JP7602861B2 - Composite powder, skin external application composition, and method for enhancing fluorescence intensity of inorganic fluorescent powder - Google Patents
Composite powder, skin external application composition, and method for enhancing fluorescence intensity of inorganic fluorescent powder Download PDFInfo
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- JP7602861B2 JP7602861B2 JP2018200695A JP2018200695A JP7602861B2 JP 7602861 B2 JP7602861 B2 JP 7602861B2 JP 2018200695 A JP2018200695 A JP 2018200695A JP 2018200695 A JP2018200695 A JP 2018200695A JP 7602861 B2 JP7602861 B2 JP 7602861B2
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- fluorescent powder
- oxide
- inorganic fluorescent
- inorganic
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- 239000008269 hand cream Substances 0.000 description 1
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- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
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- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 229940091554 lauryl peg-9 polydimethylsiloxyethyl dimethicone Drugs 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
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- 229920001778 nylon Polymers 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- RUOPINZRYMFPBF-UHFFFAOYSA-N pentane-1,3-diol Chemical compound CCC(O)CCO RUOPINZRYMFPBF-UHFFFAOYSA-N 0.000 description 1
- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 description 1
- 229910052628 phlogopite Inorganic materials 0.000 description 1
- 229920001523 phosphate polymer Polymers 0.000 description 1
- 229920003217 poly(methylsilsesquioxane) Polymers 0.000 description 1
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- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 229940113124 polysorbate 60 Drugs 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- FWFUWXVFYKCSQA-UHFFFAOYSA-M sodium;2-methyl-2-(prop-2-enoylamino)propane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(C)(C)NC(=O)C=C FWFUWXVFYKCSQA-UHFFFAOYSA-M 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
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- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 description 1
- MLXDKRSDUJLNAB-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F MLXDKRSDUJLNAB-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Cosmetics (AREA)
Description
本発明は、無機蛍光粉体と非蛍光粉体の複合粉体、それを含有する皮膚外用組成物、及び無機蛍光粉体の蛍光強度増強方法に関する。 The present invention relates to a composite powder of an inorganic fluorescent powder and a non-fluorescent powder, a skin topical composition containing the composite powder, and a method for enhancing the fluorescence intensity of an inorganic fluorescent powder.
化粧料では、目的に応じて様々な粉体が含有されている。特にメーキャップ化粧料や日焼け止め化粧料においては、粉体によってツヤ感、ソフトフォーカス性、色補正、紫外線防御能等の効果を付与することが一般的である。 Cosmetics contain a variety of powders depending on the purpose. In particular, in makeup and sunscreen cosmetics, powders are commonly used to impart effects such as gloss, soft focus, color correction, and UV protection.
粉体の中で、蛍光粉体は、一般にディスプレイや照明、遊具や塗料等の用途に使用されているが、化粧料においてもメーキャップ効果を高める目的で使用されている。例えば、化粧料に蛍光粉体を用いることで、ソフトフォーカス性等の付与だけでなく、蛍光色による色補正効果の付与もできる。 Of all powders, fluorescent powders are generally used in displays, lighting, playground equipment, paints, etc., but they are also used in cosmetics to enhance the makeup effect. For example, the use of fluorescent powders in cosmetics can not only impart soft focus properties, but also provide color correction effects through the use of fluorescent colors.
特許文献１では無機蛍光粉体であるアルミネート複合酸化物を含有させることでソフトフォーカス性を向上させた化粧料が開示されている。特許文献２では非晶質シリカ粒子を含んだ青色蛍光粉体が開示されており、化粧料への適用についても記載されている。しかし、特許文献１や特許文献２に記載されている蛍光粉体は発光強度が十分でないため、化粧料として効果を発揮するには配合量を多くする必要があった。また、これらの蛍光粉体はソフトフォーカス性が高いため、ツヤ感を高める効果をもたせた化粧料には不向きであった。 Patent Document 1 discloses a cosmetic product that has improved soft focus properties by including an inorganic fluorescent powder, an aluminate complex oxide. Patent Document 2 discloses a blue fluorescent powder that includes amorphous silica particles, and also describes its application to cosmetics. However, the fluorescent powders described in Patent Documents 1 and 2 do not have sufficient luminescence intensity, so a large amount needs to be blended to be effective as a cosmetic product. In addition, because these fluorescent powders have high soft focus properties, they are unsuitable for cosmetics that have the effect of enhancing luster.
そのような中、蛍光粉体において、その蛍光強度を増強させることで、メーキャップ効果を高める技術が開発されている。例えば特許文献３には、無機蛍光粉体と他の粉体を含有させることで発光強度がより効果的に高められた化粧料が開示されている。しかし、この文献に記載の技術では、蛍光粉体の蛍光強度の増強効果が不十分である場合がある。 In light of this, technology has been developed to enhance the makeup effect of fluorescent powders by increasing their fluorescence intensity. For example, Patent Document 3 discloses a cosmetic product in which the luminescence intensity is more effectively increased by incorporating inorganic fluorescent powder and other powders. However, the technology described in this document may not be effective in enhancing the fluorescence intensity of the fluorescent powder.
一方、化粧料分野においては様々な複合粉体が使用されており、複合化する粉体の組み合わせ等により、様々な化粧料効果が得られることが知られている。例えば特許文献４では無機粉体上に特定の方法でシリカを複合化することでソフトフォーカス効果を高めた複合粉体が開示されている。特許文献５では窒化ホウ素に金属酸化物を複合化することでツヤを高めた複合粉体が開示されている。 On the other hand, various composite powders are used in the field of cosmetics, and it is known that various cosmetic effects can be obtained by combining composite powders. For example, Patent Document 4 discloses a composite powder that enhances the soft focus effect by compounding silica on an inorganic powder using a specific method. Patent Document 5 discloses a composite powder that enhances shine by compounding boron nitride with a metal oxide.
しかし特許文献４、５においては、蛍光粉体に関する記述は一切なく、蛍光粉体の蛍光強度を増強するという課題は、これらの文献を参考にしても解決することができない。また、色補正効果についても何ら記載されていない。 However, Patent Documents 4 and 5 contain no description whatsoever of fluorescent powders, and the problem of increasing the fluorescent intensity of fluorescent powders cannot be solved by referring to these documents. In addition, there is no description of the color correction effect.
本発明は、無機蛍光体の蛍光強度の新規増強方法、この方法を用いて得られた蛍光強度が増強された無機蛍光体、それを含有する化粧料を提供することを目的とする。 The present invention aims to provide a new method for enhancing the fluorescence intensity of an inorganic phosphor, an inorganic phosphor with enhanced fluorescence intensity obtained using this method, and a cosmetic preparation containing the same.
本発明者は上記課題を解決するために鋭意検討した結果、無機蛍光粉体の表面の少なくとも一部に非蛍光粉体を被覆させることで蛍光強度が増強することを見出した。 As a result of intensive research into solving the above problems, the inventors discovered that the fluorescence intensity can be increased by coating at least a portion of the surface of an inorganic fluorescent powder with a non-fluorescent powder.
即ち、本発明の要旨は以下の通りである。 In other words, the gist of the present invention is as follows:
［１］少なくともａ）無機蛍光粉体の表面の一部を、ｂ）非蛍光粉体が被覆していることを特徴とする複合粉体。
［２］ａ）無機蛍光粉体の有する蛍光波長が、４４０ｎｍ～５２０ｎｍ又は６４０ｎｍ～７００ｎｍの範囲内であることを特徴とする［１］に記載の複合粉体。
［３］ａ）無機蛍光粉体が、結晶母体及び／又は賦活剤としてＡｌ（アルミニウム）、Ｚｎ（亜鉛）、Ｍｇ（マグネシウム）、Ｓｉ（ケイ素）、Ｍｎ（マンガン）、Ｃａ（カルシウム）、Ｔｉ（チタン）、Ｃｅ（セリウム）、Ｂａ（バリウム）、Ｏ（酸素）、Ｐ（リン）、Ｓ（硫黄）の中から選択される少なくとも１種以上の元素を含有していることを特徴とする［１］又は［２］に記載の複合粉体。
［４］ａ）無機蛍光粉体が、酸化（Ａｌ／Ｃａ／マンガン）、酸化（Ｍｇ／マンガン／チタン）、酸化亜鉛蛍光体、及び、リン酸（Ｃａ／セリウム）からなる群より選択される少なくとも１種であることを特徴とする［１］～［３］のいずれか記載の複合粉体。
［５］ｂ）非蛍光粉体が、酸化チタン、非蛍光性酸化亜鉛、酸化鉄、酸化アルミニウム（アルミナ）、及び、シリカからなる群より選択される少なくとも１種であることを特徴とする［１］～［４］のいずれか記載の複合粉体。
［６］ａ）無機蛍光粉体の粒子径が、１μｍ以上２００μｍ以下であることを特徴とする、［１］～［５］のいずれか記載の複合粉体。
［７］ｂ）非蛍光粉体の粒子径が、１ｎｍ以上１００ｎｍ以下であることを特徴とする、［１］～［６］のいずれか記載の複合粉体。
［８］複合粉体におけるａ）無機蛍光粉体とｂ）非蛍光粉体の比率が、ａ成分：ｂ成分＝９５（重量％）：５（重量％）～７０（重量％）：３０（重量％）であることを特徴とする、［１］～［７］のいずれか記載の複合粉体。
［９］皮膚外用組成物用である、［１］～［８］のいずれか記載の複合粉体。
［１０］［１］～［９］のいずれか記載の複合粉体を含有する、皮膚外用組成物。
［１１］ａ）無機蛍光粉体の表面の一部をｂ）非蛍光粉体で被覆することを特徴とする、無機蛍光粉体の蛍光強度増強方法。
[1] A composite powder comprising a) an inorganic fluorescent powder and b) a non-fluorescent powder covering at least a portion of the surface of the inorganic fluorescent powder.
[2] a) The composite powder according to [1], characterized in that the fluorescent wavelength of the inorganic fluorescent powder is within the range of 440 nm to 520 nm or 640 nm to 700 nm.
[3] a) The composite powder according to [1] or [2], characterized in that the inorganic fluorescent powder contains at least one element selected from Al (aluminum), Zn (zinc), Mg (magnesium), Si (silicon), Mn (manganese), Ca (calcium), Ti (titanium), Ce (cerium), Ba (barium), O (oxygen), P (phosphorus), and S (sulfur) as a crystal host and/or an activator.
[4] a) The composite powder according to any one of [1] to [3], characterized in that the inorganic fluorescent powder is at least one selected from the group consisting of (Al/Ca/manganese), (Mg/manganese/titanium) oxide, zinc oxide phosphor, and (Ca/cerium) phosphate.
[5] b) The composite powder according to any one of [1] to [4], characterized in that the non-fluorescent powder is at least one selected from the group consisting of titanium oxide, non-fluorescent zinc oxide, iron oxide, aluminum oxide (alumina), and silica.
[6] The composite powder according to any one of [1] to [5], characterized in that a) the inorganic fluorescent powder has a particle size of 1 μm or more and 200 μm or less.
[7] b) The composite powder according to any one of [1] to [6], characterized in that the particle diameter of the non-fluorescent powder is 1 nm or more and 100 nm or less.
[8] The composite powder according to any one of [1] to [7], characterized in that the ratio of a) inorganic fluorescent powder and b) non-fluorescent powder in the composite powder is component a:component b=95 (wt%):5 (wt%) to 70 (wt%):30 (wt%).
[9] The composite powder according to any one of [1] to [8], which is for use in a composition for external application to skin.
[10] A composition for external use on the skin, comprising the complex powder according to any one of [1] to [9].
[11] A method for enhancing fluorescence intensity of an inorganic fluorescent powder, comprising: a) covering a part of a surface of the inorganic fluorescent powder with b) a non-fluorescent powder.
本発明によれば、ａ）無機蛍光粉体の表面の少なくとも一部にｂ）非蛍光粉体を被覆させた複合粉体とすることで、ａ）無機蛍光粉体の蛍光強度を顕著に向上させることができる。また、ａ）無機蛍光粉体の表面の少なくとも一部にｂ）非蛍光粉体を被覆させた本発明の複合粉体は、優れた発光性を示すため、化粧料に含有させることで、よりメーキャップ効果の高い化粧料を提供することができる。 According to the present invention, by forming a composite powder in which at least a portion of the surface of a) inorganic fluorescent powder is coated with b) non-fluorescent powder, the fluorescence intensity of a) inorganic fluorescent powder can be significantly improved. In addition, the composite powder of the present invention in which at least a portion of the surface of a) inorganic fluorescent powder is coated with b) non-fluorescent powder exhibits excellent luminescence, and thus, by including it in cosmetics, cosmetics with a stronger makeup effect can be provided.
以下、本発明について詳細に説明する。なお、本明細書中で使用される用語は、特に言及しない限り、当該技術分野で通常用いられる意味で解釈される。 The present invention will be described in detail below. Note that the terms used in this specification are to be interpreted as having the meanings normally used in the relevant technical field unless otherwise specified.
また、本明細書中で使用される％は、特に言及しない限り重量％を指す。 In addition, % used in this specification refers to % by weight unless otherwise specified.
＜複合粉体＞
本発明の複合粉体は、少なくともａ）無機蛍光粉体の表面の一部をｂ）非蛍光粉体が被覆していることを特徴とする。ここで、被覆とは、ａ）無機蛍光粉体の表面の少なくとも一部をｂ）非蛍光粉体が覆っていることを意味し、ａ）無機蛍光粉体の表面の一部を覆っている場合、ａ）無機蛍光粉体の表面の全部を覆っている場合のいずれも含む。本願発明の複合粉体の被覆率は３０％以上が好ましく、４０％以上がより好ましく、５０％以上がさらに好ましい。
<Composite powder>
The composite powder of the present invention is characterized in that at least a part of the surface of the inorganic fluorescent powder a) is covered with a non-fluorescent powder b). Here, "covered" means that at least a part of the surface of the inorganic fluorescent powder a) is covered with the non-fluorescent powder b), and includes both the case where a part of the surface of the inorganic fluorescent powder a) is covered and the case where the entire surface of the inorganic fluorescent powder a) is covered. The coverage of the composite powder of the present invention is preferably 30% or more, more preferably 40% or more, and even more preferably 50% or more.
本願発明における被覆率とは、ａ）無機蛍光粉体の表面積に対する、ａ）無機蛍光粉体の表面積と複合粉体における被覆されていない表面の表面積の差の割合のことであり、下記のような式で表すことができる。
被覆率を求める方法としては、例えば、走査型電子顕微鏡観察画像において複合粉体の表面を観察し、複合粉体の表面全体と、ｂ）非蛍光粉体が被覆されていない面の表面積を画像解析等により求め、上記式により各複合粉体の被覆率を算出し、複数の複合粉体の被覆率の平均値を本発明における複合粉体の被覆率とすることができる。 As a method for determining the coverage rate, for example, the surface of the composite powder is observed in a scanning electron microscope image, and the surface area of the entire surface of the composite powder and the surface area of the surface not covered with the non-fluorescent powder are determined by image analysis or the like, and the coverage rate of each composite powder is calculated using the above formula, and the average value of the coverage rates of the multiple composite powders can be regarded as the coverage rate of the composite powder in the present invention.
本発明で用いられるａ）無機蛍光粉体は、蛍光特性を有する無機粉体であればよく、形状、大きさは限定されない。 The inorganic fluorescent powder a) used in the present invention may be any inorganic powder having fluorescent properties, and there are no limitations on its shape or size.
ａ）無機蛍光粉体としては、蛍光特性を有する無機粉体であればよく、結晶母体単体で蛍光特性を有する賦活剤を含まない無機蛍光粉体でも、結晶母体と賦活剤（不純物）からなる賦活型蛍光体でもよい。本明細書における結晶母体とは、結晶体でも非晶体でもよい。また、それ以外の賦活剤等を含んでも、含まなくてもよく、賦活剤等を含まない場合においても通常用いられる結晶体及び非晶体と同等の意味で用いられる。結晶母体としては、金属酸化物、リン酸化合物、金属硫化物、金属硫酸化物、ハロリン酸化合物等が挙げられ、金属酸化物又はリン酸化合物が好ましい。 a) The inorganic fluorescent powder may be an inorganic powder having fluorescent properties, and may be an inorganic fluorescent powder containing no activator that has fluorescent properties in the crystal matrix alone, or an activated phosphor consisting of a crystal matrix and an activator (impurity). The crystal matrix in this specification may be a crystalline or amorphous body. It may also contain or not contain other activators, and even when it does not contain an activator, it is used in the same sense as the commonly used crystalline and amorphous bodies. Examples of the crystal matrix include metal oxides, phosphate compounds, metal sulfides, metal sulfates, halophosphate compounds, etc., and metal oxides or phosphate compounds are preferred.
本発明で用いられるａ）無機蛍光粉体の結晶母体としては、Ａｌ（アルミニウム）、Ｔｉ（チタン）、Ｚｎ（亜鉛）、Ｇｅ（ゲルマニウム）、Ｓｉ（ケイ素）、Ｆｅ（鉄）、Ｚｒ（ジルコニウム）、Ｍｎ（マンガン）、Ｍｇ（マグネシウム）、Ｃａ（カルシウム）、Ｚｎ（亜鉛）の中から選択される１種以上の元素を含有していることが好ましい。中でもＡｌ（アルミニウム）、Ｚｎ（亜鉛）、Ｍｇ（マグネシウム）、Ｃａ（カルシウム）、Ｔｉ（チタン）、Ｂａ（バリウム）、Ｏ（酸素）、Ｐ（リン）、Ｓ（硫黄）の中から選択される１種以上の元素を含有していることが好ましく、特にＯ（酸素）及び／又はＰ（リン）を含有し、かつＡｌ（アルミニウム）、Ｚｎ（亜鉛）、Ｍｇ（マグネシウム）、Ｃａ（カルシウム）、Ｔｉ（チタン）、Ｂａ（バリウム）から選ばれる１種以上の元素を含有していることが好ましい。 The crystalline matrix of the inorganic fluorescent powder a) used in the present invention preferably contains one or more elements selected from Al (aluminum), Ti (titanium), Zn (zinc), Ge (germanium), Si (silicon), Fe (iron), Zr (zirconium), Mn (manganese), Mg (magnesium), Ca (calcium), and Zn (zinc). In particular, it is preferable to contain one or more elements selected from Al (aluminum), Zn (zinc), Mg (magnesium), Ca (calcium), Ti (titanium), Ba (barium), O (oxygen), P (phosphorus), and S (sulfur), and it is particularly preferable to contain O (oxygen) and/or P (phosphorus) and one or more elements selected from Al (aluminum), Zn (zinc), Mg (magnesium), Ca (calcium), Ti (titanium), and Ba (barium).
本発明で用いられる賦活剤を含むａ）無機蛍光粉体の賦活剤としては、Ｍｎ（マンガン）、Ｅｕ（ユウロピウム）、Ｃｒ（クロム）、Ｃｅ（セリウム）、Ｐｒ（プラセオジム）、Ｌａ（ランタン）、Ｇｄ（ガドリニウム）、Ｔｂ（テルビウム）、Ｄｙ（ジスプロシウム）、Ｈｏ（ホルミウム）、Ｅｒ（エルビウム）、Ｔｍ（ツリウム）、Ｙｂ（イッテルビウム）、Ｆｅ（鉄）、Ｚｎ（亜鉛）、Ｔｉ（チタン）等が用いられるが、特にこれらに限定されない。 Activators for a) inorganic fluorescent powders, including the activators used in the present invention, include, but are not limited to, Mn (manganese), Eu (europium), Cr (chromium), Ce (cerium), Pr (praseodymium), La (lanthanum), Gd (gadolinium), Tb (terbium), Dy (dysprosium), Ho (holmium), Er (erbium), Tm (thulium), Yb (ytterbium), Fe (iron), Zn (zinc), Ti (titanium), etc.
本発明で用いられるａ）無機蛍光粉体は、結晶母体及び／又は賦活剤としてＡｌ（アルミニウム）、Ｚｎ（亜鉛）、Ｍｇ（マグネシウム）、Ｓｉ（ケイ素）、Ｍｎ（マンガン）、Ｃａ（カルシウム）、Ｔｉ（チタン）、Ｃｅ（セリウム）、Ｂａ（バリウム）、Ｏ（酸素）、Ｐ（リン）、Ｓ（硫黄）の中から選択される少なくとも１種以上の元素を含有していることが好ましく、特に酸化（Ａｌ／Ｃａ／マンガン）、酸化（Ｍｇ／マンガン／チタン）、酸化亜鉛蛍光体、リン酸（Ｃａ／セリウム）が好ましい。 The inorganic fluorescent powder a) used in the present invention preferably contains at least one element selected from Al (aluminum), Zn (zinc), Mg (magnesium), Si (silicon), Mn (manganese), Ca (calcium), Ti (titanium), Ce (cerium), Ba (barium), O (oxygen), P (phosphorus), and S (sulfur) as a crystal matrix and/or activator, with (Al/Ca/manganese), (Mg/manganese/titanium), zinc oxide phosphor, and (Ca/cerium) phosphate being particularly preferred.
本発明で用いられるａ）無機蛍光粉体は、いずれの色の蛍光を発するものであってよく、特に赤色蛍光粉体、緑色蛍光粉体、青色蛍光粉体が好ましい。 The inorganic fluorescent powder a) used in the present invention may emit fluorescence of any color, with red fluorescent powder, green fluorescent powder, and blue fluorescent powder being particularly preferred.
ａ）無機蛍光粉体の有する最大蛍光波長は、４４０ｎｍ～５２０ｎｍ又は６４０ｎｍ～７００ｎｍの範囲であることが好ましい。 a) The maximum fluorescent wavelength of the inorganic fluorescent powder is preferably in the range of 440 nm to 520 nm or 640 nm to 700 nm.
本発明で用いられるａ）無機蛍光粉体の市販品としては、例えば、Ｌｕｍａｔｅ Ｒ（堺化学工業社製）、Ｌｕｍａｔｅ Ｇ（堺化学工業社製）、Ｌｕｍａｔｅ Ｂ（堺化学工業社製）等が挙げられるが、特にこれらに限定されない。 Commercially available examples of the inorganic fluorescent powder a) used in the present invention include Lumate R (manufactured by Sakai Chemical Industry Co., Ltd.), Lumate G (manufactured by Sakai Chemical Industry Co., Ltd.), Lumate B (manufactured by Sakai Chemical Industry Co., Ltd.), etc., but are not limited to these.
本発明で用いられるａ）無機蛍光粉体の粒子径は特に限定されないが、０．５μｍ以上であることが好ましく、１μｍ以上であることがより好ましい。また、ａ）無機蛍光粉体の粒子径は、３００μｍ以下であり、２００μｍ以下であることが好ましく、１５０μｍ以下であることがより好ましく、１００μｍ以下であることがさらに好ましい。本発明で用いられるａ）無機蛍光粉体の粒子径としては、十分な蛍光強度が得られ、化粧料等に用いた場合に使用感に優れる等の観点から、１μｍ以上２００μｍ以下であることが好ましく、２μｍ以上１００μｍ以下であることがより好ましい。 The particle size of the inorganic fluorescent powder a) used in the present invention is not particularly limited, but is preferably 0.5 μm or more, and more preferably 1 μm or more. The particle size of the inorganic fluorescent powder a) is 300 μm or less, preferably 200 μm or less, more preferably 150 μm or less, and even more preferably 100 μm or less. From the viewpoints of obtaining sufficient fluorescent intensity and providing excellent usability when used in cosmetics, etc., the particle size of the inorganic fluorescent powder a) used in the present invention is preferably 1 μm or more and 200 μm or less, and more preferably 2 μm or more and 100 μm or less.
なお、本願発明で用いる粒子径とは、透過型電子顕微鏡で観察した時の一次粒子における平均径のことを指す。 In addition, the particle size used in this invention refers to the average diameter of primary particles when observed with a transmission electron microscope.
本発明で用いられるｂ）非蛍光粉体は、蛍光特性を有さない粉体であれば特に限定されず、無機粉体でも有機粉体でもよく、形状や大きさも限定されない。 The non-fluorescent powder b) used in the present invention is not particularly limited as long as it is a powder that does not have fluorescent properties, and may be an inorganic or organic powder, and there is no limitation on the shape or size.
無機粉体としては、酸化チタン、非蛍光性酸化亜鉛、酸化鉄（ベンガラ、黄酸化鉄、黒酸化鉄）、シリカ、酸化アルミニウム、水酸化アルミニウム、酸化セシウム、酸化クロム、水酸化クロム、硫酸バリウム、合成金雲母、マイカ、タルク、セリサイト、カオリン、グンジョウ、コンジョウ、カーボンブラック、炭酸カルシウム、炭酸マグネシウム、シリコーン、ケイ酸マグネシウム、ケイ酸アルミニウムマグネシウム、窒化ホウ素等が挙げられるが、特にこれらに限定されない。 Inorganic powders include, but are not limited to, titanium oxide, non-fluorescent zinc oxide, iron oxide (red ocher, yellow iron oxide, black iron oxide), silica, aluminum oxide, aluminum hydroxide, cesium oxide, chromium oxide, chromium hydroxide, barium sulfate, synthetic phlogopite, mica, talc, sericite, kaolin, gunjo, konjo, carbon black, calcium carbonate, magnesium carbonate, silicone, magnesium silicate, magnesium aluminum silicate, boron nitride, etc.
無機粉体の市販品としては、例えば、ＭＰ－１１３３ＡＱ（テイカ社製）、ＭＰ－１１３３ＷＰ（テイカ社製）、ＭＴ－１００ＷＰ（テイカ社製）、ＭＴ－１００ＳＡ（テイカ社製）、ＭＴ－５００Ｂ（テイカ社製）、ＭＺ－３００（テイカ社製）、ＭＴＺ－３０４０ＴＳＷ（テイカ社製）、ＭＺ－５００（テイカ社製）、ＦＩＮＥＸ－３０（堺化学工業社製）、ＦＩＮＥＸ－５０（堺化学工業社製）、ＦＩＮＥＸ－３０Ｗ（堺化学工業社製）、ＦＩＮＥＸ－５０Ｗ（堺化学工業社製）、ＦＩＮＥＸ－５０Ｗ－ＬＰ２（堺化学工業社製）、ＡＥＲＯＳＩＬ ２００（日本アエロジル社製）、ＡＥＲＯＳＩＬ Ａｌｕ Ｃ（日本アエロジル社製）、ＬＬ－１００ＨＰ（チタン工業社製）、Ｒ－５１６ＨＰ（チタン工業社製）、ＢＬ－１００ＨＰ（チタン工業社製）、セリサイトＦＳＥ（三信鉱工社製）、シリカマイクロビード Ｐ－１５００（日揮触媒化成社製）、ＫＳＰ－１００（信越化学工業社製）、ＫＳＰ－３００（信越化学工業社製）等が挙げられるが、特にこれらに限定されない。 Commercially available inorganic powders include, for example, MP-1133AQ (manufactured by Teika Corporation), MP-1133WP (manufactured by Teika Corporation), MT-100WP (manufactured by Teika Corporation), MT-100SA (manufactured by Teika Corporation), MT-500B (manufactured by Teika Corporation), MZ-300 (manufactured by Teika Corporation), MTZ-3040TSW (manufactured by Teika Corporation), MZ-500 (manufactured by Teika Corporation), FINEX-30 (manufactured by Sakai Chemical Industry Co., Ltd.), FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd.), FINEX-30W (manufactured by Sakai Chemical Industry Co., Ltd.), FINEX-50W (manufactured by Sakai Chemical Industry Co., Ltd.), FINEX-50W-LP2 (manufactured by Sakai Chemical Industry Co., Ltd.), AEROSIL 200 (manufactured by Nippon Aerosil Co., Ltd.), AEROSIL Alu C (manufactured by Nippon Aerosil Co., Ltd.), LL-100HP (manufactured by Titan Kogyo Co., Ltd.), R-516HP (manufactured by Titan Kogyo Co., Ltd.), BL-100HP (manufactured by Titan Kogyo Co., Ltd.), Sericite FSE (manufactured by Sanshin Kogyo Co., Ltd.), Silica Microbead P-1500 (manufactured by JGC Catalysts and Chemicals Co., Ltd.), KSP-100 (manufactured by Shin-Etsu Chemical Co., Ltd.), KSP-300 (manufactured by Shin-Etsu Chemical Co., Ltd.), etc., but are not limited to these.
有機粉体としては、ポリエチレン、ポリアミド、架橋ポリスチレン、ポリメタクリル酸メチル、セルロース、カルバメート、フッ素樹脂、ポリオレフィン、エポキシ樹脂、フェノール樹脂、小麦でんぷん、シルク、長鎖脂肪酸塩、セラミド、リン脂質等が挙げられるが、特にこれらに限定されない。 Organic powders include, but are not limited to, polyethylene, polyamide, cross-linked polystyrene, polymethyl methacrylate, cellulose, carbamate, fluororesin, polyolefin, epoxy resin, phenolic resin, wheat starch, silk, long-chain fatty acid salts, ceramide, phospholipids, and the like.
有機粉体の市販品としては、例えば、ガンツパールＧＭＸ－０６１０（アイカ工業社製）、ガンツパールＧＭＸ－０６１０ＡＱ（アイカ工業社製）、ＳＰ－５００（東レ社製）、Ｃｅｒａｍｉｄｅ Ｉ（Ｅｖｏｎｉｋ社製）、Ｃｅｒａｍｉｄｅ III（Ｅｖｏｎｉｋ社製）、Ｃｅｒａｍｉｄｅ VI（Ｅｖｏｎｉｋ社製）、Ｐｈｙｔｏｐｒｅｓｏｍｅ Ｃａｒｅ－Ｖ（日本精化社製）、Ｃｅｒａｍｉｄｅ ＴＩＣ－００１（高砂香料工業社製）、ＳＬＰ－ＰＣ７０（辻精油社製）、ＳＬＰ－ＰＣ９２Ｈ（辻精油社製）、ＮＩＫＫＯＬ レシノールＳ－１０（日光ケミカルズ社製）等が挙げられるが、特にこれらに限定されない。 Examples of commercially available organic powders include, but are not limited to, Ganz Pearl GMX-0610 (manufactured by Aica Kogyo Co., Ltd.), Ganz Pearl GMX-0610AQ (manufactured by Aica Kogyo Co., Ltd.), SP-500 (manufactured by Toray Industries, Inc.), Ceramide I (manufactured by Evonik Co., Ltd.), Ceramide III (manufactured by Evonik Co., Ltd.), Ceramide VI (manufactured by Evonik Co., Ltd.), Phytopresome Care-V (manufactured by Nippon Fine Chemicals Co., Ltd.), Ceramide TIC-001 (manufactured by Takasago International Corporation), SLP-PC70 (manufactured by Tsuji Oils Co., Ltd.), SLP-PC92H (manufactured by Tsuji Oils Co., Ltd.), and NIKKOL Resinol S-10 (manufactured by Nikko Chemicals Co., Ltd.).
本発明で用いられる非蛍光粉体は無機粉体が好ましく、中でも金属酸化物、金属水酸化物、ケイ酸化物が好ましい。さらに金属酸化物とケイ酸化物は好ましく、酸化チタン、非蛍光性酸化亜鉛、酸化鉄、酸化アルミニウム（アルミナ）、シリカが特に好ましい。 The non-fluorescent powder used in the present invention is preferably an inorganic powder, and among these, metal oxides, metal hydroxides, and silicates are preferred. Metal oxides and silicates are more preferred, and titanium oxide, non-fluorescent zinc oxide, iron oxide, aluminum oxide (alumina), and silica are particularly preferred.
また、本発明で用いられるｂ）非蛍光粉体の粒子径は、本願発明で用いられる無機蛍光粉体の粒子径よりも小さい方が好ましく、２５０ｎｍ以下であることが好ましく、１００ｎｍ以下の微粒子であることがより好ましい。また、本発明の複合粒子の蛍光強度を向上させる効果の観点から、０．１ｎｍ以上であることが好ましく、１ｎｍ以上であることがより好ましい。本発明で用いられる非蛍光粉体の粒子径としては、０．１ｎｍ以上１５０ｎｍ以下であることが好ましく、１ｎｍ以上１００ｎｍ以下であることがより好ましい。 The particle size of the non-fluorescent powder b) used in the present invention is preferably smaller than the particle size of the inorganic fluorescent powder used in the present invention, and is preferably 250 nm or less, and more preferably a fine particle of 100 nm or less. From the viewpoint of the effect of improving the fluorescence intensity of the composite particle of the present invention, it is preferably 0.1 nm or more, and more preferably 1 nm or more. The particle size of the non-fluorescent powder used in the present invention is preferably 0.1 nm or more and 150 nm or less, and more preferably 1 nm or more and 100 nm or less.
本願発明で用いられるａ）無機蛍光粉体及び／又はｂ）非蛍光粉体は、複合化させる粉体の組み合わせによって、粉体同士の付着性を向上させたり、得られる複合粉体の蛍光強度をより高める等の目的で、表面処理がなされていてもよい。この表面処理は、複合化前のそれぞれの粉体に対して行ってもよいし、得られた複合粉体に対して行ってもよい。 The inorganic fluorescent powder a) and/or non-fluorescent powder b) used in the present invention may be surface-treated to improve adhesion between the powders or to increase the fluorescence intensity of the resulting composite powder, depending on the combination of powders to be composited. This surface treatment may be performed on each powder before composite formation, or on the resulting composite powder.
表面処理に用いられる物質の種類としては、シリカ、アルギン酸、酸化アルミニウム（アルミナ）、ＰＯＥ／ジメチコン共重合体、ポリエチレングリコール、水酸化アルミニウム、アミノ酸、金属石ケン、パーフルオロアルキルエチルリン酸エステルジエタノールアミン酸、フッ素アルキルアクリレート／ポリアルキレングリコールアクリレートポリマー、パーフルオロポリエーテルリン酸、パーフルオロポリエーテル鎖を有するアニオン性又はカチオン性高分子、水素添加レシチン、アシル化アミノ酸、α－トコフェロールリン酸エステル酸、メチルハイドロジェンポリシロキサン、α－モノアルコキシポリジメチルシロキサン、α－ジアルコキシポリジメチルシロキサン、トリエトキシシリルエチルポリジメチルシロキシエチルジメチコン、アモジメチコン、トリエトキシカプリリルシラン、アミノプロピルトリエトキシシラン、パーフルオロオクチルエチルトリエトキシシラン、パーフルオロオクチルトリエトキシシラン、等が挙げられるが、これらに限定されない。中でも、親水性の表面処理が好ましく、特に、シリカ、アルギン酸、酸化アルミニウム（アルミナ）、ＰＯＥ／ジメチコン共重合体、ポリエチレングリコール、水酸化アルミニウムが好ましい。 Types of substances used for surface treatment include, but are not limited to, silica, alginic acid, aluminum oxide (alumina), POE/dimethicone copolymer, polyethylene glycol, aluminum hydroxide, amino acids, metal soaps, perfluoroalkylethyl phosphate ester diethanolamine acid, fluoroalkyl acrylate/polyalkylene glycol acrylate polymer, perfluoropolyether phosphate, anionic or cationic polymers with perfluoropolyether chains, hydrogenated lecithin, acylated amino acids, α-tocopherol phosphate ester acid, methylhydrogenpolysiloxane, α-monoalkoxypolydimethylsiloxane, α-dialkoxypolydimethylsiloxane, triethoxysilylethyl polydimethylsiloxyethyl dimethicone, amodimethicone, triethoxycaprylylsilane, aminopropyltriethoxysilane, perfluorooctylethyltriethoxysilane, perfluorooctyltriethoxysilane, etc. Among these, hydrophilic surface treatments are preferred, with silica, alginic acid, aluminum oxide (alumina), POE/dimethicone copolymer, polyethylene glycol, and aluminum hydroxide being particularly preferred.
また、ａ）無機蛍光粉体及び／又はｂ）非蛍光粉体に対しては、複数の表面処理がなされていてもよく、表面処理率（粉体に対する表面処理剤量の割合）や表面処理方法も特に限定されない。 In addition, a) the inorganic fluorescent powder and/or b) the non-fluorescent powder may be subjected to multiple surface treatments, and the surface treatment rate (ratio of the amount of surface treatment agent to the powder) and the surface treatment method are not particularly limited.
本発明において用いられるａ）無機蛍光粉体及び／又はｂ）非蛍光粉体は、後述する複合粉体の調製方法での湿式処理において付着力が高いという点で、表面が親水性であることが好ましい。中でも、少なくとも１つ以上の親水性の表面処理がなされていることが好ましく、最表面に親水性の表面処理がなされていることが特に好ましい。ここで、親水性の表面処理としては、例えばシリカ、アルギン酸、酸化アルミニウム（アルミナ）、水酸化アルミニウム、アミノ酸、ポリエチレングリコール、ＰＯＥ／ジメチコン共重合体処理等が挙げられるが特にこれらに限定されない。 The a) inorganic fluorescent powder and/or b) non-fluorescent powder used in the present invention preferably have a hydrophilic surface in that they have high adhesion in the wet treatment of the composite powder preparation method described below. In particular, it is preferable that at least one hydrophilic surface treatment is performed, and it is particularly preferable that the outermost surface is subjected to a hydrophilic surface treatment. Here, examples of hydrophilic surface treatments include, but are not limited to, silica, alginic acid, aluminum oxide (alumina), aluminum hydroxide, amino acid, polyethylene glycol, and POE/dimethicone copolymer treatments.
本願発明における複合粉体の調製方法は特に限定されないが、湿式処理が好ましい。 The method for preparing the composite powder in the present invention is not particularly limited, but wet processing is preferred.
湿式処理では、分散媒中にａ）無機蛍光粉体とｂ）非蛍光粉体を分散し、ｂ）非蛍光粉体をａ）無機蛍光粉体の表面の少なくとも一部に被覆させることが好ましい。また、ａ）無機蛍光粉体及び／又はｂ）非蛍光粉体を機械的撹拌力・解砕力により十分に分散させる方が好ましく、具体的にはマグネチックスターラー、ミキサー、超音波、ホモジナイザー、高圧ホモジナイザー、ディスパーミキサー、ビーズミル、コロイドミル、ローラーミル、三本ローラーミル、スタンプミル、ロッドミル、ボールミル、ジョークラッシャー、ニーダー、プラネタリーミキサー等が挙げられるが特にこれらに限定されず、２つ以上用いても構わない。 In the wet treatment, it is preferable to disperse a) inorganic fluorescent powder and b) non-fluorescent powder in a dispersion medium, and to coat at least a part of the surface of a) inorganic fluorescent powder with b) non-fluorescent powder. It is also preferable to thoroughly disperse a) inorganic fluorescent powder and/or b) non-fluorescent powder by mechanical stirring and crushing force, and specific examples of such a means include, but are not limited to, a magnetic stirrer, a mixer, an ultrasonic wave, a homogenizer, a high-pressure homogenizer, a disperser mixer, a bead mill, a colloid mill, a roller mill, a three-roller mill, a stamp mill, a rod mill, a ball mill, a jaw crusher, a kneader, a planetary mixer, etc., and two or more may be used.
また、ろ過や遠心分離、乾燥等の工程を付与してもよい。乾燥方法も特に限定されない。得られる複合粉体は、分散体やペーストとして用いてもよく、粉体として用いてもよい。 Furthermore, processes such as filtration, centrifugation, and drying may be added. The drying method is not particularly limited. The obtained composite powder may be used as a dispersion or paste, or as a powder.
湿式処理において用いる分散媒も特に限定されず、水、アルコール、炭化水素油、エステル油、シリコーン油、有機溶媒等が挙げられ、分散媒中に界面活性剤や塩、キレート剤等の成分を含有させてもよい。 The dispersion medium used in the wet treatment is not particularly limited, and examples include water, alcohol, hydrocarbon oil, ester oil, silicone oil, organic solvent, etc., and the dispersion medium may contain components such as surfactants, salts, and chelating agents.
湿式処理において用いる分散媒は、粉体同士の付着力が向上する等の理由から、親水性の分散媒が好ましく、少なくとも水を含んでいることが好ましい。 The dispersion medium used in the wet treatment is preferably a hydrophilic dispersion medium, preferably containing at least water, for reasons such as improving the adhesion between powder particles.
本発明の複合粉体におけるａ）無機蛍光粉体とｂ）非蛍光粉体の重量の割合は、ａ）無機蛍光粉体とｂ）非蛍光粉体のそれぞれの形状や大きさ等により適宜調整すればよいが、ａ成分（重量％）：ｂ成分（重量％）＝９５：５～７０：３０が好ましく、特に９０：１０～７０：３０が好ましい。また、上記割合は、例えば、複合粉体を調製する際の、ａ）成分、ｂ）成分の仕込み量（重量％）の割合としてもよい。 The weight ratio of a) inorganic fluorescent powder and b) non-fluorescent powder in the composite powder of the present invention may be adjusted appropriately depending on the shape and size of each of a) inorganic fluorescent powder and b) non-fluorescent powder, but a component a (wt%): component b (wt%) = 95:5 to 70:30 is preferable, and 90:10 to 70:30 is particularly preferable. The above ratio may also be, for example, the ratio of the amounts (wt%) of component a) and component b) charged when preparing the composite powder.
本発明の複合粉体は、蛍光強度が強いことから、様々な形態の化粧料等の皮膚外用組成物に好適に用いることができる。また、蛍光を活用できる照明や遊具、塗料等の分野においても好適に使用することができる。 The composite powder of the present invention has a strong fluorescent intensity and can therefore be suitably used in various forms of skin-applied compositions, such as cosmetics. It can also be suitably used in fields where fluorescence can be utilized, such as lighting, playground equipment, and paints.
＜皮膚外用組成物＞
本発明の外用組成物は、上述した本発明の複合粉体を含有する。本発明の複合粉体は、蛍光強度が強く、優れた発光性、色補正効果を示すため、これを含有する皮膚外用組成物は、傷痕を目立たなくしたり、肌の色味を整える、メーキャップ効果を付与する等の目的で、医薬品、医薬部外品、化粧料などの皮膚外用剤全般に使用できる。特にメーキャップ効果に優れることから、化粧品として好適に使用できる。
<Composition for external use on skin>
The composition for external use of the present invention contains the above-mentioned composite powder of the present invention. The composite powder of the present invention has a strong fluorescent intensity and exhibits excellent luminescence and color correction effects, so that the composition for external use of the skin containing the composite powder can be used in general as an external agent for the skin, such as medicines, quasi-drugs, and cosmetics, for the purpose of making scars less noticeable, adjusting the skin color, imparting makeup effects, etc. In particular, since the composite powder has an excellent makeup effect, it can be suitably used as a cosmetic.
本発明の皮膚外用組成物における複合粉体の含有量としては、０．０００１重量％以上５０重量％以下であり、０．００１重量％以上３０重量％以下であることが好ましく、０．０１重量％以上２０重量％以下であることがより好ましく、０．０１重量％以上１０重量％以下であることがさらに好ましく、０．０１重量％以上５重量％以下であることが特に好ましい。 The content of the composite powder in the topical skin composition of the present invention is from 0.0001% by weight to 50% by weight, preferably from 0.001% by weight to 30% by weight, more preferably from 0.01% by weight to 20% by weight, even more preferably from 0.01% by weight to 10% by weight, and particularly preferably from 0.01% by weight to 5% by weight.
本発明の皮膚外用組成物は、本発明の複合粉体以外に、本発明の効果を損なわない範囲で、その他の成分を含んでいてもよい。 The skin topical composition of the present invention may contain other ingredients in addition to the composite powder of the present invention, as long as the effects of the present invention are not impaired.
その他の成分としては、種々の目的に応じて、油分、親油性非イオン界面活性剤、親水性非イオン界面活性剤、その他の界面活性剤、金属イオン封鎖剤、天然の水溶性高分子、半合成の水溶性高分子、合成の水溶性高分子、無機の水溶性高分子、各種の抽出液、各種粉体、保湿成分、多価アルコール、スクラブ剤、紫外線散乱成分、収斂成分、ペプチド又はその誘導体、アミノ酸又はその誘導体、洗浄成分、角質柔軟成分、細胞賦活化成分、老化防止成分、血行促進作用成分、美白成分、ＤＮＡの損傷の予防及び／又は修復作用を有する成分、抗炎症成分、抗酸化成分、ビタミン類、皮脂吸着成分、抗菌成分等のその他の成分を、本発明の効果を損なわない範囲で含んでいてもよい。本発明の皮膚外用組成物において、これらの成分は、１種又は２種以上組み合わせて配合してもよい。なお、これらの各成分としては、医薬品、医薬部外品、化粧品分野等において使用され得るものであれば特に制限されず、任意のものを適宜選択し使用することができる。 As other components, depending on various purposes, oils, lipophilic nonionic surfactants, hydrophilic nonionic surfactants, other surfactants, metal ion sequestering agents, natural water-soluble polymers, semi-synthetic water-soluble polymers, synthetic water-soluble polymers, inorganic water-soluble polymers, various extracts, various powders, moisturizing components, polyhydric alcohols, scrubbing agents, UV scattering components, astringent components, peptides or derivatives thereof, amino acids or derivatives thereof, cleansing components, keratin softening components, cell activating components, anti-aging components, blood circulation promoting components, whitening components, components having DNA damage prevention and/or repair effects, anti-inflammatory components, antioxidant components, vitamins, sebum adsorbing components, antibacterial components, and other components may be included within a range that does not impair the effects of the present invention. In the skin topical composition of the present invention, these components may be blended in combination of one or more types. In addition, there are no particular limitations on each of these components as long as they can be used in the fields of medicines, quasi-drugs, cosmetics, etc., and any one can be appropriately selected and used.
本発明の皮膚外用組成物は、本発明の複合粉体の他に、複合化していない蛍光粉体を含んでいてもよい。 The skin topical composition of the present invention may contain a non-complexed fluorescent powder in addition to the composite powder of the present invention.
本発明の皮膚外用組成物の製造方法は特に制限されず、必須成分である本発明の複合粉体、及び上記その他の成分等から適宜選択した成分を、配合して、常法により、混合して製造することができる。 The method for producing the topical skin composition of the present invention is not particularly limited, and it can be produced by blending and mixing the essential component, the composite powder of the present invention, and components appropriately selected from the above-mentioned other components, etc., in a conventional manner.
本発明の皮膚外用組成物の具体的用途としては、例えば、化粧水、保湿液、乳液、美容液、パック、ハンドクリーム、ボディローション、ボディークリーム、リップクリームのような基礎化粧料；洗顔料、メイク落とし、ボディーシャンプーのような洗浄用化粧料；ファンデーション、化粧下地、アイカラー、アイシャドー、アイライナー、アイブロウ、ハイライト、コントロールカラー、チーク、マスカラ、口紅、ファイスパウダーのようなメーキャップ化粧料；日焼け止め化粧料等の化粧料に用いることができる。また、これら化粧料の機能を１つの製剤にまとめた多機能型製剤も挙げられる。さらに、創傷用軟膏、ニキビ用外用剤等の医薬品・医薬部外品等にも用いることができる。 Specific applications of the skin topical composition of the present invention include, for example, basic cosmetics such as lotion, moisturizing lotion, milky lotion, beauty essence, pack, hand cream, body lotion, body cream, and lip cream; cleansing cosmetics such as face wash, makeup remover, and body shampoo; makeup cosmetics such as foundation, makeup base, eye color, eye shadow, eyeliner, eyebrow, highlight, control color, blush, mascara, lipstick, and face powder; and sunscreen cosmetics. In addition, multifunctional preparations that combine the functions of these cosmetics into one preparation are also included. Furthermore, the composition can be used in pharmaceuticals and quasi-drugs such as wound ointments and topical preparations for acne.
中でも、ファンデーション、化粧下地、アイカラー、アイシャドー、アイライナー、アイブロウ、ハイライト、コントロールカラー、チーク、マスカラ、口紅、ファイスパウダーのようなメーキャップ化粧料；日焼け止め化粧料等の化粧料が、特に好ましい。 Among these, makeup cosmetics such as foundations, makeup bases, eye colors, eye shadows, eyeliners, eyebrows, highlighters, control colors, blushes, mascaras, lipsticks, and face powders; sunscreen cosmetics, and other cosmetics are particularly preferred.
＜無機蛍光粉体の蛍光強度増強方法＞
本発明は、ａ）無機蛍光粉体の表面の一部にｂ）非蛍光粉体を被覆させることを特徴とする、無機蛍光粉体の蛍光強度増強方法も含む。また、ａ）無機蛍光粉体の表面の一部にｂ）非蛍光粉体を被覆させて得られた本発明の複合粉体は、優れた発光性を示すため、化粧料に含有させることで、よりメーキャップ効果の高い化粧料を提供することができるものである。なお、無機蛍光粉体の蛍光強度増強方法におけるａ）無機蛍光粉体、ｂ）非蛍光粉体の説明、これらを用いて調製される複合粉体の具体的な説明は、「複合粉体」の項の説明を適用できる。
<Method for enhancing fluorescence intensity of inorganic fluorescent powder>
The present invention also includes a method for enhancing the fluorescence intensity of an inorganic fluorescent powder, characterized in that a) a portion of the surface of an inorganic fluorescent powder is coated with b) a non-fluorescent powder. Furthermore, the composite powder of the present invention obtained by coating a portion of the surface of an inorganic fluorescent powder with b) a non-fluorescent powder exhibits excellent luminescence, and therefore, when contained in a cosmetic product, a cosmetic product with a stronger makeup effect can be provided. Note that the explanations of a) the inorganic fluorescent powder and b) the non-fluorescent powder in the method for enhancing the fluorescence intensity of an inorganic fluorescent powder and the specific explanation of the composite powder prepared using these can be applied to the explanations in the section "Composite Powder".
次にａ）無機蛍光粉体の表面の少なくとも一部をｂ）非蛍光粉体が被覆している複合粉体について実施例を挙げ、詳細を説明するが、本発明はこれらに限定されるものではない。 Next, we will provide examples of composite powders in which a) at least a portion of the surface of an inorganic fluorescent powder is coated with b) a non-fluorescent powder, and explain the details, but the present invention is not limited to these.
（実施例１）
シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 １．０％・蛍光波長は６６０ｎｍ）４．５ｇを水４５．５ｇ中に入れ、ディスパーミルで十分に分散させ、酸化（Ａｌ／Ｃａ／マンガン）水分散体を得た。次にアルミナ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・水酸化Ａｌ処理 ６％）０．５ｇを水４９．５ｇ中に入れ、ディスパーミルで十分に分散させ、アルミナ処理微粒子酸化チタン水分散体を得た。酸化（Ａｌ／Ｃａ／マンガン）水分散体中にアルミナ処理微粒子酸化チタン水分散体を混合させ、ディスパーミルで十分に分散後、ろ過、６０℃で一晩乾燥させた。乾燥後に凝集物をミルグラインダーで解砕し、無機蛍光複合粉体を得た。
Example 1
4.5 g of silica-treated (Al/Ca/manganese) oxide (plate-shaped, particle size 40 μm, aluminum hydroxide treatment 4.5%, silica treatment 1.0%, fluorescence wavelength 660 nm) was added to 45.5 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of (Al/Ca/manganese) oxide. Next, 0.5 g of alumina-treated fine particle titanium oxide (acicular, particle size 15 nm, aluminum hydroxide treatment 6%) was added to 49.5 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of alumina-treated fine particle titanium oxide. The aqueous dispersion of alumina-treated fine particle titanium oxide was mixed with the aqueous dispersion of (Al/Ca/manganese) oxide, thoroughly dispersed with a disper mill, filtered, and dried overnight at 60° C. After drying, the aggregates were crushed with a mill grinder to obtain an inorganic fluorescent composite powder.
（比較例１）
シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 １．０％・蛍光波長は６６０ｎｍ。）４．５ｇとアルミナ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・水酸化Ａｌ処理 ６％）０．５ｇをミルグラインダーで粉砕し、無機蛍光粉体混合物を得た。
(Comparative Example 1)
An inorganic fluorescent powder mixture was obtained by pulverizing 4.5 g of silica-treated (Al/Ca/manganese) oxide (plate-shaped, particle size 40 μm, 4.5% aluminum hydroxide treatment, 1.0% silica treatment, fluorescent wavelength 660 nm) and 0.5 g of alumina-treated titanium dioxide fine particle (acicular, particle size 15 nm, 6% aluminum hydroxide treatment) in a mill grinder.
（比較例２）
比較例２として、シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 １．０％・蛍光波長は６６０ｎｍ）を用いた。
(Comparative Example 2)
As Comparative Example 2, silica-treated oxide (Al/Ca/manganese) (plate-like, particle size 40 μm, aluminum hydroxide treatment 4.5%, silica treatment 1.0%, fluorescence wavelength 660 nm) was used.
＜複合化の確認＞
走査型電子顕微鏡 ＶＥ－８８００（キーエンス社製）を用いて実施例１の無機蛍光複合粉体と比較例２の無機蛍光粉体混合物を観察した。それぞれの顕微鏡写真を図１（実施例１）、図２（比較例２）として示した。
<Confirmation of compounding>
A scanning electron microscope VE-8800 (manufactured by Keyence Corporation) was used to observe the inorganic fluorescent composite powder of Example 1 and the inorganic fluorescent powder mixture of Comparative Example 2. The respective micrographs are shown in FIG. 1 (Example 1) and FIG. 2 (Comparative Example 2).
図１と図２を比較すると、明らかに実施例１においてシリカ処理酸化（Ａｌ／Ｃａ／マンガン）の表面にアルミナ処理微粒子酸化チタンが付着し、非蛍光粉体であるアルミナ処理微粒子酸化チタンが、無機蛍光粉体であるシリカ処理酸化（Ａｌ／Ｃａ／マンガン）の表面を被覆していることを確認できた。 Comparing Figures 1 and 2, it is clear that in Example 1, alumina-treated titanium dioxide fine particles adhere to the surface of the silica-treated oxide (Al/Ca/manganese), and it was confirmed that the alumina-treated titanium dioxide fine particles, which are non-fluorescent powder, cover the surface of the silica-treated oxide (Al/Ca/manganese), which is an inorganic fluorescent powder.
＜試験１ 蛍光強度の評価＞
プレート（５０ｍｍ×５０ｍｍ ＨＥＬＩＯＰＬＡＴＥ ＨＤ６、ＨｅｌｉｏＳｃｒｅｅｎ Ｌａｂｓ製）に両面テープを貼り、刷毛で均一に試料を塗布。分光変角色差計ＧＣ－５０００（日本電色工業社製）を用い、プレートの試料が塗布された面側に入射角４５°で光をあて、正反射角の反射強度を測定した。ａ）成分の蛍光波長における強度において、ａ）無機蛍光粉体のみの時の強度を１とした時の、各試料の蛍光波長における強度を比較した。
<Test 1: Evaluation of fluorescence intensity>
Double-sided tape was applied to a plate (50 mm x 50 mm, HELIOPLATE HD6, manufactured by HelioScreen Labs), and the sample was applied evenly with a brush. Using a GC-5000 spectroscopic goniochromator (manufactured by Nippon Denshoku Industries Co., Ltd.), light was applied to the side of the plate on which the sample was applied at an incident angle of 45°, and the reflection intensity at the regular reflection angle was measured. The intensity at the fluorescent wavelength of the component a) was compared when the intensity when only the inorganic fluorescent powder a) was present was taken as 1.
比較例２：ａ）無機蛍光粉体単体と、比較例１：ａ）無機蛍光粉体とｂ）非蛍光粉体の単純混合の、蛍光波長６６０ｎｍにおける反射強度を比較すると、ａ）無機蛍光粉体とｂ）非蛍光粉体を単純混合するだけでも約９倍に蛍光強度が増加した。実施例１：ａ）無機蛍光粉体とｂ）非蛍光粉体を複合粉体は、比較例１の約１４倍の強度を示し、複合化により、さらに蛍光強度が増加することが確認できた。 Comparing the reflection intensity at a fluorescent wavelength of 660 nm between a) inorganic fluorescent powder alone (Comparative Example 2) and a simple mixture of a) inorganic fluorescent powder and b) non-fluorescent powder (Comparative Example 1), the fluorescence intensity increased by about 9 times just by mixing a) inorganic fluorescent powder and b) non-fluorescent powder. Example 1: A composite powder of a) inorganic fluorescent powder and b) non-fluorescent powder showed an intensity about 14 times that of Comparative Example 1, and it was confirmed that the fluorescence intensity increased further by combining the two.
また、蛍光波長（６６０ｎｍ）の場合と、蛍光波長（４００ｎｍ）の場合で、蛍光強度を比較すると、蛍光波長（６６０ｎｍ）の方がより、蛍光強度が増加しており、ａ）成分の蛍光波長において、より顕著な強度増加が確認された。蛍光波長６６０ｎｍの蛍光強度が顕著に増強されることにより、赤味の映える粉体となった。 In addition, when comparing the fluorescence intensity at a fluorescent wavelength (660 nm) with that at a fluorescent wavelength (400 nm), the fluorescence intensity was greater at the fluorescent wavelength (660 nm), and a more significant increase in intensity was confirmed at the fluorescent wavelength of component a). The significant increase in fluorescence intensity at the fluorescent wavelength of 660 nm resulted in a powder with a striking reddish hue.
（実施例２）
シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 １．０％・蛍光波長６６０ｎｍ）０．９５ｇを水４９．０５ｇ中に入れ、ディスパーミルで十分に分散させ、酸化（Ａｌ／Ｃａ／マンガン）水分散体を得た。次にアルミナ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・水酸化Ａｌ処理 ６％）０．０５ｇを水４９．９ｇ中に入れ、ディスパーミルで十分に分散させ、アルミナ処理微粒子酸化チタン水分散体を得た。酸化（Ａｌ／Ｃａ／マンガン）水分散体中にアルミナ処理微粒子酸化チタン水分散体を混合させ、ディスパーミルで十分に分散後、ろ過、６０℃で一晩乾燥させた。乾燥後に凝集物をミルグラインダーで解砕し、無機蛍光複合粉体を得た。
Example 2
0.95 g of silica-treated (Al/Ca/manganese) oxide (plate-shaped, particle size 40 μm, aluminum hydroxide treatment 4.5%, silica treatment 1.0%, fluorescence wavelength 660 nm) was added to 49.05 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of (Al/Ca/manganese) oxide. Next, 0.05 g of alumina-treated fine particle titanium oxide (needle-shaped, particle size 15 nm, aluminum hydroxide treatment 6%) was added to 49.9 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of alumina-treated fine particle titanium oxide. The aqueous dispersion of alumina-treated fine particle titanium oxide was mixed with the aqueous dispersion of (Al/Ca/manganese) oxide, thoroughly dispersed with a disper mill, filtered, and dried overnight at 60° C. After drying, the aggregates were crushed with a mill grinder to obtain an inorganic fluorescent composite powder.
（実施例３）
シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 １．０％・蛍光波長６６０ｎｍ）０．８０ｇを水４９．２０ｇ中に入れ、ディスパーミルで十分に分散させ、酸化（Ａｌ／Ｃａ／マンガン）水分散体を得た。次にアルミナ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・水酸化Ａｌ処理 ６％）０．２０ｇを水４９．８０ｇ中に入れ、ディスパーミルで十分に分散させ、アルミナ処理微粒子酸化チタン水分散体を得た。酸化（Ａｌ／Ｃａ／マンガン）水分散体中にアルミナ処理微粒子酸化チタン水分散体を混合させ、ディスパーミルで十分に分散後、ろ過、６０℃で一晩乾燥させた。乾燥後に凝集物をミルグラインダーで解砕し、無機蛍光複合粉体を得た。
Example 3
0.80 g of silica-treated (Al/Ca/manganese) oxide (plate-shaped, particle size 40 μm, aluminum hydroxide treatment 4.5%, silica treatment 1.0%, fluorescence wavelength 660 nm) was added to 49.20 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of (Al/Ca/manganese) oxide. Next, 0.20 g of alumina-treated fine particle titanium oxide (needle-shaped, particle size 15 nm, aluminum hydroxide treatment 6%) was added to 49.80 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of alumina-treated fine particle titanium oxide. The aqueous dispersion of alumina-treated fine particle titanium oxide was mixed with the aqueous dispersion of (Al/Ca/manganese) oxide, thoroughly dispersed with a disper mill, filtered, and dried overnight at 60° C. After drying, the aggregates were crushed with a mill grinder to obtain an inorganic fluorescent composite powder.
（実施例４）
シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 １．０％・蛍光波長６６０ｎｍ）０．７０ｇを水４９．３０ｇ中に入れ、ディスパーミルで十分に分散させ、酸化（Ａｌ／Ｃａ／マンガン）水分散体を得た。次にアルミナ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・水酸化Ａｌ処理 ６％）０．３０ｇを水４９．７０ｇ中に入れ、ディスパーミルで十分に分散させ、アルミナ処理微粒子酸化チタン水分散体を得た。酸化（Ａｌ／Ｃａ／マンガン）水分散体中にアルミナ処理微粒子酸化チタン水分散体を混合させ、ディスパーミルで十分に分散後、ろ過、６０℃で一晩乾燥させた。乾燥後に凝集物をミルグラインダーで解砕し、無機蛍光複合粉体を得た。
Example 4
0.70 g of silica-treated (Al/Ca/manganese) oxide (plate-shaped, particle size 40 μm, aluminum hydroxide treatment 4.5%, silica treatment 1.0%, fluorescence wavelength 660 nm) was added to 49.30 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of (Al/Ca/manganese) oxide. Next, 0.30 g of alumina-treated fine particle titanium oxide (acicular, particle size 15 nm, aluminum hydroxide treatment 6%) was added to 49.70 g of water and thoroughly dispersed with a disper mill to obtain an aqueous dispersion of alumina-treated fine particle titanium oxide. The aqueous dispersion of alumina-treated fine particle titanium oxide was mixed with the aqueous dispersion of (Al/Ca/manganese) oxide, thoroughly dispersed with a disper mill, filtered, and dried overnight at 60° C. After drying, the aggregates were crushed with a mill grinder to obtain an inorganic fluorescent composite powder.
複合化処理を行った実施例１～４の蛍光強度を、複合化前のａ）無機蛍光粉体である比較例２の強度を１として、比較した。結果は表２に示す。 The fluorescence intensities of Examples 1 to 4, which had been subjected to the composite treatment, were compared with the intensity of Comparative Example 2, which was inorganic fluorescent powder a) before composite treatment, set at 1. The results are shown in Table 2.
（実施例５）
実施例１のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）を、粒子径１０μｍのシリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径１０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 ３．０％・蛍光波長６６０ｎｍ）に変え、無機蛍光複合粉体を得た。
Example 5
The silica-treated oxide (Al/Ca/manganese) of Example 1 was changed to silica-treated oxide (Al/Ca/manganese) having a particle diameter of 10 μm (plate-like, particle diameter 10 μm, aluminum hydroxide treatment 4.5%, silica treatment 3.0%, fluorescent wavelength 660 nm), to obtain an inorganic fluorescent composite powder.
（実施例６）
実施例３のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）を、粒子径１０μｍのシリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径１０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 ３．０％・蛍光波長６６０ｎｍ）に変え、無機蛍光複合粉体を得た。
Example 6
The silica-treated oxide (Al/Ca/manganese) of Example 3 was changed to silica-treated oxide (Al/Ca/manganese) having a particle diameter of 10 μm (plate-like, particle diameter 10 μm, aluminum hydroxide treatment 4.5%, silica treatment 3.0%, fluorescent wavelength 660 nm), to obtain an inorganic fluorescent composite powder.
（実施例７）
実施例４のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）を、粒子径１０μｍのシリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径１０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 ３．０％・蛍光波長６６０ｎｍ）に変え、無機蛍光複合粉体を得た。
(Example 7)
The silica-treated oxide (Al/Ca/manganese) of Example 4 was changed to silica-treated oxide (Al/Ca/manganese) having a particle diameter of 10 μm (plate-like, particle diameter 10 μm, aluminum hydroxide treatment 4.5%, silica treatment 3.0%, fluorescent wavelength 660 nm), to obtain an inorganic fluorescent composite powder.
（比較例３）
比較例３として、シリカ処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径１０μｍ・水酸化アルミニウム処理 ４．５％後、シリカ処理 ３．０％・蛍光波長６６０ｎｍ）を用いた。
(Comparative Example 3)
As Comparative Example 3, silica-treated oxide (Al/Ca/manganese) (plate-like, particle size 10 μm, aluminum hydroxide treatment 4.5%, silica treatment 3.0%, fluorescence wavelength 660 nm) was used.
複合化処理を行った実施例５～７の蛍光強度を、複合化前のａ）無機蛍光粉体である比較例３の強度を１として、比較した。結果を表３に示す。 The fluorescence intensity of Examples 5 to 7, which had undergone the composite treatment, was compared with the intensity of Comparative Example 3, which was inorganic fluorescent powder a) before composite treatment, set at 1. The results are shown in Table 3.
実施例１～４と比較例２より、ａ）成分とｂ）成分の比率を変えても、複合化により、蛍光強度の増強が確認できた。 From Examples 1 to 4 and Comparative Example 2, it was confirmed that the fluorescence intensity was enhanced by the conjugation even when the ratio of components a) and b) was changed.
また、ａ）成分の粒子径を変えても（実施例５～７）同様に、複合化により、蛍光強度の増強が確認できた。特にａ：ｂ＝９０：１０～７０：３０において顕著に蛍光強度が上昇した。 Furthermore, even when the particle size of component a) was changed (Examples 5 to 7), it was confirmed that the fluorescence intensity was enhanced by the complexation. In particular, the fluorescence intensity increased significantly when the a:b ratio was between 90:10 and 70:30.
（実施例８）
実施例１のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）をアルギン酸処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・アルギン酸処理 ３％・蛍光波長は６６０ｎｍ）に変え、無機蛍光複合粉体を得た。
(Example 8)
The silica-treated oxide (Al/Ca/manganese) in Example 1 was changed to alginic acid-treated oxide (Al/Ca/manganese) (plate-like, particle size 40 μm, alginic acid treatment 3%, fluorescent wavelength 660 nm), to obtain an inorganic fluorescent composite powder.
（実施例９）
実施例８のアルミナ処理微粒子酸化チタンをシリカ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・シリカ処理 ３０％）に変え、無機複合粉体を得た。
(Example 9)
An inorganic composite powder was obtained by changing the alumina-treated fine particle titanium dioxide of Example 8 to a silica-treated fine particle titanium dioxide (acicular, particle diameter 15 nm, silica treatment 30%).
（実施例１０）
実施例１のアルミナ処理微粒子酸化チタンをアルミナ（略球状・粒子径１３ｎｍ・表面処理なし）に変え、無機蛍光複合粉体を得た。
(Example 10)
The alumina-treated titanium oxide fine particle of Example 1 was changed to alumina (approximately spherical, particle diameter 13 nm, no surface treatment), to obtain an inorganic fluorescent composite powder.
（実施例１１）
実施例１のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）をアルギン酸処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・アルギン酸処理 １％・蛍光波長は６６０ｎｍ）に変え、さらにアルミナ処理微粒子酸化チタンをシリカ（略球状・粒子径１２ｎｍ・表面処理なし）に変え、無機蛍光複合粉体を得た。
Example 11
The silica-treated titanium dioxide (Al/Ca/manganese) in Example 1 was changed to an alginic acid-treated titanium dioxide (Al/Ca/manganese) (plate-like, particle size 40 μm, 1% alginic acid treatment, fluorescent wavelength 660 nm), and the alumina-treated titanium dioxide fine particle was changed to silica (approximately spherical, particle size 12 nm, no surface treatment), to obtain an inorganic fluorescent composite powder.
（実施例１２）
実施例３のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）をアルギン酸処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４０μｍ・アルギン酸処理 １％・蛍光波長は６６０ｎｍ）に変え、さらにアルミナ処理微粒子酸化チタンをシリカ処理顔料級酸化チタン（略球状・粒子径２５０ｎｍ・水酸化Ａｌ処理 ２．６％後にシリカ処理 ５．０％）に変え、無機複合粉体を得た。
Example 12
The silica-treated titanium dioxide (Al/Ca/manganese) in Example 3 was changed to alginic acid-treated titanium dioxide (Al/Ca/manganese) (plate-like, particle size 40 μm, 1% alginic acid treatment, fluorescence wavelength 660 nm), and the alumina-treated fine particle titanium dioxide was changed to silica-treated pigment-grade titanium dioxide (approximately spherical, particle size 250 nm, 2.6% Al hydroxide treatment followed by 5.0% silica treatment) to obtain an inorganic composite powder.
（実施例１３）
実施例１２のシリカ処理顔料級酸化チタンをＰＯＥ・ジメチコン共重合体処理微粒子酸化亜鉛（略球状・粒子径３５ｎｍ・トリエトキシカプリリルシラン処理 ３．６％後、ポリオキシエチレン・メチルポリシロキサン共重合体処理 １０．０％）に変え、無機蛍光複合粉体を得た。
Example 13
The silica-treated pigment-grade titanium oxide of Example 12 was changed to fine particle zinc oxide treated with a POE-dimethicone copolymer (approximately spherical, particle size 35 nm, treated with 3.6% triethoxycaprylylsilane, and then treated with 10.0% polyoxyethylene-methylpolysiloxane copolymer), to obtain an inorganic fluorescent composite powder.
（比較例４）
比較例４として、アルギン酸処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４μｍ・アルギン酸処理 ３％・蛍光波長６６０ｎｍ）を用いた。
(Comparative Example 4)
As Comparative Example 4, alginic acid-treated oxide (Al/Ca/manganese) (plate-like, particle size 4 μm, alginic acid treatment 3%, fluorescence wavelength 660 nm) was used.
（比較例５）
比較例５として、アルギン酸処理酸化（Ａｌ／Ｃａ／マンガン）（板状・粒子径４μｍ・アルギン酸処理 １％・蛍光波長６６０ｎｍ）を用いた。
(Comparative Example 5)
As Comparative Example 5, alginic acid-treated oxide (Al/Ca/manganese) (plate-like, particle size 4 μm, alginic acid treatment 1%, fluorescence wavelength 660 nm) was used.
それぞれの実施例で得られた無機蛍光複合粉体において、複合していないａ）無機蛍光粉体と蛍光強度を１として比較した結果は表４のようになった（実施例８、９は比較例４と、実施例１０は比較例２と、実施例１１～１３は比較例５で強度の比を求めた）。 The inorganic fluorescent composite powders obtained in each Example were compared with the non-composite a) inorganic fluorescent powder, with the fluorescence intensity set at 1, and the results are shown in Table 4 (the intensity ratio was calculated for Examples 8 and 9 with Comparative Example 4, for Example 10 with Comparative Example 2, and for Examples 11 to 13 with Comparative Example 5).
（実施例１４）
実施例１のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）をリン酸（Ｃａ／セリウム）（Ｌｕｍａｔｅ Ｂ（堺化学工業社製、最大蛍光波長 ４６０ｎｍ））に変え、無機蛍光複合粉体を得た。
(Example 14)
The silica-treated oxide (Al/Ca/manganese) in Example 1 was changed to phosphate (Ca/cerium) (Lumate B (manufactured by Sakai Chemical Industry Co., Ltd., maximum fluorescent wavelength 460 nm)), to obtain an inorganic fluorescent composite powder.
（実施例１５）
実施例１のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）を酸化亜鉛蛍光体（Ｌｕｍａｔｅ Ｇ（堺化学工業社製、最大蛍光波長 ５００ｎｍ））に変え、アルミナ処理微粒子酸化チタンをシリカ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・シリカ処理 ３０％）に変え、無機蛍光複合粉体を得た。
(Example 15)
The silica-treated oxide (Al/Ca/manganese) in Example 1 was changed to a zinc oxide phosphor (Lumate G (manufactured by Sakai Chemical Industry Co., Ltd., maximum fluorescent wavelength 500 nm)), and the alumina-treated titanium dioxide fine particle was changed to a silica-treated titanium dioxide fine particle (acicular, particle diameter 15 nm, silica treatment 30%), to obtain an inorganic fluorescent composite powder.
（実施例１６）
実施例１のシリカ処理酸化（Ａｌ／Ｃａ／マンガン）を酸化（Ｍｇ／マンガン／チタン）（Ｌｕｍａｔｅ Ｒ（堺化学工業社製、最大蛍光波長６６０ｎｍ））に変え、アルミナ処理微粒子酸化チタンをシリカ処理微粒子酸化チタン（針状・粒子径１５ｎｍ・シリカ処理 ３０％）に変え、無機蛍光複合粉体を得た。
(Example 16)
The silica-treated oxide (Al/Ca/manganese) in Example 1 was changed to oxide (Mg/manganese/titanium) (Lumate R (manufactured by Sakai Chemical Industry Co., Ltd., maximum fluorescent wavelength 660 nm)), and the alumina-treated titanium dioxide fine particle was changed to silica-treated titanium dioxide fine particle (acicular, particle diameter 15 nm, silica treatment 30%), to obtain an inorganic fluorescent composite powder.
（比較例６）
比較例６として、リン酸（Ｃａ／セリウム）（Ｌｕｍａｔｅ Ｂ（堺化学工業社製、最大蛍光波長 ４６０ｎｍ））を用いた。
(Comparative Example 6)
In Comparative Example 6, calcium/cerium phosphate (Lumate B (manufactured by Sakai Chemical Industry Co., Ltd., maximum fluorescent wavelength 460 nm)) was used.
（比較例７）
比較例７として、酸化亜鉛蛍光体（Ｌｕｍａｔｅ Ｇ（堺化学工業社製、最大蛍光波長 ５００ｎｍ））を用いた。
(Comparative Example 7)
In Comparative Example 7, a zinc oxide phosphor (Lumate G (manufactured by Sakai Chemical Industry Co., Ltd., maximum fluorescent wavelength 500 nm)) was used.
（比較例８）
比較例８として、酸化（Ｍｇ／マンガン／チタン）（Ｌｕｍａｔｅ Ｒ（堺化学工業社製、最大蛍光波長６６０ｎｍ）を使用。）を用いた。
(Comparative Example 8)
In Comparative Example 8, Mg/manganese/titanium oxide (Lumate R (manufactured by Sakai Chemical Industry Co., Ltd., maximum fluorescent wavelength 660 nm) was used).
実施例１４と比較例６の４６０ｎｍにおける蛍光強度の比較と、実施例１５と比較例７の５００ｎｍにおける蛍光強度の比較、実施例１６と比較例８の６６０ｎｍにおける蛍光強度の比較をそれぞれ行った結果は表５のようになった。いずれも比較例の強度を１として強度比を求めた。 The results of comparing the fluorescence intensity at 460 nm between Example 14 and Comparative Example 6, the fluorescence intensity at 500 nm between Example 15 and Comparative Example 7, and the fluorescence intensity at 660 nm between Example 16 and Comparative Example 8 are shown in Table 5. In all cases, the intensity ratio was calculated by setting the intensity of the comparative example to 1.
＜化粧料への応用例＞
次に無機蛍光複合粉体を配合した皮膚外用組成物（化粧料）の処方例を示すが、これらに限定されるものではない。
<Application to cosmetics>
Next, examples of formulations of skin external compositions (cosmetics) containing the inorganic fluorescent complex powder are shown below, but the present invention is not limited to these.
［パウダーファンデーション］
成分名 配合量［％］
シリコーン処理タルク 残余
フッ素処理セリサイト ５
シリコーン処理顔料級酸化チタン ５
シリコーン処理微粒子酸化チタン ５
窒化ホウ素 ３
（ビニルジメチコン／メチコンシルセスキオキサン）クロスポリマー ２
ナイロン末 １
ステアリン酸Ｍｇ １
実施例１の無機蛍光複合粉体 ３
メチルフェニルポリシロキサン ７
パラメトキシケイヒ酸２－エチルヘキシル ５
ビスエチルヘキシルオキシフェノールメトキシフェニルトリアジン １
イソステアリン酸ソルビタン ０．５
着色顔料 適量
防腐剤 適量
合計 １００
[Powder Foundation]
Ingredient name Amount [%]
Silicone-treated talc Residual fluorine-treated sericite 5
Silicone-treated pigment-grade titanium dioxide 5
Silicone-treated titanium dioxide particles 5
Boron nitride 3
(Vinyl dimethicone/methicone silsesquioxane) crosspolymer 2
Nylon powder 1
Magnesium stearate 1
Inorganic fluorescent composite powder of Example 1 3
Methylphenylpolysiloxane 7
2-Ethylhexyl paramethoxycinnamate 5
Bis-ethylhexyloxyphenol methoxyphenyl triazine 1
Sorbitan isostearate 0.5
Color pigment (appropriate amount)
Preservatives (appropriate amount)
Total 100
メーキャップ効果の優れたパウダーファンデーションが得られた。 A powder foundation with excellent makeup effects was obtained.
［ルースパウダー］
成分名 配合量［％］
シリコーン処理タルク 残余
フッ素処理セリサイト ５
ポリメチルシルセスキオキサン ７
実施例１の無機蛍光複合粉体 ５
シリコーン処理顔料級酸化チタン ３
雲母チタン ３
着色顔料 適量
防腐剤 適量
合計 １００
[Loose powder]
Ingredient name Amount [%]
Silicone-treated talc Residual fluorine-treated sericite 5
Polymethylsilsesquioxane 7
Inorganic fluorescent composite powder of Example 1 5
Silicone-treated pigment-grade titanium dioxide 3
Mica Titanium 3
Color pigment (appropriate amount)
Preservatives (appropriate amount)
Total 100
［化粧下地］
成分名 配合量［％］
水 残余
ＢＧ １０
１，３－ペンタンジオール １
キサンタンガム ０．１
ヒドロキシプロピルメチルセルロース ０．２
（アクリル酸ヒドロキシエチル／アクリロイルジメチルタウリンＮａ）コポリマー
０．５
ポリソルベート６０ １．５
ステアリン酸グリセリル １．５
パラメトキシケイヒ酸２－エチルヘキシル ８
イソステアリン酸処理微粒子酸化亜鉛 ２
ジエチルアミノヒドロキシ安息香酸ヘキシル ３
イソノナン酸イソノニル ３
メチルポリシロキサン ３
実施例３の無機蛍光複合粉体 １
雲母チタン １
着色顔料 適量
防腐剤 適量
合計 １００
[Makeup base]
Ingredient name Amount [%]
Water Residual BG 10
1,3-Pentanediol 1
Xanthan gum 0.1
Hydroxypropyl methylcellulose 0.2
(Hydroxyethyl acrylate/Sodium acryloyldimethyltaurate) copolymer
0.5
Polysorbate 60 1.5
Glyceryl stearate 1.5
2-Ethylhexyl paramethoxycinnamate 8
Isostearic acid treated zinc oxide particles 2
Hexyl diethylaminohydroxybenzoate 3
Isononyl isononanoate 3
Methylpolysiloxane 3
Inorganic fluorescent composite powder of Example 3 1
Mica titanium 1
Color pigment (appropriate amount)
Preservatives (appropriate amount)
Total 100
メーキャップ効果の優れた化粧下地が得られた。 A makeup base with excellent makeup effects was obtained.
［サンスクリーン］
成分名 配合量［％］
シクロペンタシロキサン 残余
メチルフェニルポリシロキサン ５
パラメトキシケイヒ酸２－エチルヘキシル ６
ビスエチルヘキシルオキシフェノールメトキシフェニルトリアジン ３
イソノナン酸イソノニル ７
シリコーン処理微粒子酸化亜鉛 ３
ラウリルＰＥＧ－９ポリジメチルシロキシエチルジメチコン ２
イソステアリン酸ソルビタン １
ステアリン酸処理した実施例１の無機蛍光複合粉体 １
水 ２５
ＤＰＧ ５
キサンタンガム ０．１
エタノール ５
防腐剤 適量
合計 １００
[Sunscreen]
Ingredient name Amount [%]
Cyclopentasiloxane Residual methylphenylpolysiloxane 5
2-Ethylhexyl paramethoxycinnamate 6
Bis-ethylhexyloxyphenol methoxyphenyl triazine 3
Isononyl isononanoate 7
Silicone-treated zinc oxide microparticles 3
Lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone 2
Sorbitan isostearate 1
Inorganic fluorescent composite powder of Example 1 treated with stearic acid 1
Water 25
DPG 5
Xanthan gum 0.1
Ethanol 5
Preservatives (appropriate amount)
Total 100
メーキャップ効果の優れたサンスクリーンが得られた。 A sunscreen with excellent makeup effects was obtained.
本発明によれば、無機蛍光粉体が本来有する蛍光強度を顕著に向上させた複合粉体を提供することができる。また、本発明の複合粉体は、優れた発光性を示すため、化粧料に含有させることで、よりメーキャップ効果の高い様々な形態の化粧料を提供することができる。さらに化粧料だけでなく、照明や遊具、塗料等の分野においても使用することができる。 According to the present invention, it is possible to provide a composite powder that significantly improves the fluorescence intensity inherent to inorganic fluorescent powders. Furthermore, since the composite powder of the present invention exhibits excellent luminescence, by incorporating it into cosmetics, it is possible to provide cosmetics in various forms with a stronger makeup effect. Furthermore, it can be used not only in cosmetics, but also in fields such as lighting, play equipment, and paints.
Claims (7)
ｂ）非蛍光粉体が、酸化チタン、非蛍光性酸化亜鉛、マイカ、シリカ、酸化アルミニウム、水酸化アルミニウム、酸化セシウム、硫酸バリウム、タルク、セリサイト、カオリン、炭酸カルシウム、炭酸マグネシウム、シリコーン、ケイ酸マグネシウム、ケイ酸アルミニウムマグネシウム、窒化ホウ素、ポリエチレン、ポリアミド、架橋ポリスチレン、ポリメタクリル酸メチル、セルロース、カルバメート、フッ素樹脂、ポリオレフィン、エポキシ樹脂、フェノール樹脂、小麦でんぷん、シルク、長鎖脂肪酸塩、セラミド、及びリン脂質からなる群より選択される少なくとも１種であることを特徴とする皮膚外用組成物用複合粉体（但し、ａ）無機蛍光粉体が、酸窒化物または窒化物で形成された蛍光体であるもの、及びＹ３Ａｌ５Ｏ１２：Ｃｅ３＋である蛍光体であるものを除く）。 At least a part of the surface of the inorganic fluorescent powder a) is covered with the non-fluorescent powder b), and the ratio of the inorganic fluorescent powder a) to the non-fluorescent powder b) is component a:component b=90 (wt%):10 (wt%) to 70 (wt%):30 (wt%) ;
b) A composite powder for a composition for external application to skin, characterized in that the non-fluorescent powder is at least one selected from the group consisting of titanium oxide, non-fluorescent zinc oxide, mica, silica, aluminum oxide, aluminum hydroxide, cesium oxide, barium sulfate, talc, sericite, kaolin, calcium carbonate, magnesium carbonate, silicone, magnesium silicate, magnesium aluminum silicate, boron nitride, polyethylene, polyamide, cross-linked polystyrene, polymethyl methacrylate, cellulose, carbamate, fluororesin, polyolefin, epoxy resin, phenolic resin, wheat starch, silk, long-chain fatty acid salt, ceramide, and phospholipid (however, excluding a) the inorganic fluorescent powder which is a phosphor formed of an oxynitride or nitride , and a phosphor which is Y3Al5O12 : Ce3 + ).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006518398A (en) | 2003-02-20 | 2006-08-10 | パテント−トロイハント−ゲゼルシヤフト フユール エレクトリツシエ グリユーラムペン ミツト ベシユレンクテル ハフツング | Coated phosphor, light-emitting device having this type of phosphor, and method for manufacturing the same |
| JP2008150518A (en) | 2006-12-19 | 2008-07-03 | Sharp Corp | Wavelength converting member and light-emitting device |
| JP2014201648A (en) | 2013-04-04 | 2014-10-27 | パナソニック株式会社 | Phosphor body, production method of phosphor body, and led element |
| WO2017142057A1 (en) | 2016-02-18 | 2017-08-24 | ロート製薬株式会社 | Topical dermatological composition |
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| JP5870611B2 (en) * | 2010-11-05 | 2016-03-01 | 日亜化学工業株式会社 | Light emitting device and manufacturing method thereof |
| JP2015089898A (en) * | 2013-11-05 | 2015-05-11 | 信越化学工業株式会社 | Inorganic phosphor powder, curable resin composition using inorganic phosphor powder, wavelength conversion member, and optical semiconductor device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006518398A (en) | 2003-02-20 | 2006-08-10 | パテント−トロイハント−ゲゼルシヤフト フユール エレクトリツシエ グリユーラムペン ミツト ベシユレンクテル ハフツング | Coated phosphor, light-emitting device having this type of phosphor, and method for manufacturing the same |
| JP2008150518A (en) | 2006-12-19 | 2008-07-03 | Sharp Corp | Wavelength converting member and light-emitting device |
| JP2014201648A (en) | 2013-04-04 | 2014-10-27 | パナソニック株式会社 | Phosphor body, production method of phosphor body, and led element |
| WO2017142057A1 (en) | 2016-02-18 | 2017-08-24 | ロート製薬株式会社 | Topical dermatological composition |
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