JPWO2017018358A1 - 硬化シリコーン粒子、これを配合した化粧料 - Google Patents
硬化シリコーン粒子、これを配合した化粧料 Download PDFInfo
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- JPWO2017018358A1 JPWO2017018358A1 JP2017530846A JP2017530846A JPWO2017018358A1 JP WO2017018358 A1 JPWO2017018358 A1 JP WO2017018358A1 JP 2017530846 A JP2017530846 A JP 2017530846A JP 2017530846 A JP2017530846 A JP 2017530846A JP WO2017018358 A1 JPWO2017018358 A1 JP WO2017018358A1
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- UNZSHUCNBUBSGW-IFNWOZJISA-M sodium;(9z,12z,15z)-octadeca-9,12,15-trienoate Chemical compound [Na+].CC\C=C/C\C=C/C\C=C/CCCCCCCC([O-])=O UNZSHUCNBUBSGW-IFNWOZJISA-M 0.000 description 1
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- 150000003751 zinc Chemical class 0.000 description 1
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- GBFLQPIIIRJQLU-UHFFFAOYSA-L zinc;tetradecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O GBFLQPIIIRJQLU-UHFFFAOYSA-L 0.000 description 1
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- QUEDXNHFTDJVIY-DQCZWYHMSA-N γ-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-DQCZWYHMSA-N 0.000 description 1
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
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Abstract
Description
(A)平均式:
[RaRb 2SiO(Rb 2SiO)n]4Si
(式中、nは0以上の数であり、但し、一分子中、少なくとも1個のnは1以上の数であり、Raは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基もしくは2〜12個の炭素原子を有するアルケニル基であり、但し、一分子中、少なくとも2個のRaは前記アルケニル基であり、Rbは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基、2〜12個の炭素原子を有するアルケニル基、もしくは6〜20個の炭素原子を有するアリール基である。)
で表されるポリオルガノシロキサン
(B)(B−1)平均単位式:
(Rc 3SiO1/2)p(Rc 2SiO2/2)q(RdSiO3/2)r
(式中、Rcは、同じか又は異なる、水素原子、1〜6個の炭素原子を有するアルキル基、もしくは6〜20個の炭素原子を有するアリール基であり、但し、一分子中、少なくとも2個のRcは水素原子であり、Rdは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基もしくは6〜20個の炭素原子を有するアリール基であり、p、q、rは、それぞれ、0より大きい数で、p+q+r=1を満たす数である。)
で表されるポリオルガノシロキサン及び/又は(B−2)平均式:
HRd 2SiO(Rd 2SiO)mSiRd 2H
(式中、mは0より大きい数であり、Rdは前記と同じである。)
で表されるポリオルガノシロキサン
(C)ヒドロシリル化反応用触媒
(A)平均式:
[RaRb 2SiO(Rb 2SiO)n]4Si
(式中、nは0以上の数であり、但し、一分子中、少なくとも1個のnは1以上の数であり、Raは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基もしくは2〜12個の炭素原子を有するアルケニル基であり、但し、一分子中、少なくとも2個のRaは前記アルケニル基であり、Rbは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基、2〜12個の炭素原子を有するアルケニル基、もしくは6〜20個の炭素原子を有するアリール基である。)
で表されるポリオルガノシロキサン
(B)(B−1)平均単位式:
(Rc 3SiO1/2)p(Rc 2SiO2/2)q(RdSiO3/2)r
(式中、Rcは、同じか又は異なる、水素原子、1〜6個の炭素原子を有するアルキル基、もしくは6〜20個の炭素原子を有するアリール基であり、但し、一分子中、少なくとも2個のRcは水素原子であり、Rdは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基もしくは6〜20個の炭素原子を有するアリール基であり、p、q、rは、それぞれ、0より大きい数で、p+q+r=1を満たす数である。)
で表されるポリオルガノシロキサン及び/又は(B−2)平均式:
HRd 2SiO(Rd 2SiO)mSiRd 2H
(式中、mは0より大きい数であり、Rdは前記と同じである。)
で表されるポリオルガノシロキサン
(C)ヒドロシリル化反応用触媒
(Rc 3SiO1/2)p(Rc 2SiO2/2)q(RdSiO3/2)r
で表されるポリオルガノシロキサン及び/又は(B−2)一般式:
HRd 2SiO(Rd 2SiO)mSiRd 2H
で表されるポリオルガノシロキサンである。
ReRd 2SiO(Rd 2SiO)kSiRd 2Re
で表されるポリオルガノシロキサン(D)を含むことができる。
水は、人体に有害な成分を含有せず、清浄であればよく、水道水、精製水、ミネラルウォーター、及び海洋深層水が例示される。本発明の化粧料が水系である場合、水相には本発明の効果を損なわない範囲で任意に水溶性の添加成分を配合することができる。また、化粧料の保存安定性等を改善する目的で、公知のpH調整剤、防腐剤、抗菌剤又は酸化防止剤を適宜配合することもできる。
(X,Y)2−3(Si,Al)4O10(OH)2Z1/3・nH2O
(但し、Xは、Al、Fe(III)、Mn(III)、又は、Cr(III)であり、Yは、Mg、Fe(II)、Ni、Zn、又はLiであり、Zは、K、Na、又はCaである。)
で表されるものが例示される。このような無機系水溶性高分子として、具体的には、ベントナイト、モンモリロナイト、パイデライト、ノントロナイト、サポナイト、ヘクトライト、ケイ酸アルミニウムマグネシウム、及び無水ケイ酸が例示され、これらは天然物及び合成物のいずれであってもよい。
塩類として、無機塩、有機酸塩、アミン塩及びアミノ酸塩が挙げられる。無機塩としては、例えば、塩酸、硫酸、炭酸、硝酸等の無機酸のナトリウム塩、カリウム塩、マグネシウム塩、カルシウム塩、アルミニウム塩、ジルコニウム塩、及び亜鉛塩等;有機酸塩としては、例えば、酢酸、デヒドロ酢酸、クエン酸、りんご酸、コハク酸、アスコルビン酸、及びステアリン酸等の有機酸類の塩;並びにアミン塩及びアミノ酸塩としては、例えば、トリエタノールアミン等のアミン類の塩、及びグルタミン酸等のアミノ酸類の塩等が挙げられる。また、その他、ヒアルロン酸、コンドロイチン硫酸等の塩、アルミニウムジルコニウムグリシン錯体等、及び化粧品処方の中で使用される酸−アルカリの中和塩等も使用することができる。
本発明のシリコーン粉末およびその製造方法を、実施例および比較例により詳細に説明する。ただし、本発明はそれらの実施例のみに限定されるものではない。実施例中の粘度は25℃における値である。また、硬化シリコーン粒子の特性を次のようにして測定した。
硬化シリコーン粒子の原料である硬化性シリコーン組成物を加熱オーブンにて150℃で1時間加熱して、シート状に硬化させた。この硬さをJIS K6301に規定されるJIS A硬度計により測定した。
白金触媒を添加する前のエマルジョンを、レーザー回折式粒度分布測定器(ベックマン・コールター社のLS−230)により測定し、そのメジアン径(累積分布の50%に相当する粒径、50%粒径)を平均粒子径とした。
エタノールを分散媒として、レーザー回折式粒度分布測定器(堀場製作所のLA−750)で硬化シリコーン粒子の粒径を測定し、エタノール中での硬化シリコーン粒子のメジアン径(累積分布の50%に相当する粒径、D50、μm)、90%粒径(累積分布の90%に相当する粒径、D90、μm)や算術分散度(粒径分布の分散度合いを示す、SD、μm2)の値を得た。測定試料は、300mLのカップに硬化シリコーン粒子(1g)とエタノール(100mL)を撹拌装置や超音波振動機を用いて分散した。
以下の式において、Viはビニル基、Meはメチル基を示す。
[化1−1]
平均式:
[ViMe2SiO(Me2SiO)n]4Si
で表されるポリオルガノシロキサン(nの値は平均で約10.0〜11.0の数、ビニル基の含有量は3.15質量%、粘度は35mPa・s)
[化1−2]
平均式:
[ViMe2SiO(Me2SiO)n]4Si
で表されるポリオルガノシロキサン(nの値は平均で約30.0、ビニル基の含有量は1.16質量%、粘度は120mPa・s)
[化1−3]
式:
ViMe2SiO(Me2SiO)165SiMe2Vi
で表されるポリオルガノシロキサン(ビニル基の含有量は0.457質量%、粘度は450mPa・s)
[化1−4]
平均式:
[ViMe2SiO(Me2SiO)n]4Si
で表されるポリオルガノシロキサン(nの値は平均で0.46、粘度は20mPa・s)
[化1−5]
式:
ViMe2SiO(Me2SiO)130(ViMeSiO)2SiMe2Vi
で表されるポリオルガノシロキサン(ビニル基の含有量は1.08質量%、粘度は370mPa・s)
[化2−1]
式:
HMe2SiO(Me2SiO)14SiMe2H
で表されるポリオルガノシロキサン(ケイ素原子結合水素原子の含有量は0.15質量%、粘度は15mPa・s)
[化2−2]
平均単位式:
(Me3SiO1/2)0.10(Me2SiO2/2)0.33(HMeSiO2/2)0.52(MeSiO3/2)0.05
で表されるポリオルガノシロキサン(ケイ素原子結合水素原子の含有量は0.825質量%、粘度は15mPa・s)
[化2−3]
平均式:
Me3SiO(Me2SiO)33.7(HMeSiO)11.5SiMe3
で表されるポリオルガノシロキサン(ケイ素原子結合水素原子の含有量は0.44質量%、粘度は50mPa・s)
[化2−4]
平均式:
Me3SiO(Me2SiO)51.3(HMeSiO)6.3SiMe3
で表されるポリオルガノシロキサン(ケイ素原子結合水素原子含有量は0.146質量%、粘度は57mPa・s)
[化1−1]のポリオルガノシロキサン 51.7質量部、[化2−1]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性をシリコーン組成物に調製した。次に、この組成物をポリオキシエチレンアルキル(C12―14)エーテル0.4質量部と純水50質量部からなる25℃の水溶液中に分散し、さらにコロイドミルにより均一に乳化した後、純水350質量部を加えて希釈してエマルジョンを調製した。次に、塩化白金酸のイソプロピルアルコール溶液(本組成物中、白金金属が質量単位で10ppmとなる量)をポリオキシエチレンアルキル(C12―14)エーテルと純粋で水分散液として、エマルジョンに加えて攪拌した後、このエマルジョンを50℃で3時間静置して、シリコーンゴム粒子の均一な水系サスペンジョンを調製した。次に、この水系サスペンジョンを小型スプレードライヤー(アシザワニロ社製)で乾燥し、硬化シリコーン粒子を得た。
[化1−2]のポリオルガノシロキサン 94.9質量部、[化2−2]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−1]のポリオルガノシロキサン 45.0質量部、[化1−3]のポリオルガノシロキサン 45.0質量部、[化2−2]のポリオルガノシロキサン(前記ポリオルガノシロキサンの合計中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−4]のポリオルガノシロキサン 14.3質量部、[化2−1]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−1]のポリオルガノシロキサン 87.6質量部、[化2−2]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−1]のポリオルガノシロキサン 45.0質量部、[化1−3]のポリオルガノシロキサン 45.0質量部、[化2−2]のポリオルガノシロキサン(前記ポリオルガノシロキサンの合計中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。ポリオキシエチレンアルキル(C12―14)エーテル0.1質量部と純水50質量部からなる25℃の水溶液中に分散し、次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−2]のポリオルガノシロキサン 90.8質量部、[化2−3]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−5]のポリオルガノシロキサン 78.5質量部、[化2−4]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
[化1−3]のポリオルガノシロキサン 97.9質量部、[化2−2]のポリオルガノシロキサン(前記ポリオルガノシロキサン中のビニル基に対する本成分中のケイ素原子結合水素原子の比率が1.0となる量)を室温で均一に混合して付加反応硬化性シリコーン組成物を調製した。次に、この組成物を実施例1と同様にして、硬化シリコーン粒子を得た。
表2に、硬化シリコーン粒子とデカメチルシクロペンタシロキサンの混合物の粘度を示す。
300mLカップに硬化シリコーン粒子(6g)とデカメチルシクロペンタシロキサン(58g)を計量し、ディスパーにて4000rpmで2分間攪拌した。その後、のBM型回転粘度計(東機産業社製)で、ローターNo.2で60rpmの条件で、1分後の値を粘度とした。
実施例3及び比較例1の硬化シリコーン粒子を用いて表―3に示すスキンクリームを調整し、専門評価パネル10名により、肌に塗布後、肌へのなじみ感が得られたかを下記基準にて3段階評価し、さらにその平均点から判定した。比較例5に比べて実施例10が、肌なじみが良いことを確認した。
5点: 非常に肌なじみ感がよかった
3点: 普通
1点: まったく肌なじみ感がなかった
○: 平均点4.0以上
△: 平均点2.0点以上4.0点未満
×: 平均点2.0点未満
実施例3、実施例5及び比較例1の硬化シリコーン粒子を用いて表―4に示すボディーパウダーを調整し、専門評価パネル10名により、肌に塗布する時の塗り伸ばしやすさと塗布後にさらさら感が得られたかを下記基準にて3段階評価し、さらにその平均点から判定した。比較例6に比べて、実施例11と実施例12が、塗り伸ばしやすさ、さらさら感が優れていることを確認した。
5点:塗り伸ばしやすい
3点: 普通
1点: 塗り伸ばしにくい
○: 平均点4.0以上
△: 平均点2.0点以上4.0点未満
×: 平均点2.0点未満
5点:塗布後の肌にさらさら感を感じる
3点: 普通
1点: 塗布後の肌にさらさら感を感じない
○: 平均点4.0以上
△: 平均点2.0点以上4.0点未満
×: 平均点2.0点未満
(成分)
相A
1)ラウリルPEG/PPG−18/18ジメチコン(注1) 4質量部
2)カプリリルメチコン(注2) 14質量部
3)メトキシケイヒ酸エチルヘキシル(注3) 7.5質量部
4)ジエチルアミノヒドロキシベンゾイル安息香酸ヘキシル(注4) 1.5質量部
5)サリチル酸エチルヘキシル 2.5質量部
6)トリメチルシロキシケイ酸、ポリプロピルシルセスキオキサン(注5) 2質量部
7)実施例のシリコーン架橋体 3質量部
8)酢酸トコフェロール 0.5質量部
相B
9)アスコルビルリン酸ナトリウム 0.5質量部
10)グリセリン 8質量部
11)塩化ナトリウム 0.7質量部
12)精製水 39.8質量部
相C
13)酸化チタン 5.6質量部
14)黄色酸化鉄(注6) 0.25質量部
15)赤色酸化鉄(注7) 0.1質量部
16)黒色酸化鉄(注8) 0.05質量部
17)フェニルトリメチコン(注9) 9.2質量部
18)酸化亜鉛(注10) 0.8質量部
注1:東レ・ダウコーニング社製5200 Formulation Aid
注2:東レ・ダウコーニング社製FZ−3196
注3:BASF社製ユビナールMC80N
注4:BASF社製ユビナールA Plus Glanular
注5:東レ・ダウコーニング社製MQ−1640 Flake Resin
注6:三次化成社製SA−IOY−8
注7:三次化成社製SA−IOR−8
注8:三次化成社製SA−IOB−8
注9:東レ・ダウコーニング社製SH556
注10:BASF社製Z−Cote
1.成分1〜8を混合する。
2.成分9〜12を混合する。
3.成分13〜18を混合する。
4.工程1で得られる相Aと工程3で得られる相Cを混合する。
5.工程4で得られる混合物を撹拌しながら工程2で得られる相Bをゆっくり加え乳化す
る。
(成分)
(1)酸化亜鉛(注1) 6質量部
(2)メトキシケイヒ酸エチルヘキシル(注2) 7.5質量部
(3)ジメチコン、ジメチコンクロスポリマー(注3) 24質量部
(4)シクロペンタシロキサン(注4) 60.5質量部
(5)実施例のシリコーン架橋体 2質量部
注1:TAYCA製MZ−303S
注2:BASF社製ユビナールMC80N
注3:東レ・ダウコーニング社製9041 Silicone Elastomer Blend
注4:東レ・ダウコーニング社製SH245
1.成分4と成分5を均一になるまで攪拌する。
2.成分3に上記1を加えて均一になるまで攪拌する。
3.成分1と成分2を混合する。
4.上記2と3を均一になるまで攪拌する。
(成分)
相A
(1)精製水 残余
(2)メタクリル酸メチルクロスポリマー(注1) 5質量部
相B
(3)シクロペンタシロキサン、シクロヘキサシロキサン(注2) 35質量部
(4)実施例のシリコーン架橋体 5質量部
(5)(アクリル酸ヒドロキシエチル/アクリロイルジメチルタウリンNa)コポリマー 、スクワラン、ポリソルベート80 、水、オレイン酸ソルビタン(注3) 0.7質量部
(6)(アクリル酸ヒドロキシエチル/アクリロイルジメチルタウリンNa)コポリマー 、イソヘキサデカン、ポリソルベート60 、水、イソステアリン酸ソルビタン(注4) 0.7質量部
相C
(7)ジメチコン 5質量部
(8)ジパルミトイルヒドロキシプロリン(注5) 0.5質量部
相D
(9)ワイン抽出物(注6) 0.01質量部
(10)香料 0.2質量部
相E
(11)フェノキシエタノール 0.9質量部
注1:SEPPIC S.A. 社製 Micropearl M305
注2:東レ・ダウコーニング社製DC345
注3:SEPPIC S.A. 社製 Simulgel EG
注4:SEPPIC S.A. 社製 Simulgel NS
注5:SEPPIC S.A. 社製 Sepilift DPHP
注6:SEPPIC S.A. 社製 Sepivinol R
1.成分2を成分1に分散させる。
2.成分4を成分3に分散させる。
3.成分5と成分6を上記2に加え、混合する。
4.成分8を成分7に溶解させる。
5.上記1を攪拌しながら、上記3、4およびPhase Dを加え、乳化する。
6.上記1を攪拌しながら、上記3、4およびPhase Dを加え、乳化する。
(成分)
相A
1)シクロペンタシロキサン(注1) 11質量部
2)実施例のシリコーン架橋体 10質量部
3)ラウリルPEG/PPG−18/18ジメチコン(注2) 0.5質量部
4)PEG−12ジメチコン(注3) 4質量部
相B
5)精製水 72.5質量部
相C
6)ポリアクリルアミド、水、(C13,14)イソパラフィン 、ラウレス−7(注4) 2質量部
注1:東レ・ダウコーニング社製SH245
注2:東レ・ダウコーニング社製5200 Formulation Aid
注3:東レ・ダウコーニング社製OFX−5329
注4:SEPPIC S.A. 社製Simulgel 305
1.Phase Aを均一になるまで混合する。
2.Phase Bを攪拌しながら上記1をゆっくり加える。
3.上記2にPhase Cを加えて均一になるまで混合する。
(成分)
相A
1)シクロペンタシロキサン、シクロヘキサシロキサン(注1) 4質量部
2)セチルジメチコン(注2) 2質量部
3)ステアリルジメチコン(注3) 6質量部
4)アルキル(C30−45)メチコン、オレフィン(C30−45)(注4) 3質量部
5)ビーズワックス(注5) 8質量部
6)シクロペンタシロキサン、ポリプロピルシルセスキオキサン(注6) 5質量部
7)防腐剤 0.5質量部
相B
8)シクロペンタシロキサン(注7) 44質量部
9)酸化鉄赤(注8) 1.5質量部
10)酸化鉄黄(注9) 2.5質量部
11)酸化鉄黒(注10) 0.75質量部
12)酸化鉄茶(注11) 5.75質量部
相C
13)シリカ(注12) 1質量部
14)実施例のシリコーン架橋体 6質量部
15)オクテニルコハク酸トウモロコシデンプンAl(注13) 4質量部
16)タルク 2質量部
17)アラントイン(注14) 1質量部
18)酸化チタン(注15) 3質量部
注1:東レ・ダウコーニング社製DC345
注2:東レ・ダウコーニング社製 2502 COSMETIC FLUID
注3:東レ・ダウコーニング社製2503 COSMETIC WAX
注4:東レ・ダウコーニング社製AMS−C30 COSMETIC WAX
注5:Baerlocher France S.A.社製Cerabeil White No 1
注6:東レ・ダウコーニング社製 670 FLUID
注7:東レ・ダウコーニング社製SH245
注8:Sensient Cosmetic Technologies社製Unipure Red LC 381 AS−EM
注9:Sensient Cosmetic Technologies社製Unipure Yellow LC 182 AS−EM
注10:Sensient Cosmetic Technologies社製Unipure Black LC 989 AS−EM
注11:Sensient Cosmetic Technologies社製Unipure Brown LC 881
注12:Sensient Cosmetic Technologies社製LDP 1500
注13:National Starch & Chemical Company社製Dry Flo Plus
注14:Allantoin / ISP
注15:Sensient Cosmetic Technologies社製Matlake OPA−AS
1.Phase Aを80℃に加温し、溶解させる。
2.成分9〜12を均一になるまで混合する。
3.成分8に上記2を分散させる。
4.Phase Cを均一になるまで混合する。
5.上記3と上記4を混合する。
6. 上記1を攪拌しながら上記5を加えて攪拌する(80℃)。
7.容器に移して冷やし固める。
(成分)
相A
1)セチルジグリセリルトリス(トリメチルシロキシ)シリルエチルジメチコン(注1) 2質量部
2)ジメチコン(注2) 10質量部
3)実施例のシリコーン架橋体 2質量部
4)フェニルトリメチコン(注3) 4質量部
相B
5)オクタクロロハイドレックスグリシン(Al/ジルコニウム)、水(注4)45質量部
6)グリセリン 5.5質量部
7)プロパンジオール 12.5質量部
8)精製水 18.5質量部
9)防腐剤 0.5質量部
注1:東レ・ダウコーニング社製ES−5600 SILICONE GLYCEROL EMULSIFIER
注2:東レ・ダウコーニング社製SH200C FLUID 2CS
注3:東レ・ダウコーニング社製556 FLUID
注4:Summit Reheis社製Reach AZO 956G
1.Phase Aを均一になるまで混合する。
2.Phase Bを均一になるまで混合する。
3.上記1を攪拌しながら、ゆっくり上記2を加えて乳化する。
(成分)
1)シクロペンタシロキサン(注1) 45質量部
2)実施例のシリコーン架橋体 2.7質量部
3)カプリリルメチコン(注2) 20質量部
4)アルガンオイル 0.1質量部
5)オリーブオイル 0.1質量部
6)フェニルトリメチコン(注3) 2質量部
7)シクロペンタシロキサン、ジメチコノール(注4) 30質量部
8)香料 0.1質量部
注1:東レ・ダウコーニング社製SH245
注2:東レ・ダウコーニング社製SS−3408
注3:東レ・ダウコーニング社製556 FLUID
注4:東レ・ダウコーニング社製PMX−1501 Fluid
1. 成分2を成分1に分散させる。
2. 上記1に残りの成分3〜8を加えて混合する。
Claims (8)
- 次の(A)乃至(C)成分から少なくともなる硬化性シリコーン組成物を硬化させてなる、平均粒子径が0.1〜500μmである硬化シリコーン粒子。
(A)平均式:
[RaRb 2SiO(Rb 2SiO)n]4Si
(式中、nは0以上の数であり、但し、一分子中、少なくとも1個のnは1以上の数であり、Raは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基もしくは2〜12個の炭素原子を有するアルケニル基であり、但し、一分子中、少なくとも2個のRaは前記アルケニル基であり、Rbは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基、2〜12個の炭素原子を有するアルケニル基、もしくは6〜20の炭素原子を有するアリール基である。)
で表されるポリオルガノシロキサン
(B)(B−1)平均単位式:
(Rc 3SiO1/2)p(Rc 2SiO2/2)q(RdSiO3/2)r
(式中、Rcは、同じか又は異なる、水素原子、1〜6個の炭素原子を有するアルキル基もしくは6〜20個の炭素原子を有するアリール基であり、但し、一分子中、少なくとも2個のRcは水素原子であり、Rdは、同じか又は異なる、1〜6個の炭素原子を有するアルキル基もしくは6〜20個の炭素原子を有するアリール基であり、p、q、rは、それぞれ、0より大きい数で、p+q+r=1を満たす数である。)
で表されるポリオルガノシロキサン及び/又は(B−2)平均式:
HRd 2SiO(Rd 2SiO)mSiRd 2H
(式中、mは0より大きい数であり、Rdは前記と同じである。)
で表されるポリオルガノシロキサン
(C)ヒドロシリル化反応用触媒 - 平均式:
ReRd 2SiO(Rd 2SiO)kSiRd 2Re
(式中、Reは、同じか又は異なる2〜12個の炭素原子を有するアルケニル基であり、Rdは前記と同じ基であり、kは0より大きい数である。)
で表されるポリオルガノシロキサン(D)をさらに含む硬化性シリコーン組成物を硬化させてなる、請求項1記載の硬化シリコーン粒子。 - (A)成分と(B)成分の混合物を微粒子化し、次いで、この微粒子に(C)成分を配合して硬化性シリコーン組成物の微粒子を調製した後、該組成物を硬化反応することを特徴とする、請求項1又は2記載の硬化シリコーン粒子の製造方法。
- (A)成分と(B)成分と(C)成分を混合して硬化シリコーン組成物とし、次いで、その微粒子を調製した後、該組成物を硬化反応することを特徴とする、請求項1又は2記載の硬化シリコーン粒子の製造方法。
- 水性媒体又は油性媒体に請求項1又は2記載の硬化シリコーン粒子を分散した、化粧品原料。
- 請求項1又は2記載の硬化シリコーン粒子を含有する化粧料。
- 皮膚用化粧料である、請求項6に記載の化粧料。
- メークアップ化粧料又はサンスクリーン剤である、請求項7に記載の化粧料。
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