JP4979995B2 - Non-interfering color flop powder exhibiting a beige hue and a cosmetic comprising the same - Google Patents
Non-interfering color flop powder exhibiting a beige hue and a cosmetic comprising the same Download PDFInfo
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- JP4979995B2 JP4979995B2 JP2006174733A JP2006174733A JP4979995B2 JP 4979995 B2 JP4979995 B2 JP 4979995B2 JP 2006174733 A JP2006174733 A JP 2006174733A JP 2006174733 A JP2006174733 A JP 2006174733A JP 4979995 B2 JP4979995 B2 JP 4979995B2
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- Prior art keywords
- angle
- powder
- color
- coating layer
- color flop
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000843 powder Substances 0.000 title claims description 138
- 239000002537 cosmetic Substances 0.000 title claims description 42
- 230000001747 exhibiting effect Effects 0.000 title description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 70
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 68
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 62
- 239000002245 particle Substances 0.000 claims description 58
- 239000011247 coating layer Substances 0.000 claims description 55
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 44
- 239000000377 silicon dioxide Substances 0.000 claims description 35
- 239000000758 substrate Substances 0.000 claims description 35
- 235000012239 silicon dioxide Nutrition 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 28
- 239000004408 titanium dioxide Substances 0.000 claims description 25
- 239000010445 mica Substances 0.000 claims description 18
- 229910052618 mica group Inorganic materials 0.000 claims description 18
- 230000008859 change Effects 0.000 claims description 9
- 238000004040 coloring Methods 0.000 claims description 8
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 3
- 238000004611 spectroscopical analysis Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 34
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- 239000000049 pigment Substances 0.000 description 23
- 230000000694 effects Effects 0.000 description 21
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- 239000002585 base Substances 0.000 description 18
- 239000011248 coating agent Substances 0.000 description 17
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- 238000002156 mixing Methods 0.000 description 11
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- 239000000126 substance Substances 0.000 description 11
- 239000000725 suspension Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 10
- 230000007062 hydrolysis Effects 0.000 description 9
- 238000006460 hydrolysis reaction Methods 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 238000000149 argon plasma sintering Methods 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 7
- 238000011160 research Methods 0.000 description 7
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
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- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- 239000003086 colorant Substances 0.000 description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 5
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- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- -1 methyl hydrogen Chemical compound 0.000 description 4
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 4
- 229920001220 nitrocellulos Polymers 0.000 description 4
- 238000012643 polycondensation polymerization Methods 0.000 description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000454 talc Substances 0.000 description 4
- 229910052623 talc Inorganic materials 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 2
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
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- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
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- 239000004115 Sodium Silicate Substances 0.000 description 1
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
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- SFVJVIQIWGMENJ-UHFFFAOYSA-N butan-1-olate;iron(3+) Chemical compound [Fe+3].CCCC[O-].CCCC[O-].CCCC[O-] SFVJVIQIWGMENJ-UHFFFAOYSA-N 0.000 description 1
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
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Description
本発明は、マイカ等の鱗片状基材の表面に酸化鉄、二酸化珪素、二酸化チタン等の被覆層を形成してなる、ベージュ色の色相を呈する非干渉性のカラーフロップ粉体およびこれを配合してなる化粧料に関するものである。 The present invention relates to a non-interfering color flop powder having a beige hue formed by forming a coating layer of iron oxide, silicon dioxide, titanium dioxide or the like on the surface of a scaly substrate such as mica and the like. This is related to cosmetics.
従来、パウダーファンデーション等の化粧料には、マイカ、タルク、セリサイト等の鱗片状粉体が配合されている。この鱗片状粉体を化粧料に配合した場合の効果は、化粧料の皮膚上での延展性を向上させると共に、着色顔料の皮膚上での分散性を向上させ、さらに皮膚への付着力を高めることなどであり、メークアップ用化粧料には欠かせないものである。
また、主としてマイカの表面にある一定厚さの酸化チタンを被覆したものは、パール顔料と呼ばれ、化粧料や塗料等に使用されている。このパール顔料は、光の干渉を利用して光の入射角に対するある一定の反射角において各層の厚さに応じて色調が変化し、かつ強い光沢を有するものである。この光沢が強いほど、見る角度による明度の変化は大きくなり、その性質はフリップフロップ性と呼ばれている。
Conventionally, scaly powders such as mica, talc, and sericite are blended in cosmetics such as powder foundation. The effect of blending this scaly powder into a cosmetic improves the spreadability of the cosmetic on the skin, improves the dispersibility of the colored pigment on the skin, and further improves the adhesion to the skin. It is essential to make up cosmetics.
In addition, what is coated with a certain thickness of titanium oxide mainly on the surface of mica is called a pearl pigment and is used in cosmetics and paints. This pearl pigment has a strong luster that changes its color tone according to the thickness of each layer at a certain reflection angle with respect to the incident angle of light by utilizing interference of light. The stronger the gloss, the greater the change in brightness depending on the viewing angle, and this property is called flip-flop.
光の干渉により生じる色は、ベンガラ、群青等、一般の着色顔料の色と比較して明度は高いが、その着色力は非常に弱いことが知られている。この着色力を向上させる方法として、前記した酸化チタン層の上に酸化鉄等の可視光域のある特定範囲の波長を吸収する金属酸化物を被覆することが提案されている（特許文献1）。しかしながら、この方法では、ある特定の色を強める効果や光沢に起因する明度の変化を大きくする効果は得られるが、見る角度によって色相が変わるという効果は余り期待できない。
また、逆にマイカの表面にまず酸化第二鉄を被覆し、その上に一定の厚さの酸化チタン層を設けたものも提案されている（特許文献２）。しかし、当該被覆粉体においても、見る角度によって色相を変える効果はやはり小さいものであった。
It is known that the color produced by the light interference has higher brightness than the color of common color pigments such as Bengala and ultramarine blue, but its coloring power is very weak. As a method for improving the coloring power, it has been proposed to coat a metal oxide that absorbs a wavelength in a specific range of visible light, such as iron oxide, on the titanium oxide layer (Patent Document 1). . However, with this method, an effect of enhancing a specific color and an effect of increasing the change in lightness due to gloss can be obtained, but an effect that the hue changes depending on the viewing angle cannot be expected.
On the other hand, there has also been proposed a method in which the surface of mica is first coated with ferric oxide and a titanium oxide layer having a certain thickness is provided thereon (Patent Document 2). However, the effect of changing the hue depending on the viewing angle was also small in the coated powder.
さらに、特許文献３には、薄片状の金属基体上に、屈折率１．８以下の無色の被覆層、次に屈折率２．０以上の選択的に光を吸収する被覆層、更に必要に応じて無色または選択的に光を吸収する被覆層を順次形成してなる光沢顔料が提案されており、前記金属基体としてはアルミニウムまたはその合金、第1層である前記被覆層の物質としてはシリカ、酸化アルミニウム等、第２層である前記被覆層の物質としては酸化鉄、酸化クロム、酸化チタン（ＴｉＯ2のアンモニア還元物等を含む）等が例示されている。また、この明細書中には、当該被覆粉体によれば、見る角度によって色調が異なる効果が挙げられているものの、この光沢顔料は色調変化を強める目的で金属基材を使用しているため、強い金属光沢を有すると記載されている。従って、光沢を押さえた自然な外観を有する化粧料を得ることが困難であり、また隠蔽性も高すぎるという問題点がある。 Further, Patent Document 3 discloses a colorless coating layer having a refractive index of 1.8 or less on a flaky metal substrate, then a coating layer selectively absorbing light having a refractive index of 2.0 or more, and further required. Accordingly, a luster pigment is proposed in which a coating layer that absorbs light or selectively absorbs light in sequence is proposed, and the metal substrate is aluminum or an alloy thereof, and the coating layer material that is the first layer is silica. Examples of the material of the coating layer, which is the second layer, such as aluminum oxide, include iron oxide, chromium oxide, titanium oxide (including ammonia reduction product of TiO 2 ), and the like. In addition, in this specification, according to the coating powder, although the effect that the color tone is different depending on the viewing angle is mentioned, this glossy pigment uses a metal base material for the purpose of enhancing the color tone change. It is described as having a strong metallic luster. Therefore, it is difficult to obtain a cosmetic having a natural appearance with reduced gloss, and there is a problem that the concealing property is too high.
また、上記のような問題点を解決するため、本出願人は、鱗片状基材に少なくとも２つの着色層を積層被覆した複合粉体を開発し、これを出願している（特許文献４）。この複合粉体によれば、見る角度によって色相が変わり、しかも過度の光沢がなく自然な外観を得ることができるものの、２つの着色層を有していることから、実質的に色彩が濃いものであった。従って、ベースメーキャップ化粧料に配合した場合、濃い色彩のファンデーションには配合できるが、薄い色彩のファンデーションへの配合には制約があり、配合量を落とすと、色相、彩度、明度のバランスからなる色彩の調整が可能となるが、所望のカラーフロップ効果が得られないという問題があった。 Further, in order to solve the above-mentioned problems, the present applicant has developed a composite powder in which at least two colored layers are laminated and coated on a scaly substrate, and has applied for this (Patent Document 4). . According to this composite powder, although the hue changes depending on the viewing angle, and it can obtain a natural appearance without excessive gloss, it has two colored layers, so it is substantially dark in color. Met. Therefore, when blended into base makeup cosmetics, it can be blended into a dark-colored foundation, but there are restrictions on blending into a light-colored foundation. Although the color can be adjusted, there is a problem that a desired color flop effect cannot be obtained.
さらに、特許文献５には、内側の雲母の芯、第１の外側の有色顔料層、第２の外側の透明層、および第３の最も外側の有色顔料層の４つの異なる層を有する干渉性のシャドー顔料が提案されており、前記第1層としては酸化鉄を含む赤色顔料層、前記第２層としては透明シリカからなる透明層、前記第３層としては二酸化チタンと酸化鉄を含む黄色顔料層などが例示されている。また、この明細書中には、当該被覆粉体によれば、特定の反射角度で見たときには顔料が黄色に見え、他の反射角度で見たときには赤味を帯びており、全体としてはオレンジ色／茶色を呈し、これをファンデーションに配合して使用した場合は、ほお骨の突起を引き出し又は鼻の外観をほっそりとさせる効果があるものの、上記と同様にこのオレンジ色／茶色の色では他の色彩、例えばピンク色等をつくることが難しいと記載されている。そこで、この問題点を解決するために、該シャドー顔料に標準の有色、または無色の干渉顔料を組み合わせることにより、所望の明から暗に変化する効果を維持しつつ、様々な色彩に調整する方法が提案されている。 Further, Patent Document 5 discloses an interference property having four different layers: an inner mica core, a first outer colored pigment layer, a second outer transparent layer, and a third outermost colored pigment layer. The first layer is a red pigment layer containing iron oxide, the second layer is a transparent layer made of transparent silica, and the third layer is a yellow layer containing titanium dioxide and iron oxide. A pigment layer and the like are illustrated. Further, in this specification, according to the coating powder, the pigment appears yellow when viewed at a specific reflection angle, and is reddish when viewed at other reflection angles, and as a whole is orange. When it is used in a foundation with a color / brown color, it has the effect of pulling out the protrusions of the cheekbones or making the appearance of the nose slender. It is described that it is difficult to produce colors such as pink. Therefore, in order to solve this problem, a method of adjusting to various colors while maintaining the desired effect of changing from light to dark by combining a standard colored or colorless interference pigment with the shadow pigment. Has been proposed.
しかしながら、この発明では、前記シャドー顔料とほぼ同量の標準の干渉顔料を配合せねばならず、経済的でなかった。また、このように干渉性のシャドー顔料と標準の干渉材料を組み合わせた場合、過度の光沢が避けられないという問題があった。
上記のように、特別な制限を受けることなく一種類の材料の配合のみで、見る角度によって色が変わり、しかも過度の光沢がなく自然な外観を得ることができるファンデーション用の材料は未だ知られていないのが現状である。
However, in the present invention, it is necessary to blend the same amount of standard interference pigment as the shadow pigment, which is not economical. In addition, when the interference shadow pigment and the standard interference material are combined in this way, there is a problem that excessive gloss is inevitable.
As mentioned above, there are still no known materials for foundations that can change the color depending on the viewing angle and have a natural appearance without excessive luster, by combining only one kind of material without any special restrictions. The current situation is not.
本発明者らは、上記のような問題点を解決することを目的として鋭意研究を続けたところ、特別な構成からなるカラーフロップ粉体を使用すればよいことを見出し、本発明を完成するに至った。すなわち、本発明は、見る角度によって彩度と明度が変わり、しかもベージュ色の色相を呈し自然な肌の色を得ることのできる非干渉性のカラーフロップ粉体を提供することを目的としている。さらに、本発明は、このカラーフロップ粉体を使用して、顔、その他の立体的な構造を一つの材料で光沢を抑えて自然なつやを付与しながらも、色相の変化なく、彩度と明度の変化により強調することのできる化粧料、特にベースメークアップ用化粧料を提供することを目的としている。
The inventors of the present invention have conducted intensive research for the purpose of solving the above-mentioned problems, and found that a color flop powder having a special configuration may be used to complete the present invention. It came. That is, an object of the present invention is to provide a non-interfering color flop powder that changes in saturation and lightness depending on the viewing angle, and has a beige hue and can obtain a natural skin color. Furthermore, the present invention uses this color flop powder to suppress the luster of the face and other three-dimensional structures with a single material to give natural gloss, but without changing the hue and saturation. An object of the present invention is to provide a cosmetic that can be emphasized by a change in lightness, particularly a cosmetic for base makeup.
本発明によるカラーフロップ粉体は、鱗片状基材の表面に、赤褐色の酸化第二鉄、無彩色の二酸化珪素および無彩色の二酸化チタンを順次積層してなる、ベージュ色の色相を呈する非干渉性の粉体であることを特徴としている。
前記鱗片状基材は、マイカまたは合成マイカであることが好ましい。
また、前記鱗片状基材は、平均粒子径１〜４０μｍおよび平均厚さ０．０５〜１．０μｍの大きさを有することが好ましい。
The color flop powder according to the present invention is a non-interfering material having a beige hue formed by sequentially laminating red-brown ferric oxide, achromatic silicon dioxide, and achromatic titanium dioxide on the surface of a scaly substrate. It is a characteristic powder.
The scaly substrate is preferably mica or synthetic mica.
The scaly substrate preferably has an average particle diameter of 1 to 40 μm and an average thickness of 0.05 to 1.0 μm.
前記カラーフロップ粉体は、前記酸化第二鉄を０．５〜５重量％、前記二酸化珪素２〜３０重量％、前記二酸化チタン５〜３０重量％および前記鱗片状基材をバランスで含むことが好ましい。
前記酸化第二鉄の被覆層は、１０ｎｍ以下であり、しかも必要な着色力を備えた厚さであることが好ましい。
また、前記二酸化珪素の被覆層は、１００ｎｍ以下であり、しかも必要な透過光散乱力を備えた厚さであることが好ましい。
さらに、前記二酸化チタンの被覆層は、４０ｎｍ以下であり、しかも必要な光反射力を備えた厚さであることが好ましい。
The color flop powder may contain 0.5 to 5% by weight of the ferric oxide, 2 to 30% by weight of the silicon dioxide, 5 to 30% by weight of the titanium dioxide, and the scaly substrate in a balance. preferable.
It is preferable that the ferric oxide coating layer has a thickness of 10 nm or less and a necessary coloring power.
The silicon dioxide coating layer preferably has a thickness of 100 nm or less and a necessary transmission light scattering force.
Furthermore, it is preferable that the titanium dioxide coating layer has a thickness of 40 nm or less and a necessary light reflectivity.
本発明によるカラーフロップ粉体は、日本工業規格番号ＪＩＳ Ｚ ８７２９ ５.２ に規定される彩度Ｃ* abが、正反射角付近では２０以下、正反射角より少しずれた拡散反射角付近では２１以上であり、日本工業規格番号ＪＩＳ Ｚ ８７３０ ７．１ に規定される色差△Ｅ* abが１８以上であることを特徴としている。
また、前記カラーフロップ粉体が、正反射角付近に干渉光による発色を呈さず、反射強度が１０〜８０の範囲にあることが好ましい。
一方、本発明による化粧料は、上記のカラーフロップ粉体を配合してなるものであることを特徴としている。
また、前記化粧料は、ベースメークアップ用化粧料であることが好ましい。
The color flop powder according to the present invention has a saturation C * ab specified by Japanese Industrial Standard No. JIS Z 8729 5.2 of 20 or less near the regular reflection angle, and near the diffuse reflection angle slightly deviated from the regular reflection angle. The color difference ΔE * ab specified in Japanese Industrial Standard No. JIS Z 8730 7.1 is 18 or more, and is characterized by 18 or more.
Further, it is preferable that the color flop powder does not exhibit coloration due to interference light in the vicinity of the regular reflection angle and has a reflection intensity in the range of 10-80.
On the other hand, the cosmetic material according to the present invention is characterized by comprising the above-mentioned color flop powder.
Further, the cosmetic is preferably a base makeup cosmetic.
本発明のカラーフロップ粉体によれば、他の顔料などと組み合わせることなくこれ自体で、見る角度によって彩度と明度が変わり、しかもベージュ色の色相を呈し自然な肌の色を得ることができる。
また、本発明による化粧料、特にベースメークアップ用化粧料は、顔、その他の立体的な構造を、一つの材料で光沢を抑えて自然なつやを付与しながらも、色相の変化なく、彩度と明度の変化により強調することができるという利点を有している。
According to the color flop powder of the present invention, it is possible to obtain a natural skin color by changing the saturation and lightness depending on the viewing angle and exhibiting a beige hue without combining with other pigments. .
Further, the cosmetics according to the present invention, especially the cosmetics for base make-up, have a face and other three-dimensional structures with a single material that suppresses gloss and gives natural gloss, but without changing the hue. It has the advantage that it can be emphasized by changes in brightness and brightness.
以下、本発明のカラーフロップ粉体および該カラーフロップ粉体を配合してなる化粧料について具体的に説明する。 Hereinafter, the color flop powder of the present invention and a cosmetic comprising the color flop powder will be specifically described.
〔カラーフロップ粉体〕
本発明によるカラーフロップ粉体は、鱗片状基材の表面に、赤褐色の酸化第二鉄、無彩色の二酸化珪素および無彩色の二酸化チタンを順次積層してなる、ベージュ色の色相を呈する非干渉性の無機酸化物粉体である。
本発明で使用される鱗片状基材としては、特に制限されるものではないが、マイカ、タルク、セリサイト等の天然鉱物や、合成マイカ、合成セリサイト、板状シリカ、板状酸化アルミニウム、板状酸化チタン等の合成物である無機酸化物が挙げられる。この中でも、マイカまたは合成マイカを使用することが好ましい。
[Color flop powder]
The color flop powder according to the present invention is a non-interfering material having a beige hue formed by sequentially laminating red-brown ferric oxide, achromatic silicon dioxide, and achromatic titanium dioxide on the surface of a scaly substrate. Inorganic oxide powder.
The scale-like substrate used in the present invention is not particularly limited, but natural minerals such as mica, talc, sericite, synthetic mica, synthetic sericite, plate-like silica, plate-like aluminum oxide, An inorganic oxide which is a synthetic material such as plate-like titanium oxide can be used. Among these, it is preferable to use mica or synthetic mica.
前記鱗片状基材の大きさは、平均粒子径が概ね１〜４０μｍ、好ましくは５〜３０μｍであることが望ましい。
前記平均粒子径が１μｍ未満では、得られるカラーフロップ粉体の粒子径が小さすぎて、所望のカラーフロップ性が得られ難く、また前記平均粒子径が４０μｍを超えると、得られるカラーフロップ粉体の光沢が強すぎてギラついた外観となることがあるので、好ましくない。
さらに、前記鱗片状基材の平均厚さは０．０５〜１μｍ、好ましくは０．１〜０．５μｍであることが望ましい。ここで、前記鱗片状基材の平均厚さが０．０５μｍ未満では、延展性が低下する他、嵩高くなって、吸油量が大幅に増加することになり、また前記平均厚さが１μｍを超えると、延展性が低下するので好ましくない。
The scale-like base material has an average particle diameter of approximately 1 to 40 μm, preferably 5 to 30 μm.
If the average particle size is less than 1 μm, the particle size of the obtained color flop powder is too small, and it is difficult to obtain the desired color flop property. If the average particle size exceeds 40 μm, the resulting color flop powder is obtained. Since the gloss of the film is too strong, it may have a glaring appearance.
Furthermore, the average thickness of the scaly substrate is 0.05 to 1 μm, preferably 0.1 to 0.5 μm. Here, if the average thickness of the scaly substrate is less than 0.05 μm, the spreadability is lowered, and the bulkiness is increased, so that the amount of oil absorption is greatly increased, and the average thickness is 1 μm. Exceeding this is not preferable because the spreadability is lowered.
本発明で使用される酸化第二鉄は、化学式Ｆe 2Ｏ3で表され、前記鱗片状基材の上部に赤褐色の着色層を形成するために使用される。また、前記酸化第二鉄としては、α−Ｆe 2Ｏ3またはγ−Ｆe 2Ｏ3を使用することが好ましい。
前記鱗片状基材の表面に被覆される前記酸化第二鉄は、得られるカラーフロップ粉体に対し０．５〜５重量％、好ましくは１〜３重量％の範囲で含まれていることが好ましい。
ここで、前記含有量が０．５重量％未満では、着色力が不充分となり、所望のカラーフロップ性が得られないことがある。一方、前記含有量が５重量％を超えると、粉体自体の色彩が濃すぎることとなり、通常のファンデーションのシェード中で特に彩度が低い色彩に調整できないことがあるので好ましくない。
The ferric oxide used in the present invention is represented by the chemical formula Fe 2 O 3 and is used to form a reddish brown colored layer on the scale-like substrate. Further, as the ferric oxide, it is preferable to use the α-Fe 2 O 3 or γ-Fe 2 O 3.
The ferric oxide coated on the surface of the scaly substrate is contained in an amount of 0.5 to 5% by weight, preferably 1 to 3% by weight, based on the obtained color flop powder. preferable.
Here, if the content is less than 0.5% by weight, the coloring power becomes insufficient, and the desired color flop property may not be obtained. On the other hand, if the content exceeds 5% by weight, the color of the powder itself will be too dark, and it may not be possible to adjust to a color with particularly low saturation in the shade of a normal foundation.
また、前記酸化第二鉄の被覆層の厚さは、１０ｎｍ以下、好ましくは１〜５ｎｍの範囲とすることが望ましい。
ここで、前記被覆層の厚さが１０ｎｍを超えると、赤みが強くなりすぎる他、有色の干渉光が発現することがある。この干渉光が発現すると、特に正反射光域での酸化第二鉄層の赤褐色が変化してベージュ色の色相を呈さなくなるので好ましくない。すなわち、前記干渉光が赤色の場合は、酸化第二鉄層の赤褐色が増幅されて、赤みが強くなりすぎることになり、また前記干渉光が緑色の場合は、赤みを打ち消しあって、赤みが低くなりすぎることになり、また前記干渉光が青色、黄色の場合は、色相がそれぞれ紫色、オレンジ色に変化することになる。さらに、このような粉体を配合した化粧料を塗った肌は、不自然に見えることがある。
一方、前記被覆層の厚さの下限値については、測定限界を超えているためこれを正確に規定することはできないが、少なくとも１ｎｍ未満の厚さでは、着色力が低下して、所望のカラーフロップ性が得られない他、ベージュ色の色相を呈さなくなるため、前記酸化第二鉄による効果（所謂、着色力）を期待することは難しいものと察せられる。
The ferric oxide coating layer has a thickness of 10 nm or less, preferably 1 to 5 nm.
Here, when the thickness of the coating layer exceeds 10 nm, reddishness becomes too strong and colored interference light may appear. When this interference light appears, the reddish brown color of the ferric oxide layer in the specular reflection light region changes and does not exhibit a beige hue, which is not preferable. That is, when the interference light is red, the reddish brown color of the ferric oxide layer is amplified and the redness becomes too strong. When the interference light is green, the redness is canceled and redness is lost. If the interference light is blue or yellow, the hue changes to purple or orange, respectively. Furthermore, skin coated with a cosmetic containing such a powder may appear unnatural.
On the other hand, the lower limit value of the thickness of the coating layer cannot be accurately defined because it exceeds the measurement limit. However, if the thickness is less than 1 nm, the coloring power is reduced and the desired color is reduced. In addition to not being able to obtain flop, it is considered difficult to expect the effect (so-called coloring power) by the ferric oxide because it does not exhibit a beige hue.
本発明で使用される二酸化珪素は、化学式ＳｉＯ2で表され、前記酸化第二鉄の被覆層の上部に透明な透過光散乱層（無彩色層）を形成するために使用される。
前記透過光散乱層は、以下に述べる二酸化チタンの被覆層を透過した光が、該透過光散乱層を透過する際にその透過光を散乱させ、さらに上記で述べた酸化第二鉄の被覆層で反射された光が再び該透過光散乱層を透過する際にその透過光を散乱させるための機能を有している。
Silicon dioxide used in the present invention is represented by the chemical formula SiO 2 and is used to form a transparent transmitted light scattering layer (achromatic layer) on the ferric oxide coating layer.
The transmitted light scattering layer scatters the transmitted light when the light transmitted through the titanium dioxide coating layer described below passes through the transmitted light scattering layer, and the ferric oxide coating layer described above. When the light reflected by the light passes through the transmitted light scattering layer again, it has a function of scattering the transmitted light.
前記酸化第二鉄の被覆層の上部に被覆される二酸化珪素は、得られるカラーフロップ粉体に対し２〜３０重量％、好ましくは５〜２０重量％の範囲で含まれていることが好ましい。
ここで、前記含有量が２重量％未満では、透過光散乱層を透過する際の散乱が不充分となり、色相の変化が小さくなる他、下層の酸化第二鉄と上層の二酸化チタンが固溶体のチタン鉄化合物を形成し、色相がより黄色味に変化することによりベージュ色の色相を呈さなくなり、また前記含有量が３０重量％を超えると、粉体自体の厚さが増して延展性が低下することがある。
Silicon dioxide coated on the ferric oxide coating layer is preferably contained in an amount of 2 to 30% by weight, preferably 5 to 20% by weight, based on the color flop powder obtained.
Here, if the content is less than 2% by weight, scattering during transmission through the transmitted light scattering layer becomes insufficient, and the change in hue becomes small. In addition, the lower ferric oxide and the upper titanium dioxide are solid solutions. Forms a titanium-iron compound and the hue changes to a yellowish color so that it does not exhibit a beige hue. If the content exceeds 30% by weight, the thickness of the powder itself increases and the spreadability decreases. There are things to do.
また、前記二酸化珪素の被覆層の厚さは、１００ｎｍ以下、好ましくは３〜２０ｎｍの範囲とすることが望ましい。ここで、前記被覆層の厚さが１００ｎｍを超えると、この粉体を配合した化粧料を塗った肌の感触が低下することがあるので好ましくない。
一方、前記被覆層の厚さの下限値については、測定限界を超えているためこれを正確に規定することはできないが、少なくとも３ｎｍ未満の厚さでは、光がこの層を透過する際の散乱が不充分となって、彩度の変化が小さくなるため、前記二酸化珪素による効果（所謂、透過光散乱力）を期待することは難しいものと察せられる。
The thickness of the silicon dioxide coating layer is 100 nm or less, preferably 3 to 20 nm. Here, when the thickness of the coating layer exceeds 100 nm, it is not preferable because the feel of the skin coated with the cosmetic containing the powder may be lowered.
On the other hand, the lower limit value of the thickness of the coating layer cannot be accurately defined because it exceeds the measurement limit. However, when the thickness is less than 3 nm, the scattering of light passing through this layer is not possible. Is insufficient, and the change in saturation is small, so it is difficult to expect the effect of silicon dioxide (so-called transmitted light scattering force).
本発明で使用される二酸化チタンは、化学式ＴｉＯ2で表され、前記二酸化珪素の被覆層の上部に非干渉性の光反射層（無彩色層）を形成するために使用される。また、前記二酸化チタンとしては、アナターゼ型またはルチル型の結晶性酸化チタンを使用することが好ましい。
前記二酸化珪素の表面に被覆される前記二酸化チタンは、得られるカラーフロップ粉体に対し５〜３０重量％、好ましくは１０〜２０重量％の範囲で含まれていることが望ましい。
ここで、前記含有量が５重量％未満では、反射率が低下して、所望のカラーフロップ性が得られない他、適度なつやを付与できなくなることがある。一方、前記含有量が３０重量％を超えると、逆に反射率が高くなりすぎて、ぎらぎらした外観となる他、隠蔽性が高くなりすぎることとなる。
Titanium dioxide used in the present invention is represented by the chemical formula TiO 2 and is used to form an incoherent light reflecting layer (achromatic layer) on the silicon dioxide coating layer. As the titanium dioxide, it is preferable to use anatase type or rutile type crystalline titanium oxide.
The titanium dioxide coated on the surface of the silicon dioxide is desirably contained in an amount of 5 to 30% by weight, preferably 10 to 20% by weight, based on the obtained color flop powder.
Here, when the content is less than 5% by weight, the reflectance is lowered, and a desired color flop property may not be obtained, and an appropriate gloss may not be imparted. On the other hand, if the content exceeds 30% by weight, conversely, the reflectivity becomes too high, resulting in a gritty appearance, and the concealability becomes too high.
また、前記二酸化チタンの被覆層の厚さは、４０ｎｍ以下、好ましくは５〜３０ｎｍの範囲とすることが望ましい。
ここで、前記被覆層の厚さが４０ｎｍを超えると、有色の干渉光が発現することがある。この干渉光が発現すると、特に正反射域で無彩色を呈さなくなるので好ましくない。すなわち、前記干渉光が赤色、黄色の場合は、酸化第二鉄層の赤褐色とのコントラストが低下し、カラーフロップ性が低下することになり、また前記干渉光が緑色、青色の場合は、赤味、黄色味を打ち消しあうため、この粉体を配合した化粧料を塗った肌が不自然に見えることがある。
一方、前記被覆層の厚さの下限値については、測定限界を超えているためこれを正確に規定することはできないが、少なくとも５ｎｍ未満の厚さでは、反射率が低下して、所望のカラーフロップ性が得られない他、適度なつやを付与できなくなるため、前記二酸化チタンによる効果（所謂、光反射力）を期待することは難しいものと察せられる。
The thickness of the titanium dioxide coating layer is 40 nm or less, preferably 5 to 30 nm.
Here, when the thickness of the coating layer exceeds 40 nm, colored interference light may appear. When this interference light appears, an achromatic color is not exhibited particularly in the regular reflection region, which is not preferable. That is, when the interference light is red or yellow, the contrast with the reddish brown color of the ferric oxide layer is lowered, and the color flop property is lowered. When the interference light is green or blue, the contrast is red. In order to counteract the taste and yellowness, the skin coated with a cosmetic containing this powder may appear unnatural.
On the other hand, the lower limit value of the thickness of the coating layer exceeds the measurement limit and cannot be accurately defined. However, if the thickness is less than 5 nm, the reflectance decreases and the desired color is reduced. In addition to not being able to obtain a flop property, it becomes impossible to provide an appropriate gloss, and therefore it is difficult to expect the effect of titanium dioxide (so-called light reflectivity).
このようにして、鱗片状基材の表面に、赤褐色の酸化第二鉄、無彩色の二酸化珪素および無彩色の二酸化チタンを順次積層してなる、本発明のカラーフロップ粉体は、鱗片状基材と同様に鱗片状の形状を有している。
本発明でいう鱗片状基材とは、板状、薄片状、うろこ状などの形状を有する粉体粒子（以下、単に「粒子」という場合がある）を意味し、本発明のカラーフロップ粉体も同様な形状を有する粉体粒子（これについても同様に、単に「粒子」という場合がある）である。しかし、前記鱗片状基材および前記カラーフロップ粉体は、本発明の明細書中に規定される平均粒子径および平均厚さを有していることが望まれる。
Thus, the color flop powder of the present invention, in which red-brown ferric oxide, achromatic silicon dioxide, and achromatic titanium dioxide are sequentially laminated on the surface of the flaky substrate, has a flaky substrate. Like the material, it has a scaly shape.
The scale-like base material as used in the present invention means powder particles having a plate shape, a flake shape, a scaly shape, or the like (hereinafter sometimes simply referred to as “particles”), and the color flop powder of the present invention. Are powder particles having the same shape (also referred to simply as “particles”). However, it is desirable that the scale-like substrate and the color flop powder have an average particle diameter and an average thickness as defined in the specification of the present invention.
前記カラーフロップ粉体の平均粒子径は、５〜４０μｍ、好ましくは１０〜３０μｍの範囲にあることが望ましい。
ここで、前記粉体の平均粒子径が５μｍ未満では、この粉体を配合した化粧料を塗った肌の感触が不良となることがある。一方、前記平均粒子径が４０μｍを超えると、光沢が強過ぎてギラついた外観となって好ましくない。特に、平均粒子径が１０〜３０μｍの範囲にあるカラーフロップ粉体を配合すれば、延展性に優れた感触の良い化粧料が得られる。
また、前記カラーフロップ粉体の平均厚さは、前記鱗片状基材の厚さと前記被覆層の厚さに依存するが、０．０５〜１μｍの範囲にあることが好ましい。
The average particle size of the color flop powder is desirably 5 to 40 μm, preferably 10 to 30 μm.
Here, if the average particle size of the powder is less than 5 μm, the skin feel may be poor when a cosmetic containing the powder is applied. On the other hand, if the average particle diameter exceeds 40 μm, the gloss is too strong and the appearance is glaring. In particular, if a color flop powder having an average particle size in the range of 10 to 30 μm is blended, a cosmetic with excellent spreadability and good touch can be obtained.
Moreover, although the average thickness of the said color flop powder is dependent on the thickness of the said scale-like base material, and the thickness of the said coating layer, it is preferable to exist in the range of 0.05-1 micrometer.
本発明によるカラーフロップ粉体は、日本工業規格番号ＪＩＳ Ｚ ８７２９ ５.２ に規定される彩度Ｃ* abが、正反射角付近では２０以下、好ましくは１０〜２０の範囲、正反射角より少しずれた拡散反射角付近では２１以上、好ましくは３０以上であり、日本工業規格番号ＪＩＳ Ｚ ８７３０ ７．１に規定される色差△Ｅ* abが１８以上、好ましくは２２以上であることが望まれる。
ここで、前記正反射角付近の彩度Ｃ* abが２０を超えると、粉体自体の彩度が濃すぎることとなり、通常のファンデーションのシェード中で特に彩度が低い色彩に調整できなくなることがある。一方、前記正反射角付近の彩度Ｃ* abが１０未満では、粉体自体の彩度が薄いことから、所望のカラーフロップ性が得られなくなることがある。また前記正反射角より少しずれた拡散反射角付近の彩度Ｃ* abが上記の範囲外であると、カラーフロップ性が低下して、所望の効果が得られなくなる。また、前記色差△Ｅ* abが１８未満では、上記と同様に、カラーフロップ性が低下して、所望の効果が得られなくなる。
In the color flop powder according to the present invention, the saturation C * ab specified in Japanese Industrial Standard No. JIS Z 8729 5.2 has a specular reflection angle of 20 or less, preferably in the range of 10 to 20, from the specular reflection angle. It is 21 or more, preferably 30 or more in the vicinity of a slightly different diffuse reflection angle, and the color difference ΔE * ab defined in Japanese Industrial Standard No. JIS Z 8730 7.1 is 18 or more, preferably 22 or more. It is.
Here, if the saturation C * ab near the specular reflection angle exceeds 20, the saturation of the powder itself is too dark, and it becomes impossible to adjust to a color with particularly low saturation in the shade of a normal foundation. There is. On the other hand, if the saturation C * ab near the regular reflection angle is less than 10, the powder itself has a low saturation, so that a desired color flop property may not be obtained. On the other hand, if the saturation C * ab near the diffuse reflection angle slightly deviated from the regular reflection angle is outside the above range, the color flop property is lowered and the desired effect cannot be obtained. On the other hand, if the color difference ΔE * ab is less than 18, the color flop property is lowered as described above, and a desired effect cannot be obtained.
さらに、前記カラーフロップ粉体は、日本工業規格番号ＪＩＳ Ｚ ８７２９ ５．３に規定される色相角ｈabが、正反射角付近では５６°〜９６°、好ましくは６６°〜８６°であり、正反射角より少しずれた拡散反射角付近の色相角ｈabとの色相角差△ｈabが−１０°〜１０°、好ましくは−５°〜５°であることが望ましい。
ここで、前記正反射角付近の色相角ｈabが上記の範囲外であると、ベージュ色を呈さないこととなり、また前記色相角差△ｈabが上記の範囲外であると、色相が変わって見えることから、この粉体を配合した化粧料を塗った肌が不自然に見えることがある。
Further, the color flop powder, hue angle h ab which is defined in Japanese Industrial Standard No. JIS Z 8729 5.3 is, 56 ° to 96 ° in the vicinity of the regular reflection angle, preferably 66 ° -86 °, hue angle difference between the hue angle h ab near diffuse reflection angle slightly deviated from the regular reflection angle △ h ab is -10 ° to 10 °, it is desirable that preferably -5 ° to 5 °.
Here, if the hue angle hab near the regular reflection angle is out of the above range, a beige color is not exhibited, and if the hue angle difference Δhab is out of the above range, the hue changes. Therefore, the skin coated with a cosmetic containing this powder may appear unnatural.
また、前記カラーフロップ粉体は、正反射角付近に干渉光による発色を呈さず、反射強度が１０〜８０、好ましくは２０〜６０であることが望ましい。
ここで、前記反射強度が８０を超えると、過度の光沢があり、この粉体を配合した化粧料を塗った肌が不自然に見えることがある。また、前記反射強度が１０未満では、光沢が低すぎて、この粉体を配合した化粧料を塗った肌に程度な艶を付与できないことがある。
Further, it is desirable that the color flop powder does not exhibit coloration due to interference light near the regular reflection angle and has a reflection intensity of 10 to 80, preferably 20 to 60.
Here, when the reflection intensity exceeds 80, there is excessive gloss, and the skin coated with a cosmetic containing this powder may appear unnatural. On the other hand, if the reflection intensity is less than 10, the gloss is too low, and the skin coated with the cosmetic containing this powder may not be given a moderate gloss.
前記彩度Ｃ* abおよび前記色差△Ｅ* ab、ならびに前記色相角差△ｈabは、前記粉体３ｇをニトロセルロースラッカー（遠藤化学工業所製）１２ｇによく分散させ塗料化し、バーコーターＮｏ．１８を用いて白色の隠蔽率試験紙に塗付して調製した塗膜を、Ｄ６５／２の光源を持ち、煽り角を１０°に設定した三次元変角分光光度計（村上色彩技術研究所製、ＧＣＭＳ−４）を用いて、入射角０゜の条件にて受光角１０゜での正反射角付近の反射光（以下、単に「正反射光」という場合がある。）と４５゜での拡散反射光のＬ*、ａ*、ｂ*の変化を測定し、その結果を次式に入力することによって求められる。
Ｃ* ab＝［（ａ*）2 ＋（ｂ*）2］1/2
△Ｅ* ab＝［（△Ｌ*）2 ＋（△ａ*）2 ＋（△ｂ*）2］1/2
ｈab＝ｔａｎ-1（ｂ*／ａ*）
△ｈab＝（ｈab45°−ｈab10°）
The saturation C * ab, the color difference ΔE * ab , and the hue angle difference Δh ab are obtained by dispersing 3 g of the powder in 12 g of nitrocellulose lacquer (manufactured by Endo Chemical Co., Ltd.) to obtain a paint. . A three-dimensional variable angle spectrophotometer (Murakami Color Research Laboratory) with a D65 / 2 light source and a tilt angle set to 10 °. Using GCMS-4), the reflected light near the regular reflection angle at a light receiving angle of 10 ° under the condition of an incident angle of 0 ° (hereinafter sometimes simply referred to as “regular reflected light”) and 45 °. Is measured by measuring changes in L * , a * , and b * of the diffusely reflected light and inputting the result into the following equation.
C * ab = [(a * ) 2 + (b * ) 2 ] 1/2
ΔE * ab = [(ΔL * ) 2 + (Δa * ) 2 + (Δb * ) 2 ] 1/2
h ab = tan −1 (b * / a * )
△ h ab = (h ab45 ° -h ab10 °)
本発明でいう反射強度とは、前記粉体３ｇをニトロセルロースラッカー（遠藤化学工業所製）１２ｇによく分散させ塗料化し、バーコーターＮｏ．１８を用いて黒色の隠蔽率試験紙に塗付して調製した塗膜を、Ｄ６５／２の光源を持ち、煽り角を０°に設定した三次元変角光度計（村上色彩技術研究所製、ＧＰ−２００）を用いて、入射角０゜の条件にて受光角５゜での正反射角付近の反射光（以下、単に「正反射光」という場合がある。）を測定した反射強度をいう。 In the present invention, the reflection intensity means that 3 g of the above powder is well dispersed in 12 g of nitrocellulose lacquer (manufactured by Endo Chemical Industries) to form a paint. A three-dimensional goniophotometer (manufactured by Murakami Color Research Laboratory) with a D65 / 2 light source and a tilt angle set to 0 ° was prepared by applying a black concealment rate test paper using 18 , GP-200), the reflection intensity measured in the vicinity of the regular reflection angle (hereinafter sometimes referred to simply as “regular reflection light”) at a light receiving angle of 5 ° under the condition of an incident angle of 0 °. Say.
また、正反射角付近の干渉光による発色の有無は、黒色の隠蔽率試験紙に貼った平滑性の高い透明両面テープの粘着面に前記粉体を塗布した試料を、Ｄ６５／２の光源を持ち、煽り角を１０°に設定した三次元変角分光光度計（村上色彩技術研究所製、ＧＣＭＳ−４）を用いて、入射角−４５゜、受光角４５゜の条件にて、３８０ｎｍから７６０ｎｍの波長における反射率を測定し、有色の干渉光に由来する反射率のおおきなうねりの有無にて確認することができる。すなわち、有色の干渉光を発するものは、特定波長の吸収と反射が起こることから、大きくループしたプロットを辿り、一方、無彩色の場合は、当該波長の吸収と反射が起こらないことから、フラットなプロットを辿るので、その有無を判断することができる。
In addition, the presence or absence of coloring due to interference light near the specular reflection angle was determined by using a sample obtained by applying the powder on the adhesive surface of a transparent smooth double-sided tape affixed to a black concealment rate test paper, and using a D65 / 2 light source. Using a three-dimensional variable angle spectrophotometer (GCMS-4, manufactured by Murakami Color Research Laboratory) with a tilt angle set to 10 °, from 380 nm under the conditions of an incident angle of −45 ° and a light receiving angle of 45 ° The reflectance at a wavelength of 760 nm can be measured and confirmed by the presence or absence of a significant swell of the reflectance derived from colored interference light. In other words, those that emit colored interference light follow a largely looped plot because absorption and reflection at a specific wavelength occur, while in the case of an achromatic color, absorption and reflection at that wavelength do not occur. Since a simple plot is traced, the presence or absence can be determined.
〔カラーフロップ粉体の調製〕
以下、本発明のカラーフロップ粉体の調製方法について具体的に説明する。
酸化第二鉄被覆層の形成
鱗片状基材の表面に、酸化第二鉄の被覆層を形成する方法としては、従来公知の被膜形成方法を採用することができる。その方法の事例を簡単に述べれば、以下の通りである。
ａ）鱗片状基材の分散液（溶媒は水および／または有機溶媒）に、酸化第二鉄の前駆物質である塩化第二鉄、硝酸第二鉄、硫酸第二鉄等の鉄塩をアルカリで中和して基材上に析出させる方法。
ｂ）鱗片状基材の分散液（溶媒は水および／または有機溶媒）に、トリエトキシアイアン、トリブトキシアイアン等の有機鉄化合物、またはこれらの部分加水分解物を所定量添加し、必要に応じて加水分解用触媒の存在下で加水分解さらには縮重合し、加水分解・縮重合物を基材上に析出させる方法。
[Preparation of color flop powder]
Hereafter, the preparation method of the color flop powder of this invention is demonstrated concretely.
Formation of Ferric Oxide Coating Layer As a method for forming a ferric oxide coating layer on the surface of the scaly substrate, a conventionally known coating formation method can be employed. An example of the method is briefly described as follows.
a) An iron salt such as ferric chloride, ferric nitrate, ferric sulfate, or the like, which is a ferric oxide precursor, is alkalinized in a dispersion of a scaly substrate (the solvent is water and / or an organic solvent). A method of neutralizing and precipitating on the substrate.
b) A predetermined amount of an organic iron compound such as triethoxy iron or tributoxy iron, or a partial hydrolyzate thereof is added to a dispersion of a scaly base material (the solvent is water and / or an organic solvent), and if necessary In this method, hydrolysis and condensation polymerization are carried out in the presence of a hydrolysis catalyst, and the hydrolysis / condensation polymer is precipitated on the substrate.
二酸化珪素被覆層の形成
前記酸化第二鉄の被覆層の上部（表面）に二酸化珪素の被覆層を形成する方法としては、従来公知の被膜形成方法を採用することができる。その方法の事例を簡単に述べれば、以下の通りである。
ａ）上記の方法で酸化第二鉄を被覆した鱗片状基材の分散液（溶媒は水および／または有機溶媒）に、二酸化珪素層の前駆物質である四塩化珪素等の珪素塩、珪酸ナトリウム等の珪酸塩、珪酸液等の珪酸をアルカリ、または酸で中和して基材上に析出させる方法。
ｂ）上記の方法で酸化第二鉄を被覆した鱗片状基材の分散液（溶媒は水および／または有機溶媒）に、テトラメトキシシラン、テトラエトキシシラン等の有機系素化合物、またはこれらの部分加水分解物を所定量添加し、必要に応じて加水分解用触媒の存在下で加水分解さらには縮重合し、加水分解・縮重合物を前記酸化第二鉄被覆層の上部に析出させる方法。
Formation of Silicon Dioxide Coating Layer As a method of forming a silicon dioxide coating layer on the upper part (surface) of the ferric oxide coating layer, a conventionally known coating film forming method can be employed. An example of the method is briefly described as follows.
a) A dispersion of a scaly substrate coated with ferric oxide by the above method (the solvent is water and / or an organic solvent), a silicon salt such as silicon tetrachloride as a precursor of the silicon dioxide layer, sodium silicate A method of neutralizing silicic acid such as silicate and silicic acid solution with an alkali or acid and depositing on the substrate.
b) A dispersion of a scaly substrate coated with ferric oxide by the above method (the solvent is water and / or an organic solvent), an organic elemental compound such as tetramethoxysilane or tetraethoxysilane, or a portion thereof. A method in which a predetermined amount of a hydrolyzate is added, and if necessary, hydrolysis and condensation polymerization are performed in the presence of a hydrolysis catalyst, and the hydrolysis / condensation polymer is deposited on the ferric oxide coating layer.
二酸化チタン被覆層の形成
前記二酸化珪素の被覆層の上部（表面）に二酸化チタンの被覆層を形成する方法としては、従来公知の被膜形成方法を採用することができる。その方法の事例を簡単に述べれば、以下の通りである。
ａ）上記の方法で酸化第二鉄および二酸化珪素を被覆した鱗片状基材の分散液（溶媒は水および／または有機溶媒）に、二酸化チタン層の前駆物質である四塩化チタン、硫酸チタン等のチタン塩、ペルオキソチタン酸等の過酸化物をアルカリ、または酸で中和して基材上に析出させる方法。
ｂ）上記の方法で酸化第二鉄および二酸化珪素を被覆した鱗片状基材の分散液（溶媒は水および／または有機溶媒）に、テトライソプロポキシチタン、テトラブトキシチタン等の有機チタン化合物またはこれらの部分加水分解物を所定量添加し、必要に応じて加水分解用触媒の存在下で加水分解さらには縮重合し、加水分解・縮重合物を前記二酸化珪素被覆層の上部に析出させる方法。
Formation of Titanium Dioxide Coating Layer As a method for forming a titanium dioxide coating layer on the upper surface (surface) of the silicon dioxide coating layer, a conventionally known coating film forming method can be employed. An example of the method is briefly described as follows.
a) A dispersion of a scaly substrate coated with ferric oxide and silicon dioxide by the above method (the solvent is water and / or an organic solvent), titanium tetrachloride, titanium sulfate, etc., which are precursors of the titanium dioxide layer A method in which a peroxide such as titanium salt or peroxotitanic acid is neutralized with an alkali or acid and deposited on a substrate.
b) An organic titanium compound such as tetraisopropoxy titanium or tetrabutoxy titanium or a dispersion of a scaly base material coated with ferric oxide and silicon dioxide by the above method (the solvent is water and / or an organic solvent) A method in which a predetermined amount of the partial hydrolyzate is added and, if necessary, hydrolysis and condensation polymerization are performed in the presence of a hydrolysis catalyst, and the hydrolysis / condensation polymerization product is deposited on the silicon dioxide coating layer.
〔化粧料〕
以下に、本発明に係る化粧料、特にベースメークアップ用化粧料について具体的に説明する。
本発明によるベースメークアップ用化粧料は、本発明に係る前記カラーフロップ粉体と、以下に述べる各種化粧料成分とを配合して得られるものである。
前記カラーフロップ粉体の配合量は、調製すべき化粧料の種類や配合すべき化粧料成分等によっても異なるが、前記化粧料に対し１〜５０重量％、好ましくは５〜４０重量％の範囲にあることが望ましい。
ここで、前記配合量が１重量％未満では、顔などの被塗布体に対する外観上の効果が得られなくなる。すなわち、本発明に係る化粧料によれば、見る角度によって彩度と明度が変わり、しかもベージュ色の色相を呈することから、違和感なく顔等の立体感を強調することができるが、前記配合量が１重量％未満では、このような効果は得られない。一方、前記配合量が５０重量％を越えると、本来、ベースメークアップ用化粧料に求められるその他の重要な機能、例えば、隠蔽性、光散乱性、透明性、感触、紫外線防御機能、化粧もち等を付与する各種化粧料成分を配合できる比率が低下し、トータルバランスの取れた商品設計が困難となることから好ましくない。
[Cosmetics]
Hereinafter, the cosmetic according to the present invention, particularly the cosmetic for base makeup, will be described in detail.
The base makeup cosmetic according to the present invention is obtained by blending the color flop powder according to the present invention and various cosmetic ingredients described below.
The blending amount of the color flop powder varies depending on the type of cosmetic to be prepared, the cosmetic ingredients to be blended, etc., but is in the range of 1 to 50% by weight, preferably 5 to 40% by weight with respect to the cosmetic. It is desirable to be in
Here, when the blending amount is less than 1% by weight, an effect on the appearance to the coated body such as the face cannot be obtained. That is, according to the cosmetic according to the present invention, the saturation and lightness change depending on the viewing angle, and also exhibits a beige hue, so that the three-dimensional effect such as the face can be emphasized without a sense of incongruity. If it is less than 1% by weight, such an effect cannot be obtained. On the other hand, if the blending amount exceeds 50% by weight, other important functions originally required for base makeup cosmetics such as concealment, light scattering, transparency, touch, UV protection, The ratio at which various cosmetic ingredients imparting the like can be blended is lowered, which makes it difficult to design a product with a total balance.
前記の各種化粧料成分としては、例えば、高級脂肪族アルコール、高級脂肪酸、エステル油、パラフィン油、ワックス等の油分、エチルアルコール、プロピレングリコール、ソルビトール、グリセリンなどのアルコール類、ムコ多糖類、コラーゲン類、ＰＣＡ塩、乳酸塩などの保湿剤、ノニオン系、カチオン系、アニオン系または両性の各種界面活性剤、アラビアガム、キサンタンガム、ポリビニルピロリドン、エチルセルローズ、カルボキシメチルセルローズ、カルボキシビニルポリマー、変性又は未変性の粘土鉱物などの増粘剤、酢酸エチル、アセトン、トルエンなどの溶剤、無機顔料、有機顔料、有機染料、ＢＨＴ、トコフェロールなどの酸化防止剤、水、薬剤、紫外線吸収剤、ｐＨ緩衝剤、キレート化剤、防腐剤、香料などが挙げられる。 Examples of the various cosmetic ingredients include oils such as higher fatty alcohols, higher fatty acids, ester oils, paraffin oils, waxes, alcohols such as ethyl alcohol, propylene glycol, sorbitol, glycerin, mucopolysaccharides, collagens, and the like. , Moisturizers such as PCA salt and lactate, nonionic, cationic, anionic or amphoteric surfactants, gum arabic, xanthan gum, polyvinylpyrrolidone, ethyl cellulose, carboxymethyl cellulose, carboxyvinyl polymer, modified or unmodified Thickeners such as clay minerals, solvents such as ethyl acetate, acetone, toluene, inorganic pigments, organic pigments, organic dyes, antioxidants such as BHT, tocopherol, water, chemicals, UV absorbers, pH buffering agents, chelates Agent, preservative, fragrance, etc. That.
また、本発明に係るベースメークアップ用化粧料には、シリカ、タルク、カオリン、マイカなどの無機系充填剤、体質顔料、各種有機樹脂等から選ばれた物質を一種類以上を含んでいてもよい。
さらに、前記化粧料に配合される前記カラーフロップ粉体は、その表面をシリコーンやフッ素化合物等で予め処理しておいてもよい。
なお、本発明のベースメークアップ用化粧料は、従来公知の方法で製造することができる。このようにして製造された化粧料は、粉末状、ケーキ状、液状、クリーム状などの各種形態で使用され、さらに具体的に述べれば、パウダーファンデーション、リキッドファンデーション、クリームファンデーション、ムースファンデーションなどが挙げられる。
しかし、本発明のカラーフロップ粉体は、その他の化粧料、例えばアイシャドウ、アイライナー、マスカラ、口紅、リップグロス、ネイルエナメル等のポイントメークアップ化粧料、ローション、乳液、クリーム、化粧下地等のスキンケア化粧料にも好適に使用することができる。
Further, the base makeup cosmetic according to the present invention may contain one or more substances selected from inorganic fillers such as silica, talc, kaolin and mica, extender pigments and various organic resins. Good.
Furthermore, the surface of the color flop powder blended in the cosmetic may be pretreated with silicone, a fluorine compound, or the like.
The base makeup cosmetic of the present invention can be produced by a conventionally known method. The cosmetics thus produced are used in various forms such as powder, cake, liquid, and cream, and more specifically, powder foundation, liquid foundation, cream foundation, mousse foundation, etc. It is done.
However, the color flop powder of the present invention can be used for other cosmetics such as eye shadow, eyeliner, mascara, lipstick, lip gloss, nail enamel and other makeup products, lotions, emulsions, creams, makeup bases, etc. It can also be suitably used for skin care cosmetics.
〔測定方法〕
次に、本発明の実施例その他で採用された測定方法を具体的に述べれば、以下の通りである。
（１）鱗片状基材およびカラーフロップ粉体の平均粒子径
前記鱗片状基材または前記カラーフロップ粉体の試料をレーザー回折・散乱式粒度分布測定装置（堀場製作所製ＬＡ―３００）にかけて、その平均粒子径を測定した。
（２）鱗片状基材およびカラーフロップ粉体の厚さ
前記鱗片状基材または前記カラーフロップ粉体の試料から選ばれた１００個の粒子を走査型電子顕微鏡（日立製作所製S-5200N）を用いて写真撮影し、その厚さの平均値を測定した。
〔Measuring method〕
Next, the measurement methods employed in the examples and others of the present invention will be specifically described as follows.
(1) Average particle diameter of scaly base material and color flop powder A sample of the scaly base material or the color flop powder was subjected to a laser diffraction / scattering type particle size distribution measuring device (LA-300 manufactured by Horiba, Ltd.). The average particle size was measured.
(2) Thickness of scaly substrate and color flop powder 100 particles selected from the sample of scaly substrate or color flop powder were scanned with a scanning electron microscope (S-5200N manufactured by Hitachi, Ltd.). The photograph was taken and the average value of the thickness was measured.
（３）カラーフロップ粉体の被覆層の厚さ
前記カラーフロップ粉体の試料をエポキシ樹脂（BUEHLHER製EPO-KWICK）に均一混合して常温で硬化させた後、ミクロトーム（Reichert-Nissei製ULTRACUT N）を用いて超薄切片の試料を調製した。次に、これをＦＥ−ＴＥＭ（日立製作所製HF-2200）を用いて観察し、そのＴＥＭ−ＥＤＳ分析から各酸化物層の厚さを測定した。
（４）カラーフロップ粉体の組成
前記カラーフロップ粉体の試料を誘導結合プラズマ発光分光分析装置（セイコー電子製SPS-1200A）を用いて、酸化第二鉄、二酸化珪素、二酸化チタンおよび鱗片状基材の組成を測定して、カラーフロップ粉体の組成から該基材の組成を差し引いて各組成を求めた。
(3) Thickness of coating layer of color flop powder The sample of color flop powder was uniformly mixed with epoxy resin (EPO-KWICK made by BUEHLHER) and cured at room temperature, and then microtome (ULTRACUT N made by Reichert-Nissei) ) Was used to prepare ultrathin section samples. Next, this was observed using FE-TEM (Hitachi Ltd. HF-2200), and the thickness of each oxide layer was measured from the TEM-EDS analysis.
(4) Composition of color flop powder Using a sample of the color flop powder using an inductively coupled plasma emission spectrometer (SPS-1200A manufactured by Seiko Denshi), ferric oxide, silicon dioxide, titanium dioxide and scaly groups The composition of the material was measured, and each composition was determined by subtracting the composition of the substrate from the composition of the color flop powder.
（５）カラーフロップ粉体の光学特性
前記カラーフロップ粉体３ｇをニトロセルロースラッカー（遠藤化学工業所製）１２ｇによく分散させ塗料化し、バーコーターＮｏ．１８を用いて白色の隠蔽率試験紙に塗付し、室温で乾燥させた。この試験紙上に形成された塗膜（厚さは約６μｍ）を、Ｄ６５／２の光源を持ち、煽り角を１０°に設定した三次元変角分光光度計（村上色彩技術研究所製、ＧＣＭＳ−４）を用いて、入射角０゜の条件にて受光角１０゜の正反射光と４５゜の拡散反射光のＬ*、ａ*、ｂ*の変化を測定し、上記の方法で求めた。
(5) Optical properties of color flop powder 3 g of the color flop powder was well dispersed in 12 g of nitrocellulose lacquer (manufactured by Endo Chemical Industries) to form a paint. 18 was applied to white hiding test paper and dried at room temperature. A three-dimensional variable angle spectrophotometer (GCMS, manufactured by Murakami Color Research Laboratory, Inc.) having a D65 / 2 light source and a turning angle set to 10 ° is formed on the test paper (thickness is about 6 μm). -4) is used to measure the changes in L * , a * , b * of the specularly reflected light with a light receiving angle of 10 ° and the diffusely reflected light of 45 ° under the condition of an incident angle of 0 ° and obtained by the above method. It was.
（６）カラーフロップ粉体の光沢性
前記カラーフロップ粉体３ｇをニトロセルロースラッカー（遠藤化学工業所製）１２ｇによく分散させ塗料化し、バーコーターＮｏ．１８を用いて黒色の隠蔽率試験紙に塗付し、室温で乾燥させた。この試験紙上に形成された塗膜（厚さは約６μｍ）を、Ｄ６５／２の光源を持ち、光束絞りを５．０、受光絞りを３．０、ＳＥＮＳＩＴＩＶＩＴＹ ＡＤＪ．を９５０、ＨＩＧＨＴ ＶＯＬＴ．を４２５、煽り角を０°に設定した三次元変角光度計（村上色彩技術研究所製、ＧＰ−２００）を用いて、入射角０゜の条件にて受光角５゜の正反射光の反射強度を測定した。
(6) Gloss of color flop powder 3 g of the above color flop powder was well dispersed in 12 g of nitrocellulose lacquer (manufactured by Endo Chemical Industries) to form a paint. 18 was applied to black concealment rate test paper and dried at room temperature. A coating film (thickness of about 6 μm) formed on this test paper was provided with a light source of D65 / 2, a light beam stop of 5.0, a light receiving stop of 3.0, SENSITIVITY ADJ. 950, HIGH VOLT. 425, and a three-dimensional variable angle photometer (GP-200, manufactured by Murakami Color Research Laboratory) with a tilt angle set to 0 °, the specularly reflected light with a receiving angle of 5 ° under the condition of an incident angle of 0 °. The reflection intensity was measured.
（７）カラーフロップ粉体の干渉性
前記カラーフロップ粉体を黒色の紙に貼った平滑性の高い透明両面テープの粘着面に付着させた試料を、Ｄ６５／２の光源を持ち、煽り角を１０°に設定した三次元変角分光光度計（村上色彩技術研究所製、ＧＣＭＳ−４）を用いて、入射角−４５゜、受光角４５゜の条件にて、３８０ｎｍから７６０ｎｍの波長における反射率を測定し、有色の干渉光に由来する反射率のうねりの有無を確認した。
以下、実施例に基づき本発明を更に具体的に説明する。しかし、本発明は、これらの実施例に記載された範囲に限定されるものではない。
(7) Interference of color flop powder A sample obtained by adhering the color flop powder to the adhesive surface of a highly smooth transparent double-sided tape with black paper pasted on it has a light source of D65 / 2 and has a turning angle. Using a three-dimensional variable angle spectrophotometer (GCMS-4, manufactured by Murakami Color Research Laboratory) set to 10 °, reflection at a wavelength of 380 nm to 760 nm under conditions of an incident angle of −45 ° and a light receiving angle of 45 °. The rate was measured and the presence or absence of the swell of the reflectance derived from the colored interference light was confirmed.
Hereinafter, the present invention will be described more specifically based on examples. However, the present invention is not limited to the scope described in these examples.
酸化第二鉄の被覆工程
平均粒子径２１μｍ、厚さ０．２μmのマイカ（（株）キララ製）１００ｇを純水１０００ｃｃに加えて十分に攪拌した後、６０℃の温度まで昇温し、これに５重量％濃度の塩酸水溶液を添加してｐＨ２．９の懸濁液を調製した。
この懸濁液に、Ｆｅ2Ｏ3換算基準で１０重量％濃度に調整した塩化第二鉄（和光純薬（株）製）の水溶液２５．６ｇを、１５重量％濃度のアンモニア水溶液を加えてｐＨを２．９に保持しながら、６．４ｇ／時間の速度で添加した。次いで、添加終了後そのまま１時間放置し、室温まで冷却した後、該懸濁液中に含まれる固形分を濾過、洗浄した。
次に、得られた固形分を１５０℃の温度で１５時間乾燥して、マイカの表面に酸化第二鉄を被覆した被覆粉体(1)を得た。
Coating process of ferric oxide 100 g of mica (manufactured by Kirara Co., Ltd.) having an average particle size of 21 μm and a thickness of 0.2 μm was added to 1000 cc of pure water and stirred sufficiently, and then the temperature was raised to a temperature of 60 ° C. A 5 wt% aqueous hydrochloric acid solution was added to the suspension to prepare a pH 2.9 suspension.
To this suspension, 25.6 g of an aqueous solution of ferric chloride (manufactured by Wako Pure Chemical Industries, Ltd.) adjusted to a concentration of 10% by weight on the basis of Fe 2 O 3 was added, and an aqueous ammonia solution of 15% by weight was added. While maintaining the pH at 2.9, it was added at a rate of 6.4 g / hr. Then, after completion of the addition, the mixture was allowed to stand for 1 hour and cooled to room temperature, and then the solid content contained in the suspension was filtered and washed.
Next, the obtained solid content was dried at a temperature of 150 ° C. for 15 hours to obtain a coated powder (1) in which the surface of mica was coated with ferric oxide.
二酸化珪素の被覆工程
前記被覆粉体(1)１００ｇを取り出して純水１０００ｃｃに加えて十分に攪拌した後、７０℃の温度まで昇温し、これに１５重量％濃度のアンモニア水溶液を添加してｐＨ９．４の懸濁液を調製した。
この懸濁液に、ＳｉＯ2換算基準で５重量％濃度に調整した珪酸（触媒化成工業（株）製）の水溶液２２２ｇを、１５重量％濃度のアンモニア水溶液を加えてｐＨを９．４に保持しながら、１３．８ｇ／時間の速度で添加した。次いで、添加終了後そのまま１時間放置し、室温まで冷却した後、該懸濁液中に含まれる固形分を濾過、洗浄した。
次に、得られた固形分を１５０℃の温度で１５時間乾燥して、マイカの表面に酸化第二鉄および二酸化珪素を被覆した被覆粉体(2)を得た。
Silicon dioxide coating process
100 g of the coated powder (1) was taken out and added to 1000 cc of pure water and stirred sufficiently. Then, the temperature was raised to a temperature of 70 ° C., and a 15 wt% aqueous ammonia solution was added thereto to add a suspension of pH 9.4. A suspension was prepared.
To this suspension, 222 g of an aqueous solution of silicic acid (manufactured by Catalyst Kasei Kogyo Co., Ltd.) adjusted to a concentration of 5% by weight in terms of SiO 2 was added, and an aqueous ammonia solution of 15% by weight was added to maintain the pH at 9.4. However, it was added at a rate of 13.8 g / hr. Then, after completion of the addition, the mixture was allowed to stand for 1 hour and cooled to room temperature, and then the solid content contained in the suspension was filtered and washed.
Next, the obtained solid content was dried at a temperature of 150 ° C. for 15 hours to obtain a coated powder (2) in which the surface of mica was coated with ferric oxide and silicon dioxide.
二酸化チタンの被覆工程
前記被覆粉体(2)１００ｇを取り出して純水１０００ｃｃに加えて十分に攪拌した後、６０℃の温度まで昇温し、これに１５重量％濃度のアンモニア水溶液を添加してｐＨ２．３の懸濁液を調製した。
この懸濁液に、ＴｉＯ2換算基準で１０重量％濃度に調整した硫酸チタニル（和光純薬（株）製）の水溶液２２２ｇを、１５重量％濃度のアンモニア水溶液を加えてｐＨを２．３に保持しながら、１１ｇ／時間の速度で添加した。次いで、添加終了後そのまま１時間放置し、室温まで冷却した後、該懸濁液中に含まれる固形分を濾過、洗浄した。
次に、得られた固形分を１５０℃の温度で１５時間乾燥して、マイカの表面に酸化第二鉄、二酸化珪素および二酸化チタンを被覆した被覆粉体(3)を得た。
Titanium dioxide coating step 100 g of the coated powder (2) was taken out and added to 1000 cc of pure water and stirred sufficiently. The temperature was raised to 60 ° C., and a 15 wt% aqueous ammonia solution was added thereto. A pH 2.3 suspension was prepared.
To this suspension was added 222 g of an aqueous solution of titanyl sulfate (manufactured by Wako Pure Chemical Industries, Ltd.) adjusted to a concentration of 10% by weight on the basis of TiO 2 , and an aqueous ammonia solution of 15% by weight was added to adjust the pH to 2.3. While holding, it was added at a rate of 11 g / hr. Then, after completion of the addition, the mixture was allowed to stand for 1 hour and cooled to room temperature, and then the solid content contained in the suspension was filtered and washed.
Next, the obtained solid content was dried at a temperature of 150 ° C. for 15 hours to obtain a coated powder (3) in which the surface of mica was coated with ferric oxide, silicon dioxide and titanium dioxide.
焼成工程
前記被覆粉体(3)を、電気炉（ヤマト科学（株）製）中に入れて、７５０℃の温度で３時間焼成した。次いで、この焼成粉体をジューサーミキサー（日立製作所（株）製）にかけて凝集物を解砕して、本発明のカラーフロップ粉体である実施例粉体Ａを得た。
Firing step The coated powder (3) was placed in an electric furnace (manufactured by Yamato Kagaku Co., Ltd.) and fired at a temperature of 750 ° C. for 3 hours. Then, the fired powder was passed through a juicer mixer (manufactured by Hitachi, Ltd.) to break up the agglomerates to obtain Example Powder A which is a color flop powder of the present invention.
このようにして得られた実施例粉体Ａについて、上記の測定方法を用いて平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
さらに、前記実施例粉体Ａを黒色紙に塗布して、正面から観察すると、シルバー色で有色の干渉色は確認されず、過度の光沢もなかった。また、側面から観察すると、ベージュ色を呈し、見る角度で色調が異なることが観察された。
With respect to Example Powder A thus obtained, the average particle diameter, particle composition, optical characteristics (regularity of reflected light C * ab , hab , reflection intensity, and coherence were measured using the above measurement method. Table 1, Table 2 and Table 3 show the results of measuring the presence / absence, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc.) and the thickness of the particle coating layer, respectively.
Furthermore, when the said Example powder A was apply | coated to black paper and it observed from the front, the colored interference color by silver was not confirmed, and there was no excessive glossiness. Moreover, when observed from the side, it was observed that the color was beige and the color tone was different depending on the viewing angle.
実施例１に示す前記酸化第二鉄被覆工程において、塩化第二鉄水溶液を３６．３ｇとし、その添加速度を９．１ｇ／時間に代えた以外は、実施例１と同様な操作を行って、実施例粉体Ｂを得た。
このようにして得られた実施例粉体Ｂについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
さらに、前記実施例粉体Ｂを黒色紙に塗布して、正面から観察すると、シルバー色で有色の干渉色は確認されず、過度の光沢もなかった。また、側面から観察すると、ベージュ色を呈し、見る角度で色調が異なることが観察された。
In the ferric oxide coating step shown in Example 1, the same operation as in Example 1 was performed, except that the aqueous ferric chloride solution was 36.3 g and the addition rate was changed to 9.1 g / hour. Example powder B was obtained.
As for Example Powder B thus obtained, the average particle diameter, particle composition, optical properties (saturation C * ab , hab , reflection intensity and interference of specular reflection light) were the same as in Example 1. Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
Furthermore, when the said Example powder B was apply | coated to black paper and it observed from the front, the colored interference color by silver was not confirmed and there was no excessive glossiness. Moreover, when observed from the side, it was observed that the color was beige and the color tone was different depending on the viewing angle.
実施例１に示す前記酸化第二鉄被覆工程において、塩化第二鉄水溶液を１２．７ｇとし、その添加速度を３．２ｇ／時間に代えた以外は、実施例１と同様な操作を行って、実施例粉体Ｃを得た。
このようにして得られた実施例粉体Ｃについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
さらに、前記実施例粉体Ｃを黒色紙に塗布して、正面から観察すると、シルバー色で有色の干渉色は確認されず、過度の光沢もなかった。また、側面から観察すると、ベージュ色を呈し、見る角度で色調が異なることが観察された。
In the ferric oxide coating step shown in Example 1, the same operation as in Example 1 was performed, except that the ferric chloride aqueous solution was 12.7 g and the addition rate was changed to 3.2 g / hour. Example powder C was obtained.
For Example Powder C thus obtained, as in Example 1, the average particle size, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
Furthermore, when the said Example powder C was apply | coated to black paper and observed from the front, the colored interference color by silver was not confirmed, and there was no excessive glossiness. Moreover, when observed from the side, it was observed that the color was beige and the color tone was different depending on the viewing angle.
実施例１に示す前記酸化第二鉄被覆工程において、平均粒子径９μｍ、厚さ０．２μmのマイカ（（株）山口雲母工業所製）を使用した以外は、実施例１と同様な操作を行って、実施例粉体Ｄを得た。
このようにして得られた実施例粉体Ｄについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
さらに、前記実施例粉体Ｄを黒色紙に塗布して、正面から観察すると、シルバー色で有色の干渉色は確認されず、過度の光沢もなかった。また、側面から観察すると、ベージュ色を呈し、見る角度で色調が異なることが観察された。
In the ferric oxide coating step shown in Example 1, the same operation as in Example 1 was performed except that mica having an average particle diameter of 9 μm and a thickness of 0.2 μm was used (manufactured by Yamaguchi Mica Industry Co., Ltd.). Example powder D was obtained.
For Example Powder D thus obtained, as in Example 1, the average particle size, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
Furthermore, when the said Example powder D was apply | coated to black paper and it observed from the front, the colored interference color by silver was not confirmed and there was no excessive glossiness. Moreover, when observed from the side, it was observed that the color was beige and the color tone was different depending on the viewing angle.
実施例１に示す前記酸化第二鉄被覆工程において、平均粒子径２９μｍ、厚さ０．３μmのマイカ（（株）山口雲母工業所製）を使用した以外は、実施例１と同様な操作を行って、実施例粉体Ｅを得た。
このようにして得られた実施例粉体Ｅについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
さらに、前記実施例粉体Ｅを黒色紙に塗布して、正面から観察すると、シルバー色で有色の干渉色は確認されず、過度の光沢もなかった。また、側面から観察すると、ベージュ色を呈し、見る角度で色調が異なることが観察された。
In the ferric oxide coating step shown in Example 1, the same operation as in Example 1 was performed except that mica having an average particle diameter of 29 μm and a thickness of 0.3 μm was used (manufactured by Yamaguchi Mica Industry Co., Ltd.). Example powder E was obtained.
For Example Powder E thus obtained, as in Example 1, the average particle size, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
Furthermore, when the said Example powder E was apply | coated to black paper and observed from the front, the interference color of a silver color was not confirmed, and there was no excessive glossiness. Moreover, when observed from the side, it was observed that the color was beige and the color tone was different depending on the viewing angle.
実施例１に示す前記酸化第二鉄被覆工程において、平均粒子径１３μｍ、厚さ０．４μmの合成マイカ（トピー工業（株）製）を使用した以外は、実施例１と同様な操作を行って、実施例粉体Ｆを得た。
このようにして得られた実施例粉体Ｆについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
さらに、前記実施例粉体Ｆを黒色紙に塗布して、正面から観察すると、シルバー色で有色の干渉色は確認されず、過度の光沢もなかった。また、側面から観察すると、ベージュ色を呈し、見る角度で色調が異なることが観察された。
In the ferric oxide coating step shown in Example 1, the same operation as in Example 1 was performed except that synthetic mica having an average particle diameter of 13 μm and a thickness of 0.4 μm was used (Topy Industries, Ltd.). Example powder F was obtained.
As for Example Powder F thus obtained, the average particle diameter, particle composition, optical properties (saturation C * ab , hab , reflection intensity and interference of specular reflection light) were the same as in Example 1. Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
Furthermore, when the said Example powder F was apply | coated to black paper and it observed from the front, the colored interference color by silver was not confirmed, and there was no excessive glossiness. Moreover, when observed from the side, it was observed that the color was beige and the color tone was different depending on the viewing angle.
実施例１で得られた実施例粉体Ａをメチルハイドロジェンポリシロキサン（信越化学（株）製ＫＦ−９９０１）で表面処理したシリコーン処理粉体（シリコーン３重量％処理品）を用いて、以下の組成（重量％）からなるリキッドファンデーションを調製した。
（１） シリコーン処理粉体（カラーフロップ粉体） １０．００
（２） シクロペンタシロキサン／ＰＥＧ−１０ジメチコン／ジステアリルジモニウムヘクトライト ８．００
（３） シクロペンタシロキサン １５．００
（４） ジメチコン ５．００
（５） トリエチルヘキサノイン ５．００
（６） 酸化チタン（顔料） ４．５０
（７） ベンガラ（顔料） ０．０６
（８） 酸化鉄（黄色顔料） ０．５５
（９） 酸化鉄（黒色顔料） ０．１０
（１０） ブチレングリコール １０．００
（１１） メチルパラベン ０．２０
（１２） 水 ４１．５９
上記の配合成分において、前記（２）は、日光ケミカル（株）製のニコムルスWOを使用し、また前記（６）〜（９）は、触媒化成工業（株）製のSYMPHOLIGHTシリーズを使用した。
Example powder A obtained in Example 1 was treated with methyl hydrogen polysiloxane (KF-9901 manufactured by Shin-Etsu Chemical Co., Ltd.) and treated with silicone (powder 3% by weight) and the following. A liquid foundation having the composition (% by weight) was prepared.
(1) Silicone-treated powder (color flop powder) 10.00
(2) Cyclopentasiloxane / PEG-10 dimethicone / distearyldimonium hectorite 8.00
(3) Cyclopentasiloxane 15.00
(4) Dimethicone 5.00
(5) Triethylhexanoin 5.00
(6) Titanium oxide (pigment) 4.50
(7) Bengala (pigment) 0.06
(8) Iron oxide (yellow pigment) 0.55
(9) Iron oxide (black pigment) 0.10
(10) Butylene glycol 10.00
(11) Methylparaben 0.20
(12) Water 41.59
In said compounding component, said (2) used Nikomuls WO by Nikko Chemical Co., Ltd., and said (6)-(9) used SYMPHOLIGHT series by a catalyst chemical industry Co., Ltd.
なお、前記リキッドファンデーションの調製は、以下のように行った。
（ａ）前記（１）〜（５）の成分を混合し、７０℃の温度に加熱して十分に撹拌混合した。
（ｂ）前記（６）〜（１２）の成分をホモミキサーを用いて混合し、５０００ｒｐｍの回転速度で１５分間、撹拌して、これに含まれる固形分を分散させた。
（ｃ）前記（ａ）で得られた混合物を、前記（ｂ）のホモミキサーの中に入れて混合し、５０００ｒｐｍの回転速度で３分間、撹拌して乳化させた。
（ｄ）前記（ｃ）で得られた乳化物を室温まで冷却し、次いで真空容器中に入れて脱泡した。
The liquid foundation was prepared as follows.
(A) The components (1) to (5) were mixed, heated to a temperature of 70 ° C., and sufficiently stirred and mixed.
(B) The components (6) to (12) were mixed using a homomixer and stirred at a rotational speed of 5000 rpm for 15 minutes to disperse the solid content contained therein.
(C) The mixture obtained in (a) was put into the homomixer of (b) and mixed, and the mixture was stirred and emulsified at a rotational speed of 5000 rpm for 3 minutes.
(D) The emulsion obtained in (c) was cooled to room temperature, and then put in a vacuum vessel to degas.
次に、得られたリキッドファンデーションを、実際に腕の皮膚に塗布してみたところ、正反射角周辺ではシルバーの色味が確認され、それ以外では皮膚の色に近い肌色が観察された。また、このリキッドファンデーションを実際に顔に塗布したところ、市販のファンデーションと比較して、鼻筋がスッキリと見え、且つ顔全体の立体感を強調する効果があることを確認された。 Next, when the obtained liquid foundation was actually applied to the skin of the arm, the color of silver was confirmed around the regular reflection angle, and the skin color close to the color of the skin was observed otherwise. Moreover, when this liquid foundation was actually applied to the face, it was confirmed that the nasal muscles were clearly visible and had an effect of enhancing the three-dimensional effect of the entire face as compared with a commercially available foundation.
実施例１で得られた実施例粉体Ａをメチルハイドロジェンポリシロキサン（信越化学（株）製ＫＦ−９９０１）で表面処理したシリコーン処理粉体（シリコーン３重量％処理品）を用いて、以下の組成（重量％）からなるパウダーファンデーションを調製した。
（１） シリコーン処理粉体（カラーフロップ粉体） ２０．００
（２） タルクのシリコーン処理粉体 ３３．５５
（３） マイカのシリコーン処理粉体 ２０．００
（４） 球状シリカ ３．００
（５） 酸化チタン（顔料） ８．００
（６） ベンガラ（顔料） ０．３５
（７） 酸化鉄（黄色顔料） １．７５
（８） 酸化鉄（黒色顔料） ０．１５
（９） メチルパラベン ０．２０
（１０） ジイソステアリン酸ポリグリセリル １．００
（１１） ジメチコン ５．００
（１２） 流動パラフィン ４．００
（１３） トリエチルヘキサノイン ３．００
上記の配合成分において、前記（４）は、触媒化成工業（株）製シリカマイクロビードＰ−１５００のシリコーン５重量％処理品を使用し、また前記（５）は、石原産業（株）製タイペークＣＲ−５０シリコーン２重量％処理品を使用し、（６）〜（８）は、チタン工業（株）製のTAROXシリーズのシリコーン２重量％処理品を使用した。
Example powder A obtained in Example 1 was treated with methyl hydrogen polysiloxane (KF-9901 manufactured by Shin-Etsu Chemical Co., Ltd.) and treated with silicone (powder 3% by weight) and the following. A powder foundation having the composition (% by weight) was prepared.
(1) Silicone-treated powder (color flop powder) 20.00
(2) Talc silicone-treated powder 33.55
(3) Mica silicone-treated powder 20.00
(4) Spherical silica 3.00
(5) Titanium oxide (pigment) 8.00
(6) Bengala (pigment) 0.35
(7) Iron oxide (yellow pigment) 1.75
(8) Iron oxide (black pigment) 0.15
(9) Methylparaben 0.20
(10) Polyglyceryl diisostearate 1.00
(11) Dimethicone 5.00
(12) Liquid paraffin 4.00
(13) Triethylhexanoin 3.00
In the above blending component, (4) uses a 5% by weight treated product of silica microbead P-1500 manufactured by Catalyst Kasei Kogyo Co., Ltd., and (5) indicates a typeque manufactured by Ishihara Sangyo Co., Ltd. A CR-50 silicone treated product with 2% by weight was used. For (6) to (8), a TAROX series silicone treated product with 2% by weight manufactured by Titanium Industry Co., Ltd. was used.
なお、前記パウダーファンデーションの調製は、以下のように行った。
（ａ）前記（１）〜（９）の成分を混合し、十分に撹拌混合した。
（ｂ）前記（１０）〜（１３）の成分を十分に混合した後、前記（ａ）の混合物に加えて、均一になるまで撹拌混合した。
（ｃ）前記（ｂ）で得られた混合物１２ｇを５５ｍｍ×４７ｍｍの金皿に載せ、これを１．５ｋｇ／ｃｍ2の圧力でプレスしてケーキ状ファンデーションに成形した。
The powder foundation was prepared as follows.
(A) The above components (1) to (9) were mixed and sufficiently stirred and mixed.
(B) After sufficiently mixing the components (10) to (13), the mixture was added to the mixture (a) and stirred until uniform.
(C) 12 g of the mixture obtained in the above (b) was placed on a 55 mm × 47 mm metal pan, and pressed with a pressure of 1.5 kg / cm 2 to form a cake-like foundation.
次に、得られたパウダーファンデーションを、実際に腕の皮膚に塗布してみたところ、正反射角周辺ではシルバーの色味が確認され、それ以外では皮膚の色に近い肌色が観察された。また、このパウダーファンデーションを実際に顔に塗布したところ、市販のファンデーションと比較して、鼻筋がスッキリと見え、且つ顔全体の立体感を強調する効果があることを確認された。 Next, when the obtained powder foundation was actually applied to the skin of the arm, the color of silver was confirmed around the specular reflection angle, and the skin color close to the color of the skin was observed otherwise. Moreover, when this powder foundation was actually applied to the face, it was confirmed that the nose muscles were clearly seen and the effect of enhancing the three-dimensional effect of the entire face was enhanced compared to a commercially available foundation.
実施例１に示す前記酸化第二鉄被覆工程において、塩化第二鉄水溶液を８１．１ｇに代えた以外は、実施例１と同様な操作を行って、比較例粉体Ａを得た。
このようにして得られた比較例粉体Ａについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
その結果、受光角１０°での正反射光の彩度Ｃ* abが２０を超えていることが確認された。また、当該比較例粉体Ａを用いて、実施例７と同様にリキッドファンデーションを調製した。この際、同実施例（７）のベンガラ、（８）の酸化鉄の配合量を種々変更したが、結果的に濃い色彩のものしか得られなかった。
Comparative Example powder A was obtained by performing the same operation as in Example 1 except that the ferric chloride aqueous solution was replaced with 81.1 g in the ferric oxide coating step shown in Example 1.
About the comparative example powder A thus obtained, as in Example 1, the average particle diameter, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
As a result, it was confirmed that the saturation C * ab of specularly reflected light at a light receiving angle of 10 ° exceeds 20. A liquid foundation was prepared in the same manner as in Example 7 using the comparative example powder A. At this time, the blending amounts of Bengala of Example (7) and iron oxide of (8) were variously changed. As a result, only dark colors were obtained.
実施例１に示す前記酸化チタン被覆工程において、硫酸チタニル水溶液を６６６．６ｇとし、その添加速度を４１．７ｇ／時間に代えた以外は、実施例１と同様な操作を行って、比較例粉体Ｂを得た。
このようにして得られた比較例粉体Ｂについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
その結果、受光角１０°での正反射光の彩度Ｃ* abが８と非常に小さくなっており、また青みを帯びた干渉色が確認された。また、当該比較例粉体Ｂを用いて、実施例７と同様にリキッドファンデーションを調製し、肌に塗付してみたところ、青味を帯びた光が血色の悪い印象を与えて不自然であった。
In the titanium oxide coating step shown in Example 1, the same operation as in Example 1 was performed except that 666.6 g of the titanyl sulfate aqueous solution was changed to 41.7 g / hour, and Comparative Example Powder was used. Body B was obtained.
As for Comparative Example Powder B thus obtained, the average particle diameter, particle composition, optical properties (saturation C * ab , hab , reflection intensity and interference of specular reflection light) were the same as in Example 1. Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
As a result, the saturation C * ab of specular reflection light at a light receiving angle of 10 ° was as very small as 8, and a bluish interference color was confirmed. Further, using the comparative powder B, a liquid foundation was prepared in the same manner as in Example 7, and when applied to the skin, the bluish light gave an unpleasant impression and was unnatural. there were.
実施例１に示す前記酸化チタン被覆工程において、硫酸チタニル水溶液を１０．１ｇとし、その添加速度を２．５ｇ／時間に代えた以外は、実施例１と同様な操作を行って、比較例粉体Ｃを得た。
このようにして得られた比較例粉体Ｃについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
その結果、受光角１０°での正反射光の彩度Ｃ* abが２０を超えており、また、色差△Ｅ* abが１８未満であることが確認された。また、当該比較例粉体Ｃを用いて、実施例７と同様にリキッドファンデーションを調製した。この際、同実施例（７）のベンガラ、（８）の酸化鉄の配合量を種々変更したが、結果的に濃い色彩のものしか得られなかった。また、顕著なカラーフロップ性も確認できなかった。
In the titanium oxide coating step shown in Example 1, the same procedure as in Example 1 was carried out except that the titanyl sulfate aqueous solution was changed to 10.1 g and the addition rate was changed to 2.5 g / hour. Body C was obtained.
About the comparative example powder C thus obtained, as in Example 1, the average particle diameter, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
As a result, it was confirmed that the chroma C * ab of specular reflection light at a light receiving angle of 10 ° exceeds 20 and the color difference ΔE * ab is less than 18. In addition, a liquid foundation was prepared in the same manner as in Example 7 using the comparative powder C. At this time, the blending amounts of Bengala of Example (7) and iron oxide of (8) were variously changed. As a result, only dark colors were obtained. In addition, a remarkable color flop property could not be confirmed.
実施例１に示す前記二酸化珪素被覆工程を省略（すなわち、珪酸水溶液の添加操作なし）した以外は、実施例１と同様な操作を行って、比較例粉体Ｄを得た。
このようにして得られた比較例粉体Ｄについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
その結果、受光角１０°での正反射光の彩度Ｃ* abが２０を超えており、また、色差△Ｅ* abが１８未満であることが確認された。また、当該比較例粉体Ｄを用いて、実施例７と同様にリキッドファンデーションを調製した。この際、同実施例（７）のベンガラ、（８）の酸化鉄の配合量を種々変更したが、結果的に濃い色彩のものしか得られなかった。また、顕著なカラーフロップ性も確認できなかった。
Comparative Example powder D was obtained by performing the same operation as in Example 1 except that the silicon dioxide coating step shown in Example 1 was omitted (that is, no addition operation of an aqueous silicic acid solution).
About the comparative example powder D thus obtained, as in Example 1, the average particle size, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
As a result, it was confirmed that the chroma C * ab of specular reflection light at a light receiving angle of 10 ° exceeds 20 and the color difference ΔE * ab is less than 18. In addition, a liquid foundation was prepared in the same manner as in Example 7 using the comparative powder D. At this time, the blending amounts of Bengala of Example (7) and iron oxide of (8) were variously changed. As a result, only dark colors were obtained. In addition, a remarkable color flop property could not be confirmed.
実施例１に示す前記酸化第二鉄被覆工程において、平均粒子径４９μｍ、厚さ０．３μmのマイカを使用した以外は、実施例１と同様な操作を行って、比較例粉体Ｅを得た。
このようにして得られた比較例粉体Ｅについて、実施例1の場合と同様に、平均粒子径、粒子組成、光学特性（正反射光の彩度Ｃ* ab、ｈab、反射強度および干渉性の有無、拡散反射光の彩度Ｃ* ab、色差△Ｅ* ab、色相角差△ｈab等）および粒子被覆層の厚さを測定した結果をそれぞれ表1、表２および表３に示す。
その結果、反射強度が検出上限の８９を超えていることが確認された。また、当該比較例粉体Ｅを用いて、実施例７と同様にリキッドファンデーションを調製し、肌に塗付してみたところ、極めて光沢が高く、不自然な仕上がりとなった。
Comparative Example Powder E was obtained by performing the same operation as in Example 1 except that mica having an average particle diameter of 49 μm and a thickness of 0.3 μm was used in the ferric oxide coating step shown in Example 1. It was.
As for Comparative Example Powder E thus obtained, in the same manner as in Example 1, the average particle diameter, particle composition, optical characteristics (regular reflection light saturation C * ab , hab , reflection intensity and interference) Table 1, Table 2 and Table 3 show the results of measuring the thickness of the particle coating layer, the presence or absence of color, the saturation C * ab of diffuse reflected light, the color difference ΔE * ab , the hue angle difference Δhab, etc. Show.
As a result, it was confirmed that the reflection intensity exceeded the upper detection limit of 89. Further, when a liquid foundation was prepared using the comparative example powder E in the same manner as in Example 7 and applied to the skin, it was extremely glossy and had an unnatural finish.
Claims (11)
前記鱗片状基材が、平均粒子径１〜４０μｍおよび平均厚さ０．０５〜１．０μｍの大きさを有し、
前記酸化第二鉄を０．５〜５重量％、前記二酸化珪素を２〜３０重量％、前記二酸化チタンを５〜３０重量％含むことを特徴とするカラーフロップ粉体。 Non-interference with a beige hue formed by sequentially laminating a reddish brown ferric oxide coating layer , an achromatic silicon dioxide coating layer, and an achromatic titanium dioxide coating layer on the surface of a scaly substrate Color flop powder ,
The scaly substrate has an average particle size of 1 to 40 μm and an average thickness of 0.05 to 1.0 μm,
A color flop powder comprising 0.5 to 5% by weight of the ferric oxide, 2 to 30% by weight of the silicon dioxide, and 5 to 30% by weight of the titanium dioxide .
日本工業規格番号ＪＩＳ Ｚ ８７２９ ５．２ に規定される彩度Ｃ* abが、正反射角付近では２０以下、正反射角より少しずれた拡散反射角付近では２１以上であり、
日本工業規格番号ＪＩＳ Ｚ ８７３０ ７．１ に規定される色差△Ｅ* ab （ここで、△Ｅ * ab は、Ｄ６５／２の光源を持ち、煽り角を１０°に設定した三次元変角分光光度計を用いて、入射角０°の条件にて受光角１０°での正反射角付近の反射光と４５°での拡散反射光のＬ * 、ａ * 、ｂ * の変化を測定し、その結果を式△Ｅ * ab ＝［（△Ｌ * ） 2 ＋（△ａ * ） 2 ＋（△ｂ * ） 2 ］ 1/2 に入力することにより求められる。）が１８以上であり、
正反射光域に干渉光による発色を呈さず、さらに
Ｄ６５／２の光源を持ち、煽り角を０°に設定した三次元変角光度計を用いて、入射角０°の条件にて受光角５°での正反射角付近の反射光を測定したときの反射強度が、１０〜８０の範囲にある
ことを特徴とするカラーフロップ粉体。 On the surface of the scaly substrate, a coating layer of reddish brown ferric oxide, a coating layer of achromatic silicon dioxide and a coating layer of achromatic titanium dioxide are sequentially laminated,
The saturation C * ab specified in Japanese Industrial Standard No. JIS Z 8729 5.2 is 20 or less near the regular reflection angle, and 21 or more near the diffuse reflection angle slightly deviated from the regular reflection angle.
Color difference ΔE * ab defined in Japanese Industrial Standard No. JIS Z 8730 7.1 (where ΔE * ab is a three-dimensional variable angle spectroscopy with a D65 / 2 light source and a tilt angle set to 10 °. Using a photometer , the change in L * , a * , b * of the reflection light near the regular reflection angle at the light receiving angle of 10 ° and the diffuse reflection light at 45 ° under the condition of the incident angle of 0 ° is measured. As a result of formula △ E * ab = [(△ L *) 2 + (△ a *) 2 + (△ b *) 2] obtained by inputting to 1/2.) Ri der 18 or more,
Does not exhibit coloring due to interference light in the specular reflection region, and
Using a three-dimensional variable angle photometer with a D65 / 2 light source and a tilt angle set to 0 °, the reflected light near the regular reflection angle at a light receiving angle of 5 ° was measured under the condition of an incident angle of 0 °. The color flop powder characterized by having a reflection intensity in the range of 10-80 .
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