JP2015532659A - 水性シリコーン分散液及びフィルム並びにその調製 - Google Patents
水性シリコーン分散液及びフィルム並びにその調製 Download PDFInfo
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- JP2015532659A JP2015532659A JP2015524703A JP2015524703A JP2015532659A JP 2015532659 A JP2015532659 A JP 2015532659A JP 2015524703 A JP2015524703 A JP 2015524703A JP 2015524703 A JP2015524703 A JP 2015524703A JP 2015532659 A JP2015532659 A JP 2015532659A
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- dispersion
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- alkenyl
- silicone
- aqueous
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- LOIYMIARKYCTBW-UHFFFAOYSA-N trans-urocanic acid Natural products OC(=O)C=CC1=CNC=N1 LOIYMIARKYCTBW-UHFFFAOYSA-N 0.000 description 1
- 229960001727 tretinoin Drugs 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 description 1
- DHWLRNPWPABRBG-UHFFFAOYSA-N tridecyl 2,2-dimethylpropanoate Chemical compound CCCCCCCCCCCCCOC(=O)C(C)(C)C DHWLRNPWPABRBG-UHFFFAOYSA-N 0.000 description 1
- MZHULIWXRDLGRR-UHFFFAOYSA-N tridecyl 3-(3-oxo-3-tridecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCC MZHULIWXRDLGRR-UHFFFAOYSA-N 0.000 description 1
- HTJNEBVCZXHBNJ-XCTPRCOBSA-H trimagnesium;(2r)-2-[(1s)-1,2-dihydroxyethyl]-3,4-dihydroxy-2h-furan-5-one;diphosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.OC[C@H](O)[C@H]1OC(=O)C(O)=C1O HTJNEBVCZXHBNJ-XCTPRCOBSA-H 0.000 description 1
- 229940117985 trimethyl pentaphenyl trisiloxane Drugs 0.000 description 1
- AQZSPJRLCJSOED-UHFFFAOYSA-M trimethyl(octyl)azanium;chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(C)C AQZSPJRLCJSOED-UHFFFAOYSA-M 0.000 description 1
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 1
- 229940030300 trolamine salicylate Drugs 0.000 description 1
- 239000012588 trypsin Substances 0.000 description 1
- 229960001322 trypsin Drugs 0.000 description 1
- 229940035936 ubiquinone Drugs 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 229960005356 urokinase Drugs 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 1
- 235000012141 vanillin Nutrition 0.000 description 1
- 229960003048 vinblastine Drugs 0.000 description 1
- JXLYSJRDGCGARV-XQKSVPLYSA-N vincaleukoblastine Chemical compound C([C@@H](C[C@]1(C(=O)OC)C=2C(=CC3=C([C@]45[C@H]([C@@]([C@H](OC(C)=O)[C@]6(CC)C=CCN([C@H]56)CC4)(O)C(=O)OC)N3C)C=2)OC)C[C@@](C2)(O)CC)N2CCC2=C1NC1=CC=CC=C21 JXLYSJRDGCGARV-XQKSVPLYSA-N 0.000 description 1
- OGWKCGZFUXNPDA-XQKSVPLYSA-N vincristine Chemical compound C([N@]1C[C@@H](C[C@]2(C(=O)OC)C=3C(=CC4=C([C@]56[C@H]([C@@]([C@H](OC(C)=O)[C@]7(CC)C=CCN([C@H]67)CC5)(O)C(=O)OC)N4C=O)C=3)OC)C[C@@](C1)(O)CC)CC1=C2NC2=CC=CC=C12 OGWKCGZFUXNPDA-XQKSVPLYSA-N 0.000 description 1
- 229960004528 vincristine Drugs 0.000 description 1
- OGWKCGZFUXNPDA-UHFFFAOYSA-N vincristine Natural products C1C(CC)(O)CC(CC2(C(=O)OC)C=3C(=CC4=C(C56C(C(C(OC(C)=O)C7(CC)C=CCN(C67)CC5)(O)C(=O)OC)N4C=O)C=3)OC)CN1CCC1=C2NC2=CC=CC=C12 OGWKCGZFUXNPDA-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000009492 vitamin B5 Nutrition 0.000 description 1
- 239000011675 vitamin B5 Substances 0.000 description 1
- 235000019158 vitamin B6 Nutrition 0.000 description 1
- 239000011726 vitamin B6 Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 235000020334 white tea Nutrition 0.000 description 1
- 229940118846 witch hazel Drugs 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 235000013904 zinc acetate Nutrition 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
- CPYIZQLXMGRKSW-UHFFFAOYSA-N zinc;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+3].[Fe+3].[Zn+2] CPYIZQLXMGRKSW-UHFFFAOYSA-N 0.000 description 1
- OJYLAHXKWMRDGS-UHFFFAOYSA-N zingerone Chemical compound COC1=CC(CCC(C)=O)=CC=C1O OJYLAHXKWMRDGS-UHFFFAOYSA-N 0.000 description 1
- UZFLPKAIBPNNCA-FPLPWBNLSA-N α-ionone Chemical compound CC(=O)\C=C/C1C(C)=CCCC1(C)C UZFLPKAIBPNNCA-FPLPWBNLSA-N 0.000 description 1
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Abstract
Description
≡Si−CH2−CH(Y)−(A)a−Si≡
のシロキサン鎖の間の連結により特徴付けられ、
示されるSi原子は、各々、異なるシロキサン鎖の部分を形成し、a=0又は1であり、Aが存在する場合、通常1〜4個の炭素原子を有する炭化水素連鎖を表し、Yは、水素又は1又は2個の炭素原子を有するアルキル基を表す。アルケニル含有オルガノポリシロキサン(a)及びSiH含有シロキサン(b)は、実質的に完全に反応させられ得、よって分散液に存在する反応生成物は、実質的に未反応のアルケニル基を含まないか、又は実質的に未反応のSiH基(すなわち、立体障害又は他の理由のため反応するのが遅い任意の残存性SiH及び/又はアルケニルを除いて反応した)を含まないか、のいずれかであり、又は部分的に反応させられ得る。
この実施例は、米国特許第−B−6306411号の実施例1に基づく。105.11gの脱イオン水及びAshlandにより供給された3.97gのヒドロキシエチルセルロースの溶液を、まず調製した。64gのDOW CORNING(登録商標)9509シリコーンエラストマー懸濁液を、歯科用カップに計量して、続いてヒドロキシエチルセルロース溶液を計量して、Speedmixer(登録商標)DAC 450ミキサの中に配置し、カップを1分間最大速度で素早く回転させた。次いで、12.93gのAvalure(登録商標)UR450(これは何であろうか)及び2gのグリセロールをカップ中に引き続いて添加し、1分間最大速度で素早く回転させた。
9.09gのDow Corning(登録商標)9701の化粧品粉末(ジメチコン/ビニルジメチコンクロスポリマー、及びシリカを含み、日本国特許公開公報第JP−A−10/175816号に記載されるプロセスにより製造された)を、歯科用カップに計量して、18重量%の溶液中の6.03gのMowiol 18〜88及び11.25gの水を続いて計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。
およそ50,000mPa.sの粘度を有する29.89gのビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.167gの水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。非イオン性界面活性剤としての0.56gのポリオキシエチレン(6)トリデシルエーテル、及び0.09gのSyloff 4000の触媒(15ppmの白金を提供)を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。1.25gの脱イオン水をカップ中に添加し、カップを1分間最大速度で素早く回転させた。したがって、形成された濃縮されたエマルションを、必要な量の脱イオン水で漸増式に希釈し、合計は41.23gに到達した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.s(cPs)の粘度を有する64.96%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、0.36重量%の水素化官能基を含有する7mPa secの0.47%の水素化官能性シロキサンオリゴマーを続いて計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。6.7%のMowiol 18〜88ポリビニルアルコール(88%加水分解され18mPa.sの粘度)の18%の活性溶液、及び0.2%のSyloff 4000の触媒(15ppmの白金を提供)を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。1.6%の脱イオン水をカップ中に添加し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.40%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18〜88の18%の活性溶液、及び0.13%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
実施例2を、Mowiol 18〜88の18%の活性溶液の量を増加させそれを用いて繰り返した。この溶液の量は、実施例3及び4で、それぞれ、15%及び30%である。
実施例2を、以下のポリビニルアルコールの異なる純度の様々な量を用いることで繰り返した。
実施例5−20.0%のMowiol 20〜98の10%溶液(98%加水分解され20mPa.sの粘度)
実施例6−20.2%のMowiol 8〜88の10%溶液(88%加水分解され8mPa.sの粘度)
実施例7−19.7%のMowiol 30〜88の10%溶液(88%加水分解され30mPa.sの粘度)
実施例8−20.2%のMowiol 30〜92の10%溶液(92%加水分解され30mPa.sの粘度)
実施例2を、0.36重量%の水素化官能基を含有する7mPa.sの水素化官能性シロキサンオリゴマーの様々な量を用いることで繰り返した。実施例9、10、11、12、及び13のための水素化官能性シロキサンの量は、それぞれ、0.47%、0.51%、0.57%、0.30%、及び0.81%であった。SiH基とビニル基との間のモル比を、各実施例のために計算し表1に示す。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて1.66重量%の水素化官能基を含有する粘度30mPa.sの0.07%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18〜88の18%の活性溶液、及び0.06%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.21%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.41%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。15%のMowiol 18〜88の18%活性溶液、0.18%のポリオキシエチレン(6)トリデシルエーテル、及び0.2%のSyloff 4000の触媒をまた、カップ中に添加した。PVA対非イオン性界面活性剤の重量比は、15:1であった。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.15%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.41%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。14.7%のMowiol 18〜88の18%活性溶液、及びカチオン性界面活性剤としての塩化アンモニウムセチルの3.4%の30%活性溶液、及び0.2%のSyloff 4000の触媒をまた、カップ中に添加した。PVA対非イオン性界面活性剤の重量比は、2.7:1であった。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.40%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18〜88の18%の活性溶液、及び0.13%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、必要な量の脱イオン水で漸増式に希釈し、合計は90%に到達した。各水の添加の後、カップを最大速度で1分間撹拌した。10%のグリセロールを、次いで漸増式に添加し、各添加の後、カップを最大速度で1分間撹拌した。
実施例20のグリセロールを、カプリン酸及びカプリル酸トリグリセリド(tryglicerides)の混合物(実施例21)又はペトロラタム(実施例22)に置換することで繰り返した。調製されたフィルムの機械抵抗は、表3に列挙され、十分であることが分かる。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.40%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18〜88の18%の活性溶液、及び0.13%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、必要な量の脱イオン水で漸増式に希釈し、合計は94%に到達した。各水の添加の後、カップを最大速度で1分間撹拌した。6%のポリエチレングリコールPEG400(分子量400)を、次いで漸増式に添加し、各添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて、0.36重量%の水素化官能基と10%のDow Corning(登録商標)200流体350とを含有する7mPa.sの0.40%の水素化官能性シロキサンオリゴマー、運動性粘度が0.00035m2/秒(350 cSt)のトリメチルシリル末端封鎖ポリジメチルシロキサン、を計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。15.00%のMowiol 18〜88の18%の活性溶液、及び0.13%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて、0.36重量%の水素化官能基と5%のDow Corning(登録商標)200流体10000とを含有する7mPa.sの0.40%の水素化官能性シロキサンオリゴマー、運動性粘度が0.01m2/秒(10000 cSt)のトリメチルシリル末端封鎖ポリジメチルシロキサン、を計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18−88の18%の活性溶液、及び0.13%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する59.58%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.40%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18〜88の18%の活性溶液、及び0.13%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、必要な量の脱イオン水で漸増式に希釈し、合計は95.98%に到達した。各水の添加の後、カップを最大速度で1分間撹拌した。4.02%のDow Corning(登録商標)9701の化粧品的粉末(ジメチコン/ビニルジメチコンクロスポリマー及びシリカを含む)を、次いで添加し、粉末の添加後、カップを最大速度で1分間撹拌した。
およそ50,000mPa.sの粘度を有する85.04%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.62%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。14.27%のMowiol 18〜88の18%活性溶液、及び0.07%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。
およそ50,000mPa.sの粘度を有する79.36%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて0.36重量%の水素化官能基を含有する7mPa.sの0.56%の水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。20.02%のMowiol 18〜88の18%の活性溶液、及び0.07%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。
豚の耳を地元の畜殺場から入手し、冷たい流水下で洗浄した。解剖用メスで皮膚を切除し、電気皮膚採取器(Zimmer(商標) Electric Dermatome,Dover,Ohio)で750μmの厚さに切断した。皮膚を〜9cm2片に切断し、個別にParafilm(商標)に包んで、使用前に最長3ヶ月間−20℃で保管した。
●セルのサイズ:個別校正毎に、内部直径=15mm、浸透面=1.77cm2、受容体の体積〜12ml。
●受容体の溶液及び種類:リン酸緩衝生理食塩水、pH 7.4
●試料採取パラメータ:
○出水5.0mL
○廃棄物1.0mL
○試料1.0mL
○廃棄物に戻る:あり
○置換体積:10.2mL
●膜上に堆積した製剤の量:セル当たり〜50〜〜70mgの範囲の重量の差分により重力測定的に判定される。
●膜の種類:皮膚採取した豚の皮膚(750μm)
●試験温度:32℃
●試料採取予定:1、2、3、4、5、6時間
およそ50,000mPa.sの粘度を有する59.59%のビニル末端官能性直鎖状シロキサンを、歯科用カップ中に計量し、続いて、0.18重量%の水素化官能基を含有する10mPa.sの1.17%の直鎖状水素化官能性シロキサンオリゴマーを計量した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。10.00%のMowiol 18〜88の18%の活性溶液、及び0.05%のSyloff 4000の触媒を、カップ中に添加した。カップを閉じて、Speedmixer(登録商標)DAC 450ミキサ内に配置し、カップを1分間最大速度で素早く回転させた。厚い相の組成物を、合計100%に到達するために必要とされる量の脱イオン水で漸増式に希釈した。各水の添加の後、カップを最大速度で1分間撹拌した。ヒドロシリル化反応生成物の分散液を形成した。
請求項1の手順を踏まえて、表6に示される試薬からシリコーン分散液を調製した。Si−ビニルポリマーは、およそ50,000mPa.sの粘度を有するビニル末端官能性直鎖状シロキサンであった。SI−Hポリマーは、0.36重量%の水素化官能基(%)を含有する粘度7mPa.sの水素化官能性シロキサンオリゴマーであった。分散液の調製後、固体シリコーン粒子を、その中に分散させた。各固体シリコーン粒子は、ジメチコン/ビニルジメチコンクロスポリマーを含んだ。1つの種類の粒子において、このクロスポリマーをシリカとブレンドする。別の種類の粒子において、クロスポリマーを、C12〜14パレス−12、すなわち、合成二級C12〜14脂肪族アルコールと平均12個のモルのエチレンオキシドとの混合物のポリエチレングリコールエーテルとブレンドする。固体シリコーン粒子を含有する実施例31〜35の分散液の中央粒径を測定したものを表6に示す。
Claims (21)
- 水性シリコーン分散液の調製のための方法であって、前記方法が、(a)分子当たり平均少なくとも2個のアルケニル基を有するアルケニル含有オルガノポリシロキサンと、(b)分子当たり平均少なくとも2個のSiH部分を有するSiH含有シロキサンと、を混合することと、得られた混合物をポリビニルアルコール水溶液中で乳化させて水性シリコーンエマルションを形成することと、を含み、ヒドロシリル化触媒が、前記ポリビニルアルコール水溶液の添加と同時に添加されるか、又は続いて前記水性シリコーンエマルションに添加され、前記アルケニル含有オルガノポリシロキサン(a)と前記SiH含有シロキサン(b)とが、前記水性シリコーンエマルション中で一緒に反応し、前記アルケニル含有オルガノポリシロキサン(a)と前記SiH含有シロキサン(b)とそれらの反応生成物とが、前記水相中に溶解されたポリビニルアルコールによって分散液形態で安定化される、方法。
- 前記アルケニル含有オルガノポリシロキサンが、分子当たり平均少なくとも2個のビニル又はヘキセニル基を含有するポリジオルガノシロキサンである、請求項1に記載の方法。
- 前記アルケニル含有オルガノポリシロキサンが、25℃にてASTM D1084に記載されるように試験されたときに、100〜100,000,000ミリパスカル秒(mPa.s)の動的粘度を有する、請求項1又は2に記載の方法。
- 前記アルケニル含有オルガノポリシロキサンが、式CH2=CH−Si(CH3)2O−[Si(CH3)2O]n−Si(CH3)2−CH=CH2のビニルで末端封鎖されたポリジメチルシロキサンであり、式中、nが、100〜10000の平均数である、請求項1に記載の方法。
- 前記SiH含有シロキサンが、分子当たり平均2個を超えるSiH部分を有する、請求項1〜4のいずれか一項に記載の方法。
- 賦形剤油が、アルケニル含有オルガノポリシロキサン(a)とSiH含有シロキサン(b)との前記混合物が乳化される前に、前記アルケニル含有オルガノポリシロキサン(a)と前記SiH含有シロキサン(b)と共に混合される、請求項1〜5のいずれか一項に記載の方法。
- 前記水性シリコーン分散液が、いかなる非ポリマー界面活性剤も存在しない中で調製される、請求項1〜6のいずれか一項に記載の方法。
- フィルムを形成するために有用な水性分散液であって、前記分散液が、水相中に分散されたシリコーン組成物を含み、前記シリコーン組成物が、(a)分子当たり平均少なくとも2個のアルケニル基を有するアルケニル含有オルガノポリシロキサンと、(b)分子当たり平均少なくとも2個のSiH部分を有するSiH含有シロキサンとの反応の生成物を含み、前記分散液組成物がまた、ヒドロシリル化触媒とポリビニルアルコールとを含み、前記アルケニル含有オルガノポリシロキサン(a)と前記SiH含有シロキサン(b)とが、部分的に一緒に反応し、前記シリコーン組成物が、前記水相中に溶解された前記ポリビニルアルコールによって分散液形態で安定化され、前記分散液がいかなる非ポリマー界面活性剤をも欠く、水性分散液。
- 水相中に分散されたシリコーン組成物の液滴を含む水性分散液であって、前記シリコーン組成物が、(a)分子当たり平均少なくとも2個のアルケニル基を有するアルケニル含有オルガノポリシロキサンと、(b)分子当たり平均少なくとも2個のSiH部分を有するSiH含有シロキサンとの反応の生成物を含み、前記エマルション組成物がまた、ヒドロシリル化触媒とポリビニルアルコールとを含み、前記アルケニル含有オルガノポリシロキサン(a)と前記SiH含有シロキサン(b)とが、部分的に一緒に反応し、前記シリコーン組成物が、前記ポリビニルアルコールによって分散液形態で安定化され、前記分散液が、平らなホウケイ酸ガラス基板上に試験用多層フィルムを形成することができるものとして特徴付けることができ、前記多層フィルムが、前記基板と外側のポリ(ビニルアルコール)層との間に挟まれ、それらと機能的に接触している、内部シリコーン層を含み、前記内部シリコーン層が、前記分散液の前記液滴の集合体を含み、前記外側のポリ(ビニルアルコール)層が、試験用水滴がその上に堆積された30秒後、θがASTM D7334−08に従って測定されたときの、80度(°)未満の水接触角(θ)により特徴付けることができる、水性分散液。
- 前記ポリビニルアルコールが、前記水性シリコーン分散液の総重量の1〜10%で存在する、請求項8又は9に記載の分散液。
- 前記ポリビニルアルコール水溶液が、少なくとも5:1のポリビニルアルコール対非イオン性界面活性剤の重量比で、非イオン性界面活性剤を含有するか、又は、少なくとも2.5:1のポリビニルアルコール対カチオン性若しくはアニオン性界面活性剤の重量比で、カチオン性若しくはアニオン性界面活性剤を含有する、請求項8〜10のいずれか一項に記載の分散液。
- それぞれ、請求項8〜11のいずれか一項に記載の分散液と、医薬品的に又は化粧品的に活性な成分との混和物を含む、医薬品又は化粧品組成物。
- ポリ(ビニルアルコール)層と機能的に接触しているシリコーン層を含む多層フィルムであって、前記シリコーン層が、請求項8〜12のいずれか一項に記載の分散液の分散相の集合体を含み、前記ポリ(ビニルアルコール)層が、試験用水滴がその上に堆積された30秒後、水接触角(θ)がASTM D7334−08に従って測定されるときの、80度(°)未満のθにより特徴付けることができる、多層フィルム。
- 前記シリコーン層が、前記アルケニル含有オルガノポリシロキサン(a)と前記SiH含有シロキサン(b)との反応により形成されるエラストマー性シリコーン材料である、請求項13に記載の多層フィルム。
- 前記シリコーン層が、前記多層フィルムの60〜99重量%を成す、請求項13又は14に記載の多層フィルム。
- それぞれ、請求項13〜15のいずれか一項に記載の多層フィルムを含み、かつ医薬品的に又は化粧品的に活性な成分を更に含有する、医薬品的に又は化粧品的に活性な多層フィルム。
- 請求項13〜16のいずれか一項に記載の多層フィルムでコーティングされた基板であって、前記シリコーン層を、前記基板と前記ポリ(ビニルアルコール)層との間に挟むように、前記多層フィルムの前記シリコーン層が、前記基板と接触している、基板。
- 多層フィルムで基板をコーティングする方法であって、請求項8〜12のいずれか一項に記載の分散液で前記基板をコーティングすることと、前記水相中の水を前記基板上の前記コーティングから蒸発させることと、を含む、方法。
- 哺乳類の疾患又は状態の治療を必要とする哺乳類の疾患又は状態を治療する方法であって、治療的に有効な量の請求項12に記載の組成物、又は治療的に有効な量の請求項16に記載の多層フィルムを前記哺乳類の皮膚の一部に局部的に塗布することを含む、方法。
- 哺乳類の皮膚のしわのマスク処置を必要とする哺乳類の皮膚のしわをマスクする方法であって、有効な量の請求項8〜12のいずれか一項に記載の分散液を前記哺乳類の皮膚に局部的に塗布することを含む、方法。
- 皮膚のしわをマスクするための皮膚ケアにおける請求項8〜12のいずれか一項に記載の分散液の使用。
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CN104395377A (zh) | 2015-03-04 |
US20180369390A1 (en) | 2018-12-27 |
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