JP2008137921A - Pigment powder for water- and oil-repellent cosmetic, and cosmetic containing the same - Google Patents
Pigment powder for water- and oil-repellent cosmetic, and cosmetic containing the same Download PDFInfo
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Abstract
Description
本発明は、ファンデーション、アイシャドー、ほほ紅等に代表されるメークアップ化粧料あるいはサンスクリーン化粧料に配合されて好適な撥水撥油性化粧料用顔料粉体およびそれを含有する化粧料に関するものである。 The present invention relates to a water and oil repellent cosmetic pigment powder suitable for use in makeup cosmetics or sunscreen cosmetics represented by foundations, eye shadows, cheeks and the like, and cosmetics containing the same. It is.
従来、下記一般化学式（１）：
（ＲｆＣｎＨ２ｎ）ａＳｉ（ＯＣｍＨ２ｍ＋１）ｂ ・・・・・（１）
（式中、Ｒｆは炭素数３〜２１のパーフルオロアルキル基を示し、直鎖状あるいは分岐状であって、単一鎖長のものであっても複合鎖長のものであってもよい。ｎは１〜１２の整数を示し、ｍは１〜３の整数を示す。また、ａ，ｂは１〜３の整数を示し、ａ＋ｂ＝４である。）
にて示されるパーフルオロアルキルアルコキシシラン化合物による天然あるいは人工粘土鉱物からなる化粧料用顔料粉体への表面処理は、両者を直接混合するといった方法、あるいは前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物を適当な有機溶剤に溶解もしくは分散させた溶液と、天然あるいは人工粘土鉱物からなる化粧料用顔料粉体とを混合した後に有機溶剤を除去するといった方法で行われている。
Conventionally, the following general chemical formula (1):
(RfC n H 2n ) a Si (OC m H 2m + 1 ) b (1)
(In the formula, Rf represents a perfluoroalkyl group having 3 to 21 carbon atoms, and may be linear or branched, and may have a single chain length or a complex chain length. n represents an integer of 1 to 12, m represents an integer of 1 to 3, and a and b represent an integer of 1 to 3, and a + b = 4.)
The surface treatment of the cosmetic pigment powder made of natural or artificial clay mineral with the perfluoroalkylalkoxysilane compound represented by formula (1) can be carried out by a method of directly mixing the two, or by the method of the general chemical formula (1). It is carried out by a method in which a solution in which a fluoroalkylalkoxysilane compound is dissolved or dispersed in a suitable organic solvent and a cosmetic pigment powder made of natural or artificial clay mineral are mixed and then the organic solvent is removed.
しかしながら、前述したような表面処理方法により得られた従来の撥水撥油性化粧料用顔料粉体は、十分な撥水撥油性を有していないという問題点がある。このため、天然あるいは人工粘土鉱物からなる化粧料用顔料粉体に対して前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物が表面処理された撥水撥油性化粧料用顔料粉体において十分な撥水撥油性を示すものが望まれている。 However, the conventional water and oil repellent cosmetic pigment powder obtained by the surface treatment method as described above has a problem that it does not have sufficient water and oil repellent properties. Therefore, water and oil repellent cosmetic pigment powder obtained by surface-treating the perfluoroalkylalkoxysilane compound represented by the general chemical formula (1) on a cosmetic pigment powder made of natural or artificial clay minerals. In this case, a material exhibiting sufficient water and oil repellency is desired.
本発明は、このような問題点に鑑みてなされたもので、天然あるいは人工粘土鉱物からなる化粧料用顔料粉体に対してパーフルオロアルキルアルコキシシラン化合物が表面処理された撥水撥油性化粧料用顔料粉体において十分な撥水撥油性を示す撥水撥油性化粧料用顔料粉体およびそれを含有する化粧料を提供することを目的とするものである。 The present invention has been made in view of such problems, and is a water- and oil-repellent cosmetic material in which a perfluoroalkylalkoxysilane compound is surface-treated on a cosmetic pigment powder made of natural or artificial clay mineral. It is an object of the present invention to provide a water and oil repellent cosmetic pigment powder exhibiting sufficient water and oil repellency in a pigment powder and a cosmetic containing the same.
本発明者は、天然あるいは人工粘土鉱物からなる化粧料用顔料粉体に対して、下記一般化学式（１）：
（ＲｆＣｎＨ２ｎ）ａＳｉ（ＯＣｍＨ２ｍ＋１）ｂ ・・・・・（１）
（式中、Ｒｆは炭素数３〜２１のパーフルオロアルキル基を示し、直鎖状あるいは分岐状であって、単一鎖長のものであっても複合鎖長のものであってもよい。ｎは１〜１２の整数を示し、ｍは１〜３の整数を示す。また、ａ，ｂは１〜３の整数を示し、ａ＋ｂ＝４である。）
にて示されるパーフルオロアルキルアルコキシシラン化合物による表面処理を行う前に、その化粧料用顔料粉体に対して水酸化アルミニウムを表面処理することにより、十分な撥水撥油性を示す撥水撥油性化粧料用顔料粉体を得ることができることを見出し本発明を完成するに至ったものである。
The present inventor has the following general chemical formula (1) for cosmetic pigment powders made of natural or artificial clay minerals:
(RfC n H 2n ) a Si (OC m H 2m + 1 ) b (1)
(In the formula, Rf represents a perfluoroalkyl group having 3 to 21 carbon atoms, and may be linear or branched, and may have a single chain length or a complex chain length. n represents an integer of 1 to 12, m represents an integer of 1 to 3, and a and b represent an integer of 1 to 3, and a + b = 4.)
Before the surface treatment with the perfluoroalkylalkoxysilane compound shown in the above, the surface of the pigment powder for cosmetics is treated with aluminum hydroxide to provide sufficient water and oil repellency. The present inventors have found that a pigment powder for cosmetics can be obtained and have completed the present invention.
要するに、前記目的を達成するために、第１発明による撥水撥油性化粧料用顔料粉体は、
天然あるいは人工粘土鉱物からなる化粧料用顔料粉体に水酸化アルミニウムを表面処理した後、更に前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物で表面処理してなることを特徴とするものである。
In short, in order to achieve the above object, the water- and oil-repellent cosmetic pigment powder according to the first invention comprises:
A cosmetic pigment powder made of natural or artificial clay mineral is surface treated with aluminum hydroxide and then surface treated with a perfluoroalkylalkoxysilane compound represented by the general chemical formula (1). To do.
次に、第２発明による化粧料は、
第１発明に係る撥水撥油性化粧料用顔料粉体を含有してなることを特徴とするものである。
Next, the cosmetic according to the second invention is:
It contains the pigment powder for water- and oil-repellent cosmetics according to the first invention.
第１発明の撥水撥油性化粧料用顔料粉体によれば、天然あるいは人工粘土鉱物からなる化粧料用顔料粉体に対して前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物による表面処理が行われる前に、その化粧料用顔料粉体に対して水酸化アルミニウムが表面処理されるので、十分な撥水撥油性を示す撥水撥油性化粧料用顔料粉体を得ることができる。 According to the water- and oil-repellent cosmetic pigment powder of the first invention, the perfluoroalkylalkoxysilane compound represented by the general chemical formula (1) with respect to the cosmetic pigment powder made of natural or artificial clay minerals Before the surface treatment is performed, the aluminum hydroxide is surface-treated with respect to the cosmetic pigment powder, so that a water and oil repellency cosmetic pigment powder exhibiting sufficient water and oil repellency can be obtained. Can do.
また、第２発明の化粧料によれば、十分な撥水撥油性を示す第１発明の撥水撥油性化粧料用顔料粉体が含有されるので、撥水撥油性に優れて化粧持ちの良い化粧料を得ることができる。 Further, according to the cosmetic of the second invention, since the pigment powder for the water / oil / oil repellent cosmetic of the first invention showing sufficient water / oil repellency is contained, it has excellent water / oil repellency and has a long-lasting makeup. Good cosmetics can be obtained.
次に、本発明による撥水撥油性化粧料用顔料粉体およびそれを含有する化粧料の具体的な実施の形態について説明する。 Next, specific embodiments of the water and oil repellent cosmetic pigment powder and the cosmetic containing the same according to the present invention will be described.
本発明において、天然あるいは人工粘土鉱物からなる化粧料用顔料粉体に対して水酸化アルミニウムを表面処理する方法としては、例えば、化粧料用顔料粉体を水に分散させた顔料粉体スラリーにアルミン酸ソーダ水溶液または塩化アルミニウム水溶液を添加し、次いで顔料粉体スラリーを中和した後、乾燥粉砕するという方法が挙げられる。 In the present invention, as a method for surface-treating aluminum hydroxide on cosmetic pigment powder made of natural or artificial clay mineral, for example, pigment powder slurry in which cosmetic pigment powder is dispersed in water is used. A method of adding a sodium aluminate aqueous solution or an aluminum chloride aqueous solution, then neutralizing the pigment powder slurry, and then drying and pulverizing may be mentioned.
本発明において、水酸化アルミニウムで表面処理された化粧料用顔料粉体（以下、「水酸化アルミニウム処理顔料粉体」と称する。）に対して、下記一般化学式（１）：
（ＲｆＣｎＨ２ｎ）ａＳｉ（ＯＣｍＨ２ｍ＋１）ｂ ・・・・・（１）
（式中、Ｒｆは炭素数３〜２１のパーフルオロアルキル基を示し、直鎖状あるいは分岐状であって、単一鎖長のものであっても複合鎖長のものであってもよい。ｎは１〜１２の整数を示し、ｍは１〜３の整数を示す。また、ａ，ｂは１〜３の整数を示し、ａ＋ｂ＝４である。）
にて示されるパーフルオロアルキルアルコキシシラン化合物を表面処理する方法としては、例えば、（Ａ）水酸化アルミニウム処理顔料粉体と前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物とを直接混合するといった方法や、（Ｂ）前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物を適当な有機溶剤に溶解もしくは分散させた溶液と、水酸化アルミニウム処理顔料粉体とを混合した後に有機溶剤を除去するといった方法などが挙げられる。なお、（Ｂ）の表面処理方法において用いられる有機溶剤としては、例えばメタノール、エタノール、イソプロピルアルコール、イソブタノール、アセトン、酢酸エチル、酢酸ブチル、メチルエチルケトン、ジクロロメタン、クロロホルムに代表される極性有機溶剤や、ノルマルヘキサン、トルエン、キシレンのような炭化水素系有機溶剤が適当である。
In the present invention, a cosmetic powder powder surface-treated with aluminum hydroxide (hereinafter referred to as “aluminum hydroxide-treated pigment powder”) has the following general chemical formula (1):
(RfC n H 2n ) a Si (OC m H 2m + 1 ) b (1)
(In the formula, Rf represents a perfluoroalkyl group having 3 to 21 carbon atoms, and may be linear or branched, and may have a single chain length or a complex chain length. n represents an integer of 1 to 12, m represents an integer of 1 to 3, and a and b represent an integer of 1 to 3, and a + b = 4.)
As a method for surface-treating the perfluoroalkylalkoxysilane compound represented by (1), for example, (A) an aluminum hydroxide-treated pigment powder and the perfluoroalkylalkoxysilane compound represented by the general chemical formula (1) are directly used. A method of mixing, or (B) a solution obtained by dissolving or dispersing a perfluoroalkylalkoxysilane compound represented by the general chemical formula (1) in an appropriate organic solvent, and an aluminum hydroxide-treated pigment powder were mixed. The method of removing an organic solvent later is mentioned. Examples of the organic solvent used in the surface treatment method (B) include polar organic solvents such as methanol, ethanol, isopropyl alcohol, isobutanol, acetone, ethyl acetate, butyl acetate, methyl ethyl ketone, dichloromethane, and chloroform, Hydrocarbon organic solvents such as normal hexane, toluene and xylene are suitable.
本発明において、化粧料用顔料粉体に対する水酸化アルミニウムの表面処理量は、顔料粉体の粒子径にもよるが、０．０５〜２０重量％の範囲が適当である。表面処理量が０．０５重量％未満であると、得られた撥水撥油性化粧料用顔料粉体の撥水撥油性が十分に発現されない可能性がある。一方、表面処理量が２０重量％を超えると、得られた撥水撥油性化粧料用顔料粉体の感触を損ない、化粧料に配合する上で好ましくないものとなってしまう可能性がある。 In the present invention, the surface treatment amount of aluminum hydroxide relative to the pigment powder for cosmetics is suitably in the range of 0.05 to 20% by weight, although it depends on the particle diameter of the pigment powder. When the surface treatment amount is less than 0.05% by weight, the water / oil repellency of the obtained pigment powder for water / oil repellency cosmetic may not be sufficiently exhibited. On the other hand, if the surface treatment amount exceeds 20% by weight, the feel of the obtained water- and oil-repellent pigment powder for cosmetics may be impaired, which may be undesirable in blending with cosmetics.
本発明において、前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物の化粧料用顔料粉体に対する表面処理量は、顔料粉体の粒子径や顔料粉体に対する水酸化アルミニウムの表面処理量にもよるが、０．１〜２５重量％の範囲が適当である。表面処理量が０．１重量％未満であると、得られた撥水撥油性化粧料用顔料粉体の撥水撥油性が十分に発現されない可能性がある。一方、表面処理量が２５重量％を超えると、処理剤同士の反応が過度に進んで凝集やべたつき感が発生し、化粧料に配合する上で好ましくないものとなってしまう可能性がある。 In the present invention, the surface treatment amount of the perfluoroalkylalkoxysilane compound represented by the general chemical formula (1) for the pigment powder for cosmetics is the particle diameter of the pigment powder or the surface treatment of aluminum hydroxide for the pigment powder. Depending on the amount, a range of 0.1 to 25% by weight is suitable. If the surface treatment amount is less than 0.1% by weight, the water / oil repellency of the obtained pigment powder for water / oil repellency cosmetic may not be sufficiently exhibited. On the other hand, when the amount of surface treatment exceeds 25% by weight, the reaction between the treating agents proceeds excessively to cause agglomeration and stickiness, which may be undesirable when blended in cosmetics.
本発明で用いられる天然あるいは人工粘土鉱物からなる化粧料用顔料粉体としては、例えばセリサイト、タルク、マイカ、カオリン、シリカ、ガラスフレーク等が挙げられる。 Examples of cosmetic pigment powders made of natural or artificial clay minerals used in the present invention include sericite, talc, mica, kaolin, silica, glass flakes and the like.
本発明で用いられる前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物としては、例えばトリフルオロプロピルトリメトキシシラン、トリデカフルオロオクチルトリメトキシシラン、トリフルオロプロピルトリエトキシシラン、トリデカフルオロオクチルトリエトキシシラン、ヘプタデカデシルトリエトキシシラン等が挙げられる。なお、これら例示されたもののうち、トリデカフルオロオクチルトリエトキシシランは、デグサ社（株）から商品名：Ｆ８２６１として市販されている。 Examples of the perfluoroalkylalkoxysilane compound represented by the general chemical formula (1) used in the present invention include trifluoropropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, trifluoropropyltriethoxysilane, and tridecafluoro. Examples include octyltriethoxysilane, heptadecadecyltriethoxysilane, and the like. Of these examples, tridecafluorooctyltriethoxysilane is commercially available from Degussa Co., Ltd. under the trade name: F8261.
次に、本発明による撥水撥油性化粧料用顔料粉体およびそれを含有する化粧料の具体的な実施例について説明する。なお、本発明は以下に述べる実施例に限定されるものではない。 Next, specific examples of the water- and oil-repellent cosmetic pigment powder and the cosmetics containing the same according to the present invention will be described. In addition, this invention is not limited to the Example described below.
（製造実施例１）
撹拌装置および加熱装置を有する反応釜に水１０Ｌ（リットル）を入れ、撹拌しながらセリサイト１ｋｇを続いて投入して顔料粉体スラリーを作製した。よく撹拌した後、アルミン酸ソーダ３２．４ｇを水６００ｇに溶解させたアルミン酸ソーダ水溶液をゆっくりと添加してしばらく撹拌した。その後、ゆっくりと時間をかけて約７．５％硫酸水溶液で中和した。そして、反応釜の温度を７０℃以上に上げて熟成を行い、その後、水洗濾過工程、乾燥工程および粉砕工程を順にそれぞれ行うことにより、セリサイトに対して２％の水酸化アルミニウムが表面処理された水酸化アルミニウム処理セリサイトを得た。こうして得られた水酸化アルミニウム処理セリサイト９００ｇをミキサーに入れて撹拌しながら、トリデカフルオロオクチルトリエトキシシラン（デグサ社（株）製：Ｆ８２６１）２７ｇをイソプロピルアルコール１８０ｇに溶解させた溶液を添加した。イソプロピルアルコール除去のため、ミキサーを加温し必要に応じてミキサー槽内を減圧した。その後、１３０℃で乾燥した後粉砕を行うことにより、水酸化アルミニウム処理セリサイトにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性セリサイトを得た。
(Production Example 1)
10 L (liter) of water was put into a reaction kettle having a stirrer and a heating device, and 1 kg of sericite was continuously added while stirring to prepare a pigment powder slurry. After stirring well, a sodium aluminate aqueous solution in which 32.4 g of sodium aluminate was dissolved in 600 g of water was slowly added and stirred for a while. Then, it neutralized with about 7.5% sulfuric acid aqueous solution over time slowly. Then, the temperature of the reaction kettle is increased to 70 ° C. or more, and aging is performed. Thereafter, a washing process, a drying process, and a pulverization process are sequentially performed, so that 2% aluminum hydroxide is surface-treated with respect to sericite. An aluminum hydroxide-treated sericite was obtained. While stirring 900 g of the aluminum hydroxide-treated sericite thus obtained in a mixer, a solution in which 27 g of tridecafluorooctyltriethoxysilane (Degussa Co., Ltd .: F8261) was dissolved in 180 g of isopropyl alcohol was added. . In order to remove isopropyl alcohol, the mixer was heated and the inside of the mixer tank was depressurized as necessary. Then, after drying at 130 ° C., pulverization was performed to obtain water- and oil-repellent sericite in which tridecafluorooctyltriethoxysilane was surface-treated on aluminum hydroxide-treated sericite.
（製造実施例２）
撹拌装置および加熱装置を有する反応釜に水１０Ｌを入れ、撹拌しながらセリサイト１ｋｇを続いて投入して顔料粉体スラリーを作製した。よく撹拌した後、アルミン酸ソーダ８１．０ｇを水１５００ｇに溶解させたアルミン酸ソーダ水溶液をゆっくりと添加してしばらく撹拌した。その後、ゆっくりと時間をかけて約７．５％硫酸水溶液で中和した。そして、反応釜の温度を７０℃以上に上げて熟成を行い、その後、水洗濾過工程、乾燥工程および粉砕工程を順にそれぞれ行うことにより、セリサイトに対して５％の水酸化アルミニウムが表面処理された水酸化アルミニウム処理セリサイトを得た。その後、製造実施例１と同様にして、水酸化アルミニウム処理セリサイトにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性セリサイトを得た。
(Production Example 2)
10 L of water was put into a reaction kettle having a stirrer and a heating device, and 1 kg of sericite was continuously added while stirring to prepare a pigment powder slurry. After stirring well, a sodium aluminate aqueous solution in which 81.0 g of sodium aluminate was dissolved in 1500 g of water was slowly added and stirred for a while. Then, it neutralized with about 7.5% sulfuric acid aqueous solution over time slowly. Then, the temperature of the reaction kettle is increased to 70 ° C. or more, and aging is performed. Thereafter, the water washing filtration process, the drying process, and the pulverization process are sequentially performed, so that 5% aluminum hydroxide is surface-treated with respect to sericite. An aluminum hydroxide-treated sericite was obtained. Thereafter, in the same manner as in Production Example 1, water- and oil-repellent sericite in which tridecafluorooctyltriethoxysilane was surface-treated on aluminum hydroxide-treated sericite was obtained.
（製造実施例３）
撹拌装置および加熱装置を有する反応釜に水１０Ｌを入れ、撹拌しながらセリサイト１ｋｇを続いて投入して顔料粉体スラリーを作製した。よく撹拌した後、アルミン酸ソーダ１２１．５ｇを水２２５０ｇに溶解させたアルミン酸ソーダ水溶液をゆっくりと添加してしばらく撹拌した。その後、ゆっくりと時間をかけて約７．５％硫酸水溶液で中和した。そして、反応釜の温度を７０℃以上に上げて熟成を行い、その後、水洗濾過工程、乾燥工程および粉砕工程を順にそれぞれ行うことにより、セリサイトに対して７．５％の水酸化アルミニウムが表面処理された水酸化アルミニウム処理セリサイトを得た。その後、製造実施例１と同様にして、水酸化アルミニウム処理セリサイトにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性セリサイトを得た。
(Production Example 3)
10 L of water was put into a reaction kettle having a stirrer and a heating device, and 1 kg of sericite was continuously added while stirring to prepare a pigment powder slurry. After stirring well, a sodium aluminate aqueous solution in which 121.5 g of sodium aluminate was dissolved in 2250 g of water was slowly added and stirred for a while. Then, it neutralized with about 7.5% sulfuric acid aqueous solution over time slowly. Then, the temperature of the reaction kettle is increased to 70 ° C. or more and aging is performed, and then the water washing filtration process, the drying process and the pulverization process are sequentially performed, so that 7.5% of aluminum hydroxide is surfaced with respect to sericite. A treated aluminum hydroxide-treated sericite was obtained. Thereafter, in the same manner as in Production Example 1, water- and oil-repellent sericite in which tridecafluorooctyltriethoxysilane was surface-treated on aluminum hydroxide-treated sericite was obtained.
（製造実施例４）
撹拌装置および加熱装置を有する反応釜に水１０Ｌを入れ、撹拌しながらマイカ１ｋｇを続いて投入して顔料粉体スラリーを作製した。よく撹拌した後、アルミン酸ソーダ８１．０ｇを水１５００ｇに溶解させたアルミン酸ソーダ水溶液をゆっくりと添加してしばらく撹拌した。その後、ゆっくりと時間をかけて約７．５％硫酸水溶液で中和した。そして、反応釜の温度を７０℃以上に上げて熟成を行い、その後、水洗濾過工程、乾燥工程および粉砕工程を順にそれぞれ行うことにより、マイカに対して５％の水酸化アルミニウムが表面処理された水酸化アルミニウム処理マイカを得た。その後、製造実施例１と同様にして、水酸化アルミニウム処理マイカにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性マイカを得た。
(Production Example 4)
10 L of water was put into a reaction kettle having a stirring device and a heating device, and 1 kg of mica was continuously added while stirring to prepare a pigment powder slurry. After stirring well, a sodium aluminate aqueous solution in which 81.0 g of sodium aluminate was dissolved in 1500 g of water was slowly added and stirred for a while. Then, it neutralized with about 7.5% sulfuric acid aqueous solution over time slowly. Then, the temperature of the reaction kettle was increased to 70 ° C. or more, and aging was performed. Thereafter, a water-washing filtration process, a drying process, and a pulverization process were sequentially performed, whereby 5% aluminum hydroxide was surface-treated with respect to mica. Aluminum hydroxide-treated mica was obtained. Thereafter, in the same manner as in Production Example 1, water- and oil-repellent mica in which aluminum hydroxide-treated mica was surface-treated with tridecafluorooctyltriethoxysilane was obtained.
（製造実施例５）
撹拌装置および加熱装置を有する反応釜に水１０Ｌを入れ、撹拌しながらマイカ１ｋｇを続いて投入して顔料粉体スラリーを作製した。よく撹拌した後、アルミン酸ソーダ１２１．５ｇを水２２５０ｇに溶解させたアルミン酸ソーダ水溶液をゆっくりと添加してしばらく撹拌した。その後、ゆっくりと時間をかけて約７．５％硫酸水溶液で中和した。そして、反応釜の温度を７０℃以上に上げて熟成を行い、その後、水洗濾過工程、乾燥工程および粉砕工程を順にそれぞれ行うことにより、マイカに対して７．５％の水酸化アルミニウムが表面処理された水酸化アルミニウム処理マイカを得た。その後、製造実施例１と同様にして、水酸化アルミニウム処理マイカにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性マイカを得た。
(Production Example 5)
10 L of water was put into a reaction kettle having a stirring device and a heating device, and 1 kg of mica was continuously added while stirring to prepare a pigment powder slurry. After stirring well, a sodium aluminate aqueous solution in which 121.5 g of sodium aluminate was dissolved in 2250 g of water was slowly added and stirred for a while. Then, it neutralized with about 7.5% sulfuric acid aqueous solution over time slowly. Then, the temperature of the reaction kettle is increased to 70 ° C. or more, and aging is performed. Thereafter, the water washing filtration process, the drying process, and the pulverization process are sequentially performed, so that 7.5% of aluminum hydroxide is surface-treated with respect to mica. An aluminum hydroxide-treated mica was obtained. Thereafter, in the same manner as in Production Example 1, water- and oil-repellent mica in which aluminum hydroxide-treated mica was surface-treated with tridecafluorooctyltriethoxysilane was obtained.
（製造比較例１）
水酸化アルミニウムが表面処理されていないセリサイト９００ｇをミキサーに入れて撹拌しながら、トリデカフルオロオクチルトリエトキシシラン（デグサ社（株）製：Ｆ８２６１）２７ｇをイソプロピルアルコール１８０ｇに溶解させた溶液を添加した。イソプロピルアルコール除去のため、ミキサーを加温し必要に応じてミキサー槽内を減圧した。その後、１３０℃で乾燥した後粉砕を行うことにより、セリサイトにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性セリサイトを得た。
(Production Comparative Example 1)
While stirring 900 g of sericite with no surface treatment of aluminum hydroxide in a mixer, a solution in which 27 g of tridecafluorooctyltriethoxysilane (Degussa Co., Ltd .: F8261) was dissolved in 180 g of isopropyl alcohol was added. did. In order to remove isopropyl alcohol, the mixer was heated and the inside of the mixer tank was depressurized as necessary. Then, after drying at 130 ° C., pulverization was performed to obtain water- and oil-repellent sericite in which tridecafluorooctyltriethoxysilane was surface-treated.
（製造比較例２）
水酸化アルミニウムが表面処理されていないマイカ９００ｇをミキサーに入れて撹拌しながら、トリデカフルオロオクチルトリエトキシシラン（デグサ社（株）製：Ｆ８２６１）２７ｇをイソプロピルアルコール１８０ｇに溶解させた溶液を添加した。イソプロピルアルコール除去のため、ミキサーを加温し必要に応じてミキサー槽内を減圧した。その後、１３０℃で乾燥した後粉砕を行うことにより、マイカにトリデカフルオロオクチルトリエトキシシランが表面処理された撥水撥油性マイカを得た。
(Production Comparative Example 2)
While stirring 900 g of mica not surface-treated with aluminum hydroxide in a mixer, a solution in which 27 g of tridecafluorooctyltriethoxysilane (Degussa, Inc .: F8261) was dissolved in 180 g of isopropyl alcohol was added. . In order to remove isopropyl alcohol, the mixer was heated and the inside of the mixer tank was depressurized as necessary. Then, after drying at 130 ° C., pulverization was performed to obtain a water- and oil-repellent mica whose surface was treated with tridecafluorooctyltriethoxysilane.
製造実施例１〜３の撥水撥油性セリサイト、製造実施例４，５の撥水撥油性マイカ、製造比較例１の撥水撥油性セリサイトおよび製造比較例２の撥水撥油性マイカについてそれぞれ水と流動パラフィンによる接触角を測定した。その結果が表１に示されている。 Water- and oil-repellent sericite of Production Examples 1 to 3, Water- and oil-repellent mica of Production Examples 4 and 5, Water- and oil-repellent sericite of Production Comparative Example 1, and Water- and oil-repellent mica of Production Comparative Example 2 The contact angles with water and liquid paraffin were measured. The results are shown in Table 1.
表１から明らかなように、予め水酸化アルミニウムで表面処理した後に、更にトリデカフルオロオクチルトリエトキシシランで表面処理した製造実施例１〜３の撥水撥油性セリサイトおよび製造実施例４，５の撥水撥油性マイカは、予め水酸化アルミニウムで表面処理せずにトリデカフルオロオクチルトリエトキシシランを表面処理した製造比較例１の撥水撥油性セリサイトおよび製造比較例２の撥水撥油性マイカと比べて、撥水性および撥油性が共に優れていることが分かる。なお、製造実施例１〜５の撥水撥油性化粧料用顔料はいずれも、測定の際に滴下される水滴および油滴が時間とともに顔料粉体に吸収されることなく安定していた。 As is apparent from Table 1, the water- and oil-repellent sericite of Production Examples 1 to 3 and Production Examples 4 and 5 which were previously surface-treated with aluminum hydroxide and further surface-treated with tridecafluorooctyltriethoxysilane. The water- and oil-repellent mica was prepared by subjecting tridecafluorooctyltriethoxysilane to a surface treatment in advance without surface treatment with aluminum hydroxide. It can be seen that both water repellency and oil repellency are superior to mica. In addition, all the water- and oil-repellent cosmetic pigments of Production Examples 1 to 5 were stable without being absorbed by the pigment powder over time with water droplets and oil droplets dropped during the measurement.
（実施例１）
製造実施例１で得られた撥水撥油性セリサイトと、製造比較例１，２と同様に水酸化アルミニウムで表面処理することなくトリデカフルオロオクチルトリエトキシシランを表面処理して得られた撥水撥油性タルク、撥水撥油性酸化チタン、撥水撥油性黄酸化鉄、撥水撥油性ベンガラおよび撥水撥油性黒酸化鉄とを用いて以下のようにパウダーファンデーションを作製した。
まず、パウダーベースを以下の配合にて調製した。
＜パウダーベース配合＞
撥水撥油性セリサイト（製造実施例１） ６０．０
撥水撥油性タルク ２７．０
撥水撥油性酸化チタン １０・０
撥水撥油性黄酸化鉄 ２．０
撥水撥油性ベンガラ ０・６
撥水撥油性黒酸化鉄 ０・３
メチルパラベン ０・１
合計１００．０
次に、バインダーベースを以下の配合にて調製した。
＜バインダーベース配合＞
ジメチコン トリメトキシシリケート ２９．８５
ジメチコン（２０） ７０．００
フェノキシエタノール ０・１０
トコフェノール ０・０５
合計１００．００
これらパウダーベースおよびバインダーベースをそれぞれ９０％および１０％の配合比になるようにミキサーで混合してパウダーファンデーションを得た。
(Example 1)
The water- and oil-repellent sericite obtained in Production Example 1 and tridecafluorooctyltriethoxysilane obtained by surface treatment without surface treatment with aluminum hydroxide as in Production Comparative Examples 1 and 2 were obtained. A powder foundation was prepared using water / oil repellent talc, water / oil repellent titanium oxide, water / oil repellent yellow iron oxide, water / oil repellent bengara and water / oil repellent black iron oxide as follows.
First, a powder base was prepared with the following composition.
<Powder base formulation>
Water / oil repellent sericite (Production Example 1) 60.0
Water and oil repellent talc 27.0
Water / oil repellent titanium oxide 10.0
Water and oil repellent yellow iron oxide 2.0
Water and oil repellent Bengala 0.6
Water and oil repellent black iron oxide 0.3
Methylparaben 0.1
Total 100.0
Next, a binder base was prepared with the following formulation.
<Binder base formulation>
Dimethicone Trimethoxysilicate 29.85
Dimethicone (20) 70.00
Phenoxyethanol 0 · 10
Tocophenol 0.05
Total 100.00
These powder base and binder base were mixed with a mixer so as to have a blending ratio of 90% and 10%, respectively, to obtain a powder foundation.
（比較例１）
製造実施例１の撥水撥油性セリサイトに代えて製造比較例１の撥水撥油性セリサイトを用いて実施例１と同様にしてパウダーファンデーションを作製した。
(Comparative Example 1)
A powder foundation was prepared in the same manner as in Example 1 using the water / oil / oil repellent sericite of Production Comparative Example 1 instead of the water / oil / oil repellent sericite of Production Example 1.
実施例１のパウダーファンデーションおよび比較例１のパウダーファンデーションは肌での延びや使用感に大きな違いは見られなかったが、実施例１のパウダーファンデーションの方が撥水撥油性に優れるため、化粧崩れが抑制されて化粧持ちが良かった。 The powder foundation of Example 1 and the powder foundation of Comparative Example 1 showed no significant difference in skin extension or feeling of use. Was suppressed and the makeup was good.
以上のことから、セリサイトやマイカなどに代表される天然あるいは人工粘土鉱物からなる化粧料用顔料粉体を水酸化アルミニウムで表面処理した後、更に前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物で表面処理して得られた撥水撥油性化粧料用顔料粉体を含有してなる化粧料は、水酸化アルミニウムで表面処理されていない化粧料用顔料粉体に前記一般化学式（１）にて示されるパーフルオロアルキルアルコキシシラン化合物を表面処理して得られた撥水撥油性化粧料用顔料粉体を含有してなる化粧料よりも撥水撥油性に優れ、化粧持ちが良いことが分かった。 From the above, after subjecting cosmetic pigment powders made of natural or artificial clay minerals such as sericite and mica to surface treatment with aluminum hydroxide, the perfluoro represented by the above general chemical formula (1) A cosmetic comprising a water- and oil-repellent cosmetic pigment powder obtained by surface treatment with an alkylalkoxysilane compound is a cosmetic pigment powder not surface-treated with aluminum hydroxide. It is superior in water and oil repellency to a cosmetic comprising the water- and oil-repellent pigment powder for cosmetics obtained by surface treatment of the perfluoroalkylalkoxysilane compound represented by (1), and has a long-lasting makeup. I found it good.
Claims (2)
（ＲｆＣｎＨ２ｎ）ａＳｉ（ＯＣｍＨ２ｍ＋１）ｂ ・・・・・（１）
（式中、Ｒｆは炭素数３〜２１のパーフルオロアルキル基を示し、直鎖状あるいは分岐状であって、単一鎖長のものであっても複合鎖長のものであってもよい。ｎは１〜１２の整数を示し、ｍは１〜３の整数を示す。また、ａ，ｂは１〜３の整数を示し、ａ＋ｂ＝４である。）
にて示されるパーフルオロアルキルアルコキシシラン化合物で表面処理してなることを特徴とする撥水撥油性化粧料用顔料粉体。 A cosmetic pigment powder made of natural or artificial clay mineral is surface-treated with aluminum hydroxide, and then the following general chemical formula (1):
(RfC n H 2n ) a Si (OC m H 2m + 1 ) b (1)
(In the formula, Rf represents a perfluoroalkyl group having 3 to 21 carbon atoms, and may be linear or branched, and may have a single chain length or a complex chain length. n represents an integer of 1 to 12, m represents an integer of 1 to 3, and a and b represent an integer of 1 to 3, and a + b = 4.)
A water- and oil-repellent cosmetic pigment powder, which is surface-treated with a perfluoroalkylalkoxysilane compound represented by
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105456048A (en) * | 2016-01-04 | 2016-04-06 | 上海蔻沣生物科技有限公司 | Preparing method for hydrophobic and oleophobic cosmetic pigment powder |
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| JPH04330007A (en) * | 1991-02-01 | 1992-11-18 | Daito Kasei Kogyo Kk | Cosmetic |
| JPH09143032A (en) * | 1995-11-27 | 1997-06-03 | Narisu Keshohin:Kk | Powder for cosmetic and cosmetic |
| JP2002146238A (en) * | 2000-08-31 | 2002-05-22 | Miyoshi Kasei Kk | Novel composite powder and cosmetic incorporating the same |
| JP2002194247A (en) * | 2000-11-06 | 2002-07-10 | Merck Patent Gmbh | Post-coating of pearlescent pigment by hydrophobic coupling agent |
| JP2003081733A (en) * | 2001-07-05 | 2003-03-19 | Shiseido Co Ltd | Powdery composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04330007A (en) * | 1991-02-01 | 1992-11-18 | Daito Kasei Kogyo Kk | Cosmetic |
| JPH09143032A (en) * | 1995-11-27 | 1997-06-03 | Narisu Keshohin:Kk | Powder for cosmetic and cosmetic |
| JP2002146238A (en) * | 2000-08-31 | 2002-05-22 | Miyoshi Kasei Kk | Novel composite powder and cosmetic incorporating the same |
| JP2002194247A (en) * | 2000-11-06 | 2002-07-10 | Merck Patent Gmbh | Post-coating of pearlescent pigment by hydrophobic coupling agent |
| JP2003081733A (en) * | 2001-07-05 | 2003-03-19 | Shiseido Co Ltd | Powdery composition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105456048A (en) * | 2016-01-04 | 2016-04-06 | 上海蔻沣生物科技有限公司 | Preparing method for hydrophobic and oleophobic cosmetic pigment powder |
| CN105456048B (en) * | 2016-01-04 | 2017-02-01 | 上海蔻沣生物科技有限公司 | Preparing method for hydrophobic and oleophobic cosmetic pigment powder |
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