JP3726843B2 - Emulsified cosmetics - Google Patents
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Description
【０００１】
【産業上の利用分野】
本発明は、乳化化粧料において、使用感が良好で、塗布後時間が経過してもべたつかず、密着性が長時間持続され、塗布直後の色変化及び時間が経過した後に起こるくすみを防止し化粧塗布直後の仕上がりの色を長時間維持する効果を有する乳化化粧料に関する。更に詳しくは、低沸点炭化水素又は低沸点シリコーン油の１種又は２種以上の揮発性油剤と微粒子酸化チタン含有の板状ケイ素粉体とを配合することにより、塗布直後の色変化及びくすみ防止効果を高め、化粧料塗布直後の仕上がりの色を長時間維持する効果を有しなおかつ塗布時のさっぱり感・肌への密着性が良好で、塗布後時間がたってもべたつきのない乳化化粧料に関する。
【０００２】
【従来の技術及び発明が解決しようとする課題】
従来の乳化化粧料では、不揮発性の炭化水素類、油脂類、高級アルコール、高級脂肪酸、エステル類等の不揮発性の油剤からなる油相と水相とを界面活性剤を用いて乳化した乳化物が化粧料に応用されている。一般に、乳化化粧料は、塗布時に乳化化粧料中の水の蒸発により清涼感が付与されてさっぱりとした使用感を与えたり、残留する油剤により肌を保護するとともにしっとりとした使用感を与えたりすることから、とても優れた化粧品の形態の一つであると言われている。
【０００３】
しかしながら、上記不揮発性の油剤は、肌や毛髪等に塗布した際に毛髪上に残留するため、べたつきが気になったり、いつまでもヌルヌルとした嫌な感触が残ったりするという欠点を有していた。そこで、近年では、乳化化粧料中に低沸点炭化水素又は低沸点シリコーン油等の揮発性油剤を油相の一部として用いることにより、油剤の残留による好ましくない感触を低減させた乳化化粧料が提案されている。低沸点炭化水素又は低沸点シリコーン油等の揮発性油剤を含有した油中水型エマルジョンとして、例えば、特開昭６１−２６３６３１号公報等が知られている。しかし、メークアップ化粧料等として、これらの低沸点炭化水素又は低沸点シリコーン油等の揮発性油剤を含有した乳化化粧料に着色剤として粉体を配合した場合、塗布後揮発性油剤が蒸発することにより、肌や毛髪上に残留する粉体と油剤との比率が変化し粉体の割合が多くなっていくこととなる。そのため、塗布直後では使用感及び仕上がり感がともに良好なものであっても、塗布後（比較的）短時間の間に粉体が油剤に濡れている状態から乾いた状態に変化していき、粉体の表面での光の散乱が増加して仕上がりの色が白っぽくなってしまう。更に、時間が経過して皮脂が分泌されると、今度は粉体が皮脂により濡れていき、粉体の表面での光の散乱が減少するので仕上がりの色が暗くなり、くすみと呼ばれる好ましくない現象が発生してくるといった欠点を有していた。
【０００４】
また、メークアップ化粧料におけるくすみを防止する目的で、濡れたり乾いたりした時の粉体自身の色変化の少ない粉体として、板状の窒化ホウ素や合成マイカを添加することが知られている（特開昭６１−１００５０８号公報、特開昭６３−１８５８１０号公報）。しかしながら、これらの粉体を乳化化粧料に用いても、完全に色変化が発生しないというものではなく、また、同時に配合される他の着色剤の色変化を防止することはできないために、くすまない乳化化粧料としては満足のいくものではなかった。
【０００５】
一方、微粒子酸化チタン含有の板状二酸化ケイ素粉体としては、特開平１−１４３８２１号公報や特開平６−１１６１１９号公報で紫外線防止効果の面から化粧品への配合が提案されているが、いずれも粉体固形化粧料に関するものであり、水の蒸発による清涼感が付与されないためさっぱりとした使用感に欠けるものであった。
【０００６】
従って、本発明の目的は、塗布直後の仕上がりの色の変化が少なく、高いくすみ抑制効果があり、さっぱり感に優れ、べたつきの無い乳化化粧料を提供することにある。
【０００７】
【課題を解決するための手段】
本発明者らは、鋭意検討した結果、（Ａ）特定の揮発性油剤と、（Ｂ）微粒子酸化チタン含有の板状二酸化ケイ素粉体とを含有する乳化化粧料が、上記目的を達成し得ることを知見した。
【０００８】
本発明は、上記知見に基づきなされたもので、下記（Ａ）及び（Ｂ）成分を含有し、下記（Ａ）成分の含有量が乳化化粧料全体中０．５〜６０重量％であり、下記（Ｂ）成分の含有量が乳化化粧料全体中０．１〜５０重量％である乳化化粧料を提供するものである。
（Ａ）大気圧下での沸点が２４０℃以下で、炭素数６〜１５の直鎖、分岐又は環状の低沸点炭化水素及び粘度が２５℃で５c.s.以下で、大気下での沸点が２４０℃以下の直鎖、分岐又は環状の低沸点シリコーン油からなる群から選ばれた１種又は２種以上の揮発性油剤
（Ｂ）微粒子酸化チタンを５〜５０重量％含有の平均粒径が４．５〜１２．８μｍで厚みが０．１５〜０．９μｍである板状二酸化ケイ素粉体
【０００９】
以下、本発明の乳化化粧料について詳しく述べる。
【００１０】
本発明に用いられる（Ａ）成分は、低沸点炭化水素及び低沸点シリコーン油からなる群から選ばれた１種又は２種以上の揮発性油剤である。
【００１１】
上記低沸点炭化水素としては、炭素数６〜１５の直鎖、分岐又は環状の炭化水素が用いられる。炭素数は８〜１５が好ましい。上記低沸点炭化水素の中でも、特に炭素数１０〜１３のイソパラフィンが好ましく、該イソパラフィンは他の揮発性油剤に比べて乳化のしやすさ及び乳化後の安定性等の点で優れている。また、上記低沸点炭化水素は、大気圧下での沸点が２４０℃以下のものである。なお、上記低沸点炭化水素として、市販品を用いることもでき、具体例としては、アイソバーＣ（ＥＳＳＯ）、シェルソル７１(Shell）等が挙げられる。
【００１２】
上記低沸点シリコーン油としては、大気圧下での沸点が２４０℃以下の直鎖、分岐又は環状のシリコーン油が用いられる。例えば、ジメチルポリシロキサン、環状のシクロジメチルポリシロキサン等が挙げられる。また、上記低沸点シリコーン油の粘度は２５℃で、５c.s.以下である。なお、上記低沸点シリコーン油として、市販品を用いることもでき、具体例としては、ＳＨ２４４、ＳＨ２４５（東レ・ダウコーニング）、ＫＦ９６Ｌ−２ｃｓ、ＫＦ９６Ｌ−１ｃｓ（信越シリコーン）等が挙げられる。
【００１３】
本発明においては、上記揮発性油剤〔（Ａ）成分〕と共に、必要ならば、他の油剤を併用してもよい。上記他の油剤としては、通常の乳化化粧料に使用されるものでよく、例えば、炭化水素類（上記揮発性油剤〔（Ａ）成分〕以外のもの）、油脂類、ワックス類、高級アルコール類、高級脂肪酸類、エステル類等種々のものが挙げられ、用途に応じてこれらの１種又は２種以上を組み合わせて用いられる。
【００１４】
上記揮発性油剤〔（Ａ）成分〕の含有量は、本発明の乳化化粧料全体中、０．５〜６０％（％は重量基準、以下同じ）であり、好ましくは１〜５５％、より好ましくは２〜５０％である。上記含有量が、０．５％未満であると、さっぱりとした使用感及びべたつきのなさを満足することができなくなり、一方、６０％を超えると、油剤が多くなりすぎ水の蒸発による清涼感が低下する。また、本発明における揮発性成分〔上記（Ａ）成分及び上記他の油剤のうち揮発性のもの〕の含有量は、上記（Ａ）成分と上記他の油剤とを含む油剤全体中、好ましくは５％以上、より好ましくは１０％以上である。
【００１５】
本発明に用いられる（Ｂ）成分である微粒子酸化チタン含有の板状二酸化ケイ素粉体の形態は、微粒子酸化チタンが板状二酸化ケイ素粉体中に分散した複合体の形態でも、微粒子酸化チタン及び板状二酸化ケイ素粉体が均一に混合した多成分系の形態でも良い。
上記微粒子酸化チタンの粒径を制御することで、微粒子酸化チタン表面での光散乱を利用して、より高いくすみ抑制効果が得られるので上記の複合体の形態の微粒子酸化チタン含有の板状二酸化ケイ素粉体を用いるのが好ましい。
【００１６】
上記微粒子酸化チタンの平均粒径は、好ましくは１０〜１０００ｎｍ、より好ましくは１０〜３００ｎｍである。上記平均粒径が、１０ｎｍ未満であると、微粒子酸化チタンの透明性が高くなりすぎ、皮脂に濡れた時に白色度が増す効果が不十分であり、一方、１０００ｎｍを超えると板状二酸化ケイ素粉体中に均一に分散した複合体の形態の粉体を得にくくなる傾向にある。
【００１７】
上記板状二酸化ケイ素粉体〔（Ｂ）成分〕における微粒子酸化チタンの含有量は、５〜５０％である。上記含有量が、５％未満であると、くすみ抑制能力が十分ではなく、一方、５０％を超えると、塗布直後に前記揮発性油剤が蒸発して粉体がやや乾燥した状態になった時に白色度が高くなり過ぎ、また、くすみ抑制能力も低下してしまう。
【００１８】
また、上記微粒子酸化チタン含有の板状二酸化ケイ素粉体〔（Ｂ）成分〕中に、微粒子酸化チタン及び板状二酸化ケイ素以外の成分を添加して、各種特性を改善しても良いが、上記微粒子酸化チタン含有の板状二酸化ケイ素粉体のくすみ抑制能や安定性などの点から、微粒子酸化チタン及び板状二酸化ケイ素の合計量は８０％以上でなければならない。上記微粒子酸化チタン含有の板状二酸化ケイ素粉体中に添加し得る他の成分（２０％未満）としては、酸化鉄、アルミナ、ジルコニア等が挙げられる。
【００１９】
上記板状二酸化ケイ素粉体〔（Ｂ）成分〕の平均粒径は、４．５〜１２．８μｍである。
【００２０】
上記板状二酸化ケイ素粉体〔（Ｂ）成分〕の粒子の厚みは、０．１５〜０．９μｍである。
【００２１】
上記板状二酸化ケイ素粉体〔（Ｂ）成分〕の含有量は、本発明の乳化化粧料全体中、０．１〜５０％であり、好ましくは０．３〜４０％、より好ましくは０．５〜３０％である。上記含有量が、０．１％未満であると、くすみ抑制効果が発揮されず、一方、５０％を超えると、粉体成分が多くなりすぎ化粧塗布膜が粉っぽくなる。
【００２２】
本発明における上記（Ａ）成分と上記（Ｂ）成分との含有量の比は、重量比で（Ａ）／（Ｂ）が好ましくは０．０１／１〜８０／１、より好ましくは０．０５／１〜４０／１である。上記含有量の比が、０．０１／１未満であると、微粒子酸化チタン含有の板状二酸化ケイ素粉体の比率が大きくなりすぎ粉っぽくなってしまい、一方、８０／１を超えると、微粒子酸化チタン含有の板状二酸化ケイ素粉体の比率が少なくなりすぎるため、仕上がりの色変化を防止できなくなるので好ましくない。
【００２３】
上記（Ｂ）成分である微粒子酸化チタン含有の板状二酸化ケイ素粉体は、配合の対照となる乳化化粧料の目的に応じて適宜疎水化処理をしても構わない。
【００２４】
上記疎水化処理の方法としては、メチルハイドロジェンポリシロキサン、高粘度シリコーンオイル、シリコーン樹脂等のシリコーン化合物による処理、アニオン活性剤、カチオン活性剤等の界面活性剤による処理、ナイロン、ポリメチルメタクリレート、ポリエチレン、テフロン、ポリアミノ酸等の高分子化合物による処理、パーフロオロ基含有化合物、レシチン、コラーゲン、金属石鹸、親油性ワックス、多価アルコール部分エステル又は完全エステル等による処理等の方法が挙げられる。但し、一般に粉末の疎水化処理に適用できる方法であれば良く、これらの方法に限定されるものではない。
【００２５】
本発明の乳化化粧料には、前記揮発性油剤〔（Ａ）成分〕及び前記微粒子酸化チタン含有の板状二酸化ケイ素粉体〔（Ｂ）成分〕の他に、通常化粧料に用いられる他の成分を必要に応じて適宜配合することができる。
上記他の成分としては、例えば、タルク、カオリン、セリサイト、白雲母、金雲母、紅雲母、黒雲母、リチア雲母、合成フッ素金雲母、バーミキュライト、炭酸マグネシウム、炭酸カルシウム、珪ソウ土、ケイ酸マグネシウム、ケイ酸カルシウム、ケイ酸アルミニウム、ケイ酸バリウム、硫酸バリウム、ケイ酸ストロンチウム、タングステン酸金属塩、シリカ、ヒドロキシアパタイト、ゼオライト、窒化ホウ素、セラミックスパウダー等の無機粉末、ナイロンパウダー、ポリエチレンパウダー、ポリスチレンパウダー、ベンゾグアナミンパウダー、ポリ四弗化エチレンパウダー、ジスチレンベンゼンポリマーパウダー、エポキシパウダー、アクリルパウダー、微結晶性セルロース等の有機粉体、酸化チタン、酸化亜鉛等の無機白色顔料、酸化鉄（ベンガラ）、チタン酸鉄等の無機赤色系顔料、γ酸化鉄等の無機褐色系顔料、黄酸化鉄、黄土等の無機黄色系顔料、黒酸化鉄、カーボンブラック等の無機黒色系顔料、マンゴバイオレット、コバルトバイオレット等の無機紫色系顔料、酸化クロム、水酸化クロム、チタン酸コバルト等の無機緑色系顔料、群青、紺青等の無機青色系顔料、酸化チタン被覆雲母、酸化チタン被覆オキシ塩化ビスマス、オキシ塩化ビスマス、酸化チタン被覆タルク、魚鱗箔、着色酸化チタン被覆雲母等のパール顔料、アルミニウムパウダー、カッパーパウダー等の金属粉末顔料、赤色２０１号、赤色２０２号、赤色２０４号、赤色２０５号、赤色２２０号、赤色２２６号、赤色２２８号、赤色４０５号、橙色２０３号、橙色２０４号、黄色２０５号、黄色４０１号及び青色４０４号等の有機顔料、赤色３号、赤色１０４号、赤色１０６号、赤色２２７号、赤色２３０号、赤色４０１号、赤色５０５号、橙色２０５号、黄色４号、黄色５号、黄色２０２号、黄色２０３号、緑色３号及び青色１号のジルコニウム、バリウム又はアルミニウムレーキ等の有機顔料、クロロフィル、β−カロチン等の天然色素、スクワラン、不揮発性の流動パラフィン、ワセリン、マイクロクリスタリンワックス、オゾケライト、セレシン、ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸、イソステアリン酸、セチルアルコール、ヘキサデシルアルコール、オレイルアルコール、２−エチルヘキサン酸セチル、パルミチン酸−２−エチルヘキシル、ミリスチン酸−２−オクチルドデシル、ジ−２−エチルヘキサン酸ネオペンチルグリコール、トリ−２−エチルヘキサン酸グリセロール、オレイン酸−２−オクチルドデシル、ミリスチン酸イソプロピル、トリイソステアリン酸グリセロール、トリヤシ油脂肪酸グリセロール、トリ−２−エチルヘキサン酸グリセロール、オレイン酸−２−オクチルドデシル、ミリスチン酸イソプロピル、トリイソステアリン酸グリセロール、トリヤシ油脂肪酸グリセロール、オリーブ油、アボガド油、ミツロウ、ミリスチン酸ミリスチル、ミンク油、ラノリン等の各種不揮発性の炭化水素、不揮発性のシリコーン油、パーフルオロポリエーテル、高級脂肪酸、油脂類、エステル類、高級アルコール、ロウ類等の油性成分、アルキッド樹脂、尿素樹脂等の樹脂、カンファ、クエン酸トリブチル等の可塑剤、紫外線吸収剤、酸化防止剤、防腐剤、界面活性剤、保湿剤、香料、増粘剤等が挙げられる。
【００２６】
本発明の乳化化粧料は、常法により種々の形態で使用され、その形態には特に制限されないが、乳化型ファンデーション、クリーム状ファンデーション、乳化型マスカラ、乳化型アイシャドー、クリーム状アイシャドー等のメイクアップ化粧料、プレメイクアップ化粧料、サンスクリーン乳液等として使用される。
【００２７】
【実施例】
以下、実施例及び比較例により、本発明の乳化化粧料を更に詳細に説明する。しかしながら、本発明は、これらの実施例に限定されるものではない。
【００２８】
まず、本発明の乳化化粧料（実施例１〜２３）に用いられる微粒子酸化チタン含有の板状二酸化ケイ素粉体〔（Ｂ）成分〕の製造例（製造例１〜８）を示すが、上記板状二酸化ケイ素粉体の製造方法は、これらに限定されるものではない。なお、本発明に係る上記（Ｂ）成分である微粒子酸化チタン含有の板状二酸化ケイ素粉体としては、日本板硝子株式会社製のＴＳＧフレーク３０〔微粒子酸化チタン（平均粒径４４ｎｍ）３０％含有の板状二酸化ケイ素粉体、平均厚み＝０．５μｍ、平均粒径＝１０μｍ〕が市販されており、該市販品を使用してもよく、また、熱分解法等の常法いずれでも製造可能で、これにより製造したものを使用してもよい。
【００２９】
製造例１〔微粒子酸化チタン５％含有の板状二酸化ケイ素粉体〕
テトラブトキシシラン〔（Ｃ4 Ｈ9 Ｏ）4 Ｓｉ〕５１０重量部（以下、「部」と略す）にブタノール１２００部を混合し、これに、更に微粒子酸化チタン（平均粒径３５ｎｍ）を５部混合し、十分に攪拌する。この溶液を、表面を研磨して平滑にした、厚さ１mmのステンレス板の上に塗布した後、１００℃で１時間乾燥し、更に９００℃で１０時間加熱処理して薄膜を得る。この薄膜を常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを５％含有しており、厚みが０．１８μｍであり、平均粒径が７．２μｍである板状二酸化ケイ素粉体であった。
【００３０】
製造例２〔微粒子酸化チタン１０％含有の板状二酸化ケイ素粉体〕
テトラメトキシシラン〔（ＣＨ3 Ｏ）4 Ｓｉ〕２２８部にエタノール５００部及び０．１規定硝酸２２０部を混合し、これに、更に微粒子酸化チタン（平均粒径３５ｎｍ）を１０部混合し、攪拌しながら４０℃で２０時間反応させた。この溶液に、表面を研磨して平滑にした、厚さ１mmのステンレス板を浸漬し、毎分４０cmの一定速度で引き上げて、製膜した。この製膜を大気中で５分間乾燥し、更に１００℃で２分間乾燥した。この乾燥行程により、ステンレス板に塗布された膜は、完全に剥離し、フレーク状のゲルとなった。このフレーク状ゲルを毎分１００℃の昇温速度で１０００℃まで加熱し、更に１０００℃で２時間加熱処理した。処理後、このフレーク状ゲルを常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを１０％含有しており、厚みが０．６μｍであり、平均粒径が４．５μｍである板状二酸化ケイ素粉体であった。
【００３１】
製造例３〔微粒子酸化チタン２０％含有の板状二酸化ケイ素粉体〕
テトラメトキシシラン〔（ＣＨ3 Ｏ）4 Ｓｉ〕２００部にエタノール４００部及び０．１規定硝酸２００部を混合し、これに、更に微粒子酸化チタン（平均粒径３５ｎｍ）を２０部混合し、攪拌しながら４０℃で２０時間反応させた。この溶液に、表面を研磨して平滑にした、厚さ１mmのステンレス板を浸漬し、毎分４０cmの一定速度で引き上げて、製膜した。この製膜を大気中で５分間乾燥し、更に１００℃で２分間乾燥した。この乾燥行程により、ステンレス板に塗布された膜は、完全に剥離し、フレーク状のゲルとなった。このフレーク状ゲルを毎分１００℃の昇温速度で１０００℃まで加熱し、更に１０００℃で２時間加熱処理した。処理後、このフレーク状ゲルを常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを２０％含有しており、厚みが０．５μｍであり、平均粒径が４．７μｍである板状二酸化ケイ素粉体であった。
【００３２】
製造例４〔微粒子酸化チタン４０％含有の板状二酸化ケイ素粉体〕
テトラブトキシシラン〔（Ｃ4 Ｈ9 Ｏ）4 Ｓｉ〕３２０部にブタノール７００部を混合し、これに、更に微粒子酸化チタン（平均粒径２１ｎｍ）を４０部混合し、十分に攪拌する。この溶液を、表面を研磨して平滑にした、厚さ１mmのステンレス板の上に塗布した後、１００℃で１時間乾燥し、更に９００℃で１０時間加熱処理して薄膜を得る。この薄膜を常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを４０％含有しており、厚みが０．１５μｍであり、平均粒径が４．７μｍである板状二酸化ケイ素粉体であった。
【００３３】
製造例５〔微粒子酸化チタン５０％含有の板状二酸化ケイ素粉体〕
テトラブトキシシラン〔（Ｃ4 Ｈ9 Ｏ）4 Ｓｉ〕２６６部にブタノール５５０部を混合し、これに、更に微粒子酸化チタン（平均粒径３５ｎｍ）を５０部混合し、十分に攪拌する。この溶液を、表面を研磨して平滑にした、厚さ１mmのステンレス板の上に塗布した後、１００℃で１時間乾燥し、更に９００℃で１０時間加熱処理して薄膜を得る。この薄膜を常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを５０％含有しており、厚みが０．２μｍであり、平均粒径が６．６μｍである板状二酸化ケイ素粉体であった。
【００３４】
製造例６〔微粒子酸化チタン３０％及びベンガラ５％含有の板状二酸化ケイ素粉体〕
テトラメトキシシラン〔（ＣＨ3 Ｏ）4 Ｓｉ〕１６５部にエタノール３３０部及び０．１規定硝酸１６０部を混合し、これに、更に微粒子酸化チタン（平均粒径５０ｎｍ）を３０部混合し、次いでベンガラ５部を混合し、攪拌しながら４０℃で２０時間反応させた。この溶液に、表面を研磨して平滑にした、厚さ１mmのステンレス板を浸漬し、毎分２０cmの一定速度で引き上げて、製膜した。この製膜を大気中で５分間乾燥し、更に１００℃で２分間乾燥した。この乾燥行程により、ステンレス板に塗布された膜は、完全に剥離し、フレーク状のゲルとなった。このフレーク状ゲルを毎分１００℃の昇温速度で１０００℃まで加熱し、更に１０００℃で２時間加熱処理した。処理後、このフレーク状ゲルを常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを３０％含有しベンガラを５％含有しており、厚みが０．９μｍ、平均粒径が１０．５μｍである板状二酸化ケイ素粉体であった。
【００３５】
製造例７〔微粒子酸化チタン３０％及びジルコニア５％含有の板状二酸化ケイ素粉体〕
テトラメトキシシラン〔（ＣＨ3 Ｏ）4 Ｓｉ〕１６５部にエタノール３３０部及び０．１規定硝酸１６０部を混合し、これに、更に微粒子酸化チタン（平均粒径５０ｎｍ）を３０部混合し、次いでジルコニア５部を混合し、攪拌しながら４０℃で２０時間反応させた。この溶液に、表面を研磨して平滑にした、厚さ１mmのステンレス板を浸漬し、毎分３０cmの一定速度で引き上げて、製膜した。この製膜を大気中で５分間乾燥し、更に１００℃で２分間乾燥した。この乾燥行程により、ステンレス板に塗布された膜は、完全に剥離し、フレーク状のゲルとなった。このフレーク状ゲルを毎分１００℃の昇温速度で１０００℃まで加熱し、更に１０００℃で２時間加熱処理した。処理後、このフレーク状ゲルを常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを３０％含有しジルコニアを５％含有しており、厚みが０．７μｍ、平均粒径が１１．１μｍである板状二酸化ケイ素粉体であった。
【００３６】
製造例８〔微粒子酸化チタン３０％及びアルミナ５％含有の板状二酸化ケイ素粉体〕
テトラメトキシシラン〔（ＣＨ3 Ｏ）4 Ｓｉ〕１６５部にエタノール３３０部及び０．１規定硝酸１６０部を混合し、これに、更に微粒子酸化チタン（平均粒径５０ｎｍ）を３０部混合し、次いでアルミナ５部を混合し、攪拌しながら４０℃で２０時間反応させた。この溶液に、表面を研磨して平滑にした、厚さ１mmのステンレス板を浸漬し、毎分３０cmの一定速度で引き上げて、製膜した。この製膜を大気中で５分間乾燥し、更に１００℃で２分間乾燥した。この乾燥行程により、ステンレス板に塗布された膜は、完全に剥離し、フレーク状のゲルとなった。このフレーク状ゲルを毎分１００℃の昇温速度で１０００℃まで加熱し、更に１０００℃で２時間加熱処理した。処理後、このフレーク状ゲルを常温まで放冷し、粉砕し、分級して目的の粉体を得た。得られた粉体は、微粒子酸化チタンを３０％含有しアルミナを５％含有しており、厚みが０．８μｍ、平均粒径が１２．８μｍである板状二酸化ケイ素粉体であった。
【００３７】
次に、実施例及び比較例を挙げて本発明の乳化化粧料を更に詳細に説明するが、本発明はこれらの実施例に限定されるものではない。
なお、乳化化粧料の性能評価は、下記〔表１〕に挙げた項目について、専門パネル１５名による５段階評価（平均値）で行った。また、塗布直後の仕上がりの変化については、塗布１５分後の仕上がりを塗布１分後の仕上がりと比較評価を行い、くすみ抑制効果については、塗布後６時間経過後に評価を行った。評価結果は、下記〔表２〕の基準に従って、その記号により示す。
【００３８】
【表１】
【表２】
実施例１〜１９及び比較例１〜７〔二層乳化型ファンデーション〕
下記〔表３〕、〔表４〕及び〔表５〕に示す成分(1) 〜(10)のうち、各評価サンプルに応じて必要なものを混合する。これとは別に粉体成分(11)〜(24)のうち同様に必要なものをヘンシェルミキサーで混合する。予め混合しておいた上記成分(1) 〜(10)に、粉体成分(11)〜(24)の混合物を加え攪拌機で分散混合する。この混合物に、成分(25)〜(27)の混合物を３０分かけてゆっくりと攪拌しながら添加し、更に１０分間ホモミキサーで攪拌して乳化する。この乳化物を脱泡してボトルに充填し、二層乳化型ファンデーションを調製した。得られた二層乳化型ファンデーションの性能評価をそれぞれ行い、それらの結果を下記〔表６〕、〔表７〕及び〔表８〕に示す。
【００４１】
【表３】
【表４】
【表５】
【表６】
【表７】
【表８】
上記〔表６〕、〔表７〕及び〔表８〕の結果から次のことが明らかである。
特定の揮発性油剤及び微粒子酸化チタン含有板状二酸化ケイ素粉体を含有してなる本発明の乳化化粧料〔二層乳化型ファンデーション：実施例１〜１９〕は、塗布直後の仕上がりの色の変化が少なく、高いくすみ抑制効果があり、さっぱり感に優れ、べたつきの無いものであった。一方、比較例１〜７は、塗布直後の仕上がりの色の変化が起こり、くすみ抑制効果が低く、さっぱり感に劣り、べたつきやすいという点で満足のいくものではなかった。
【００４８】
実施例２０〔乳液状ファンデーション〕
下記成分(1) 〜(6) を混合する。これとは別に下記成分(7) 〜(12)をヘンシェルミキサーで混合し、これを予め混合しておいた成分(1) 〜(6) の混合物に加え攪拌機で分散混合する。これに、下記成分(13)〜(16)の混合物を３０分かけてゆっくりと攪拌しながら添加し、更に１０分間ホモミキサーで攪拌して乳化する。得られた乳化物を脱泡してボトルに充填し、乳液状ファンデーションを調製した。
本発明に係る特定の揮発性油剤及び微粒子酸化チタン含有板状二酸化ケイ素粉体を含有してなる上記乳液状ファンデーションは、塗布直後の仕上がりの色の変化が少なく、高いくすみ抑制効果があり、さっぱり感に優れ、べたつきの無い乳液状ファンデーションであった。
【００４９】
実施例２１〔クリーム状ファンデーション〕
下記成分 (1)〜(8) を８０℃にて加熱混合する。これとは別に成分 (9)〜(12)をヘンシェルミキサーで混合し、これを予め混合しておいた成分 (1)〜(8) の混合物に加え攪拌機で分散混合する。これに、８０℃に加熱した下記成分(13)〜(15)の混合物を３０分かけてゆっくりと攪拌しながら添加し、更に１０分間ホモミキサーで攪拌して乳化する。得られた乳化物をゆっくりと攪拌しながら常温まで冷却し、脱泡してボトルに充填し、クリーム状ファンデーションを調製した。
本発明に係る特定の揮発性油剤及び微粒子酸化チタン含有板状二酸化ケイ素粉体を含有してなる上記クリーム状ファンデーションは、塗布直後の仕上がりの色の変化が少なく、高いくすみ抑制効果があり、さっぱり感に優れ、べたつきの無いクリーム状ファンデーヨンであった。
【００５１】
実施例２２〔サンスクリーン乳液〕
下記成分 (11) 〜(15)を８０℃にて加熱混合する。この混合物に、別に下記成分 (1)〜(10)を予め８０℃にて加熱混合しておいたものを３０分かけてゆっくりと攪拌しながら添加し、更に１０分間ホモミキサーで攪拌して乳化する。得られた乳化物をゆっくりと攪拌しながら常温まで冷却し、脱泡してボトルに充填し、サンスクリーン乳液を調製した。
本発明に係る特定の揮発性油剤及び微粒子酸化チタン含有板状二酸化ケイ素粉体を含有してなる上記サンスクリーン乳液は、塗布直後の仕上がりが白くならず、さっぱり感に優れ、べたつきの無いサンスクリーン乳液であった。また、市販のパウダーファンデーションを重ねて塗布して用いた場合、このサンスクリーン乳液には高いくすみ抑制効果があった。
【００５３】
実施例２３〔クリーム状アイシャドー〕
下記成分 (1)〜(7) を８０℃にて加熱混合する。これとは別に下記成分 (8)〜(13)をヘンシェルミキサーで混合し、これを予め混合しておいた成分 (1)〜(7) の混合物に加え攪拌機で分散混合する。これに、８０℃に加熱した下記成分(14)〜(16)の混合物を３０分かけてゆっくりと攪拌しながら添加し、更に１０分間ホモミキサーで攪拌して乳化する。得られた乳化物をゆっくりと攪拌しながら常温まで冷却し、脱泡してボトルに充填し、クリーム状アイシャドーを調製した。
本発明に係る特定の揮発性油剤及び微粒子酸化チタン含有板状二酸化ケイ素粉体を含有してなる上記クリーム状アイシャドーは、塗布直後の仕上がりの色の変化が少なく、高いくすみ抑制効果があり、さっぱり感に優れ、べたつきの無いクリーム状アイシャドーであった。
【００５５】
【発明の効果】
本発明の乳化化粧料は、揮発性油剤及び微粒子酸化チタン含有板状二酸化ケイ素粉体を含有することにより、塗布直後の仕上がりの色の変化が少なく、高いくすみ抑制効果があり、さっぱり感に優れ、べたつきの無いものである。[0001]
[Industrial application fields]
The present invention provides an emulsified cosmetic material that has a good feeling of use, does not become sticky even after the application time has passed, has a long-lasting adhesion, and prevents dullness that occurs after the color change and time has passed immediately after application. The present invention relates to an emulsified cosmetic having an effect of maintaining a finished color immediately after applying cosmetics for a long time. More specifically, by blending one or more volatile oils of low-boiling hydrocarbons or low-boiling silicone oils with plate-like silicon powder containing fine titanium oxide, color change and dullness prevention immediately after coating are prevented. It relates to emulsified cosmetics that have the effect of enhancing the effect and maintaining the finished color immediately after application of cosmetics for a long time, and also have a refreshing feeling and good adhesion to the skin, and have no stickiness even after application. .
[0002]
[Prior art and problems to be solved by the invention]
In conventional emulsified cosmetics, an emulsion obtained by emulsifying an oil phase and a water phase composed of nonvolatile oils such as nonvolatile hydrocarbons, fats and oils, higher alcohols, higher fatty acids, esters, and the like using a surfactant. Has been applied to cosmetics. In general, emulsified cosmetics have a refreshing feeling due to the evaporation of water in the emulsified cosmetics when applied, giving a refreshing feeling of use, and protecting the skin with residual oils and giving a moist feeling of use. Therefore, it is said to be one of the most excellent cosmetic forms.
[0003]
However, since the non-volatile oil agent remains on the hair when applied to the skin, hair, etc., it has the disadvantage that the stickiness is worrisome and the unpleasant feel that remains forever remains. . Therefore, in recent years, emulsified cosmetics in which an unpleasant feel due to residual oils is reduced by using volatile oils such as low-boiling hydrocarbons or low-boiling silicone oils as part of the oil phase in the emulsified cosmetics. Proposed. As a water-in-oil emulsion containing a volatile oil such as a low-boiling hydrocarbon or a low-boiling silicone oil, for example, JP-A-61-266331 is known. However, when a powder is blended as a colorant in an emulsified cosmetic containing a volatile oil such as a low-boiling hydrocarbon or low-boiling silicone oil as a makeup cosmetic, the volatile oil evaporates after application. As a result, the ratio of the powder and the oil remaining on the skin and hair changes, and the ratio of the powder increases. Therefore, even if the feeling of use and finish are both good immediately after application, the powder will change from a wet state to a dry state in a relatively short time after application, The scattering of light on the surface of the powder increases and the finished color becomes whitish. Furthermore, if sebum is secreted over time, the powder is now wetted by the sebum, and the scattering of light on the surface of the powder is reduced, resulting in a darker finished color, which is not preferred as dullness. It had the disadvantage that the phenomenon occurred.
[0004]
In addition, for the purpose of preventing dullness in makeup cosmetics, it is known to add plate-like boron nitride or synthetic mica as a powder with little color change of the powder itself when wet or dry. (Japanese Unexamined Patent Publication Nos. 61-100508 and 63-185810). However, even if these powders are used in emulsified cosmetics, color change does not occur completely, and color change of other colorants blended at the same time cannot be prevented. No emulsifying cosmetic was not satisfactory.
[0005]
On the other hand, as a plate-like silicon dioxide powder containing fine particle titanium oxide, blending into cosmetics has been proposed in Japanese Patent Laid-Open No. 1-143821 and Japanese Patent Laid-Open No. 6-116119. Is also related to powder solid cosmetics and lacks a refreshing feeling because it does not give a refreshing feeling due to evaporation of water.
[0006]
Accordingly, an object of the present invention is to provide an emulsified cosmetic that has little change in the finished color immediately after application, has a high dullness suppressing effect, is excellent in refreshing feeling, and has no stickiness.
[0007]
[Means for Solving the Problems]
As a result of intensive studies, the inventors of the present invention can achieve the above object by an emulsified cosmetic containing (A) a specific volatile oil agent and (B) a plate-like silicon dioxide powder containing fine titanium oxide. I found out.
[0008]
The present invention has been made based on the above findings, and contains the following components (A) and (B) The content of the following component (A) is 0.5 to 60% by weight in the whole emulsified cosmetic, and the content of the following (B) component is 0.1 to 50% by weight in the whole emulsified cosmetic. The emulsified cosmetic is provided.
(A) Boiling point under atmospheric pressure is 240 ° C. or less And having 6 to 15 carbon atoms, straight, branched or cyclic Low boiling point hydrocarbons and viscosity of 5 c.s. or less at 25 ° C A linear, branched or cyclic boiling point of 240 ° C. or less in the atmosphere One or more volatile oils selected from the group consisting of low boiling point silicone oils
(B) Plate-like silicon dioxide powder containing 5 to 50% by weight of fine particle titanium oxide and having an average particle size of 4.5 to 12.8 μm and a thickness of 0.15 to 0.9 μm
[0009]
Hereinafter, the emulsified cosmetic of the present invention will be described in detail.
[0010]
The component (A) used in the present invention is one or more volatile oils selected from the group consisting of low-boiling hydrocarbons and low-boiling silicone oils.
[0011]
As said low boiling point hydrocarbon, C6-C1 Of 5 Linear, branched or cyclic hydrocarbons Used. 8-15 carbon atoms preferable. Among the low-boiling hydrocarbons, an isoparaffin having 10 to 13 carbon atoms is particularly preferable, and the isoparaffin is superior to other volatile oils in terms of ease of emulsification and stability after emulsification. The low boiling point hydrocarbons are Pressure The boiling point below is 240 ° C. or lower. Commercially available products may be used as the low-boiling hydrocarbons, and specific examples include Isobar C (ESSO), Shell Sol 71 (Shell), and the like.
[0012]
Examples of the low boiling point silicone oil include linear, branched or cyclic silicone oils having a boiling point of 240 ° C. or less under atmospheric pressure. Used. Examples thereof include dimethylpolysiloxane and cyclic cyclodimethylpolysiloxane. The viscosity of the low-boiling silicone oil is 25 c or less and 5 c.s. or less. In addition, a commercial item can also be used as said low boiling point silicone oil, As a specific example, SH244, SH245 (Toray Dow Corning), KF96L-2cs, KF96L-1cs (Shin-Etsu silicone) etc. are mentioned.
[0013]
In the present invention, other oil agents may be used in combination with the volatile oil agent (component (A)) if necessary. The other oils may be those used in ordinary emulsified cosmetics, for example, hydrocarbons (other than the volatile oil [component (A)]), fats and oils, waxes, higher alcohols. , Higher fatty acids, esters, and the like. These may be used alone or in combination of two or more depending on the application.
[0014]
Content of the said volatile oil agent ((A) component) is in the whole emulsified cosmetics of this invention. , 0 . 5-60% (% is based on weight, the same applies hereinafter) And good 1 to 55% Than Preferably it is 2 to 50%. When the content is less than 0.5%, it is impossible to satisfy a refreshing feeling of use and no stickiness. On the other hand, when the content exceeds 60%, the oil agent becomes too much and a refreshing feeling due to evaporation of water. Decrease The In addition, the content of the volatile component in the present invention [volatile among the above component (A) and the other oil agent] is preferably in the whole oil agent including the component (A) and the other oil agent. It is 5% or more, more preferably 10% or more.
[0015]
The form of the particulate silicon oxide-containing plate-like silicon dioxide powder that is the component (B) used in the present invention is the form of a composite in which the particulate titanium oxide is dispersed in the plate-like silicon dioxide powder. A multicomponent system in which plate-like silicon dioxide powder is uniformly mixed may be used.
By controlling the particle size of the fine particle titanium oxide, light scattering on the surface of the fine particle titanium oxide can be used to obtain a higher dullness suppressing effect. Therefore, the plate-like dioxide containing the fine particle titanium oxide in the form of the above composite is obtained. It is preferable to use silicon powder.
[0016]
The average particle diameter of the fine particle titanium oxide is preferably 10 to 1000 nm, more preferably 10 to 300 nm. When the average particle size is less than 10 nm, the transparency of the fine particulate titanium oxide becomes too high, and the effect of increasing the whiteness when wetted with sebum is insufficient. It tends to be difficult to obtain powder in the form of a composite that is uniformly dispersed in the body.
[0017]
The content of fine particle titanium oxide in the plate-like silicon dioxide powder [component (B)] , 5 to 50%. The content is 5 If it is less than%, dullness suppressing ability is not sufficient, 50 If it exceeds 50%, the volatile oil will evaporate immediately after application and the powder will become slightly dry, and the whiteness will be too high, and the dullness suppressing ability will also be reduced.
[0018]
In addition, in the plate-like silicon dioxide powder containing the fine particle titanium oxide [component (B)], various properties may be improved by adding components other than the fine particle titanium oxide and the plate-like silicon dioxide. From the viewpoint of dullness suppression ability and stability of the plate-like silicon dioxide powder containing fine particle titanium oxide, the total amount of fine particle titanium oxide and plate-like silicon dioxide must be 80% or more. Examples of other components (less than 20%) that can be added to the fine titanium oxide-containing plate-like silicon dioxide powder include iron oxide, alumina, and zirconia.
[0019]
The average particle diameter of the plate-like silicon dioxide powder [component (B)] is: 4.5-12.8 μm.
[0020]
The thickness of the plate-like silicon dioxide powder [component (B)] is as follows: 0.15-0.9 μm.
[0021]
The content of the plate-like silicon dioxide powder [component (B)] is in the whole emulsified cosmetic of the present invention. , 0 . 1-50% And good Preferably 0.3-40%, Than Preferably it is 0.5 to 30%. When the content is less than 0.1%, the dullness suppressing effect is not exhibited. On the other hand, when the content exceeds 50%, the powder component becomes too much and the cosmetic coating film becomes powdery. Ru .
[0022]
In the present invention, the content ratio of the component (A) to the component (B) is preferably (A) / (B) in a weight ratio of 0.01 / 1 to 80/1, more preferably 0.8. 05/1 to 40/1. When the content ratio is less than 0.01 / 1, the ratio of the plate-like silicon dioxide powder containing fine particle titanium oxide becomes too large and powdery, while when it exceeds 80/1, Since the ratio of the plate-like silicon dioxide powder containing fine particle titanium oxide is too small, it is not preferable because it is impossible to prevent the finished color change.
[0023]
The plate-like silicon dioxide powder containing fine titanium oxide, which is the component (B), may be appropriately hydrophobized according to the purpose of the emulsified cosmetic used as a blending control.
[0024]
Examples of the hydrophobizing treatment include methylhydrogenpolysiloxane, high-viscosity silicone oil, treatment with a silicone compound such as a silicone resin, treatment with a surfactant such as an anionic surfactant and a cationic surfactant, nylon, polymethyl methacrylate, Examples thereof include treatment with a polymer compound such as polyethylene, Teflon and polyamino acid, treatment with a perfluoro group-containing compound, lecithin, collagen, metal soap, lipophilic wax, polyhydric alcohol partial ester or complete ester. However, any method can be used as long as it is generally applicable to powder hydrophobization treatment, and the method is not limited to these methods.
[0025]
In the emulsified cosmetic of the present invention, in addition to the volatile oil agent (component (A)) and the fine silicon dioxide-containing plate-like silicon dioxide powder (component (B)), other commonly used cosmetics The components can be appropriately blended as necessary.
Examples of the other components include talc, kaolin, sericite, muscovite, phlogopite, saucite, biotite, lithia mica, synthetic fluorophlogopite, vermiculite, magnesium carbonate, calcium carbonate, siliceous earth, silicic acid. Magnesium, calcium silicate, aluminum silicate, barium silicate, barium sulfate, strontium silicate, metal tungstate, silica, hydroxyapatite, zeolite, boron nitride, ceramic powder and other inorganic powders, nylon powder, polyethylene powder, polystyrene Powder, benzoguanamine powder, polytetrafluoroethylene powder, distyrenebenzene polymer powder, epoxy powder, acrylic powder, organic powder such as microcrystalline cellulose, inorganic white pigment such as titanium oxide and zinc oxide, oxidation (Bengara), inorganic red pigments such as iron titanate, inorganic brown pigments such as γ iron oxide, inorganic yellow pigments such as yellow iron oxide and ocher, inorganic black pigments such as black iron oxide and carbon black, mango Inorganic purple pigments such as violet and cobalt violet, inorganic green pigments such as chromium oxide, chromium hydroxide and cobalt titanate, inorganic blue pigments such as ultramarine and bitumen, titanium oxide coated mica, titanium oxide coated bismuth oxychloride, Pearl pigments such as bismuth oxychloride, titanium oxide coated talc, fish scale foil, colored titanium oxide coated mica, metal powder pigments such as aluminum powder, copper powder, red 201, red 202, red 204, red 205, red 220, red 226, red 228, red 405, orange 203, orange 204, yellow 205, yellow 401 No. and Blue No. 404 organic pigments, Red No. 3, Red No. 104, Red No. 106, Red No. 227, Red No. 230, Red No. 401, Red No. 505, Orange No. 205, Yellow No. 4, Yellow No. 5, Organic pigments such as yellow 202, yellow 203, green 3 and blue 1 zirconium, barium or aluminum lake, natural pigments such as chlorophyll, β-carotene, squalane, non-volatile liquid paraffin, petrolatum, microcrystalline wax , Ozokerite, ceresin, myristic acid, palmitic acid, stearic acid, oleic acid, isostearic acid, cetyl alcohol, hexadecyl alcohol, oleyl alcohol, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, 2-octyl myristate Dodecyl, di-2-ethylhexanoic acid Opentyl glycol, glycerol tri-2-ethylhexanoate, -2-octyldodecyl oleate, isopropyl myristate, glycerol triisostearate, triglyceride fatty acid glycerol, glycerol tri-2-ethylhexanoate, -2-octyl oleate Various non-volatile hydrocarbons such as dodecyl, isopropyl myristate, glycerol triisostearate, triglyceride fatty acid glycerol, olive oil, avocado oil, beeswax, myristyl myristate, mink oil, lanolin, non-volatile silicone oil, perfluoropolyether Oily components such as higher fatty acids, fats and oils, esters, higher alcohols, waxes, resins such as alkyd resins and urea resins, plasticizers such as camphor and tributyl citrate, UV absorbers, antioxidants Examples thereof include a stopper, an antiseptic, a surfactant, a moisturizer, a fragrance, and a thickener.
[0026]
The emulsified cosmetic of the present invention is used in various forms by a conventional method, and the form is not particularly limited, but emulsified foundations, creamy foundations, emulsified mascaras, emulsified eyeshadows, creamy eyeshadows, etc. Used as makeup cosmetics, pre-makeup cosmetics, sunscreen emulsions and the like.
[0027]
【Example】
Hereinafter, the emulsified cosmetic of the present invention will be described in more detail with reference to Examples and Comparative Examples. However, the present invention is not limited to these examples.
[0028]
First, although the manufacture example (manufacture examples 1-8) of the plate-like silicon dioxide powder [(B) component] containing fine particle titanium oxide used for the emulsified cosmetics (Examples 1-23) of this invention is shown, the above-mentioned The method for producing the plate-like silicon dioxide powder is not limited to these. In addition, as the plate-like silicon dioxide powder containing fine particle titanium oxide as the component (B) according to the present invention, TSG flake 30 manufactured by Nippon Sheet Glass Co., Ltd. [fine particle titanium oxide (average particle size 44 nm) containing 30% (Plate-like silicon dioxide powder, average thickness = 0.5 μm, average particle size = 10 μm) is commercially available, and the commercially available product may be used, and can be produced by any conventional method such as thermal decomposition. What was manufactured by this may be used.
[0029]
Production Example 1 [Plate-like silicon dioxide powder containing 5% fine particle titanium oxide]
Tetrabutoxysilane [(C Four H 9 O) Four Si] 510 parts by weight (hereinafter abbreviated as “parts”) is mixed with 1200 parts of butanol, and further 5 parts of finely divided titanium oxide (average particle size: 35 nm) is further mixed, followed by thorough stirring. This solution was applied onto a 1 mm thick stainless steel plate that had been smoothed by polishing the surface, dried at 100 ° C. for 1 hour, and further heat-treated at 900 ° C. for 10 hours to obtain a thin film. The thin film was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 5% of fine particle titanium oxide, having a thickness of 0.18 μm and an average particle diameter of 7.2 μm.
[0030]
Production Example 2 [Plate-like silicon dioxide powder containing 10% fine particle titanium oxide]
Tetramethoxysilane [(CH Three O) Four Si] 228 parts were mixed with 500 parts of ethanol and 220 parts of 0.1 N nitric acid, and further 10 parts of fine particle titanium oxide (average particle size 35 nm) was mixed, and reacted at 40 ° C. for 20 hours with stirring. . A stainless steel plate having a thickness of 1 mm, which had been polished and smoothed, was immersed in this solution, and pulled up at a constant speed of 40 cm per minute to form a film. This film was dried in air for 5 minutes and further dried at 100 ° C. for 2 minutes. By this drying process, the film applied to the stainless steel plate was completely peeled off to form a flaky gel. This flaky gel was heated to 1000 ° C. at a temperature rising rate of 100 ° C. per minute, and further heat-treated at 1000 ° C. for 2 hours. After the treatment, the flaky gel was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 10% of fine particle titanium oxide, a thickness of 0.6 μm, and an average particle size of 4.5 μm.
[0031]
Production Example 3 [Plate-like silicon dioxide powder containing 20% fine particle titanium oxide]
Tetramethoxysilane [(CH Three O) Four Si] was mixed with 200 parts of ethanol and 200 parts of 0.1N nitric acid, and further 20 parts of fine particle titanium oxide (average particle size: 35 nm) was mixed therewith and reacted at 40 ° C. for 20 hours with stirring. . A stainless steel plate having a thickness of 1 mm, which had been polished and smoothed, was immersed in this solution, and pulled up at a constant speed of 40 cm per minute to form a film. This film was dried in air for 5 minutes and further dried at 100 ° C. for 2 minutes. By this drying process, the film applied to the stainless steel plate was completely peeled off to form a flaky gel. This flaky gel was heated to 1000 ° C. at a temperature rising rate of 100 ° C. per minute, and further heat-treated at 1000 ° C. for 2 hours. After the treatment, the flaky gel was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 20% fine particle titanium oxide, having a thickness of 0.5 μm and an average particle size of 4.7 μm.
[0032]
Production Example 4 [Plate-like silicon dioxide powder containing fine titanium oxide 40%]
Tetrabutoxysilane [(C Four H 9 O) Four Si] is mixed with 320 parts of butanol, and further 40 parts of fine particle titanium oxide (average particle diameter of 21 nm) is further mixed and stirred sufficiently. This solution was applied onto a 1 mm thick stainless steel plate that had been smoothed by polishing the surface, dried at 100 ° C. for 1 hour, and further heat-treated at 900 ° C. for 10 hours to obtain a thin film. The thin film was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 40% of fine titanium oxide, a thickness of 0.15 μm, and an average particle size of 4.7 μm.
[0033]
Production Example 5 [Plate-like silicon dioxide powder containing fine titanium oxide 50%]
Tetrabutoxysilane [(C Four H 9 O) Four Si] 266 parts are mixed with 550 parts butanol, and 50 parts fine particle titanium oxide (average particle size 35 nm) is further mixed therewith and sufficiently stirred. This solution was applied onto a 1 mm thick stainless steel plate that had been smoothed by polishing the surface, dried at 100 ° C. for 1 hour, and further heat-treated at 900 ° C. for 10 hours to obtain a thin film. The thin film was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 50% fine particle titanium oxide, having a thickness of 0.2 μm and an average particle size of 6.6 μm.
[0034]
Production Example 6 [Plate-like silicon dioxide powder containing 30% fine particle titanium oxide and 5% bengara]
Tetramethoxysilane [(CH Three O) Four Si] In 165 parts, 330 parts of ethanol and 160 parts of 0.1N nitric acid were mixed, 30 parts of fine particle titanium oxide (average particle size 50 nm) was further mixed, and then 5 parts of Bengala were mixed and stirred. The reaction was carried out at 40 ° C. for 20 hours. A stainless steel plate having a thickness of 1 mm, which had been smoothed by polishing the surface, was immersed in this solution and pulled up at a constant rate of 20 cm per minute to form a film. This film was dried in air for 5 minutes and further dried at 100 ° C. for 2 minutes. By this drying process, the film applied to the stainless steel plate was completely peeled off to form a flaky gel. This flaky gel was heated to 1000 ° C. at a temperature rising rate of 100 ° C. per minute, and further heat-treated at 1000 ° C. for 2 hours. After the treatment, the flaky gel was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 30% fine particle titanium oxide and 5% bengara, having a thickness of 0.9 μm and an average particle diameter of 10.5 μm.
[0035]
Production Example 7 [Plate-like silicon dioxide powder containing 30% fine particle titanium oxide and 5% zirconia]
Tetramethoxysilane [(CH Three O) Four Si] 165 parts were mixed with 330 parts ethanol and 160 parts 0.1N nitric acid, to which 30 parts fine particle titanium oxide (average particle size 50 nm) was further mixed, and then 5 parts zirconia was mixed and stirred. The reaction was carried out at 40 ° C. for 20 hours. A stainless steel plate having a thickness of 1 mm, which had been polished and smoothed, was immersed in this solution, and pulled up at a constant speed of 30 cm per minute to form a film. This film was dried in air for 5 minutes and further dried at 100 ° C. for 2 minutes. By this drying process, the film applied to the stainless steel plate was completely peeled off to form a flaky gel. This flaky gel was heated to 1000 ° C. at a temperature rising rate of 100 ° C. per minute, and further heat-treated at 1000 ° C. for 2 hours. After the treatment, the flaky gel was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 30% fine particle titanium oxide and 5% zirconia, having a thickness of 0.7 μm and an average particle diameter of 11.1 μm.
[0036]
Production Example 8 [Plate-like silicon dioxide powder containing 30% fine particle titanium oxide and 5% alumina]
Tetramethoxysilane [(CH Three O) Four Si] In 165 parts, 330 parts of ethanol and 160 parts of 0.1N nitric acid were mixed, and further 30 parts of fine particle titanium oxide (average particle size 50 nm) were mixed, and then 5 parts of alumina were mixed and stirred. The reaction was carried out at 40 ° C. for 20 hours. A stainless steel plate having a thickness of 1 mm, which had been polished and smoothed, was immersed in this solution, and pulled up at a constant speed of 30 cm per minute to form a film. This film was dried in air for 5 minutes and further dried at 100 ° C. for 2 minutes. By this drying process, the film applied to the stainless steel plate was completely peeled off to form a flaky gel. This flaky gel was heated to 1000 ° C. at a temperature rising rate of 100 ° C. per minute, and further heat-treated at 1000 ° C. for 2 hours. After the treatment, the flaky gel was allowed to cool to room temperature, pulverized, and classified to obtain the desired powder. The obtained powder was a plate-like silicon dioxide powder containing 30% fine particle titanium oxide and 5% alumina, having a thickness of 0.8 μm and an average particle diameter of 12.8 μm.
[0037]
Next, the emulsified cosmetic of the present invention will be described in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples.
In addition, the performance evaluation of the emulsified cosmetics was performed on the items listed in [Table 1] below by a five-step evaluation (average value) by 15 specialist panels. In addition, regarding the change in the finish immediately after application, the finish after 15 minutes of application was compared with the finish after 1 minute of application, and the dull suppression effect was evaluated after 6 hours from application. The evaluation results are indicated by the symbols according to the criteria shown in [Table 2] below.
[0038]
[Table 1]
[Table 2]
Examples 1 to 19 and Comparative Examples 1 to 7 [Double-layer emulsion foundation]
Of the components (1) to (10) shown in [Table 3], [Table 4] and [Table 5] below, those necessary for each evaluation sample are mixed. Apart from this, the necessary ones of the powder components (11) to (24) are mixed with a Henschel mixer. The mixture of the powder components (11) to (24) is added to the components (1) to (10) previously mixed, and dispersed and mixed with a stirrer. To this mixture, the mixture of components (25) to (27) is added over 30 minutes with slow stirring, and the mixture is further stirred for 10 minutes with a homomixer to emulsify. The emulsion was degassed and filled into a bottle to prepare a two-layer emulsion foundation. The performance evaluation of the obtained two-layer emulsion foundation was performed, and the results are shown in [Table 6], [Table 7] and [Table 8] below.
[0041]
[Table 3]
[Table 4]
[Table 5]
[Table 6]
[Table 7]
[Table 8]
From the results of [Table 6], [Table 7] and [Table 8], the following is clear.
The emulsified cosmetic of the present invention (double-layer emulsified foundation: Examples 1 to 19) containing a specific volatile oil and fine titanium oxide-containing plate-like silicon dioxide powder changes the color of the finished product immediately after application. There were few, there was a high dullness suppression effect, it was excellent in the refreshing feeling, and it was a sticky thing. On the other hand, Comparative Examples 1 to 7 were unsatisfactory in that the finished color change immediately after application occurred, the dullness suppressing effect was low, the refreshing feeling was inferior, and the stickiness was easy.
[0048]
Example 20 [milky foundation]
The following components (1) to (6) are mixed. Separately, the following components (7) to (12) are mixed with a Henschel mixer, added to the mixture of components (1) to (6) previously mixed, and dispersed and mixed with a stirrer. To this, a mixture of the following components (13) to (16) is added with slow stirring over 30 minutes, and further stirred for 10 minutes with a homomixer to emulsify. The obtained emulsion was defoamed and filled into a bottle to prepare an emulsion foundation.
The above-mentioned emulsion foundation comprising the specific volatile oil agent and fine-plate titanium dioxide-containing plate-like silicon dioxide powder according to the present invention has little change in the finished color immediately after coating, has a high dullness suppressing effect, and is refreshing. It was a milky foundation with excellent feeling and no stickiness.
[0049]
Example 21 [Cream Foundation]
The following components (1) to (8) are heated and mixed at 80 ° C. Separately, the components (9) to (12) are mixed with a Henschel mixer, added to the mixture of the components (1) to (8) previously mixed, and dispersed and mixed with a stirrer. To this, a mixture of the following components (13) to (15) heated to 80 ° C. is added with slow stirring over 30 minutes, and further stirred for 10 minutes with a homomixer to emulsify. The obtained emulsion was cooled to room temperature while stirring slowly, defoamed and filled into a bottle to prepare a creamy foundation.
The creamy foundation comprising the specific volatile oil according to the present invention and the particulate titanium oxide-containing plate-like silicon dioxide powder has little change in the finished color immediately after application, has a high dullness suppressing effect, and is refreshing. It was a creamy foundation with excellent feeling and no stickiness.
[0051]
Example 22 [sunscreen emulsion]
The following components (11) to (15) are heated and mixed at 80 ° C. To this mixture, the following components (1) to (10) previously heated and mixed at 80 ° C. were added with slow stirring over 30 minutes, and further stirred for 10 minutes with a homomixer to emulsify. To do. The obtained emulsion was cooled to room temperature while stirring slowly, defoamed and filled into a bottle to prepare a sunscreen emulsion.
The above-mentioned sunscreen emulsion containing the specific volatile oil according to the present invention and the particulate titanium oxide-containing plate-like silicon dioxide powder is not a white finish immediately after application, has a refreshing feeling, and has no stickiness. It was an emulsion. In addition, when a commercially available powder foundation was applied in layers, this sunscreen emulsion had a high dullness suppressing effect.
[0053]
Example 23 [Cream Eye Shadow]
The following components (1) to (7) are heated and mixed at 80 ° C. Separately, the following components (8) to (13) are mixed with a Henschel mixer, added to the mixture of components (1) to (7) previously mixed, and dispersed and mixed with a stirrer. To this, a mixture of the following components (14) to (16) heated to 80 ° C. is added with slow stirring over 30 minutes, and further stirred for 10 minutes with a homomixer to emulsify. The obtained emulsion was cooled to room temperature while stirring slowly, defoamed and filled into a bottle to prepare a creamy eye shadow.
The cream eye shadow comprising the specific volatile oil according to the present invention and the particulate silicon dioxide-containing plate-like silicon dioxide powder has little change in the finished color immediately after application, and has a high dullness suppressing effect, It was a creamy eye shadow with a refreshing feel and no stickiness.
[0055]
【The invention's effect】
The emulsified cosmetic of the present invention contains a volatile oil agent and finely divided titanium oxide-containing plate-like silicon dioxide powder, so that there is little change in the finished color immediately after application, a high dullness suppressing effect, and an excellent refreshing feeling. It ’s not sticky.
Claims (2)
（Ａ）大気圧下での沸点が２４０℃以下で、炭素数６〜１５の直鎖、分岐又は環状の低沸点炭化水素及び粘度が２５℃で５c.s.以下で、大気下での沸点が２４０℃以下の直鎖、分岐又は環状の低沸点シリコーン油からなる群から選ばれた１種又は２種以上の揮発性油剤
（Ｂ）微粒子酸化チタンを５〜５０重量％含有の平均粒径が４．５〜１２．８μｍで厚みが０．１５〜０．９μｍである板状二酸化ケイ素粉体The following (A) and (B) components are contained , the content of the following (A) component is 0.5 to 60% by weight in the whole emulsified cosmetic, and the content of the following (B) component is the whole emulsified cosmetic. 0.1 to 50% by weight der Ru emulsified cosmetic in.
Boiling point at (A) atmospheric pressure at 240 ° C. or less, linear C6-15, 5C.S. below at the 25 ° C. Low-boiling hydrocarbons and a viscosity of branched or cyclic, boiling point at atmospheric Is an average particle size containing 5 to 50% by weight of one or more volatile oils (B) fine particle titanium oxide selected from the group consisting of linear, branched or cyclic low boiling point silicone oils of 240 ° C. or lower Plate-like silicon dioxide powder having a thickness of 4.5 to 12.8 μm and a thickness of 0.15 to 0.9 μm
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18316594A JP3726843B2 (en) | 1994-08-04 | 1994-08-04 | Emulsified cosmetics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18316594A JP3726843B2 (en) | 1994-08-04 | 1994-08-04 | Emulsified cosmetics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0840831A JPH0840831A (en) | 1996-02-13 |
| JP3726843B2 true JP3726843B2 (en) | 2005-12-14 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18316594A Expired - Fee Related JP3726843B2 (en) | 1994-08-04 | 1994-08-04 | Emulsified cosmetics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3726843B2 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0765656B1 (en) * | 1995-09-29 | 2001-07-04 | Shiseido Company Limited | Water-in-oil type emulsion cosmetic composition |
| JP2000505095A (en) * | 1996-08-23 | 2000-04-25 | 花王株式会社 | Aqueous skin cosmetics |
| JP3696873B2 (en) * | 1996-08-23 | 2005-09-21 | 花王株式会社 | Water based skin cosmetics |
| US6174533B1 (en) † | 1997-05-23 | 2001-01-16 | The Procter & Gamble Company | Skin care compositions and method of improving skin appearance |
| EP1512729B1 (en) * | 2002-05-24 | 2007-01-10 | Nippon Sheet Glass Co.,Ltd. | Scaly particles and cosmetic comprising the same, coating composition, resin composition and ink composition |
| KR20130027058A (en) | 2005-03-04 | 2013-03-14 | 코그니스 아이피 매니지먼트 게엠베하 | Emollients and cosmetic compositions based on special branched hydrocarbons |
| RS55276B1 (en) * | 2009-01-09 | 2017-02-28 | Syngenta Participations Ag | Stabilized agrochemical composition |
| US9408800B2 (en) | 2012-02-28 | 2016-08-09 | Kao Corporation | Cosmetic composition |
-
1994
- 1994-08-04 JP JP18316594A patent/JP3726843B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0840831A (en) | 1996-02-13 |
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