JP5580148B2 - Surface-treated powder, method for producing the same, and cosmetics containing the same - Google Patents
Surface-treated powder, method for producing the same, and cosmetics containing the same Download PDFInfo
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- JP5580148B2 JP5580148B2 JP2010196440A JP2010196440A JP5580148B2 JP 5580148 B2 JP5580148 B2 JP 5580148B2 JP 2010196440 A JP2010196440 A JP 2010196440A JP 2010196440 A JP2010196440 A JP 2010196440A JP 5580148 B2 JP5580148 B2 JP 5580148B2
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- powder
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Description
本発明は、撥水性、撥油性に優れ、且つ使用感に優れた表面処理粉体および該粉体を含有する化粧料に関する。 The present invention relates to a surface-treated powder excellent in water repellency and oil repellency, and excellent in usability, and a cosmetic containing the powder.
メーキャップ化粧料、日焼け止め化粧料、マスカラ、ネイルエナメル、口紅などの化粧料には、化粧料用粉体として様々な粉体が用いられている。汗、涙、雨、戸外でのスポーツ、海水浴などによる化粧崩れの防止、また衣類や容器などへの色移り防止など、その使用目的に合わせて、撥水性、撥油性をもたせるための表面処理に関する多くの検討がなされており、シリカコートを施した粉体を用いる方法、各種シリコーン誘導体で表面処理した粉体を用いる方法、パーフルオロ基を有する表面処理剤により表面処理をした撥水性、撥油性を有する粉体を用いる方法などが提案されている。 Various powders are used as cosmetic powders in cosmetics such as makeup cosmetics, sunscreen cosmetics, mascara, nail enamel and lipstick. For surface treatment to give water and oil repellency according to the purpose of use, such as prevention of breakup of makeup due to sweat, tears, rain, outdoor sports, sea bathing, etc., and prevention of color transfer to clothing and containers Many studies have been made, using silica-coated powders, using surface-treated powders with various silicone derivatives, and water / oil repellency treated with a surface treatment agent having a perfluoro group. There have been proposed methods using powders having the following.
パーフルオロアルキル基を有する表面処理剤により表面処理した粉体については、パーフルオロアルキルリン酸により処理する方法が知られている（特許文献１）。また、パーフルオロアルキルリン酸により処理した粉体は伸びが悪い、粉っぽい、皮膚への付着性に乏しいなどという理由から、他の表面処理剤と併用して処理した粉体を利用する方法が提案されている（特許文献２）。しかしながら、特定のパーフルオロアルキル基については安全性の問題があるため懸念されていることから、その代替となる紛体の表面処理剤が求められている。 A method of treating powder with a surface treatment agent having a perfluoroalkyl group with a perfluoroalkyl phosphoric acid is known (Patent Document 1). In addition, the powder treated with perfluoroalkyl phosphoric acid has a poor elongation, is powdery, and has poor adhesion to the skin. Has been proposed (Patent Document 2). However, since there are concerns about specific perfluoroalkyl groups due to safety problems, powder surface treatment agents that can be used instead are demanded.
それを解決する方法の一つとして、パーフルオロポリエーテル鎖を有する表面処理剤が検討されている。パーフルオロポリエーテル鎖を有する表面処理剤で処理した粉体としては、パーフルオロポリエーテルリン酸エステルで処理された粉体及びそれを含有する化粧料（特許文献３〜４）が報告されている。パーフルオロポリエーテル鎖を有するシラン化合物で処理した紛体としては、パーフルオロポリエーテル変性アミノシラン化合物で処理した紛体（特許文献５）が報告されている。さらには、パーフルオロポリエーテルを含有するアニオン性高分子が報告されている（特許文献６）。しかしながら、これらの表面処理剤を利用した紛体は、撥水性、撥油性などの面で十分のものではなく、皮膚への付着性や感触の点からも十分満足できるものではない。また、安価かつ簡単な操作で表面処理できる表面処理剤で製造した表面処理紛体も望まれている。 As one method for solving this problem, a surface treatment agent having a perfluoropolyether chain has been studied. As powders treated with a surface treatment agent having a perfluoropolyether chain, powders treated with perfluoropolyether phosphate and cosmetics containing the same (Patent Documents 3 to 4) have been reported. . As a powder treated with a silane compound having a perfluoropolyether chain, a powder treated with a perfluoropolyether-modified aminosilane compound (Patent Document 5) has been reported. Furthermore, an anionic polymer containing perfluoropolyether has been reported (Patent Document 6). However, powders using these surface treatment agents are not sufficient in terms of water repellency and oil repellency, and are not sufficiently satisfactory in terms of adhesion to the skin and feel. In addition, a surface-treated powder produced with a surface-treating agent that can be surface-treated with an inexpensive and simple operation is also desired.
本発明は、撥水性、撥油性に優れ、肌への塗布時の感触が滑らかで付着性も良好な表面処理粉体、及びこの表面処理粉体を安価かつ簡単な操作で製造すること、並びにこの表面処理粉体を配合した化粧料を提供することにある。 The present invention is a surface-treated powder excellent in water repellency and oil repellency, having a smooth feel when applied to the skin and having good adhesion, and producing the surface-treated powder by an inexpensive and simple operation; and The object is to provide a cosmetic containing the surface-treated powder.
本発明者らは、本課題に対し鋭意研究を行った結果、一般式（１）で示されるパーフルオロポリエーテルリン酸と、一般式（２）で示されるパーフルオロポリエーテル鎖を有するアニオン性高分子または一般式（３）で示されるパーフルオロポリエーテル鎖を有するカチオン性高分子とを組み合わせて基材粉体を表面処理することにより撥水性、撥油性、付着性、感触面で、相乗的な効果を見出した。また本発明の表面処理粉体を使用する事により、汗や皮脂による化粧くずれのし難い、また肌への塗布時の感触が滑らかで付着性も良好である化粧品が得られることを見出し、本発明を完成するに到った。 As a result of intensive studies on this problem, the present inventors have found that an anionic property having a perfluoropolyether phosphate represented by the general formula (1) and a perfluoropolyether chain represented by the general formula (2). By combining the polymer or a cationic polymer having a perfluoropolyether chain represented by the general formula (3), the base powder is surface-treated to achieve synergy in terms of water repellency, oil repellency, adhesion, and feel. Found an effective effect. In addition, by using the surface-treated powder of the present invention, it has been found that cosmetics that are difficult to make up by sweat and sebum and that have a smooth feel and good adhesion when applied to the skin can be obtained. The invention has been completed.
本発明により、撥水性、撥油性に優れ、肌への塗布時の感触が滑らかで付着性も良好な表面処理粉体を提供することができる。本発明の表面処理紛体は従来の撥水撥油性粉体とは異なり、化粧品で用いられる種々の粉体との混和性にも優れており、容易に感触に優れた高機能な化粧料を提供することができる。具体的には、汗や水などによる化粧崩れがおこりにくいメーキャップ化粧料や紫外線防御用化粧料、容器や衣服などに色移りしにくい口紅やファンデーションなどの化粧料を提供することができる。 According to the present invention, it is possible to provide a surface-treated powder that is excellent in water repellency and oil repellency, has a smooth feel when applied to the skin, and has good adhesion. The surface-treated powder of the present invention, unlike conventional water- and oil-repellent powders, is excellent in miscibility with various powders used in cosmetics, and easily provides a highly functional cosmetic with excellent touch. can do. Specifically, makeup cosmetics, UV protection cosmetics, and cosmetics such as lipsticks and foundations that do not easily transfer to containers or clothes can be provided.
以下、本発明の表面処理粉体について詳述する。 Hereinafter, the surface-treated powder of the present invention will be described in detail.
本発明は、一般式（１）；
さらに、一般式（２）で表されるパーフルオロポリエーテル鎖を有するアニオン性高分子および一般式（３）で表されるパーフルオロポリエーテル鎖を有するカチオン性高分子におけるＲｆ（パーフルオロポリエーテル部）は、一般式（４）；
一般式（２）で表されるパーフルオロポリエーテル鎖を有するアニオン性高分子および一般式（３）で表されるパーフルオロポリエーテル鎖を有するカチオン性高分子におけるＲu（ウレタン結合部）は、一般式（５）；
本発明は、前記表面処理成分を組み合わせて処理する事により、相乗的に粉体の機能が向上することにある。さらに実施例で詳述するが、これらの製法を制限するものでは無く、湿式法で行う事により、処理の順序により後で処理する処理剤の性質が強く出易いという傾向があるものの、従来では得られない撥油性と感触、付着性、更には他の表面処理粉体との混和性に優れた粉体が得られる。組み合わせ比率、量について制限するものではないが、本発明の表面処理成分は基材粉体１００質量部に対して、０．５以上４０質量部であることが好ましい。 The present invention is to synergistically improve the function of the powder by processing in combination with the surface treatment components. Further detailed in the examples, but these production methods are not limited, but by the wet method, the nature of the treatment agent to be treated later tends to be strong due to the order of treatment, but conventionally, A powder excellent in oil repellency, touch, adhesion, and miscibility with other surface-treated powders can be obtained. Although it does not restrict | limit about a combination ratio and quantity, It is preferable that the surface treatment component of this invention is 0.5-40 mass parts with respect to 100 mass parts of base material powder.
さらに、前記表面処理成分の比率は、５／９５から９５／５の範囲が好ましく、更に好ましくは１０／９０から９０／１０である。 Furthermore, the ratio of the surface treatment component is preferably in the range of 5/95 to 95/5, more preferably 10/90 to 90/10.
本発明に係わる一般式（１）で表されるパーフルオロポリエーテルリン酸は、特許３８８８９０２号公報に準じた方法で合成でき、製品名ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００（ポリパーフルオロエトキシメトキシジフルオロエチルＰＥＧリン酸）として日光ケミカルズ株式会社より市販されている。一般式（２）で表されるパーフルオロポリエーテル鎖を有するアニオン性高分子は、特開２００３−１２９３９４号公報に準じた方法で合成でき、製品名ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅ（ポリウレタン−２７）として日光ケミカルズ株式会社より市販されている。一般式（３）で表されるパーフルオロポリエーテル鎖を有するカチオン性高分子とは、特開２０００−３０２９３８号公報に準じた方法で合成でき、製品名ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５（ポリウレタン−２６）として、日光ケミカルズ株式会社より市販されている。 The perfluoropolyether phosphoric acid represented by the general formula (1) according to the present invention can be synthesized by a method according to Japanese Patent No. 3888902, and the product name FOMBLIN HC / P2-1000 (polyperfluoroethoxymethoxydifluoroethyl PEG). Phosphoric acid) is commercially available from Nikko Chemicals. An anionic polymer having a perfluoropolyether chain represented by the general formula (2) can be synthesized by a method according to Japanese Patent Application Laid-Open No. 2003-129394, and product name FOMBLIN HC / PU-AN5E (polyurethane-27). Is commercially available from Nikko Chemicals Corporation. The cationic polymer having a perfluoropolyether chain represented by the general formula (3) can be synthesized by a method according to Japanese Patent Application Laid-Open No. 2000-302938, and the product name FOMBLINE HC / PU-CAT5 (polyurethane-26). ) Is commercially available from Nikko Chemicals Corporation.
表面処理剤を使用して基材粉体の表面を処理する方法は、一般的には湿式法、乾式法の２方法がある。湿式法は溶剤、もしくは水／溶剤溶液に基材粉体を分散し、ここに攪拌しながら、表面処理剤を添加し、均一にコート後ろ過して、乾燥し表面処理粉体を得るものである。乾式法はヘンシェルミキサー、ボールミルなどに基材粉体を加え、溶剤に溶解した表面処理剤を加え、良く混合後乾燥、加熱して処理粉体を得るものである。 In general, there are two methods for treating the surface of the base powder using a surface treating agent, a wet method and a dry method. In the wet method, a base powder is dispersed in a solvent or a water / solvent solution, and a surface treatment agent is added to the solution while stirring. The coating is uniformly coated, filtered, and dried to obtain a surface-treated powder. is there. In the dry method, a base powder is added to a Henschel mixer, a ball mill, etc., a surface treatment agent dissolved in a solvent is added, and after mixing well, dried and heated to obtain a treated powder.
本発明における表面処理の方法は特に制限するものでは無いが、均質な表面処理をするには湿式法が好ましい。具体的には、一般式（１）で表されるパーフルオロポリエーテルリン酸と、一般式（２）で表されるパーフルオロポリエーテル鎖を含有するアニオン性高分子はアルカリ性下で、一般式（３）で表されるパーフルオロポリエーテル鎖を含有するカチオン性高分子は酸性下で水に溶解する。したがって、一般式（１）で表されるパーフルオロポリエーテルリン酸と、一般式（２）で表されるパーフルオロポリエーテル鎖を含有するアニオン性高分子で処理するためには基材粉体を水に分散し、ｐＨ８．０以上のアルカリ性下で表面処理剤を加え、良く混合して、均質に表面吸着させた後、酸性にし不溶化して表面処理に強く吸着させて、ろ過、乾燥して処理粉体を得ることができる。
同様に、一般式（３）で表されるパーフルオロポリエーテル鎖を含有するカチオン性高分子で処理するためには基材粉体を水に分散し、ｐＨ６．０以下の酸性下で表面処理剤を加え、よく混合して、均質に表面吸着させた後、アルカリ性にし不溶化して表面処理に強く吸着させて、ろ過、乾燥して処理粉体を得ることができる。
The surface treatment method in the present invention is not particularly limited, but a wet method is preferred for homogeneous surface treatment. Specifically, the anionic polymer containing the perfluoropolyether phosphoric acid represented by the general formula (1) and the perfluoropolyether chain represented by the general formula (2) is alkaline, The cationic polymer containing the perfluoropolyether chain represented by (3) is soluble in water under acidic conditions. Therefore, in order to treat with the anionic polymer containing the perfluoropolyether phosphoric acid represented by the general formula (1) and the perfluoropolyether chain represented by the general formula (2), a base powder Is dispersed in water, added with a surface treatment agent under alkalinity of pH 8.0 or higher, mixed well, and homogeneously adsorbed on the surface, then acidified and insolubilized, strongly adsorbed to the surface treatment, filtered and dried. Thus, a treated powder can be obtained.
Similarly, in order to treat with the cationic polymer containing the perfluoropolyether chain represented by the general formula (3), the base powder is dispersed in water, and the surface treatment is performed under an acidic condition of pH 6.0 or lower. The agent can be added, mixed well, and uniformly adsorbed on the surface, then rendered alkaline and insolubilized, strongly adsorbed on the surface treatment, filtered and dried to obtain a treated powder.
上述のようにして得られる本発明の表面処理粉体は撥水性、撥油性に優れ、且つ肌への塗布時の感触が滑らかで、肌との付着性にも優れる。 The surface-treated powder of the present invention obtained as described above is excellent in water repellency and oil repellency, has a smooth feel when applied to the skin, and has excellent adhesion to the skin.
また、基材粉体をあらかじめ表面処理助剤で処理することにより、本発明において、より優れた表面処理粉体を得ることができる。表面処理助剤としては、塩化鉄、塩化アルミニウム、塩化アルミニウム六水和物、水酸化アルミニウム、ケイ酸アルミニウム、リン酸アルミニウム等があり、好ましくは塩化アルミニウム六水和物である。これら表面処理助剤の使用量を限定するものではないが、本発明の効果を損なわずにより優れた表面処理粉体を得るためには、０．１から５質量部程度が好ましい。 Further, by treating the substrate powder with a surface treatment aid in advance, a more excellent surface treated powder can be obtained in the present invention. Examples of the surface treatment aid include iron chloride, aluminum chloride, aluminum chloride hexahydrate, aluminum hydroxide, aluminum silicate, and aluminum phosphate, and aluminum chloride hexahydrate is preferable. Although the usage-amount of these surface treatment adjuvants is not limited, in order to obtain the surface treatment powder which was excellent without impairing the effect of this invention, about 0.1-5 mass parts is preferable.
更に、本発明に係わる基材粉体の表面処理にあたっては、本発明の効果を損なわない範囲で、一般式（１）から（３）以外の表面処理剤を同時又は連続的に基材粉体に表面処理することができる。本発明に使用できる表面処理剤としては、例えばパーフルオロポリエーテル変性アミノシラン、パーフルオロオクチルトリエトキシシラン、炭素数９〜１５のフルオロアルコールリン酸、トリフルオロプロピルシクロペンタシロキサン、ＰＥＧ８トリフルオロプロピルジメチコンコポリマー等の本発明に係わる表面処理剤以外のフッ素系化合物、ハイドロジェンシリコーン、アミノシリコーン、反応性オルガノポリシロキサン、アルキルシランなどのシリコーン化合物、有機チタネート、ポリオレフィン、レシチン及び／又はその塩、水添レシチン及び／又はその塩などのレシチン類、アシル化アミノ酸及び／又はその塩、酸性エステル油、脂肪酸及び／又はその塩類、デキストリン脂肪酸エステル、フラクトオリゴ糖脂肪酸エステル、コラーゲン、高級アルコール、エステル、ワックス、金属石鹸などが挙げられるが、これらに限定されるものではない。 Furthermore, in the surface treatment of the base powder according to the present invention, a surface treatment agent other than those represented by the general formulas (1) to (3) may be added simultaneously or continuously within a range not impairing the effects of the present invention. Can be surface treated. Examples of the surface treatment agent that can be used in the present invention include perfluoropolyether-modified aminosilane, perfluorooctyltriethoxysilane, fluoroalcohol phosphate having 9 to 15 carbon atoms, trifluoropropylcyclopentasiloxane, and PEG8 trifluoropropyl dimethicone copolymer. Fluorine compounds other than the surface treating agent according to the present invention, such as hydrogen silicone, amino silicone, reactive organopolysiloxane, silicone compounds such as alkylsilane, organic titanate, polyolefin, lecithin and / or salt thereof, hydrogenated lecithin And / or lecithins such as salts thereof, acylated amino acids and / or salts thereof, acidic ester oils, fatty acids and / or salts thereof, dextrin fatty acid esters, fructooligosaccharide fatty acid esters Gen, higher alcohols, esters, waxes, and the like metal soaps, but not limited thereto.
上記パーフルオロポリエーテル変性アミノシランは、特開昭５８−１２２９７９号公報に準じた方法で合成できる。パーフルオロオクチルトリエトキシシランは、Ｇｅｌｅｓｔ，Ｉｎｃ．製のものを利用できる。炭素数９〜１５のフルオロアルコールリン酸は、特開２００４−２７７３８９号公報に準じた方法で合成できる。トリフルオロプロピルシクロペンタシロキサンは、信越化学工業社のＫＦ−５００２などが利用できる。ＰＥＧ８トリフルオロプロピルジメチコンは、信越化学工業社のＦＰＤ−６１３１などを利用できる。反応性オルガノポリシロキサンとしては、信越化学工業社のＫＦ９９（メチコン）、ＫＦ９９０１（ハイドロジェンジメチコン）等、ＫＦ−９９０８（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）、ＫＦ−９９０９（トリエトキシリルエチルポリジメチルシロキシエチルヘキシルジメチコン）、ＫＰ−５７４（（アクリレーツ／アクリル酸トリデシル／メタクリル酸トリエトキシシリルプロピル／メタクリル酸ジメチコン）コポリマー）、ＫＦ―７３１２（トリメチルシロキシケイ酸とシクロペンタシロキサンの混合物）、ＫＦ―９００１（トリメチルシロキシケイ酸のデカメチルシクロペンタシロキサン５０％溶液）等を使用できる。アルキルシランとしては、ダウコーニング社のＺ−６３４１（オクチルトリエトキシシラン）やデグサ社のＦ−８２６１（トリデカフルオロオクチルトリエトキシシラン）等を使用できる。有機チタネートとしては、味の素社のプレンアクトＫＲ−ＴＴＳ（イソプロピルトリイソステアロイルチタネート）等が使用できる。ポリオレフィンとしては、例えば、特開昭６３−１７９９７２号公報に記載の公知の化合物や、ポリプロピレンを酸化して得られる酸化ポリエチレン、マレイン化ポリエチレン、酸化ポリプロピレン等を使用できる。水添レシチン及び／又はその塩類としては、例えば、日光ケミカルズ社のレシノールＳ−１０（水素添加大豆リン脂質）、キユーピー社の卵黄レシチンＰＬ−１００Ｐ（水素添加卵黄リン脂質）等を使用できる。アシル化アミノ酸及び／又はその塩としては、日光ケミカル社のサルコシネートＭＮ（ミリストイルメチルアミノ酢酸ナトリウム）、アラニネートＬＮ−３０（ラウロイルメチルアラニンナトリウム）、サルコシネートＣＮ−３０（ココイルサルコシンナトリウム）、サルコシネートＯＨ（オレオイルサルコシン）等、味の素社のアミソフトＨＳ−２１（Ｎ−ステアロイル−Ｌ−グルタミン酸ニナトリウム）等、ＳＥＰＰＩＣ社のＳＥＰＩＬＩＦＴ ＤＰＨＰ（ジパルミトイルヒドロキシプロリン）等を使用できる。 The perfluoropolyether-modified aminosilane can be synthesized by a method according to Japanese Patent Application Laid-Open No. 58-122979. Perfluorooctyltriethoxysilane is available from Gelest, Inc. The one made of can be used. The fluoroalcohol phosphate having 9 to 15 carbon atoms can be synthesized by a method according to Japanese Patent Application Laid-Open No. 2004-277389. As trifluoropropylcyclopentasiloxane, KF-5002 from Shin-Etsu Chemical Co., Ltd. can be used. As PEG8 trifluoropropyl dimethicone, FPD-6131 manufactured by Shin-Etsu Chemical Co., Ltd. can be used. Examples of reactive organopolysiloxanes include KF99 (methicone) and KF9901 (hydrogen dimethicone) from Shin-Etsu Chemical Co., Ltd., KF-9908 (triethoxysilylethyl polydimethylsiloxyethyl dimethicone), and KF-9909 (triethoxylylethyl poly). Dimethylsiloxyethylhexyl dimethicone), KP-574 ((acrylates / tridecyl acrylate / triethoxysilylpropyl methacrylate / dimethicone methacrylate) copolymer), KF-7312 (mixture of trimethylsiloxysilicate and cyclopentasiloxane), KF-9001 (Decamethylcyclopentasiloxane 50% solution of trimethylsiloxysilicate) can be used. As the alkyl silane, Z-6341 (octyltriethoxysilane) manufactured by Dow Corning, F-8261 (tridecafluorooctyltriethoxysilane) manufactured by Degussa, or the like can be used. As the organic titanate, Ajinomoto Co., Ltd. Preneact KR-TTS (isopropyl triisostearoyl titanate) and the like can be used. As the polyolefin, for example, known compounds described in JP-A No. 63-179972, oxidized polyethylene obtained by oxidizing polypropylene, maleated polyethylene, polypropylene oxide, and the like can be used. As hydrogenated lecithin and / or salts thereof, for example, Resinol S-10 (hydrogenated soybean phospholipid) manufactured by Nikko Chemicals, egg yolk lecithin PL-100P (hydrogenated egg yolk phospholipid) manufactured by QP, etc. can be used. Examples of acylated amino acids and / or salts thereof include sarcosinate MN (sodium myristoylmethylaminoacetate), alaninate LN-30 (sodium lauroylmethylalanine), sarcosinate CN-30 (cocoylsarcosine sodium), sarcosinate OH (oleic acid) manufactured by Nikko Chemical Co., Ltd. Oil Sarcosine), Ajinomoto's Amisoft HS-21 (N-stearoyl-L-glutamate disodium), SEPPIC's SEPILIFT DPHP (dipalmitoyl hydroxyproline), and the like can be used.
これら表面処理剤の使用量を限定するものではないが、本発明の表面処理剤の特性を損なわない程度に使用することが好ましい。好ましくは０．１から１０質量部程度である。 Although the usage-amount of these surface treating agents is not limited, It is preferable to use it to such an extent that the characteristic of the surface treating agent of this invention is not impaired. Preferably, it is about 0.1 to 10 parts by mass.
本発明に、用いられる基材粉体としては、従来化粧料用粉体として用いられている粉体であれば特に制限されず、例えば、次のような基材粉体が挙げられる。またこれらの基材粉体は１種または２種以上を混合して用いても構わない。 The base powder used in the present invention is not particularly limited as long as it is a powder conventionally used as a powder for cosmetics, and examples thereof include the following base powder. These base powders may be used alone or in combination of two or more.
酸化鉄、酸化亜鉛、酸化チタン、酸化セリウム、酸化マグネシウム、酸化ジルコニウム、硫酸バリウム、酸化クロム、群青、ベンガラ、炭酸マグネシウム、炭酸カルシュウム、マイカ、セリサイト、タルク、シリカ、カオリン、水酸化クロム、亜鉛華、カーボンブラック、アルミナ、ケイ酸アルミニウム、ケイ酸マグネシウム、窒化ホウ素、シリカ−アルミナ粉末、ベントナイト、スメクタイトなどの無機顔料、ナイロンパウダー、ポリウレタンパウダー、ポリメチルメタクリレート、スチレン−ジビニルベンゼン共重合体、ポリエチレン粉体、シリコーン樹脂、テフロン（登録商標）パウダー、シリコーンガム、シルクパウダー、カルナバワックス、ライスワックス、デンプン、微結晶セルロースなどの有機粉体、ローダミンＢ等の有機色素、赤色２０１号、黒色４０１号、黄色４号、青色1号等のジルコニウム、バリウム又はアルミニウムレーキ等の有機着色料、雲母チタン、酸化鉄コーティング雲母などの複合粉体、表面処理がなされている粉体などが挙げられ、形状としては、球状、板状、針状、繊維状など通常化粧料に用いられる形状、粒径であれば構わない。 化粧料に使用可能な基材粉体への被覆量は、基材粉体の種類やその粒子径、吸油量、吸水量、比表面積により異なるが、基材粉体１００質量部に対する本発明に係るパーフルオロポリエーテル鎖を有する本発明の表面処理剤の処理量は０．５〜４０質量部が好ましく、更に好ましくは１〜２０質量部である。０．５質量部より少ないと十分な効果が得られず、多すぎると本発明表面処理剤の特性を失う。 Iron oxide, zinc oxide, titanium oxide, cerium oxide, magnesium oxide, zirconium oxide, barium sulfate, chromium oxide, ultramarine, bengara, magnesium carbonate, calcium carbonate, mica, sericite, talc, silica, kaolin, chromium hydroxide, zinc Hana, carbon black, alumina, aluminum silicate, magnesium silicate, boron nitride, silica-alumina powder, bentonite, smectite and other inorganic pigments, nylon powder, polyurethane powder, polymethyl methacrylate, styrene-divinylbenzene copolymer, polyethylene Powder, silicone resin, Teflon (registered trademark) powder, silicone gum, silk powder, carnauba wax, rice wax, starch, organic powder such as microcrystalline cellulose, organic color such as rhodamine B , Red 201, black 401, yellow 4 and blue 1 such as zirconium, barium or aluminum lake and other organic colorants, composite powder such as mica titanium, iron oxide coated mica, surface treated powder The shape may be any shape as long as it is a shape or particle size usually used in cosmetics, such as a spherical shape, a plate shape, a needle shape, or a fiber shape. The coating amount of the base material powder that can be used in cosmetics varies depending on the type of base material powder, its particle diameter, oil absorption, water absorption, and specific surface area. The treatment amount of the surface treatment agent of the present invention having such a perfluoropolyether chain is preferably 0.5 to 40 parts by mass, more preferably 1 to 20 parts by mass. When the amount is less than 0.5 parts by mass, a sufficient effect cannot be obtained, and when it is too much, the characteristics of the surface treatment agent of the present invention are lost.
次に本発明の化粧料について詳述する。 Next, the cosmetic of the present invention will be described in detail.
本発明の化粧料は、上述の本発明の表面処理粉体を含有するもので、その剤型は任意であり、一般に従来の化粧料用粉体を含有する化粧料はすべて含まれる。それら化粧料としては、例えば、ファンデーション、白粉、ほほ紅などのフェイシャル化粧料、アイシャドウ、マスカラ、アイライナー、眉墨、口紅、ネイルエナメルなどといったメークアップ化粧料及び日焼け止め化粧品、乳液、ローションなどの基礎化粧料等が挙げられる。また、化粧料の他、皮膚外用剤、医薬用軟膏等にも好適に使用できる。 The cosmetic of the present invention contains the above-mentioned surface-treated powder of the present invention, and its dosage form is arbitrary, and generally includes all cosmetics containing conventional cosmetic powders. Such cosmetics include, for example, facial cosmetics such as foundations, white powder, cheeks, makeup cosmetics such as eye shadows, mascaras, eye liners, eyebrows, lipsticks, nail enamels, sunscreen cosmetics, emulsions, lotions, etc. Examples include basic cosmetics. In addition to cosmetics, it can also be suitably used for external preparations for skin, ointments for pharmaceutical use and the like.
本発明の表面処理粉体の配合量は、化粧料の形態に応じて変動するが、通常、０．０１〜９９．９質量％である。化粧料として香料等の他の成分を配合させること、また、０．１質量％未満の配合量では本発明に係る表面処理粉体による撥水性、撥油効果及び好ましい感触が十分に表われないことを考え合わせると、表面処理粉体の配合量は、好ましくは０．１〜９９質量％の範囲である。なお、化粧料の種類により、例えば固形粉体化粧料には、２０〜８０質量％、クリーム状化粧料には５〜５０質量％、乳液状化粧料には２〜３０質量％、ローション類には２〜２０質量％を配合するのがさらに好ましい。 The amount of the surface-treated powder of the present invention varies depending on the form of the cosmetic, but is usually 0.01 to 99.9% by mass. Addition of other ingredients such as fragrances as cosmetics, and if the blending amount is less than 0.1% by mass, the water repellency, oil repellency and preferred feel of the surface-treated powder according to the present invention are not sufficiently exhibited. Considering this, the amount of the surface-treated powder is preferably in the range of 0.1 to 99% by mass. Depending on the type of cosmetic, for example, 20-80% by mass for solid powder cosmetics, 5-50% by mass for creamy cosmetics, 2-30% by mass for milky cosmetics, and lotions. Is more preferably 2 to 20% by mass.
本発明の化粧料に配合できる、本発明に係わる表面処理粉体以外の成分としては、目的とする化粧料の種類に応じて、通常の化粧料に配合される成分から適宜選択して使用することができる。これらの成分としては、例えば、流動パラフィン、ワセリンなどの炭化水素、植物油脂、ロウ類、合成エステル油、シリコーン系の油相成分、フッ素系の油相成分、高級アルコール類、低級アルコール、脂肪酸類、増粘剤、紫外線吸収剤、粉体、無機・有機顔料、色材、各種界面活性剤、多価アルコール、糖、高分子化合物、生理活性成分、経皮吸収促進剤、溶媒、酸化防止剤、香料、防腐剤、各種添加剤等が挙げられるがこれらに限定されるものではない。 Components other than the surface-treated powder according to the present invention that can be blended in the cosmetics of the present invention are appropriately selected and used from the components blended in normal cosmetics, depending on the type of the target cosmetics. be able to. Examples of these components include hydrocarbons such as liquid paraffin and petrolatum, vegetable oils and fats, waxes, synthetic ester oils, silicone oil phase components, fluorine oil phase components, higher alcohols, lower alcohols, and fatty acids. , Thickener, ultraviolet absorber, powder, inorganic / organic pigment, colorant, various surfactants, polyhydric alcohol, sugar, polymer compound, physiologically active ingredient, transdermal absorption promoter, solvent, antioxidant , Fragrances, preservatives, various additives and the like, but are not limited thereto.
本発明の化粧料は、通常の方法に従って製造することができる。本発明の化粧料用粉体を配合した化粧料は、耐水性・耐皮脂性に優れ、汗及び皮脂等による化粧崩れを防止し、且つ肌上への化粧料の塗布時の感触が滑らかで、付着性に優れ、しっとりした使用感を与えることができる。 The cosmetic of the present invention can be produced according to a usual method. Cosmetics containing the cosmetic powder of the present invention are excellent in water resistance and sebum resistance, prevent makeup collapse due to sweat and sebum, etc., and have a smooth feel when the cosmetic is applied on the skin. It has excellent adhesion and gives a moist feeling.
以下に実施例を挙げて本発明を具体的に説明するが、本発明の技術的範囲はこれらに限定されるものではない。 EXAMPLES The present invention will be specifically described below with reference to examples, but the technical scope of the present invention is not limited to these examples.
［実施例１］
１．製造方法
（処理粉体の製造方法１）
ビーカーにセリサイト１００ｇを秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウム水溶液を加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらにＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを２ｇ加えて３０分間混合する。塩酸でＰＨ４．５として、１０分間混合後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品１とした。
[Example 1]
1. Manufacturing method (Processed powder manufacturing method 1)
Weigh 100 g of sericite in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide aqueous solution is added here as PH10, 2g of FOMBLIN HC / P2-1000 is added, and it mixes for 30 minutes. Add 2g of FOBLIN HC / PU-AN5E and mix for 30 minutes. Adjust to pH 4.5 with hydrochloric acid, mix for 10 minutes, and filter. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer.
（処理粉体の製造方法２）
ビーカーにセリサイト１００ｇを秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウム水溶液を加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を２ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２とした。
(Processed powder production method 2)
Weigh 100 g of sericite in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide aqueous solution is added here as PH10, 2g of FOMBLIN HC / P2-1000 is added, and it mixes for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, 2 g of FOBBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out, dried at 100 ° C. for 8 hours with a dryer, and pulverized with an atomizer to obtain Product 2 of the present invention.
（処理粉体の製造方法３）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウム水溶液を加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品３とした。
(Processed powder production method 3)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. Sodium hydroxide aqueous solution is added here as PH10, 2g of FOMBLIN HC / P2-1000 is added, and it mixes for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized and pulverized to obtain Product 3 of the present invention.
（処理粉体の製造方法４）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウム水溶液を加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを２ｇ加え、更にＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加えて、３０分間混合する。塩酸を加えてＰＨ４．５とし、混合後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品４とした。
(Processed powder production method 4)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. Sodium hydroxide aqueous solution is added here as PH10, 2g of FOMBLIN HC / PU-AN5E is added, and 2g of FOMBLIN HC / P2-1000 is further added, and it mixes for 30 minutes. Hydrochloric acid is added to pH 4.5, and after mixing, it is filtered. This was taken out and dried at 100 ° C. for 8 hours in a dryer and atomized and pulverized to make Product 4 of the present invention.
（処理粉体の製造方法５）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに塩化アルミニウム六水和物を１ｇ加え、攪拌混合しながら水酸化ナトリウムを加えてＰＨ１０とし、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ、更にＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを２ｇ加えて、３０分間混合する。塩酸を加えてＰＨ４．５とし、混合後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品５とした。
(Processed powder production method 5)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. Add 1 g of aluminum chloride hexahydrate, add sodium hydroxide with stirring to PH10, add 2 g of FOMBLIN HC / P2-1000, and then add 2 g of FOMBLIN HC / PU-AN5E and mix for 30 minutes. . Hydrochloric acid is added to pH 4.5, and after mixing, it is filtered. The product was taken out and dried at 100 ° C. for 8 hours with a dryer and pulverized with an atomizer to obtain Product 5 of the present invention.
（処理粉体の製造方法６）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに塩化アルミニウム六水和物を１ｇ加え、攪拌混合しながら水酸化ナトリウム水溶液を加えてＰＨ１０とし、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を２ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品６とした。
(Processed powder production method 6)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. To this, 1 g of aluminum chloride hexahydrate is added, and while stirring and mixing, an aqueous sodium hydroxide solution is added to make PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, 2 g of FOBBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours in a dryer and atomized and pulverized as Product 6 of the present invention.
（処理粉体の製造方法７）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに塩化アルミニウム六水和物を１ｇ加え、攪拌混合しながら水酸化ナトリウム水溶液を加えてＰＨ１０とし、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ、更にＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて、３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品７とした。
(Processed powder production method 7)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. Add 1 g of aluminum chloride hexahydrate, add sodium hydroxide aqueous solution with stirring to PH10, add 2 g of FOMBLIN HC / P2-1000 and 1 g of FOMBLIN HC / PU-AN5E, and mix for 30 minutes To do. After adjusting the pH to 4.5 with hydrochloric acid, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out, dried at 100 ° C. for 8 hours with a dryer, and pulverized with an atomizer to obtain Product 7 of the present invention.
（処理粉体の製造方法８）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を４ｇ加えて、３０分間混合する。塩酸を加えてＰＨ４．５とし、混合後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを比較品１とした。
(Processed powder production method 8)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 4 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Hydrochloric acid is added to pH 4.5, and after mixing, it is filtered. This was taken out and dried at 100 ° C. for 8 hours with a drier, and then atomized by the atomizer.
（処理粉体の製造方法９）
ビーカーにセリサイト１００ｇを計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを４ｇ加え、３０分間混合する。塩酸を加えてＰＨ４．５とし、混合後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを比較品２とした。
(Processed powder production method 9)
Weigh 100 g of sericite into a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 4 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to pH 4.5, and after mixing, it is filtered. This was taken out and dried in a dryer at 100 ° C. for 8 hours and pulverized with an atomizer to make Comparative Product 2.
（処理粉体の製造方法１０）
ビーカーにセリサイト１００ｇを秤り取り、精製水１００ｇを加えてよく攪拌する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を４ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを比較品３とした。
(Processed powder production method 10)
Weigh 100 g of sericite in a beaker, add 100 g of purified water, and stir well. After adjusting the pH to 4.5 with hydrochloric acid, 4 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and filtered. This was taken out and dried in a dryer at 100 ° C. for 8 hours, followed by atomizer pulverization as Comparative product 3.
２．評価方法
（撥水性、撥油性）試料を平板な容器に入れ、１００ｋｇ／ｃｍ２の力で平坦な表面を作り、ここに水滴、スクワラン滴を静かに落として、接触角を測定した。
（付着性）上腕内側部に試料を均質に擦り付け、これを刷毛ではき取った時に付着している様子を肉眼観察し、以下の５点のスコアで評価し、その平均を求めた。
５： 未処理粉体よりも付着性に優れる
４： 未処理粉体よりも比較的付着性に優れる
３： 未処理粉体と同程度
２： 未処理粉体よりも比較的崩れやすい
１： 未処理粉体よりもかなり崩れやすい
（感触）モニター５名で、塗布時の滑らかさを以下の５点のスコアで評価し、その平均を求めた。
５： 未処理粉体よりもかなり良い
４： 未処理粉体より良い
３： 未処理粉体と同程度
２： 未処理粉体よりも比較的劣る
１： 未処理粉体よりもかなり劣る
2. Evaluation method (Water repellency, oil repellency) A sample was put in a flat container, a flat surface was made with a force of 100 kg / cm 2 , water drops and squalane drops were gently dropped thereon, and a contact angle was measured.
(Adhesiveness) The sample was uniformly rubbed against the inner side of the upper arm, and when it was scraped off with a brush, it was visually observed, evaluated with the following five points, and the average was obtained.
5: Adhesion better than untreated powder 4: Relatively better adhesion than untreated powder 3: Same as untreated powder 2: Easier to break than untreated powder 1: Not yet It was much easier to break than the treated powder. (Feel) The smoothness at the time of application was evaluated by the following five points by five monitors, and the average was obtained.
5: Much better than untreated powder 4: Better than untreated powder 3: Same as untreated powder 2: Relatively inferior to untreated powder 1: Much worse than untreated powder
３．評価結果
評価結果を表１に示す。ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００とＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅ、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００とＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５の併用、処理順序、処理方法を変えても、良好な粉体が得られた。また表面処理助剤として塩化アルミニウム六水和物を加える方法では更に良好な粉体が得られた。さらに、併用表面処理を行った本発明品１および２は、単純表面処理品比較例１、２、３に比べて、撥水性、撥油性、感触のすべてにおいて優れた結果が得られた。
［実施例２］
１．製造方法
処理粉体は、［実施例１］の（処理粉体の製造方法１）または（処理粉体の製造方法２）に準じて製造した。
[Example 2]
1. Manufacturing method The processing powder was manufactured according to (Processing powder manufacturing method 1) or (Processing powder manufacturing method 2) of [Example 1].
２．評価方法
（撥水性、撥油性）試料を平板な容器に入れ、１００ｋｇ／ｃｍ２の力で平坦な表面を作り、ここに水滴、スクワラン滴を静かに落として、接触角を測定した。
（感触）モニター５名で、塗布時の滑らかさを評価し、以下の５点のスコアで評価し、その平均を求めた。
５： 未処理粉体よりもかなり良い
４： 未処理粉体より良い
３： 未処理粉体と同程度
２： 未処理粉体よりも比較的劣る
１： 未処理粉体よりもかなり劣る
2. Evaluation method (Water repellency, oil repellency) A sample was put in a flat container, a flat surface was made with a force of 100 kg / cm 2 , water drops and squalane drops were gently dropped thereon, and a contact angle was measured.
(Feel) The smoothness at the time of application was evaluated by five monitors, and the following five points were evaluated, and the average was obtained.
5: Much better than untreated powder 4: Better than untreated powder 3: Same as untreated powder 2: Relatively inferior to untreated powder 1: Much worse than untreated powder
３．評価結果
本発明の表面処理剤は、０．５〜４０％の処理量において、その効果が現れ、２〜２０％の処理量で、撥水性、撥油性に優れ、感触にも優れた粉体が得られた。
［実施例３］
［実施例２］において、撥水／撥油性が最も優れていた４．０重量％に固定し、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００とＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅ、およびＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００とＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５の配合比率を変えた表面処理粉体の評価を行った。
[Example 3]
In [Example 2], the water / oil repellency was fixed at 4.0% by weight which was most excellent, and FOMBLIN HC / P2-1000 and FOMBLIN HC / PU-AN5E, and FOMBLIN HC / P2-1000 and FOMBLINE HC Evaluation of surface-treated powders with different ratios of / PU-CAT5.
１．製造方法
処理粉体は、［実施例１］の（処理粉体の製造方法１）または（処理粉体の製造方法２）に準じて製造した。
1. Manufacturing method The processing powder was manufactured according to (Processing powder manufacturing method 1) or (Processing powder manufacturing method 2) of [Example 1].
２．評価方法
（撥水性、撥油性）試料を平板な容器に入れ、１００ｋｇ／ｃｍ２の力で平坦な表面を作り、ここに水滴、スクワラン滴を静かに落として、接触角を測定した。
（感触）モニター５名で、塗布時の滑らかさを評価し、以下の５点のスコアで評価し、その平均を求めた。
５： 未処理粉体よりもかなり良い
４： 未処理粉体より良い
３： 未処理粉体と同程度
２： 未処理粉体よりも比較的劣る
１： 未処理粉体よりもかなり劣る
2. Evaluation method (Water repellency, oil repellency) A sample was put in a flat container, a flat surface was made with a force of 100 kg / cm 2 , water drops and squalane drops were gently dropped thereon, and a contact angle was measured.
(Feel) The smoothness at the time of application was evaluated by five monitors, and the following five points were evaluated, and the average was obtained.
5: Much better than untreated powder 4: Better than untreated powder 3: Same as untreated powder 2: Relatively inferior to untreated powder 1: Much worse than untreated powder
３．評価結果
結果を表３に示す。ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００に対して、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５ＥまたはＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５量が増えるに従って、感触に優れ、撥水撥油性に優れた粉体が得られた。ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅの配合量が０．１重量％以下になると感触が悪く、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００の配合量が０．１重量％以下になると撥油性が得れず、滑らかな感触も十分得られなかった。
［実施例４］
本発明でいうパーフルオロポリエーテル鎖を有する化合物と及びパーフルオロポリエーテルリン酸、それに一般式（１）から（３）以外の表面処理剤を別途添加し、併用での評価を行った。
[Example 4]
The compound having a perfluoropolyether chain referred to in the present invention, perfluoropolyether phosphoric acid, and a surface treating agent other than those represented by the general formulas (1) to (3) were separately added, and the combined use was evaluated.
１．製造方法
処理粉体は、［実施例１］の（処理粉体の製造方法２）に準じて製造した。
1. Production Method The treated powder was produced according to (Processed Powder Production Method 2) in [Example 1].
２．評価方法
（撥水性、撥油性）試料を平板な容器に入れ、１００ｋｇ／ｃｍ２の力で平坦な表面を作り、ここに水滴、スクワラン滴を静かに落として、接触角を測定した。
（感触）モニター５名で、塗布時の滑らかさを評価し、以下の５点のスコアで評価し、その平均を求めた。
５： 未処理粉体よりもかなり良い
４： 未処理粉体より良い
３： 未処理粉体と同程度
２： 未処理粉体よりも比較的劣る
１： 未処理粉体よりもかなり劣る
2. Evaluation method (Water repellency, oil repellency) A sample was put in a flat container, a flat surface was made with a force of 100 kg / cm 2 , water drops and squalane drops were gently dropped thereon, and a contact angle was measured.
(Feel) The smoothness at the time of application was evaluated by five monitors, and the following five points were evaluated, and the average was obtained.
5: Much better than untreated powder 4: Better than untreated powder 3: Same as untreated powder 2: Relatively inferior to untreated powder 1: Much worse than untreated powder
３．評価結果
多くの組み合わせで、シラン単独と同程度の撥水性、撥油性と感触が得られた。本実験においてもパーフルオロポリエーテルリン酸との併用により、相乗的に機能の改善が認められた。
［実施例５］ 化粧下地
１．製造方法
（処理粉体の製造方法１１）
ビーカーに（ジフェニルジメチコン／ビニルフェニルジメチコン／シルセスキオキサン）クロスポリマーを１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品１５とした。
[Example 5] Makeup base 1. Manufacturing method (Processed powder manufacturing method 11)
In a beaker, weigh 100 g of (diphenyldimethicone / vinylphenyldimethicone / silsesquioxane) crosspolymer, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer.
（処理粉体の製造方法１２）
ビーカーに酸化チタンを１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品１６とした。
(Processed powder production method 12)
Weigh 100 g of titanium oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer.
（処理粉体の製造方法１３）
ビーカーに酸化鉄を１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品１７とした。
(Processed powder production method 13)
Weigh 100 g of iron oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out, dried at 100 ° C. for 8 hours with a dryer, and pulverized with an atomizer to obtain Product 17 of the present invention.
２．処方
Ａ 水 残部（質量％）
グリセリン ５
ステアロキシＰＧヒドロキシＰＧヒドロキシエチルスルフォン酸Ｎａ ２
Ｂ パーフルオロアルキル（Ｃ４−１４）エトキシジメチコン １３
シクロメチコン １０
ジメチコン ６
メトキシケイヒ酸オクチル ４
エタノール ３
イソステアリルグリセリン ３
１−３ブチレングリコール ２
カーボマー（４％水溶液） ２
ナイロン１２ ２
表面処理（ジフェニルジメチコン／ビニルフェニルジメチコン／
シルセスキオキサン）クロスポリマー（本発明品１５） ２
表面処理酸化チタン（本発明品１６） ２
表面処理酸化鉄（本発明品１７） ２
（調製方法）Ａ相を常温にてホモミキサーにて攪拌しなら、Ｂ相を加えて乳化した。
（結果）ＳＰＦ２５／ＰＡ＋＋で、撥水性、撥油性に優れ、感触の良い化粧下地を得た。
2. Formulation A Water remainder (% by mass)
Glycerin 5
Stearoxy PG hydroxy PG hydroxyethyl sulfonate Na 2
B Perfluoroalkyl (C4-14) ethoxydimethicone 13
Cyclomethicone 10
Dimethicone 6
Octyl methoxycinnamate 4
Ethanol 3
Isostearyl glycerin 3
1-3 Butylene glycol 2
Carbomer (4% aqueous solution) 2
Nylon 12 2
Surface treatment (diphenyl dimethicone / vinyl phenyl dimethicone /
Silsesquioxane) Crosspolymer (Invention product 15) 2
Surface-treated titanium oxide (Invention product 16) 2
Surface-treated iron oxide (Invention product 17) 2
(Preparation method) If phase A was stirred with a homomixer at room temperature, phase B was added and emulsified.
(Results) A makeup base with SPF25 / PA ++, excellent in water repellency and oil repellency, and good touch was obtained.
［実施例６］ パウダーファンデーション
１．製造方法
（処理粉体の製造方法１４）
ビーカーにマイカを１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品１８とした。
Example 6 Powder Foundation Manufacturing method (Processed powder manufacturing method 14)
Weigh 100 g of mica in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer to obtain the product 18 of the present invention.
（処理粉体の製造方法１５）
ビーカーにタルクを１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品１９とした。
(Processed powder production method 15)
Weigh 100 g of talc in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out and dried in a dryer at 100 ° C. for 8 hours and pulverized with an atomizer to make a product 19 of the present invention.
（処理粉体の製造方法１６）
ビーカーに合成金雲母を１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２０とした。
(Processed powder production method 16)
Weigh 100 g of synthetic phlogopite in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out, dried at 100 ° C. for 8 hours with a dryer, and pulverized with an atomizer to make a product 20 of the present invention.
２．処方
Ａ）表面処理マイカ（本発明品１８） 残部（質量％）
表面処理タルク（本発明品１９） １５
表面処理合成金雲母（本発明品２０） １０
ナイロン１２ １０
Ｂ）ジメチコン ７
ミリスチン酸イソセチル ５
メトキシケイヒ酸オクチル ５
（ジフェニルジメチコン／ビニルフェニルジメチコン
／シルセスキオキサン）クロスポリマー ３
トリ（カプリル／カプリン酸）グリセリル ３
水添ポリイソブテン ３
（調製方法）Ｂ成分をよく混和し、Ａ成分を加えて均一になるまでさらに混和し、容器に充填して製品とした。
（結果）ＳＰＦ２５／ＰＡ++で、撥水撥油性に優れ、感触の良いファンデーションを得た。
2. Formulation A) Surface-treated mica (Invention product 18) Remainder (mass%)
Surface treatment talc (Invention product 19) 15
Surface-treated synthetic phlogopite (Invention product 20) 10
Nylon 12 10
B) Dimethicone 7
Isocetyl myristate 5
Octyl methoxycinnamate 5
(Diphenyl dimethicone / vinyl phenyl dimethicone / silsesquioxane) cross polymer 3
Tri (capryl / capric) glyceryl 3
Hydrogenated polyisobutene 3
(Preparation method) The component B was mixed well, the component A was added and further mixed until uniform, and filled into a container to obtain a product.
(Result) An SPF25 / PA ++ foundation having excellent water and oil repellency and good touch was obtained.
［実施例７］ リキッドファンデーション
１．製造方法
（処理粉体の製造方法１７）
ビーカーに酸化亜鉛を１００ｇ秤り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を１ｇ加え３０分間混合する。塩酸でＰＨ４．５とした後、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を３ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２１とした。
[Example 7] Liquid foundation Manufacturing method (Processed powder manufacturing method 17)
Weigh 100 g of zinc oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 1 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. After adjusting the pH to 4.5 with hydrochloric acid, add 3 g of FOMBLINE HC / PU-CAT5, stir for 30 minutes, and filter. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer.
２．処方
Ａ 精製水 残部（質量％）
ブチレングリコール ５．０
グリセリン ２．０
ペミュレン ０．１
フェノキシエタノール ３．０
Ｂ シクロペンタシロキサン ２０．０
表面処理酸化チタン（本発明品１６） ５．０
表面処理酸化亜鉛（本発明品２１） ６．０
ＰＥＧ−９ポリジメチルシロキシエチルジメチコン ２．０
（アクリルサンアルキル／ジメチコン）コポリマー ２．０
（ジメチコン／ビニルジメチコン）クロスポリマー ２．０
フィトステロールイソステアレート １．０
色材 ０．９
（調製方法）Ｂ相をディスパーで良く混合後、均一溶液としたＡ相にホモミキサー攪拌しながら、加えて乳化した。
（結果）撥水性、撥油性に優れた乳液状ファンデーションを得た。紫外線防御能もＳＰＦ２０、ＰＡ＋＋と高い値を示した。
2. Formulation A Purified water The remainder (mass%)
Butylene glycol 5.0
Glycerin 2.0
Pemulen 0.1
Phenoxyethanol 3.0
B cyclopentasiloxane 20.0
Surface-treated titanium oxide (Invention product 16) 5.0
Surface-treated zinc oxide (Invention product 21) 6.0
PEG-9 polydimethylsiloxyethyl dimethicone 2.0
(Acrylic Sunalkyl / Dimethicone) Copolymer 2.0
(Dimethicone / Vinyl Dimethicone) Cross Polymer 2.0
Phytosterol isostearate 1.0
Color material 0.9
(Preparation method) Phase B was thoroughly mixed with a disper, and then added to phase A, which was made into a uniform solution, while stirring with a homomixer and emulsified.
(Results) An emulsion foundation excellent in water repellency and oil repellency was obtained. The UV protection ability also showed high values such as SPF20 and PA ++.
［実施例８］ Ｗ／Ｏ紫外線防御化粧品
１．製造方法
（処理粉体の製造方法１８）
ビーカーに酸化亜鉛を１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２２とした。
[Example 8] W / O UV protection cosmetics Manufacturing method (Processed powder manufacturing method 18)
Weigh 100 g of zinc oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out, dried at 100 ° C. for 8 hours with a dryer, and pulverized with an atomizer to make the product 22 of the present invention.
（処理粉体の製造方法１９）
ビーカーに酸化チタンを１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２３とした。
(Processed powder production method 19)
Measure 100 g of titanium oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer to obtain the product 23 of the present invention.
（処理粉体の製造方法２０）
ビーカーにタルクを１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２４とした。
(Processed powder production method 20)
Weigh 100 g of talc in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. The product was taken out and dried at 100 ° C. for 8 hours with a dryer and pulverized with an atomizer to obtain a product 24 of the present invention.
（処理粉体の製造方法２１）
ビーカーに合成金雲母を１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２５とした。
(Processed powder production method 21)
Weigh 100 g of synthetic phlogopite in a beaker, add 100 g of purified water and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours in a dryer and atomized and pulverized to make Product 25 of the present invention.
２．処方
Ａ）ジメチコン １０．０
ジフェニルシロキシフェニルトリメチコン ５．０
（ジメチコン／メチコン）・コポリマー ６．０
セレシン ５．０
トリオクタン酸トリメチロールプロパン ５．０
セスキイソステアリン酸ソルビタン ４．０
カルナウバロウ １．０
表面処理酸化亜鉛（本発明品２２） １０．０
表面処理酸化チタン（本発明品２３） ２．０
表面処理タルク（本発明品２４） ２．０
表面処理合成金雲母（本発明品２５） ２．０
シクロメチコン ３．０
メトキシケイヒ酸オクチル ３．０
ミネラルオイル １．０
ワセリン １．０
Ｂ）ジプロピレングリコール ２．０
ヒアルロン酸Ｎａ ０．２
水 残部（質量％）
（調製方法）Ａ成分を７０℃に加熱し、本発明粉体以外を均一に溶解させた後、ホモミキサーまたはディスパーミキサーでゆっくりと攪拌しながらＡにＢを徐々に加えた後、強く攪拌して乳化を行う。
（結果）撥水性、撥油性に優れ、使用感の良いＷ／Ｏ型の紫外線防御化粧品が得られた。また本発明処理粉体の分散性は高く、高い紫外線防御能を示した。ＳＰＦ３０、ＰＡ＋＋＋
2. Formula A) Dimethicone 10.0
Diphenylsiloxyphenyl trimethicone 5.0
(Dimethicone / Methicone) Copolymer 6.0
Ceresin 5.0
Trimethylolpropane trioctanoate 5.0
Sorbitan sesquiisostearate 4.0
Carnauba 1.0
Surface-treated zinc oxide (Invention product 22) 10.0
Surface-treated titanium oxide (present product 23) 2.0
Surface treatment talc (Invention product 24) 2.0
Surface treated synthetic phlogopite (Invention product 25) 2.0
Cyclomethicone 3.0
Octyl methoxycinnamate 3.0
Mineral oil 1.0
Vaseline 1.0
B) Dipropylene glycol 2.0
Hyaluronic acid Na 0.2
Water balance (mass%)
(Preparation method) After heating component A to 70 ° C. and uniformly dissolving the powder of the present invention, slowly adding B to A while slowly stirring with a homomixer or dispermixer, and then stirring vigorously To emulsify.
(Results) A W / O type UV protective cosmetic product having excellent water and oil repellency and good usability was obtained. Moreover, the dispersibility of the treated powder of the present invention was high, and high UV protection ability was exhibited. SPF30, PA ++
［実施例９］ 紫外線防御機能を有するファンデーション [Example 9] Foundation having UV protection function
１．製造方法
（処理粉体の製造方法２２）
ビーカーにタルクを１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇとイソプロピルトリイソステアロイルチタネートを１ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２６とした。
1. Manufacturing method (Processed powder manufacturing method 22)
Weigh 100 g of talc in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added here to make PH10, 2 g of FOMBLIN HC / P2-1000 and 1 g of isopropyltriisostearoyl titanate are added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer.
（処理粉体の製造方法２３）
ビーカーに合成金雲母を１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇとイソプロピルトリイソステアロイルチタネートを１ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２７とした。
(Processed powder production method 23)
Weigh 100 g of synthetic phlogopite in a beaker, add 100 g of purified water and stir well. Sodium hydroxide is added here to make PH10, 2 g of FOMBLIN HC / P2-1000 and 1 g of isopropyltriisostearoyl titanate are added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours in a dryer and atomized and pulverized, and this was designated as Product 27 of the present invention.
（処理粉体の製造方法２４）
ビーカーに酸化亜鉛を１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇとイソプロピルトリイソステアロイルチタネートを１ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過する。これを取り出し乾燥機にて１００℃で８時間乾燥し、アトマイザー粉砕したものを本発明品２８とした。
(Processed powder production method 24)
Weigh 100 g of zinc oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added here to make PH10, 2 g of FOMBLIN HC / P2-1000 and 1 g of isopropyltriisostearoyl titanate are added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to obtain a pH of 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes and then filtered. This was taken out and dried at 100 ° C. for 8 hours with a dryer, and then atomized by the atomizer to make the product 28 of the present invention.
２．処方
表面処理タルク（本発明品２６） 残部（質量％）
表面処理合成金雲母（本発明品２７） １０
表面処理酸化亜鉛（本発明品２８） ５
メトキシケイヒ酸オクチル ６
ミネラルオイル ５
微粒子シリカ ３
フィトステリルイソステレート ３
ジメチコン ３
ナイロン粉末 ３
トリエチルヘキサノイン ３
水 ３
トリイソステアリン酸ポリグリセリル-２ １
色材 １
（調製方法）下記の成分をヘンシェルミキサーにて均一になるまで混合し、容器に充填して製品とした。
（結果）肌に対する伸び、滑らかさ、付着性に優れ、オイルへの分散性に優れ、色むらの無いファンデーションが得られた。ＳＰＦ２０、ＰＡ＋＋
2. Formulation Surface treatment talc (Invention product 26) Remainder (mass%)
Surface-treated synthetic phlogopite (Invention product 27) 10
Surface-treated zinc oxide (Invention product 28) 5
Octyl methoxycinnamate 6
Mineral oil 5
Particulate silica 3
Phytosteryl isosterate 3
Dimethicone 3
Nylon powder 3
Triethylhexanoin 3
Water 3
Polyglyceryl triisostearate-2 1
Color material 1
(Preparation method) The following components were mixed with a Henschel mixer until uniform, and filled into a container to obtain a product.
(Results) A foundation having excellent elongation, smoothness and adhesion to the skin, excellent dispersibility in oil, and no color unevenness was obtained. SPF20, PA ++
［実施例１０］ プロテクトエマルション
１．製造方法
（処理粉体の製造方法２５）
ビーカーに酸化チタンを１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過、乾燥する。これにハイドロジェンシリコーン（信越化学製 ＫＦ９９）１ｇを添加してヘンシェルミキサーで粉砕処理し、１３０℃で加熱処理したものを本発明品２９とした。
[Example 10] Protect emulsion 1. Manufacturing method (Processed powder manufacturing method 25)
Measure 100 g of titanium oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to adjust the pH to 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes, filtered and dried. 1 g of hydrogen silicone (KF99, manufactured by Shin-Etsu Chemical Co., Ltd.) was added thereto, pulverized with a Henschel mixer, and heat-treated at 130 ° C. to obtain the product 29 of the present invention.
（処理粉体の製造方法２６）
ビーカーに酸化鉄を１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過、乾燥する。これにハイドロジェンシリコーン（信越化学製 ＫＦ９９）１ｇを添加してヘンシェルミキサーで粉砕処理し、１３０℃で加熱処理したものを本発明品３０とした。
(Processed powder production method 26)
Weigh 100 g of iron oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to adjust the pH to 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes, filtered and dried. 1 g of hydrogen silicone (KF99, manufactured by Shin-Etsu Chemical Co., Ltd.) was added thereto, pulverized with a Henschel mixer, and heat-treated at 130 ° C. to obtain the product 30 of the present invention.
２．処方
Ａ 水 残部（質量％）
エタノール １５．０
グリセリン ６．０
ブチレングリコール ３．０
ステアロキシＰＧヒドロキシエチルセルローススルフォン酸Ｎａ １．０
シリコーンコポリオール １．０
Ｂ メトキシケイヒ酸オクチル ５．０
パーフルオロアルキル（Ｃ４−１４）エトキシジメチコン ５．０
シクロメチコン ５．０
ジメチコン ５．０
イソステアリルグリセリン ２．０
表面処理酸化チタン（本発明品２９） １５．０
表面処理酸化鉄（本発明品３０） ２．０
Ｃ カーボマー ４％水溶液 ２．５
ＰＨ調整剤 適量
香料 適量
防腐剤 適量
（調製方法）Ａ相をホモミキサーで攪拌しながら、均質に混合、分散されたＢ相を加えて乳化する。パドル攪拌に変え、Ｃ相を加えて粘度調整した。
（結果）分散性、撥水性、撥油性に優れた製剤が得られた。
2. Formulation A Water remainder (% by mass)
Ethanol 15.0
Glycerin 6.0
Butylene glycol 3.0
Stearoxy PG hydroxyethyl cellulose sodium sulfonate 1.0
Silicone copolyol 1.0
B Octyl methoxycinnamate 5.0
Perfluoroalkyl (C4-14) ethoxy dimethicone 5.0
Cyclomethicone 5.0
Dimethicone 5.0
Isostearyl glycerin 2.0
Surface-treated titanium oxide (Product 29 of the present invention) 15.0
Surface-treated iron oxide (Invention product 30) 2.0
C Carbomer 4% aqueous solution 2.5
PH adjuster appropriate amount perfume appropriate amount preservative appropriate amount
(Preparation method) While stirring A phase with a homomixer, homogeneously mixed and dispersed B phase is added and emulsified. Viscosity was adjusted by changing to paddle stirring and adding Phase C.
(Results) A preparation excellent in dispersibility, water repellency and oil repellency was obtained.
［実施例１１］ 口紅
１．製造方法
（処理粉体の製造方法２７）
ビーカーに酸化チタンを１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過、乾燥する。これにアミノシリコーンを１ｇ添加してヘンシェルミキサーで粉砕処理し、１３０℃で加熱処理したものを本発明品３１とした。
Example 11 Lipstick Manufacturing method (Processed powder manufacturing method 27)
Measure 100 g of titanium oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to adjust the pH to 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes, filtered and dried. A product obtained by adding 1 g of aminosilicone thereto, pulverizing with a Henschel mixer, and heat-treating at 130 ° C. was designated as Product 31 of the present invention.
（処理粉体の製造方法２８）
ビーカーに酸化鉄を１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過、乾燥する。これにアミノシリコーンを１ｇ添加してヘンシェルミキサーで粉砕処理し、１３０℃で加熱処理したものを本発明品３２とした。
(Processed powder production method 28)
Weigh 100 g of iron oxide in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to adjust the pH to 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes, filtered and dried. A product obtained by adding 1 g of aminosilicone thereto, pulverizing with a Henschel mixer, and heat-treating at 130 ° C. was designated as Product 32 of the present invention.
（処理粉体の製造方法２９）
ビーカーにマイカを１００ｇ計り取り、精製水１００ｇを加えてよく攪拌する。ここに水酸化ナトリウムを加えてＰＨ１０として、ＦＯＭＢＬＩＮ ＨＣ／Ｐ２−１０００を２ｇ加え、３０分間混合する。さらに、ＦＯＭＢＬＩＮ ＨＣ／ＰＵ−ＡＮ５Ｅを１ｇ加えて３０分間混合する。塩酸を加えてＰＨ４．５として、ＦＯＭＢＬＩＮＥ ＨＣ／ＰＵ−ＣＡＴ５を１ｇ加え、３０分間攪拌後ろ過、乾燥する。これにアミノシリコーンを１ｇ添加してヘンシェルミキサーで粉砕処理し、１３０℃で加熱処理したものを本発明品３３とした。
(Processed powder production method 29)
Weigh 100 g of mica in a beaker, add 100 g of purified water, and stir well. Sodium hydroxide is added thereto to obtain PH10, and 2 g of FOMBLIN HC / P2-1000 is added and mixed for 30 minutes. Furthermore, 1 g of FOMBLIN HC / PU-AN5E is added and mixed for 30 minutes. Hydrochloric acid is added to adjust the pH to 4.5, 1 g of FOMBLINE HC / PU-CAT5 is added, and the mixture is stirred for 30 minutes, filtered and dried. A product obtained by adding 1 g of aminosilicone thereto, pulverizing with a Henschel mixer, and heat-treating at 130 ° C. was designated as Product 33 of the present invention.
２．処方
ポリブテン ６０
リンゴ酸イソステアリル １０
トリオクタノイン １０
パルミチン酸デキストリン ３
トリイソステアリン酸ジグリセリン ３
テトライソステアリン酸ペンタエリスリチル ３
（ジメチコン／メチコン）コポリマー ２
ジメチコン ２
炭酸カルシウム １
ミリスチン酸デキストリン １
表面処理酸化チタン（本発明品３１） １
表面処理酸化鉄（本発明品３２） １
表面処理マイカ（本発明品３３） １
その他色材、香料 残部（質量％）
（調製方法）下記の処方にて、ロールミルを使用して、均一に混和して作成した。
（結果）顔料の分散性に優れ鮮やかな色調の口紅が得られた。付着性に優れ、容器などへの色移りし難いものが得られた。
2. Prescription Polybutene 60
Isostearyl malate 10
Trioctanoin 10
Dextrin palmitate 3
Diglycerin triisostearate 3
Pentaerythrityl tetraisostearate 3
(Dimethicone / methicone) copolymer 2
Dimethicone 2
Calcium carbonate 1
Dextrin myristate 1
Surface-treated titanium oxide (Product 31 of the present invention) 1
Surface-treated iron oxide (Invention product 32) 1
Surface-treated mica (Invention product 33) 1
Other coloring materials, fragrance The remainder (mass%)
(Preparation method) A roll mill was used and the mixture was uniformly mixed with the following formulation.
(Result) A lipstick having a vivid color tone with excellent dispersibility of the pigment was obtained. A product having excellent adhesion and difficult to transfer color to a container or the like was obtained.
Claims (6)
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| JPH08217989A (en) * | 1995-02-16 | 1996-08-27 | Nippon Saafuakutanto Kogyo Kk | Water-and oil-repellent powder and cosmetic containing it |
| JP4191314B2 (en) * | 1999-04-28 | 2008-12-03 | 株式会社コーセー | Cosmetics |
| IT1317861B1 (en) * | 2000-02-29 | 2003-07-15 | Ausimont Spa | USE OF FLUORINATED COMPOUNDS TO PROVIDE RELEASE PROPERTIES. |
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