JP6527223B2 - 日焼け止め組成物 - Google Patents
日焼け止め組成物 Download PDFInfo
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- JP6527223B2 JP6527223B2 JP2017253825A JP2017253825A JP6527223B2 JP 6527223 B2 JP6527223 B2 JP 6527223B2 JP 2017253825 A JP2017253825 A JP 2017253825A JP 2017253825 A JP2017253825 A JP 2017253825A JP 6527223 B2 JP6527223 B2 JP 6527223B2
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- Prior art keywords
- metal oxide
- weight
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- dispersion
- oxide particles
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims description 44
- 230000000475 sunscreen effect Effects 0.000 title claims description 33
- 239000000516 sunscreening agent Substances 0.000 title claims description 33
- 150000004706 metal oxides Chemical class 0.000 claims description 133
- 239000002245 particle Substances 0.000 claims description 118
- 229910044991 metal oxide Inorganic materials 0.000 claims description 100
- 239000006185 dispersion Substances 0.000 claims description 52
- 239000007771 core particle Substances 0.000 claims description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 239000000126 substance Substances 0.000 claims description 20
- 239000011247 coating layer Substances 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 229910010272 inorganic material Inorganic materials 0.000 claims description 16
- 239000011147 inorganic material Substances 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 11
- 239000000194 fatty acid Substances 0.000 claims description 11
- 229930195729 fatty acid Natural products 0.000 claims description 11
- 230000008033 biological extinction Effects 0.000 claims description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical group [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 5
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- 239000002612 dispersion medium Substances 0.000 claims description 4
- DLAHAXOYRFRPFQ-UHFFFAOYSA-N dodecyl benzoate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1 DLAHAXOYRFRPFQ-UHFFFAOYSA-N 0.000 claims description 4
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- 125000005313 fatty acid group Chemical group 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 41
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
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- 150000003839 salts Chemical class 0.000 description 6
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- 239000011787 zinc oxide Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229920000388 Polyphosphate Polymers 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
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- 125000004432 carbon atom Chemical group C* 0.000 description 4
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- TYYHDKOVFSVWON-UHFFFAOYSA-N 2-butyl-2-methoxy-1,3-diphenylpropane-1,3-dione Chemical compound C=1C=CC=CC=1C(=O)C(OC)(CCCC)C(=O)C1=CC=CC=C1 TYYHDKOVFSVWON-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 235000021314 Palmitic acid Nutrition 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 125000002877 alkyl aryl group Chemical group 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 125000003710 aryl alkyl group Chemical group 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 125000000732 arylene group Chemical group 0.000 description 3
- 229960005193 avobenzone Drugs 0.000 description 3
- 150000001735 carboxylic acids Chemical class 0.000 description 3
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 125000000392 cycloalkenyl group Chemical group 0.000 description 3
- 125000002993 cycloalkylene group Chemical group 0.000 description 3
- 239000012470 diluted sample Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
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- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
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- DXGLGDHPHMLXJC-UHFFFAOYSA-N oxybenzone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 DXGLGDHPHMLXJC-UHFFFAOYSA-N 0.000 description 3
- 229960001173 oxybenzone Drugs 0.000 description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 3
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 3
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- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
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- HEOCBCNFKCOKBX-RELGSGGGSA-N (1s,2e,4r)-4,7,7-trimethyl-2-[(4-methylphenyl)methylidene]bicyclo[2.2.1]heptan-3-one Chemical compound C1=CC(C)=CC=C1\C=C/1C(=O)[C@]2(C)CC[C@H]\1C2(C)C HEOCBCNFKCOKBX-RELGSGGGSA-N 0.000 description 2
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 description 2
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- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
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- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 2
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- SOXAGEOHPCXXIO-DVOMOZLQSA-N menthyl anthranilate Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@H]1OC(=O)C1=CC=CC=C1N SOXAGEOHPCXXIO-DVOMOZLQSA-N 0.000 description 2
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- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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- 239000010936 titanium Substances 0.000 description 2
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- LINXHFKHZLOLEI-UHFFFAOYSA-N trimethyl-[phenyl-bis(trimethylsilyloxy)silyl]oxysilane Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)C1=CC=CC=C1 LINXHFKHZLOLEI-UHFFFAOYSA-N 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 125000003161 (C1-C6) alkylene group Chemical group 0.000 description 1
- URXZKGGRKRRVDC-UHFFFAOYSA-N 1-[dimethoxy(propyl)silyl]oxyethanamine Chemical compound CCC[Si](OC)(OC)OC(C)N URXZKGGRKRRVDC-UHFFFAOYSA-N 0.000 description 1
- ZQCIPRGNRQXXSK-UHFFFAOYSA-N 1-octadecoxypropan-2-ol Chemical compound CCCCCCCCCCCCCCCCCCOCC(C)O ZQCIPRGNRQXXSK-UHFFFAOYSA-N 0.000 description 1
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- ABEXEQSGABRUHS-UHFFFAOYSA-N 16-methylheptadecyl 16-methylheptadecanoate Chemical compound CC(C)CCCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCCCC(C)C ABEXEQSGABRUHS-UHFFFAOYSA-N 0.000 description 1
- JSOVGYMVTPPEND-UHFFFAOYSA-N 16-methylheptadecyl 2,2-dimethylpropanoate Chemical compound CC(C)CCCCCCCCCCCCCCCOC(=O)C(C)(C)C JSOVGYMVTPPEND-UHFFFAOYSA-N 0.000 description 1
- 229940043268 2,2,4,4,6,8,8-heptamethylnonane Drugs 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- KIHBGTRZFAVZRV-UHFFFAOYSA-N 2-Hydroxyoctadecanoic acid Natural products CCCCCCCCCCCCCCCCC(O)C(O)=O KIHBGTRZFAVZRV-UHFFFAOYSA-N 0.000 description 1
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- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical group CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 description 1
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 description 1
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 0.000 description 1
- OZWKZRFXJPGDFM-UHFFFAOYSA-N tripropoxysilane Chemical compound CCCO[SiH](OCCC)OCCC OZWKZRFXJPGDFM-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Chemical group 0.000 description 1
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Description
X4-n−Si−[Lm−Y]n (1)
式中、
Yは、官能基であり、
Xは、加水分解性基であり、
Lは、連結基であり、
mは、0または1、好ましくは、1であり、ならびに
nは、1または2、好ましくは、1である。
X3−Si−Lm−N+[R2 2]R3 (Z-) (2)
式中、
X、L、およびmは、上記の式(1)で定める通りであり、
各R2は、独立して、低級(すなわち、C1−C6)アルキル、好ましくは、C1−C4アルキル、より好ましくは、C1−C2アルキル、特には、メチル基であり、
R3は、ヒドロカルビル、好ましくは、アルキルまたはアルケニル、より好ましくは、アルキル基であり、分岐鎖状または直鎖状であってよく、好ましくは、直鎖状であり、6個超、好ましくは、10個超の炭素原子、より好ましくは、12〜40個、特には、14〜24個、特に、16〜20個の範囲の炭素原子を含み、ならびに、
Z-は、アニオン、好ましくは、一価アニオン、より好ましくは、臭化物、ヨウ化物、塩化物などのハロゲン化物イオン、メチルまたはエチルサルフェートなどのアルキルサルフェートから成る群より選択される。
1)金属酸化物粒子の結晶サイズ測定
結晶サイズは、X線回折(XRD)線幅広化(line broadening)によって測定した。回折パターンは、CuKα線を用い、モノクロメーターとして作用するSol−Xエネルギー分散型検出器を備えたSiemens D5000回折計で測定した。プログラム可能スリットを用い、長さ12mmの試料からの回折を、ステップサイズ0.02°およびステップのカウント時間3秒で測定した。データの分析を、ルチル型の反射位置に対応するピーク一式があり、アナターゼ型が存在する場合は、それらの反射に対応する追加のピーク一式もある22〜48°2θの回折パターンのフィッティングによって行った。このフィッティングプロセスにより、機器による回折線形状に対する幅広化の影響を取り除くことができた。重量平均結晶サイズの値は、ルチル110反射(およそ27.4°2θ)に対して、Stokes and Wilson(B.E. Warren, “X-Ray Diffraction”, Addison-Wesley, Reading, Massachusetts, 1969, pp 254-257)の方法の原理に従い、その積分幅に基づいて決定した。
金属酸化物粒子の分散体を、7gのポリグリセリル−3ポリリシノレエートを53gのC12−C15アルキルベンゾエートと混合し、続いて40gの金属酸化物粉末をその溶液中に添加することによって作製した。この混合物を、およそ2100rpmで運転し、粉砕メディアとしてジルコニアビーズを入れた水平型ビーズミルに15分間通した。金属酸化物粒子の分散体を、イソプロピルミリステートと混合することにより、固形分2重量%まで希釈した(希釈分散体は、粒子サイズの測定の前に安定であることを確保する必要がある(必要に応じて、さらにポリグリセリル−3ポリリシノレエートを添加してもよい))。希釈サンプルを、Brookhaven BI−XDC粒子径測定装置により遠心モードで分析し、メジアン粒子体積径および粒子サイズ分布は、粒子の(例:二酸化チタンの)理論密度を用いて特定した。
Micromeritics Flowsorb II 2300を用いて、単一点BET比表面積を測定した。
日焼け止め製剤を、光沢黒色カードの表面にコーティングし、No2Kバーを用いて引き伸ばし、湿潤厚さ12ミクロンの塗膜を形成した。塗膜を室温にて10分間乾燥させ、黒色表面上のコーティングの白色度(LF)を、Minolta CR300 比色計を用いて測定した。白色度の変化ΔLを、基材の白色度(LS)をコーティングの白色度(LF)から差し引くことによって算出した。白色度指数は、標準的な二酸化チタン(=100%値)(Tayca MT 100T(テイカ株式会社より))と比較した白色度の変化ΔLのパーセントである。
15gの金属酸化物粉末を、85gのC12−15アルキルベンゾエート中へ、0.8〜1.25mmジルコニアビーズを70%充填したミニモーターミル(Eiger Torrance MK M50 VSE TFV)を用いて、5000rpmで15分間ミリングすることにより、金属酸化物分散体を作製した。新たにミリングした分散体を、65×30×6mmのアクリルセル中の直径16mm×深さ3mmのへこみ部へ充填した。石英ガラス製カバーグラスをサンプルの上に置いて大気との接触を遮断し、真鍮製留め具により適切な位置に固定した。12個までのセルを回転式プラットフォーム上に置くことができ、75W UV光源(4つのTL29D16/09Nランプを備えたPhilips HB 171/A)から12cmに配置し、120分間の照射を行った。サンプルの色(L*a*b*値)を、予め標準白色タイル(L*=97.95)で較正しておいた市販の比色計(Minolta クロマメーター CR−300)で記録した。白色度の変化ΔL*を、UV光への暴露後の基材の白色度から、UV光への暴露前の基材の白色度(L* Iinitial)を差し引くことによって算出した。光灰色化指数は、ΔL*=L* (Iinitial)−L* (120分)である。
日焼け止め製剤のサンプロテクションファクター(SPF)は、Diffey and Robson, J. Soc. Cosmet. Chem. Vol. 40, pp 127-133,1989の生体外法を用いて特定した。
金属酸化物分散体のサンプル0.1gを、100mLのシクロヘキサンで希釈した。次に、この希釈サンプルを、サンプル:シクロヘキサン 1:19の比率でさらにシクロヘキサンで希釈した。合計の希釈率は、1:20000であった。次に、この希釈サンプルを、光路長1cmで分光光度計(Perkin−Elmer Lambda 2 UV/VIS 分光光度計)中に配置し、UVおよび可視光の吸光度を測定した。吸光係数は、式A=E.c.lから算出し、式中、A=吸光度、E=リットル/グラム/cmの単位での吸光係数、c=グラム/リットルの単位での濃度、およびl=cmの単位での光路長である。
皮膚への感触は、試験サンプルに一連の感覚属性に対する%数値スコアを割り当てるというプロトコルを用いて、熟練した評価者が測定した。2mLのエマルジョンを、前腕部内側の直径およそ5cmの円形領域に広げた。広げた後、皮膚上の試験サンプルの塗布後感触を、以下の用語で特徴付けた:%「オイル様」皮膚感触;%「ロウ様」皮膚感触;%「グリース様」皮膚感触;および%「シリコーン様」皮膚感触。
酸性溶液中のチタンオキシジクロリドの1モルを、水溶液中のNaOHの3モルと反応させた。初期反応時間の後、温度を70℃超まで上昇させ、撹拌を継続した。この反応混合物を、NaOH水溶液を添加することで中和し、70℃未満まで冷却した。室温までの冷却後、混合物のpHを、pH>9に再調節し、温度を、50℃に上昇させた。pHを9超に維持した状態で、TiO2重量に対して10重量%SiO2に相当するケイ酸ナトリウム溶液を添加した。添加の間、温度を50℃に維持した。pH6.5に再中和し、30分間撹拌した後、この混合物を、60℃に加熱し、pHをpH9.5に調節した。TiO2重量に対して7.5%に相当する3−アミノプロピルトリエトキシシランを添加した。この混合物を30分間撹拌し、その後、温度を75℃に上昇させた。熱水に溶解したステアリン酸ナトリウム(TiO2に対して7.5重量%のステアリン酸ナトリウムに相当)を添加した。
(a)分散体粒子サイズ
i)D(v,0.5)=48nm、
ii)粒子の10体積%が、28nm未満の体積径を有し、
iii)粒子の16体積%が、31nm未満の体積径を有し、
iv)粒子の30体積%が、38nm未満の体積径を有し、
v)粒子の70体積%が、62nm未満の体積径を有し、
vi)粒子の84体積%が、83nm未満の体積径を有し、および
vii)粒子の90体積%が、305nm未満の体積径を有する。
(b)吸光係数;
E524 E308 E360 E(max) λ(max) E308/E524
1.2 45.0 8.7 59.6 276 38.5
(c)BET比表面積=86.4m2g-1
(d)光灰色化指数=3.38
実施例1で作製した二酸化チタン分散体を用いて、以下の組成を有する日焼け止めエマルジョン製剤を作製した。
1.撹拌しながら相Bの成分を混合し、75〜80℃に加熱する。
2.これとは別に、TiO2分散体以外の相Aの成分を混合し、75〜80℃に加熱する。
3.撹拌しながら相Aの成分にTiO2分散体を添加し、少しの間75〜80℃に再加熱する。
4.強く撹拌しながら、相Bを相Aの成分にゆっくり添加する。
5.1分間ホモジナイズする。
6.40℃未満となったところで、相Cを添加し、均質となるまで混合する。
7.室温まで撹拌/冷却する。
実施例1で作製した二酸化チタン分散体を用いて、以下の組成を有する日焼け止めエマルジョン製剤を作製した;
1.撹拌しながら相Bの成分を混合し、75〜80℃に加熱する。
2.これとは別に、TiO2分散体以外の相Aの成分、およびSolaveil(商標)CZ−100を混合し、75〜80℃に加熱する。
3.相Aの成分にTiO2分散体を添加し、少しの間75〜80℃に再加熱する。
4.強く撹拌しながら、相Bを相Aの成分にゆっくり添加する。
5.1分間ホモジナイズする。
6.40℃未満となったところで、相Cを添加し、均質となるまで混合する。
7.室温まで撹拌/冷却する。
実施例1で作製した二酸化チタン分散体を用いて、以下の組成を有する日焼け止めエマルジョン製剤を作製した;
1.Keltrol SFT、Veegum Ultra、およびPricerine(商標)9091をプレミックスし、撹拌しながら水を添加する。
2.撹拌しながら残りの相Bの成分を添加し、75〜80℃に加熱する。
3.これとは別に、TiO2分散体以外の相Aの成分を混合し、75〜80℃に加熱する。
4.相Bの成分を30秒間ホモジナイズし、75〜80℃で20分間膨潤させる。
5.撹拌しながら、相Aの成分にTiO2分散体を添加し、少しの間75〜80℃に再加熱する。
4.撹拌しながら、相Aを相Bの成分に添加する。
5.1分間ホモジナイズする。
6.40℃未満となったところで、相Cを添加し、均質となるまで混合する。
7.室温まで撹拌/冷却する。
Claims (11)
- 無機物質、シランカップリング剤および疎水化剤を含む被覆層を有する金属酸化物コア粒子を含む金属酸化物粒子を含む日焼け止め組成物であって、前記被覆層が、前記金属酸化物コア粒子の重量に対して、0.5〜35重量%の無機物質、0.5〜20重量%のシランカップリング剤、および0.5〜20重量%の疎水化剤を含み、前記金属酸化物が二酸化チタンであり、前記無機物質がシリカを含み、前記シランカップリング剤がアミノシランであり、前記疎水化剤が脂肪酸である、日焼け止め組成物。
- 前記シランカップリング剤がアミノプロピルトリエトキシシランであり、前記疎水化剤がステアリン酸である、請求項1に記載の日焼け止め組成物。
- 前記金属酸化物粒子が、前記粒子の総乾燥重量に対して、82〜84重量%の金属酸化物、6.5〜7.5重量%の無機物質、4〜5.5重量%のシランカップリング剤、および4.5〜6重量%の疎水化剤を含む、請求項1または2に記載の日焼け止め組成物。
- 前記金属酸化物粒子が、0.5〜1.6L/g/cmの524nmでの吸光係数(E524)、および/または38〜55L/g/cmの308nmでの吸光係数(E308)を有する、請求項1〜3のいずれか1項に記載の日焼け止め組成物。
- 前記金属酸化物粒子が、E308/E524比が20よりも大きい、請求項1〜4のいずれか1項に記載の日焼け止め組成物。
- 前記金属酸化物粒子は分散体中のメジアン体積粒子径が30〜65nmである、請求項1〜5のいずれか1項に記載の日焼け止め組成物。
- 分散媒中に請求項1〜6のいずれか1項に記載の金属酸化物粒子を含む日焼け止め組成物に使用するための分散体。
- 少なくとも30重量%の金属酸化物粒子を含む、請求項7に記載の分散体。
- 分散剤を含む、請求項7または8に記載の分散体。
- 分散媒がアルキルベンゾエートであり、分散剤がポリグリセリル−3ポリリシノレエートである、請求項9に記載の分散体。
- 請求項7〜10のいずれか1項に記載の分散体を含む日焼け止め組成物。
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