JP7135862B2 - 皮膚化粧料 - Google Patents
皮膚化粧料 Download PDFInfo
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- JP7135862B2 JP7135862B2 JP2018549033A JP2018549033A JP7135862B2 JP 7135862 B2 JP7135862 B2 JP 7135862B2 JP 2018549033 A JP2018549033 A JP 2018549033A JP 2018549033 A JP2018549033 A JP 2018549033A JP 7135862 B2 JP7135862 B2 JP 7135862B2
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- acid
- polymer particles
- extract
- meth
- particles
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- VMPHSYLJUKZBJJ-UHFFFAOYSA-N trilaurin Chemical compound CCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCC)COC(=O)CCCCCCCCCCC VMPHSYLJUKZBJJ-UHFFFAOYSA-N 0.000 description 1
- PBSRSWFGYPZDAU-FFIPNUABSA-H trimagnesium;[(2r)-2-[(1s)-1,2-dihydroxyethyl]-3-oxido-5-oxo-2h-furan-4-yl] phosphate Chemical class [Mg+2].[Mg+2].[Mg+2].OC[C@H](O)[C@H]1OC(=O)C(OP([O-])([O-])=O)=C1[O-].OC[C@H](O)[C@H]1OC(=O)C(OP([O-])([O-])=O)=C1[O-] PBSRSWFGYPZDAU-FFIPNUABSA-H 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 229940117985 trimethyl pentaphenyl trisiloxane Drugs 0.000 description 1
- UUJLHYCIMQOUKC-UHFFFAOYSA-N trimethyl-[oxo(trimethylsilylperoxy)silyl]peroxysilane Chemical compound C[Si](C)(C)OO[Si](=O)OO[Si](C)(C)C UUJLHYCIMQOUKC-UHFFFAOYSA-N 0.000 description 1
- 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 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 229940118594 trimethylolpropane triisostearate Drugs 0.000 description 1
- DUXYWXYOBMKGIN-UHFFFAOYSA-N trimyristin Chemical compound CCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCC DUXYWXYOBMKGIN-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
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
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- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- KLNPWTHGTVSSEU-UHFFFAOYSA-N undecane-1,11-diamine Chemical compound NCCCCCCCCCCCN KLNPWTHGTVSSEU-UHFFFAOYSA-N 0.000 description 1
- 229960002703 undecylenic acid Drugs 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 229940099259 vaseline Drugs 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 229960001722 verapamil Drugs 0.000 description 1
- 239000010679 vetiver oil Substances 0.000 description 1
- LLWJPGAKXJBKKA-UHFFFAOYSA-N victoria blue B Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC(=CC=1)N(C)C)=C(C=C1)C2=CC=CC=C2C1=[NH+]C1=CC=CC=C1 LLWJPGAKXJBKKA-UHFFFAOYSA-N 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- FUSUHKVFWTUUBE-UHFFFAOYSA-N vinyl methyl ketone Natural products CC(=O)C=C FUSUHKVFWTUUBE-UHFFFAOYSA-N 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000019156 vitamin B Nutrition 0.000 description 1
- 239000011720 vitamin B Substances 0.000 description 1
- 235000019166 vitamin D Nutrition 0.000 description 1
- 239000011710 vitamin D Substances 0.000 description 1
- 150000003710 vitamin D derivatives Chemical class 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
- 229940011671 vitamin b6 Drugs 0.000 description 1
- 229940046008 vitamin d Drugs 0.000 description 1
- 239000001717 vitis vinifera seed extract Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000003357 wound healing promoting agent Substances 0.000 description 1
- 229940075420 xanthine Drugs 0.000 description 1
- ZFNVDHOSLNRHNN-UHFFFAOYSA-N xi-3-(4-Isopropylphenyl)-2-methylpropanal Chemical compound O=CC(C)CC1=CC=C(C(C)C)C=C1 ZFNVDHOSLNRHNN-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 229940105125 zinc myristate Drugs 0.000 description 1
- 229960001296 zinc oxide Drugs 0.000 description 1
- 229940043810 zinc pyrithione Drugs 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
- ZNVKGUVDRSSWHV-UHFFFAOYSA-L zinc;4-hydroxybenzenesulfonate Chemical compound [Zn+2].OC1=CC=C(S([O-])(=O)=O)C=C1.OC1=CC=C(S([O-])(=O)=O)C=C1 ZNVKGUVDRSSWHV-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
- GBFLQPIIIRJQLU-UHFFFAOYSA-L zinc;tetradecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O GBFLQPIIIRJQLU-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229930007850 β-damascenone Natural products 0.000 description 1
- 239000002446 δ-tocopherol Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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Description
1.第三角法に基づく投影図の正面図、平面図及び側面図の全てが楕円であり、下記(1)~(3)を満たす扁平楕円球状ポリマー粒子Aを含むポリマー粒子を0.1~50質量%含む皮膚化粧料。
(1)扁平部の長径(L)の平均(LAV)が、0.13≦LAV≦500μm。
(2)扁平部の短径(D)の平均(DAV)が、0.1≦DAV≦250μm。
(3)長径(L)と短径(D)とから算出されるアスペクト比(L/D)の平均(P1 AV)が、1.3<P1 AV≦50。
2.扁平楕円球状ポリマー粒子Aが、更に、下記(4)及び(5)の少なくともどちらか一方を満たす1の皮膚化粧料。
(4)短径(D)と側面の厚さ(T)とから算出されるアスペクト比(D/T)の平均(P2 AV)が、1.2<P2 AV≦100。
(5)長径(L)と側面の厚さ(T)とから算出されるアスペクト比(L/T)の平均(P3 AV)が、1.56<P3 AV≦150。
3.扁平楕円球状ポリマー粒子Aを2種以上含む1又は2の皮膚化粧料。
4.前記ポリマー粒子が、更に、扁平楕円球状ポリマー粒子Aとは異なる形状のポリマー粒子Bを1種以上含む1~3のいずれかの皮膚化粧料。
5.ポリマー粒子Bの体積平均粒子径が、LAV以下である4の皮膚化粧料。
6.ポリマー粒子Bが、球状、略球状又は楕円球状である4又は5の皮膚化粧料。
7.扁平楕円球状ポリマー粒子Aとポリマー粒子Bとの質量比が、99:1~10:90である4~6のいずれかの皮膚化粧料。
8.更に、無機粒子を含む1~7のいずれかの皮膚化粧料。
9.前記無機粒子の形状が、板状又は鱗片状である8の皮膚化粧料。
10.更に、油性成分を含む1~9のいずれかの皮膚化粧料。
本発明の皮膚化粧料は、下記扁平楕円球状ポリマー粒子Aを含むポリマー粒子を必須成分として含む。
扁平楕円球状ポリマー粒子Aは、第三角法に基づく投影図の正面図、平面図及び側面図の全てが楕円であり、下記(1)~(3)を満たすものである。
(1)扁平部の長径(L)の平均(LAV)が、0.13≦LAV≦500μm。
(2)扁平部の短径(D)の平均(DAV)が、0.1≦DAV≦250μm。
(3)長径(L)と短径(D)とから算出されるアスペクト比(L/D)の平均(P1 AV)が、1.3<P1 AV≦50。
(4)短径(D)と側面の厚さ(T)とから算出されるアスペクト比(D/T)の平均(P2 AV)が、1.2<P2 AV≦100。
(5)長径(L)と厚さ(T)とから算出されるアスペクト比(L/T)の平均(P3 AV)が、1.56<P3 AV≦150。
(6)粒子表面又は表層部に付着又は内包される微粒子の粒子径(SP)が、1/1000×DAV≦SP≦1/2×DAV。
扁平楕円球状ポリマー粒子Aは、溶液重合により一段階で製造することができ、粒子の圧縮・転写工程を含まず、バッチ法で製造できるため、複数の工程を経ることなく一括して大量生産することができる。本発明における溶液重合とは、少なくとも単量体と重合開始剤を含む媒体中で重合反応を進行させてポリマー粒子として析出又は生成させる重合方法と定義する。溶液重合法として具体的には、懸濁重合法、乳化重合法、分散重合法、シード重合法及びこれらに準ずる複合化した方法を含むものとする。
(i)スチレン、o-メチルスチレン、m-メチルスチレン、p-メチルスチレン、α-メチルスチレン、o-エチルスチレン、m-エチルスチレン、p-エチルスチレン、2,4-ジメチルスチレン、p-n-ブチルスチレン、p-tert-ブチルスチレン、p-n-ヘキシルスチレン、p-n-オクチルスチレン、p-n-ノニルスチレン、p-n-デシルスチレン、p-n-ドデシルスチレン、p-メトキシスチレン、p-フェニルスチレン、p-クロロスチレン、3,4-ジクロロスチレン等のスチレン化合物;
(ii)(メタ)アクリル酸;
(iii)(メタ)アクリル酸メチル、(メタ)アクリル酸エチル、(メタ)アクリル酸プロピル、(メタ)アクリル酸n-ブチル、(メタ)アクリル酸イソブチル、(メタ)アクリル酸ペンチル、(メタ)アクリル酸ヘキシル、(メタ)アクリル酸2-エチルヘキシル、(メタ)アクリル酸オクチル、(メタ)アクリル酸ノニル、(メタ)アクリル酸デシル、(メタ)アクリル酸ドデシル、(メタ)アクリル酸ラウリル、(メタ)アクリル酸ステアリル、(メタ)アクリル酸シクロヘキシル、(メタ)アクリル酸イソボルニル、(メタ)アクリル酸フェニル、(メタ)アクリル酸トルイル、(メタ)アクリル酸ベンジル等の炭化水素基含有(メタ)アクリル系単量体;(メタ)アクリル酸2,2,2-トリフルオロエチル、(メタ)アクリル酸3,3,3-トリフルオロプロピル、(メタ)アクリル酸2-(パーフルオロエチル)エチル、(メタ)アクリル酸2-パーフルオロエチル-2-パーフルオロブチルエチル、(メタ)アクリル酸2-パーフルオロエチル、(メタ)アクリル酸テトラフルオロプロピル、(メタ)アクリル酸パーフルオロメチル、(メタ)アクリル酸1,1,1,3,3,3-ヘキサフルオロプロパン-2-イル、(メタ)アクリル酸2-パーフルオロメチル-2-パーフルオロエチルメチル、(メタ)アクリル酸2-(パーフルオロヘキシル)エチル、(メタ)アクリル酸2-(パーフルオロデシル)エチル、(メタ)アクリル酸2-(パーフルオロヘキサデシル)エチル等のフッ素含有(メタ)アクリル系単量体;γ-(メタクリロイルオキシプロピル)トリメトキシシラン、γ-(メタクリロイルオキシプロピル)ジメトキシメチルシラン等のケイ素含有(メタ)アクリル系単量体;(ポリ)エチレングリコールモノ(メタ)アクリレート、(メタ)アクリル酸2-メトキシエチル、(メタ)アクリル酸3-メトキシブチル等のアルコキシ基含有(メタ)アクリル系単量体;(ポリ)プロピレングリコールモノ(メタ)アクリレート等の(ポリ)アルキレングリコール(メタ)アクリル系単量体;メトキシ(ポリ)エチレングリコールモノ(メタ)アクリレート、メトキシ(ポリ)プロピレングリコールモノ(メタ)アクリレート等のアルコキシ(ポリ)アルキレングリコール(メタ)アクリル系単量体;(メタ)アクリル酸2-クロロエチル、α-クロロ(メタ)アクリル酸メチル等の反応性官能基を含まない(メタ)アクリル酸エステル;
(iv)酢酸ビニル、プロピオン酸ビニル、安息香酸ビニル、酪酸ビニル、ギ酸ビニル、バレリン酸ビニル、ピバリン酸ビニル等のカルボン酸ビニルエステル;
(v)N-ビニルピロール、N-ビニルカルバゾール、N-ビニルインドール、N-ビニルピロリドン等のN-ビニル化合物;
(vi)エチレン、プロピレン等のオレフィン;
(vii)フッ化ビニル、フッ化ビニリデン、テトラフルオロエチレン、ヘキサフルオロプロピレン等のフッ化オレフィン;
(viii)ブタジエン、イソプレン等の共役ジエン
等が挙げられる。これらは、1種単独で又は2種以上を組み合わせて使用することができる。
(メタ)アクリル酸2-アミノエチル、アクリル酸-N-プロピルアミノエチル、(メタ)アクリル酸-N-エチルアミノプロピル、(メタ)アクリル酸-N-フェニルアミノエチル、(メタ)アクリル酸-N-シクロヘキシルアミノエチル等のアミノ基含有(メタ)アクリル系単量体;アリルアミン、N-メチルアリルアミン等のアリルアミン系誘導体;p-アミノスチレン等のアミノ基含有スチレン誘導体;2-ビニル-4,6-ジアミノ-S-トリアジン等のトリアジン誘導体等が挙げられる。これらの中でも、1級又は2級アミノ基を有する化合物が好ましい。
(メタ)アクリル酸、クロトン酸、ケイ皮酸、イタコン酸、マレイン酸、フマル酸等の不飽和カルボン酸;イタコン酸モノブチル等のイタコン酸モノC1~C8アルキルエステル;マレイン酸モノブチル等のマレイン酸モノC1~C8アルキルエステル;ビニル安息香酸等のビニル基含有芳香族カルボン酸等、及びこれらの塩が挙げられる。
(メタ)アクリル酸2-ヒドロキシエチル、(メタ)アクリル酸2-ヒドロキシプロピル、(メタ)アクリル酸3-ヒドロキシプロピル、(メタ)アクリル酸4-ヒドロキシブチル等のヒドロキシ基含有(メタ)アクリル系単量体;ヒドロキシエチルビニルエーテル、ヒドロキシブチルビニルエーテル等のヒドロキシアルキルビニルエーテル系単量体;アリルアルコール、2-ヒドロキシエチルアリルエーテル等のヒドロキシ基含有アリル単量体等が挙げられる。
N-(2-メルカプトエチル)アクリルアミド、N-(2-メルカプト-1-カルボキシエチル)アクリルアミド、N-(2-メルカプトエチル)メタクリルアミド、N-(4-メルカプトフェニル)アクリルアミド、N-(7-メルカプトナフチル)アクリルアミド、マレイン酸モノ2-メルカプトエチルアミド、(メタ)アクリル酸2-メルカプトエチル、(メタ)アクリル酸2-メルカプト-1-カルボキシエチル等のチオール基含有(メタ)アクリル系単量体等が挙げられる。
ビニルメチルケトン、ビニルヘキシルケトン、メチルイソプロペニルケトン等のビニル基含有ケトン等が挙げられる。
ビニルメチルエーテル、ビニルエチルエーテル、ビニルイソブチルエーテル等のビニル基含有エーテル系単量体が挙げられる。
アクリロニトリル、メタクリロニトリル、ヘキセンニトリル、4-ペンテンニトリル、p-シアノスチレン等が挙げられる。
(メタ)アクリルアミド、α-エチル(メタ)アクリルアミド、N-メチル(メタ)アクリルアミド、N-ブトキシメチル(メタ)アクリルアミド、ジアセトン(メタ)アクリルアミド、N,N-ジメチル(メタ)アクリルアミド、N,N-ジエチル(メタ)アクリルアミド、N,N-ジメチル-p-スチレンスルホンアミド、N,N-ジメチルアミノエチル(メタ)アクリルアミド、N,N-ジエチルアミノエチル(メタ)アクリルアミド、N,N-ジメチルアミノプロピル(メタ)アクリルアミド、N,N-ジエチルアミノプロピル(メタ)アクリルアミド等が挙げられる。
(メタ)アクリル酸グリシジル、(メタ)アクリル酸(β-メチル)グリシジル、(メタ)アクリル酸3,4-エポキシシクロヘキシル等のエポキシ基含有(メタ)アクリル系単量体;アリルグリシジルエーテル、3,4-エポキシビニルシクロヘキサン等のエポキシ基含有ビニル系単量体;ジ(β-メチル)グリシジルマレート、ジ(β-メチル)グリシジルフマレート等が挙げられる。
イオン性官能基としては、アニオン性官能基、カチオン性官能基のどちらでもよい。アニオン性官能基としては、例えば、カルボキシル基、スルホン酸基、リン酸基、フェノール性ヒドロキシ基及びこれらの塩等が挙げられ、カチオン性官能基としては、アミノ基、イミダゾール基、ピリジン基、アミジノ基及びこれらの塩等が挙げられる。
前記ポリマー粒子は、必要に応じて、扁平楕円球状ポリマー粒子Aとは異なる形状のポリマー粒子Bを含んでもよい。ここで述べる異なる形状とは、前記扁平楕円球状ポリマー粒子Aと形状又はサイズが異なる粒子も含まれるが、UV散乱効果、可視光領域における光散乱性、光反射性等の光学特性が安定的に得られることを考慮すると異なる形状がよい。例えば、球状、略球状、楕円球状、粉砕状、棒状、多面体、凹凸状、塊状等である。なお、略球状とは、楕円球状であって、アスペクト比が2未満のことをいう。
本発明の皮膚化粧料に含まれる前記ポリマー粒子以外の残りの成分(以下、その他の成分と称する。)としては、化粧料に通常用いられる成分を適宜使用することができる。その他の成分は、本発明の皮膚化粧料中、50~99.9質量%含まれる。
本発明の皮膚化粧料は、その他の成分として、肌への密着性、伸び、光沢、着色、隠蔽性等を適宜調整する観点から、無機粒子を含むことが好ましい。前記無機粒子としては、マイカ、タルク、カオリン、セリサイト、モンモリロナイト、カオリナイト、雲母、白雲母、金雲母、合成雲母、紅雲母、黒雲母、パーミキュライト、炭酸マグネシウム、炭酸カルシウム、ケイ酸アルミニウム、ケイ酸バリウム、ケイ酸カルシウム、ケイ酸マグネシウム、ケイ酸ストロンチウム、タングステン酸金属塩、マグネシウム、ゼオライト、硫酸バリウム、焼成硫酸カルシウム、リン酸カルシウム、フッ素アパタイト、ヒドロキシアパタイト、セラミックパウダー、ベントナイト、スメクタイト、粘土、泥、金属石鹸(例えば、ミリスチン酸亜鉛、パルミチン酸カルシウム、ステアリン酸アルミニウム)、ベンガラ、黄酸化鉄、黒酸化鉄、群青、紺青、カーボンブラック、酸化チタン、微粒子及び超微粒子酸化チタン、酸化亜鉛、微粒子及び超微粒子酸化亜鉛、アルミナ、シリカ、煙霧状シリカ(超微粒子無水ケイ酸)、雲母チタン、魚鱗箔、窒化ホウ素、ホトクロミック顔料、合成フッ素金雲母、金、アルミニウム、微粒子複合粉体等の各種の大きさ・形状の無機粒子、並びにこれらをハイドロジェンシリコーン又は環状ハイドロジェンシリコーン等のシリコーン、その他のシラン化合物、チタンカップリング剤等の各種表面処理剤で処理を行って疎水化又は親水化した無機粒子等が挙げられる。
本発明の皮膚化粧料は、その他の成分として、油性成分を含むことが好ましい。前記油性成分としては、高級アルコール類、高級脂肪酸類、油脂、ロウ類、炭化水素類、シリコーン類、脂肪酸エステル等が挙げられる。
MICROTRACK MT3000(日機装(株)製)を用いて測定した。
(2)ポリマー粒子のアスペクト比
走査電子顕微鏡((株)日立ハイテクノロジーズ製S-4800、以下、SEMという)を用い、測定可能な倍率(300~30,000倍)で写真を撮影し、得られた扁平楕円球状ポリマー粒子を二次元化した状態で、ランダムに100個の粒子を抽出し、各粒子の扁平部の長径(L)、扁平部の短径(D)及び側面の厚さ(T)の測定を行い
アスペクト比(L/D)の平均(P1 AV)、
アスペクト比(D/T)の平均(P2 AV)、
アスペクト比(L/T)の平均(P3 AV)
として算出した。
粒子の扁平部の平均長径(LAV)、平均短径(DAV)及び平均厚さ(TAV)も同様にランダムに抽出した100個の粒子について、長径(L)、短径(D)及び側面の厚さ(T)を測定して算出した。なお、図1に、扁平楕円球状ポリマー粒子Aの長径(L)、短径(D)及び厚さ(T)を表す図を示す。
(3)比表面積(SB)
自動比表面積細孔分布測定装置(BELSORP-max(日本ベル(株)製))を用い、窒素ガス吸着法により比表面積(SB)を測定した。
(4)理論比表面積(SD)
ポリマー粒子の体積平均粒子径を2r(m)、その半径をr(m)、その密度をG(g/m3)とする。このとき、半径r(m)の真球状粒子の表面積S'(m2)、体積V(m3)は、それぞれ次式で表される。
半径rの真球状粒子の表面積:S'=4πr2
半径rの真球状粒子の体積: V=4πr3/3
この場合、粒子1g当たりに含まれる粒子の個数Nは次式で表される。
粒子1g当たりに含まれる粒子の個数:N=1/VG
したがって、ポリマー粒子から算出される真球状粒子の理論比表面積SD(m2/g)は次式で表される。
SD=S'N=S'/VG=3/rG
(5)ポリマー粒子の嵩密度
三薬局方で規定されている試験法の第1法(メスシリンダーを用いる方法)を用いてゆるめ嵩密度として算出した。単位はg/mLとした。
(6)吸水量測定
乾燥させたポリマー粒子粉を約2質量%の濃度で水に分散させ、一日静置した後、再度分散させ、ガラスフィルターを用いて、減圧ろ過した。ろ過したガラスフィルターを、遠心分離機((株)日立ハイテクノロジーズ製CR-20GII)を用いて、3,000rpmで30分間遠心した後、得られたポリマー粒子粉を乾燥し、乾燥前後の粉体の質量を測定し、その差を吸水量とした。
(7)吸油量の測定
JIS K 5101に記される、煮あまに油法に準拠して測定した。
(8)pH測定
攪拌している状態の反応液にpH試験紙(Whatman社製)を浸け、その色の変化度合いで判断した。
[製造例1]
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温(25℃、以下同様)で1時間攪拌した。
水 912.0g
メタノール 45.0g
ポリプロピレングリコール(#3000) 88.0g
ポリビニルピロリドン(K-15) 56.5g
ポリエチレンオキシド(M.W.300,000) 22.5g
過酸化ベンゾイル(油溶性) 1.6g
過硫酸ナトリウム(水溶性) 3.7g
メタクリル酸メチル 524.0g
エチレングリコールジメタクリレート 6.3g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を85℃に設定し、窒素気流下で加熱、攪拌(400rpm)を開始し、8時間重合反応を行ってメタクリル酸メチル-エチレングリコールジメタクリレート共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A1を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、図2に示すように、表層部及び表面に平均粒径0.3μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは9μm、DAVは3μm、TAVは1μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 912.0g
エタノール 27.0g
ポリプロピレングリコール(#3000) 96.0g
ポリビニルピロリドン(K-15) 48.0g
ショ糖ラウリル酸エステル 9.6g
アゾビスイソブチロニトリル(AIBN)(油溶性) 2.8g
過硫酸アンモニウム(水溶性) 3.2g
メタクリル酸メチル 580.0g
エチレングリコールジメタクリレート 5.8g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を75℃に設定し、窒素気流下で加熱、攪拌(250rpm)を開始し、8時間重合反応を行ってメタクリル酸メチル-エチレングリコールジメタクリレート共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A2を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、図3に示すように、表層部及び表面に平均粒径1.2μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは35μm、DAVは8μm、TAVは2μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 930.0g
エタノール 45.5g
ポリプロピレングリコール(#3000) 68.0g
ポリビニルピロリドン(K-15) 53.5g
ショ糖ラウリル酸エステル 10.5g
2,2'-アゾビス(イソ酪酸)ジメチル(油溶性) 2.2g
過硫酸アンモニウム(水溶性) 3.6g
メタクリル酸メチル 555.0g
エチレングリコールジメタクリレート 5.6g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を75℃に設定し、窒素気流下で加熱、攪拌(400rpm)を開始し、8時間重合反応を行ってメタクリル酸メチル-エチレングリコールジメタクリレート共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A3を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、図4に示すように、表層部及び表面に平均粒径0.6μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは43μm、DAVは4μm、TAVは2μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 760.0g
エタノール 44.6g
ポリプロピレングリコール(#3000) 88.0g
ポリビニルピロリドン(K-15) 49.5g
ショ糖ラウリル酸エステル 8.6g
AIBN(油溶性) 2.4g
過硫酸アンモニウム(水溶性) 1.9g
メタクリル酸メチル 480.0g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を75℃に設定し、窒素気流下で加熱、攪拌(300rpm)を開始し、8時間重合反応を行ってポリメタクリル酸メチル粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A4を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、表層部及び表面に平均粒径0.4μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは16μm、DAVは8μm、TAVは2μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 880.0g
エタノール 52.0g
ポリプロピレングリコール(#2000) 98.0g
ポリビニルピロリドン(K-15) 46.0g
ショ糖ラウリル酸エステル 11.0g
2,2'-アゾビス(イソ酪酸)ジメチル(油溶性) 2.5g
過硫酸アンモニウム(水溶性) 3.5g
メタクリル酸メチル 684.0g
エチレングリコールジメタクリレート 10.3g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を73℃に設定し、窒素気流下で加熱、攪拌(300rpm)を開始し、8時間重合反応を行ってメタクリル酸メチル-エチレングリコールジメタクリレート共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A5を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、表層部及び表面に平均粒径0.6μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは24μm、DAVは10μm、TAVは4μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 865.0g
エタノール 42.5g
ポリプロピレングリコール(#2000) 102.0g
ポリビニルピロリドン(K-30) 22.5g
脂肪酸グリセリンエステル 13.0g
アゾビスイソバレロニトリル(油溶性) 2.0g
2,2'-アゾビス(2-メチル-N-フェニルプロピオン
アミジン)二塩酸塩(水溶性) 2.5g
メタクリル酸メチル 580.0g
ポリエチレングリコールジメタクリレート(n=4) 17.4g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を76℃に設定し、窒素気流下で加熱、攪拌(350rpm)を開始し、8時間重合反応を行ってメタクリル酸メチル-ポリエチレングリコールジメタクリレート(n=4)共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A6を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、表層部及び表面に平均粒径0.8μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは29μm、DAVは7μm、TAVは3μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 712.5g
メタノール 37.5g
ポリプロピレングリコール(#3000) 75.0g
ポリビニルピロリドン(K-30) 43.2g
ショ糖バルミチン酸エステル 10.8g
AIBN(油溶性) 3.2g
過硫酸アンモニウム(水溶性) 4.3g
メタクリル酸メチル 486.0g
メタクリル酸 54.0g
エチレングリコールジメタクリレート 10.8g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を72℃に設定し、窒素気流下で加熱、攪拌(250rpm)を開始し、8時間重合反応を行ってメタクリル酸メチル-メタクリル酸-エチレングリコールジメタクリレート共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A7を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、表層部及び表面に平均粒径1.2μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは49μm、DAVは19μm、TAVは6μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、室温で1時間攪拌した。
水 912.0g
イソプロピルアルコール 27.4g
ポリプロピレングリコール(#4000) 69.5g
ポリビニルピロリドン(K-15) 52.6g
ポリオキシエチレンラウリルエーテル 15.5g
アゾビスメチルブチロニトリル(油溶性) 2.6g
過硫酸カリウム(水溶性) 3.0g
スチレン 652.0g
ジビニルベンゼン 9.8g
このとき、液相は水系相部分と乳化相部分と油系相部分の各相が交じり合う状態であり、そのpHを測定したところ7であった。
次に、オイルバス温度を78℃に設定し、窒素気流下で加熱、攪拌(400rpm)を開始し、8時間重合反応を行ってスチレン-ジビニルベンゼン共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子A8を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、表層部及び表面に平均粒径0.5μmの粒子が付着した扁平楕円球状ポリマー粒子であった。
LAVは19μm、DAVは6μm、TAVは2μmであった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
2,000mLフラスコに、以下に示す各成分を一括で仕込み、ディスパー分散翼で1,000rpmで懸濁液を作製し、窒素気流下、オイルバス温度80℃で8時間加熱・攪拌し、粒子分散液を得た。その後、遠心分離を5回繰り返し分級・洗浄操作を行い、平均粒子径が5μmのポリメタクリル酸メチル単一の球状ポリマー粒子B1を作製した。
水 1386.5g
メタクリル酸メチル 173.4g
ラウリルパーオキサイド 8.6g
ポリビニルピロリドン(K-30) 17.3g
AIBNを用いず、過硫酸アンモニウムの使用量を14.0gに変更した以外は、製造例2と同様の方法でメタクリル酸メチル-エチレングリコールジメタクリレート共重合体粒子分散液を得た。なお、加熱開始前の反応液のpHは7、加熱開始2時間後の反応液のpHは2であり、反応終了時点の反応液のpHは1であった。
次に、公知の吸引ろ過設備にて粒子分散液をろ過し、得られたろ物について、更にメタノールにて洗浄-ろ過を5回繰り返した後、真空乾燥し、ポリマー粒子B2を得た。
得られた粒子100個をランダムに抽出してSEMにて形状を観察したところ、図5に示すように、扁平部分を有しない楕円球状(長球状)ポリマー粒子であり、その平均長径(LAV)は28μm、DAVは7μm、平均アスペクト比(P1 AV)は4であった。なお、異物について確認したが、凝集物やくっつき等の変形物は殆ど見られなかった。
[評価試験1]官能試験及び付着力評価
[参考例1-1~1-7、比較参考例1-1~1-2]
ポリマー粒子A1~A5及びB1~B2について、下記手法にて、肌触り、滑り性及び粒子付着力の評価を行った。結果を表3に示す。
(1)肌触り
各粒子を皮膚上に伸ばした際の感触を下記基準にて評価した。
(2)滑り性
黒色合皮上に各粒子1gを載せて、指で伸ばした際の長さを下記基準にて評価した。
(3)粒子付着力
黒色合皮上に各粒子1gを載せて、パフで均等に伸ばした後、合皮を3回たたき、粒子の残存量をデジタルマイクロスコープ(キーエンス社製VHX200)で観察し、下記基準にて評価した。
◎:極めて良好、○:良好、△:標準、×:不良
[参考例2-1~2-14、比較参考例2-1~2-2]
下記表4記載の組成になるように、ポリマー粒子A1~A5、ポリマー粒子B1~B2、及び精製水を混合し、0.1質量%のポリマー粒子分散液1~16を調製した。
[参考例3-1~3-2、比較参考例3-1~3-2]
下記表6記載の組成のポリマー粒子を黒色の合成皮革(5cm×8cm)に、化粧用パフでパッティングしながら均一に塗布し(0.24mg/cm2)、評価用シート1~4を作製した。次いで、自動変角光度計((株)村上色彩技術研究所製Gonio Photometer GP-200)を用い、各評価用シートに入射角45°で光を一定量照射し、反射光の光散乱分布を測定した。結果を図6に示す。
[評価試験4]粉末状ファンデーション
[実施例1~7、比較例1~2]
ポリマー粒子A1~A4、B1~B2を用い、下記表7の組成に従ってメイクアップ組成物(ファンデーション1~9)を作製した。
A:ファンデーション1がよい
B:ファンデーション2がよい
C:ファンデーション3がよい
D:ファンデーション4がよい
E:ファンデーション5がよい
F:ファンデーション6がよい
G:ファンデーション7がよい
H:ファンデーション8がよい
I:ファンデーション9がよい
J:いずれも同じ
その結果、パネラーの評価は
A:3名
B:1名
C:2名
D:2名
E:2名
F:2名
G:3名
H:0名
I:0名
J:0名
であった。
[実施例8~13、比較例3~4]
ポリマー粒子A1~A3、B1~B2を用い、下記表8の組成にしたがって、メイクアップ組成物(ファンデーション10~17)を作製した。
A:ファンデーション10がよい
B:ファンデーション11がよい
C:ファンデーション12がよい
D:ファンデーション13がよい
E:ファンデーション14がよい
F:ファンデーション15がよい
G:ファンデーション16がよい
H:ファンデーション17がよい
I:いずれも同じ
その結果、パネラーの評価は
A:3名
B:3名
C:3名
D:2名
E:2名
F:2名
G:0名
H:0名
I:0名
であった。
[処方例1~120]
化粧料全般、特に皮膚化粧料としては多数の用途や製品があるため、一般に開示されている化粧料処方をもとに、扁平楕円球状ポリマー粒子Aが皮膚化粧料として応用が可能か否か確認を行った。その結果、扁平楕円球状ポリマー粒子Aは既存のポリマー粒子や無機粒子等と同類で取り扱うことができ、かつ扁平楕円球状ポリマー粒子Aが有する固有の特性を付帯できることを確認した。
Claims (10)
- 第三角法に基づく投影図の正面図、平面図及び側面図の全てが楕円であり、下記(1)~(3)を満たす扁平楕円球状ポリマー粒子Aを含むポリマー粒子を0.1~50質量%含む皮膚化粧料。
(1)扁平部の長径(L)の平均(LAV)が、0.13≦LAV≦500μm。
(2)扁平部の短径(D)の平均(DAV)が、0.1≦DAV≦250μm。
(3)長径(L)と短径(D)とから算出されるアスペクト比(L/D)の平均(P1 AV)が、1.3<P1 AV≦50。 - 扁平楕円球状ポリマー粒子Aが、更に、下記(4)及び(5)の少なくともどちらか一方を満たす請求項1記載の皮膚化粧料。
(4)短径(D)と側面の厚さ(T)とから算出されるアスペクト比(D/T)の平均(P2 AV)が、1.2<P2 AV≦100。
(5)長径(L)と側面の厚さ(T)とから算出されるアスペクト比(L/T)の平均(P3 AV)が、1.56<P3 AV≦150。 - 扁平楕円球状ポリマー粒子Aを2種以上含む請求項1又は2記載の皮膚化粧料。
- 前記ポリマー粒子が、更に、扁平楕円球状ポリマー粒子Aとは異なる形状のポリマー粒子Bを1種以上含む請求項1~3のいずれか1項記載の皮膚化粧料。
- ポリマー粒子Bの体積平均粒子径が、LAV以下である請求項4記載の皮膚化粧料。
- ポリマー粒子Bが、球状、略球状又は楕円球状である請求項4又は5記載の皮膚化粧料。
- 扁平楕円球状ポリマー粒子Aとポリマー粒子Bとの質量比が、99:1~10:90である請求項4~6のいずれか1項記載の皮膚化粧料。
- 更に、無機粒子を含む請求項1~7のいずれか1項記載の皮膚化粧料。
- 前記無機粒子の形状が、板状又は鱗片状である請求項8記載の皮膚化粧料。
- 更に、油性成分を含む請求項1~9のいずれか1項記載の皮膚化粧料。
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US20220096356A1 (en) * | 2020-09-30 | 2022-03-31 | L'oréal | System and method for priming eye cosmetics |
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WO2024127219A1 (en) * | 2022-12-15 | 2024-06-20 | I.T.P. S.R.L. Innovation & Technology Provider | Procedure for preparing compositions with a high content of bioactive compounds |
CN117323266B (zh) * | 2023-11-20 | 2024-05-24 | 植物医生(广东)生物科技有限公司 | 一种抗糖化、抗氧化组合物及其应用 |
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JP2012001440A (ja) | 2010-06-14 | 2012-01-05 | Ohken Co Ltd | ポリエステル扁平粒子の製造方法 |
JP2015093973A (ja) | 2013-11-14 | 2015-05-18 | 日清紡ホールディングス株式会社 | 紫外線散乱剤及びその用途 |
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JP5286879B2 (ja) | 2008-03-28 | 2013-09-11 | 日清紡ホールディングス株式会社 | 微粒子含有楕円状または針状ポリマー粒子およびその製造方法 |
JP2016017048A (ja) * | 2014-07-08 | 2016-02-01 | 日清紡ホールディングス株式会社 | スクラブ剤及びその用途 |
EP3296326A4 (en) * | 2015-05-08 | 2018-12-19 | Nisshinbo Holdings Inc. | Flat elliptical polymer particles, and use thereof |
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JP2015093973A (ja) | 2013-11-14 | 2015-05-18 | 日清紡ホールディングス株式会社 | 紫外線散乱剤及びその用途 |
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