機にてろ過して7Lの水にて洗浄した後、脱水ケーキを乾燥機にて120℃にて16時間乾燥した。この時ケーキ中に温度センサーを挿入しての品温を記録したところ品温は115℃以上で7時間加熱されていた。乾燥したケーキをパルベライザーで粉砕してシリコーンゲル5%表面処理セリサイトを得た。
合成マイカPDM-9WB(トピー工業株式会社製)1kgを万能混合機に仕込み水450gとジメチコノールの水エマルジョン(製造例1)82.6gを添加して15分間混合攪拌して軟ペースト状(キャピラリー状態)とした。架橋剤としてKF-9901を10.5g添加して28%アンモニア水溶液4mlを添加して15分間混合攪拌した。軟ペーストを取り出し乾燥機にて140℃にて16時間乾燥した。この時ペースト中に温度センサーを挿入しての品温を記録したところ品温は135℃以上で8時間加熱されていた。乾燥したケーキをパルベライザーで粉砕してシリコーンゲル5%表面処理合成マイカを得た。
容量20リットルのPE製容器に水7Lと1N-NaOH水溶液を投入してpHを12.0に調整した。酸化チタンCR-50(石原産業株式会社製)1kgを添加してディスパーミキサー(プライムミクス社;AM-40)にて3000rpmで5分間分散(スラリー状態)した。次いで架橋剤として5質量%KBE-903水溶液を96g添加して2000rpmで5分間攪拌した。さらに、ジメチコノールの水エマルジョン(製造例2)97gを添加してpHを10.3以上にキープして3000rpmにて30分間攪拌した。遠心脱水機にてろ過して7Lの水にて洗浄した後、脱水ケーキを乾燥機にて120℃にて16時間乾燥した。この時ケーキ中に温度センサーを挿入しての品温を記録したところ品温は115℃以上で5時間加熱されていた。乾燥したケーキをパルベライザーで粉砕してシリコーンゲル5%表面処理酸化チタンを得た。
容量20リットルのPE製容器に水5Lと1N-NaOH水溶液を投入してpHを12.0に調整した。タルクFK300S(山口雲母工業社製)700gを添加してディスパーミキサー(プライムミクス社;AM-40)にて3000rpmで5分間分散(スラリー状態)した。(タルクスラリー)別の容器に水3Lと微粒子酸化チタンTTO-55A(石原産業株式会社製)300gを入れ1N-NaOH水溶液にてpHを12.0に調整してホモミキサーにて6000rpmで10分間分散した。(微粒子酸化チタンスラリー)タルクスラリーをディスパーミキサー3000rpm攪拌下に微粒子酸化チタンスラリーを徐添した後、架橋剤として5質量%KBE-903水溶液を116g添加して3000rpmで5分間攪拌した。さらに、ジメチコノールの水エマルジョン(製造例2)117gを添加してpHを10.3以上にキープして3000rpmにて30分間攪拌した。遠心脱水機にてろ過して8Lの水にて洗浄した後、脱水ケーキを乾燥機にて120℃にて16時間乾燥した。この時ケーキ中に温度センサーを挿入しての品温を記録したところ品温は115℃以上で5時間加熱されていた。乾燥したケーキをパルベライザーで粉砕してシリコーンゲル6%表面処理微粒子酸化チタン被覆タルクを得た。
実施例2のセリサイトを雲母チタンのTimiron Super
Red(メルク社製)に変えて以下同様にてシリコーンゲル5%表面処理Timiron Super Redを得た。
実施例4の酸化チタンを黄酸化鉄のイエローLL-100P(チタン工業社製)に変えて以下同様にてシリコーンゲル5%表面処理イエローLL-100Pを得た。
実施例4の酸化チタンを黄酸化鉄のレッドR-516PS(チタン工業社製)に変えて以下同様にてシリコーンゲル5%表面処理レッドR-516PSを得た。
実施例4の酸化チタンを黄酸化鉄のブラックBL-100P(チタン工業社製)に変えて以下同様にてシリコーンゲル5%表面処理ブラックBL-100Pを得た。
実施例1のタルクを架橋型球状ポリメタクリル酸メチル(商品名:ガンツパールGMX-0810、ガンツ化成製)に変えて以下同様にてシリコーンゲル3%表面処理ポリメタクリル酸メチルを得た。
容量20リットルのPE製容器に水7Lと1N-NaOH水溶液を投入してpHを12.5に調整した。微粒子酸化チタンTTO-S-3(石原産業株式会社製)1kgを添加してディスパーミキサー(プライムミクス社;AM-40)にて3000rpmで5分間分散(スラリー状態)した。次いで架橋剤としてKF-9901の水エマルジョン(シリコーン/ラウロイルメチルタウリンNa/水=45/5/50wt%)を21g添加して3000rpmで5分間攪拌した。さらに、ジメチコノールの水エマルジョン(製造例2)133gを添加してpHを10.5以上にキープして3000rpmにて60分間攪拌した。遠心脱水機にてろ過して7Lの水にて洗浄した後、脱水ケーキを乾燥機にて120℃にて16時間乾燥した。この時ケーキ中に温度センサーを挿入しての品温を記録したところ品温は115℃以上で6時間加熱されていた。乾燥したケーキをJETミルで粉砕してシリコーンゲル7%表面処理微粒子酸化チタンを得た。
実施例1~11で用いた表面処理剤を製造例1のジメチコノール水エマルジョンとKBE-13に代えた以外は各実施例同様の製造方法にて同量の表面処理を行い各表面処理粉体を得た。
100mlのビーカーに水を60ml入れ、各表面処理粉体を0.5g投入し24時間静置する。その後、スパーテルにて1秒間に2回の速さで50回攪拌した後、水相への表面処理粉体の移行状態を下記のように評価した。
◎:水面に浮いたままであり、水相への移行無し
〇:水面に浮いたままであるが、わずかに濁りがある
△:水面に浮いたままであるが、濁りがある
×:一部水面に浮いたままであるが、かなりの濁りがある
上腕部に各試料を0.3mg/cm2塗布し、ファンデーション用スポンジを用いて3回擦った時の滑らかで軽い使用感としっとり感の評価を行った。評価は専門評価パネル10名により、下記絶対評価にて5段階に評価し評点を付け、試料毎にパネル全員の評点合計から、その平均値を算出し、下記4段階判定基準により判定した。
(絶対評価)
(評点) : (評価)
5 : 非常に良い。
4 : 良い。
3 : 普通。
2 : やや悪い。
1 : 悪い。
上腕部に試料を0.3 mg/cm2ずつ、1つの試料に対し2箇所塗布した。1箇所に10分間38℃の水で流水し、もう1箇所は流水せずにスタンダードとした。流水箇所をスタンダードと比較し、塗布膜の変化を目視にて観察した。評価は専門評価パネル10名により、下記絶対評価にて5段階に評価し評点を付け、試料毎にパネル全員の評点合計から、その平均値を算出し、下記4段階判定基準により判定した。
(絶対評価)
(評点):(評価)
5 : 全く変化なし。
4 : 少し膜薄になり差が少しわかる。
3 : 膜薄になり差が分かる。
2 : かなり膜薄であるが、粉体は残っている。
1 : ほとんど粉体が残っていない。
A:成分1~9をヘンシェルミキサーで均一に混合する。
B:Aに成分10~13を添加し、更に混合する。
C:Bをパルベライザーにて粉砕し、金皿に圧縮成型し、パウダー
ファンデーションを得た。
なお、上記表中、実施例12は実施例1,2、4,7,8,9のものを用い、比較例12は比較例1,2、4,7,8,9のものを用いた。
A:成分1~4を加熱混合し、成分5~7を添加して均一にした。
B:成分8~9及び11を溶解した。
C:攪拌下、AにBを徐添して乳化し、冷却した後成分10を添加し
てファンデーションを得た。
なお、上記表中、実施例13は実施例3,4,7のものを用い、比較例13は比較例3,4,7のものを用いた。
A:成分1 ~ 8 をヘンシェルミキサーにて均一に混合後、成分9を
添加し、更に混合する。
B:A をパルベライザーにて粉砕する。
C:B を容器に充填して粉末状のフェイスパウダーを得た。
なお、上記表中、実施例14は実施例3,6,10のものを用い、比較例14は比較例3,6,10のものを用いた。
A:成分1~4を混合し、成分5~8を添加して均一に分散した。
B:成分9~11及び13を均一溶解した。
C:攪拌下、AにBを徐添して乳化し、成分12を添加してアイシャ
ドウを得た。
なお、上記表中、実施例15は実施例3,4,6のものを用い、比較例15は比較例3,4,6のものを用いた。
成分1~12を加熱して混合分散した後、成分13~14の混合物を添加して乳化し、容器に充填する。
なお、上記表中、実施例16は実施例9のものを用い、比較例16は比較例9のものを用いた。
工程1 成分1~11を混合分散する。
工程2 工程1で得た組成物に、成分12~15の混合物を加えて室
温にて乳化する。
なお、上記表中、実施例17は実施例1,3のものを用い、比較例17は比較例1,3のものを用いた。
A:成分1~6及び7の一部を加熱混合、溶解した。
B:成分8~10及び7の残部を均一混合し、Aに加えて均一にした。
C:Bに成分11を添加して口紅を得た。
なお、上記表中、実施例18は実施例6,8のものを用い、比較例18は比較例6,8のものを用いた。
A:成分1~4を混合し、成分5及び6を加えて均一に混合分散した。
B:成分7~10を混合した。
C:BをAに徐添して乳化し、アイライナーを得た。
なお、上記表中、実施例19は実施例3,9のものを用い、比較例19は比較例3,9のものを用いた。
A:成分1~9を加熱混合し、成分10~12を添加して均一にした。
B:成分13~14及び16を加熱溶解した。
C:攪拌下、AにBを徐添して乳化し、冷却して成分15を添加し液状乳化ファンデーションを得た。
なお、上記表中、実施例20は実施例1,3のものを用い、比較例20は比較例1,3のものを用いた。
A:成分1~6を加熱混合した。
B:成分7~15を均一に混合してAに加え均一になるよう混練した。
その後、再溶解、脱気を行い、専用容器に充填し製品を得た。
なお、上記表中、実施例21は実施例1,2,5,7,8,9のものを用い、比較例21は比較例1,2,5,7,8,9のものを用いた。
油性成分を溶解後、粉体成分を混合し、ローラーを用いてさらに混合した後、再溶解、脱気を行い、金型に充填し、冷却後とり出して容器に設置し製品を得た。
なお、上記表中、実施例22は実施例1,2,4,7,8,9のものを用い、比較例22は比較例1,2,4,7,8,9のものを用いた。
A:成分1~5を混合し、成分6,7を添加して均一に混合した。
B:成分8~9及び11を混合溶解した。
C:攪拌下、AにBを徐添して乳化した後、成分10を添加してクリーム
を得た。
なお、上記表中、実施例23は実施例3,10のものを用い、比較例23は比較例3,10のものを用いた。
A:成分4~10を混合した。
B:成分1~3を混合し、これをAに加えて攪拌乳化した。
なお、上記表中、実施例24は実施例10のものを用い、比較例24は比較例10のものを用いた。
A:成分1~6を加熱混合し、成分7,8を均一分散した。
B:成分9~11及び13を加熱混合した。
C:攪拌下、AにBを徐添して乳化し、冷却して成分12を添加し日焼け
止め乳液を得た。
なお、上記表中、実施例25は実施例6,11のものを用い、比較例25は比較例6,11のものを用いた。
A:成分1の一部に成分2を加えて均一にし、成分8を添加してビーズ
ミルで分散した。
B:成分1の残部及び3~7を混合して均一にした。
C:成分9~11及び13を混合、溶解した。
D:BにCを加えて乳化し、Aを分散させ、さらに、成分12を添加して
サンカットクリームを得た。
なお、上記表中、実施例26は実施例10,11のものを用い、比較例26は比較例10,11のものを用いた。
A:成分7~9を混合し、これに成分4~6を添加して均一に混合する。
B:Aに成分1~3を添加して混合する。
C:Bに成分10を添加混合して、ネイルエナメルを得た。
なお、上記表中、実施例27は実施例6のものを用い、比較例27は比較例6のものを用いた。
工程1 成分1~7及び成分10~11を均一に混合し、成分8~9を
添加して均一に分散する。
工程2 成分12~15及び成分17を加えて溶解する。
工程3 工程2で得た組成物を、工程1で得た組成物に徐々に添加して
乳化し、冷却する。
工程4 工程3で得た組成物に成分16を加えて攪拌混合する。
なお、上記表中、実施例28は実施例10のものを用い、比較例28は比較例10のものを用いた。
A:成分1~5及び成分11~12を加熱混合する。
B:成分6~10を加熱混合する。
C:工程1で得た組成物に、工程2で得た組成物を徐々に添加して乳化する。
なお、上記表中、実施例29は実施例10のものを用い、比較例29は比較例10のものを用いた。
成分1~6を加熱混合し、容器に充填した後、冷却する。
なお、上記表中、実施例30は実施例6のものを用い、比較例30は比較例6のものを用いた。
A:成分1~4を加温し、混合溶解する。
B:工程1で得た組成物に成分5~8を添加する。
C:工程2で得た組成物を冷却し、成分9~12を添加する。なお、
必要に応じて、成分13を添加し、pHを調製する。
なお、上記表中、実施例31は実施例10のものを用い、比較例31は比較例10のものを用いた。
A:成分1~6を加温し、混合溶解する。
B:成分7~8を加温し、混合溶解する。
C:工程1で得た組成物に工程2で得た組成物を添加し、乳化する。
D:工程3で得た組成物を冷却し、成分9および10を添加する。なお
、必要に応じて、成分11を添加する。
なお、上記表中、実施例32は実施例10のものを用い、比較例32は比較例10のものを用いた。
Claims (14)
- シリコーンゲルで表面処理した化粧料用粉体。
- 前記粉体が、無機粉体、有機粉体又はこれらの複合粉体である請求項1に記載の化粧料用粉体。
- 前記シリコーンゲルが下記式(1)で示される両末端反応性ジオルガノポリシロキサンと架橋剤としての下記式(2)の1分子中に2つ以上の加水分解性基を有するシランカップリング剤または下記式(3)の反応性オルガノポリシロキサンのいずれかを少なくとも含有するオルガノポリシロキサンとを加水分解・縮合反応させた請求項1または2に記載のシリコーンゲルで表面処理した化粧料用粉体。
- 前記シリコーンゲルが25℃で歪み率17%、剪断周波数4Hzにおける動的粘弾性測定による複素弾性率が3,000~100,000Paで損失係数tanδが1.0~2.5である請求項1~3のいずれかに記載の化粧料用粉体。
- 前記式(1)のジオルガノポリシロキサンがジメチコノールである請求項1~4のいずれかに記載の化粧料用粉体。
- 前記式(1)のジメチルシロキサン単位L数が3~1,000である前記ジメチコノールを機械乳化して得られた水エマルジョンを表面処理をするための出発原料とした請求項5に記載の化粧料用粉体。
- 前記式(1)のジメチルシロキサン単位L数が3~1、000である前記ジメチコノールを乳化重合して得られた水エマルジョンを表面処理をするための出発原料とした請求項5に記載の化粧料用粉体。
- オクタメチルシクロテトラシロキサンを出発原料として乳化重合により得られたジメチコノールの水エマルジョンを表面処理をするための出発原料とした請求項5に記載の化粧料用粉体。
- 前記ジメチコノールの水エマルジョン中に含有する界面活性剤が少なくともアシル化アミノ酸を含有する請求項6~8のいずれかに記載の化粧料用粉体。
- 前記ジメチコノールの水エマルジョン中のジメチコノール重量(A)と界面活性剤量(B)との配合重量比(B)/(A)×100が6.0未満である請求項6~9のいずれかに記載の化粧料用粉体。
- 前記式(2)のシランカップリング剤の有機基R3が、アミノ基またはフェニル基のいずれかである請求項1~10のいずれかに記載の化粧料用粉体。
- 前記シリコーンゲルと化粧料用粉体との重量比が100/0.1~100/25.0である請求項1~11のいずれかに記載の化粧料用粉体。
- 水溶性溶媒と化粧料用粉体の混合状態が、キャピラリーかスラリーのいずれかの状態にて、化粧料用粉体の存在下に前記(1)の両末端反応性ジオルガノポリシロキサンと前記(2)のシランカップリング剤または前記(3)のオルガノポリシロキサンを、別々に添加、または同時に添加する工程にて少なくとも一部を加水分解・縮合反応させる工程により得られた請求項1~12のいずれかに記載の化粧料用粉体。
- 請求項1~13のいずれかに記載のシリコーンゲルで表面処理した化粧料用粉体を0.1重量%以上含有する化粧料。
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Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS63152308A (ja) | 1986-08-23 | 1988-06-24 | Kobayashi Kooc:Kk | シリコ−ンゲル組成物並びにこれを含有する化粧料 |
JPH086035B2 (ja) | 1988-01-26 | 1996-01-24 | 株式会社コーセー | シリコーンゲル組成物並びにこれを含有する化粧料 |
JPH0948716A (ja) * | 1995-06-02 | 1997-02-18 | Miyoshi Kasei:Kk | 化粧料 |
JP2582275B2 (ja) | 1987-10-15 | 1997-02-19 | 株式会社コーセー | シリコーンゲル組成物並びにこれを含有する化粧料 |
JPH10251123A (ja) * | 1997-03-11 | 1998-09-22 | Kose Corp | 表面処理酸化チタン粉末及びそれを含有する化粧料 |
JP3079395B2 (ja) | 1991-06-26 | 2000-08-21 | 三好化成株式会社 | 有機ケイ素化合物処理顔料、その製法および化粧料 |
JP2004315468A (ja) * | 2003-04-18 | 2004-11-11 | Hakuto Co Ltd | 皮膚外用剤 |
JP3707758B2 (ja) | 1997-09-05 | 2005-10-19 | 株式会社ノエビア | 表面処理粉体及びそれを含有して成る化粧料 |
JP2006206496A (ja) | 2005-01-28 | 2006-08-10 | Shin Etsu Chem Co Ltd | 化粧品用顔料又は化粧品用体質顔料の製造法 |
JP3963635B2 (ja) | 2000-08-29 | 2007-08-22 | 触媒化成工業株式会社 | 化粧料およびその製造方法 |
JP2010163375A (ja) | 2009-01-14 | 2010-07-29 | Kao Corp | 表面処理粉体及び化粧料 |
JP2011001332A (ja) | 2009-06-22 | 2011-01-06 | Shin-Etsu Chemical Co Ltd | 複合粒子及びその製造方法、ならびに化粧料 |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4518999B1 (ja) * | 1965-07-29 | 1970-06-29 | ||
JP3675564B2 (ja) | 1996-03-19 | 2005-07-27 | 株式会社資生堂 | 固形粉末メーキャップ化粧料 |
JP2001001332A (ja) * | 1999-06-17 | 2001-01-09 | Ibiden Co Ltd | セラミック成形体の封口方法及び封口装置 |
JP2002128637A (ja) | 2000-10-26 | 2002-05-09 | Kose Corp | スラリー充填固型粉末化粧料 |
FR2867676B1 (fr) | 2004-03-22 | 2006-06-02 | Oreal | Composition cosmetique comprenant des particules concaves |
JP4763986B2 (ja) | 2004-08-23 | 2011-08-31 | 株式会社 資生堂 | ゲル状組成物及びそれを含む化粧料 |
JP4518999B2 (ja) * | 2005-05-17 | 2010-08-04 | 日本放送協会 | Mimo受信アンテナ選択装置 |
JP2009209139A (ja) | 2008-02-07 | 2009-09-17 | Shiseido Co Ltd | 固形粉末化粧料 |
KR20120046207A (ko) * | 2009-06-30 | 2012-05-09 | 가부시키가이샤 시세이도 | 고형 분말 화장료 |
JP5416493B2 (ja) | 2009-06-30 | 2014-02-12 | 株式会社 資生堂 | 固形粉末化粧料 |
JP5947065B2 (ja) | 2011-03-10 | 2016-07-06 | 株式会社コーセー | 油性睫用化粧料 |
JP5991160B2 (ja) * | 2012-11-19 | 2016-09-14 | ソニー株式会社 | ディスクカートリッジおよびチェンジャー |
JP5901799B2 (ja) * | 2012-12-26 | 2016-04-13 | 三好化成株式会社 | 表面処理した化粧料用板状粉体及びこれを配合した固形粉末化粧料 |
-
2012
- 2012-12-26 KR KR1020147036215A patent/KR102048752B1/ko active IP Right Grant
- 2012-12-26 CN CN201280074429.4A patent/CN104411285B/zh active Active
- 2012-12-26 EP EP12891123.7A patent/EP2939652B1/en active Active
- 2012-12-26 WO PCT/JP2012/008345 patent/WO2014102862A1/ja active Application Filing
- 2012-12-26 JP JP2014553882A patent/JP5901798B2/ja active Active
- 2012-12-26 US US14/424,091 patent/US9597269B2/en active Active
-
2015
- 2015-09-10 HK HK15108873.8A patent/HK1208343A1/xx unknown
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS63152308A (ja) | 1986-08-23 | 1988-06-24 | Kobayashi Kooc:Kk | シリコ−ンゲル組成物並びにこれを含有する化粧料 |
JP2582275B2 (ja) | 1987-10-15 | 1997-02-19 | 株式会社コーセー | シリコーンゲル組成物並びにこれを含有する化粧料 |
JPH086035B2 (ja) | 1988-01-26 | 1996-01-24 | 株式会社コーセー | シリコーンゲル組成物並びにこれを含有する化粧料 |
JP3079395B2 (ja) | 1991-06-26 | 2000-08-21 | 三好化成株式会社 | 有機ケイ素化合物処理顔料、その製法および化粧料 |
JPH0948716A (ja) * | 1995-06-02 | 1997-02-18 | Miyoshi Kasei:Kk | 化粧料 |
JPH10251123A (ja) * | 1997-03-11 | 1998-09-22 | Kose Corp | 表面処理酸化チタン粉末及びそれを含有する化粧料 |
JP3707758B2 (ja) | 1997-09-05 | 2005-10-19 | 株式会社ノエビア | 表面処理粉体及びそれを含有して成る化粧料 |
JP3963635B2 (ja) | 2000-08-29 | 2007-08-22 | 触媒化成工業株式会社 | 化粧料およびその製造方法 |
JP2004315468A (ja) * | 2003-04-18 | 2004-11-11 | Hakuto Co Ltd | 皮膚外用剤 |
JP2006206496A (ja) | 2005-01-28 | 2006-08-10 | Shin Etsu Chem Co Ltd | 化粧品用顔料又は化粧品用体質顔料の製造法 |
JP2010163375A (ja) | 2009-01-14 | 2010-07-29 | Kao Corp | 表面処理粉体及び化粧料 |
JP2011001332A (ja) | 2009-06-22 | 2011-01-06 | Shin-Etsu Chemical Co Ltd | 複合粒子及びその製造方法、ならびに化粧料 |
Cited By (19)
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WO2016189961A1 (ja) * | 2015-05-25 | 2016-12-01 | 三好化成株式会社 | 表面処理した化粧用粉体及び該表面処理粉体を配合したメーキャップ化粧料 |
WO2016189962A1 (ja) * | 2015-05-25 | 2016-12-01 | 三好化成株式会社 | 表面処理した化粧料用粉体及び顔料級酸化チタンを配合した、白浮きのないメーキャップ化粧料 |
JP2016216424A (ja) * | 2015-05-25 | 2016-12-22 | 三好化成株式会社 | 表面処理した化粧用粉体及び該表面処理粉体を配合したメーキャップ化粧料 |
JP2016216423A (ja) * | 2015-05-25 | 2016-12-22 | 三好化成株式会社 | 表面処理した化粧料用粉体及び顔料級酸化チタンを配合した、白浮きのないメーキャップ化粧料 |
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JP2017186316A (ja) * | 2016-03-31 | 2017-10-12 | 株式会社コーセー | 粉体化粧料 |
JP2018168130A (ja) * | 2017-03-30 | 2018-11-01 | 株式会社コーセー | 固形粉末化粧料 |
JP2018172305A (ja) * | 2017-03-31 | 2018-11-08 | 株式会社コーセー | 水中油型乳化化粧料 |
WO2019187255A1 (ja) * | 2018-03-28 | 2019-10-03 | 大阪ガスケミカル株式会社 | 疎水化無機粒子、その製造方法、化粧料添加剤、および、その製造方法 |
JP6694559B1 (ja) * | 2019-03-18 | 2020-05-13 | 株式会社ダイセル | セルロースアセテートを含む粒子、化粧品組成物、及びセルロースアセテートを含む粒子の製造方法 |
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WO2020230650A1 (ja) * | 2019-05-10 | 2020-11-19 | テイカ株式会社 | 複合表面処理無機粉体及びその製造方法、その無機粉体を配合した油性分散体及び化粧料 |
JP2020203842A (ja) * | 2019-06-17 | 2020-12-24 | 株式会社ノエビア | 表面処理粉体及び表面処理粉体を含有する化粧料 |
JP7332352B2 (ja) | 2019-06-17 | 2023-08-23 | 株式会社ノエビア | 表面処理粉体及び表面処理粉体を含有する化粧料 |
WO2021014656A1 (ja) | 2019-07-25 | 2021-01-28 | 三好化成株式会社 | 親水化無機粉体及び当該親水化無機粉体を配合した化粧料 |
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CN104411285B (zh) | 2017-07-18 |
JPWO2014102862A1 (ja) | 2017-01-12 |
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US9597269B2 (en) | 2017-03-21 |
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