JP4961082B2 - Coated zinc oxide powder, method for producing the same, and cosmetic using the same - Google Patents
Coated zinc oxide powder, method for producing the same, and cosmetic using the same Download PDFInfo
- Publication number
- JP4961082B2 JP4961082B2 JP2001295281A JP2001295281A JP4961082B2 JP 4961082 B2 JP4961082 B2 JP 4961082B2 JP 2001295281 A JP2001295281 A JP 2001295281A JP 2001295281 A JP2001295281 A JP 2001295281A JP 4961082 B2 JP4961082 B2 JP 4961082B2
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- oxide powder
- coated
- acid
- coated zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims description 89
- 239000002537 cosmetic Substances 0.000 title claims description 35
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 229920001577 copolymer Polymers 0.000 claims description 43
- 238000000576 coating method Methods 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 7
- 239000011164 primary particle Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 description 17
- 239000000843 powder Substances 0.000 description 14
- -1 and as a result Chemical compound 0.000 description 12
- 210000002374 sebum Anatomy 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 235000019198 oils Nutrition 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 4
- POJWUDADGALRAB-UHFFFAOYSA-N allantoin Chemical compound NC(=O)NC1NC(=O)NC1=O POJWUDADGALRAB-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 238000009739 binding Methods 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000006210 lotion Substances 0.000 description 4
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000015165 citric acid Nutrition 0.000 description 3
- 239000002734 clay mineral Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- GHOKWGTUZJEAQD-ZETCQYMHSA-N (D)-(+)-Pantothenic acid Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCC(O)=O GHOKWGTUZJEAQD-ZETCQYMHSA-N 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 2
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 description 2
- POJWUDADGALRAB-PVQJCKRUSA-N Allantoin Natural products NC(=O)N[C@@H]1NC(=O)NC1=O POJWUDADGALRAB-PVQJCKRUSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 241000723346 Cinnamomum camphora Species 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 2
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 229960000458 allantoin Drugs 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 229940121363 anti-inflammatory agent Drugs 0.000 description 2
- 239000002260 anti-inflammatory agent Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000003908 antipruritic agent Substances 0.000 description 2
- CUFNKYGDVFVPHO-UHFFFAOYSA-N azulene Chemical compound C1=CC=CC2=CC=CC2=C1 CUFNKYGDVFVPHO-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 2
- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 description 2
- LLEMOWNGBBNAJR-UHFFFAOYSA-N biphenyl-2-ol Chemical compound OC1=CC=CC=C1C1=CC=CC=C1 LLEMOWNGBBNAJR-UHFFFAOYSA-N 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 229960000846 camphor Drugs 0.000 description 2
- 229930008380 camphor Natural products 0.000 description 2
- QMVPMAAFGQKVCJ-UHFFFAOYSA-N citronellol Chemical compound OCCC(C)CCC=C(C)C QMVPMAAFGQKVCJ-UHFFFAOYSA-N 0.000 description 2
- OSOIQJGOYGSIMF-UHFFFAOYSA-N cyclopentadecanone Chemical compound O=C1CCCCCCCCCCCCCC1 OSOIQJGOYGSIMF-UHFFFAOYSA-N 0.000 description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical group O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 2
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 description 2
- JYGXADMDTFJGBT-VWUMJDOOSA-N hydrocortisone Chemical compound O=C1CC[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 JYGXADMDTFJGBT-VWUMJDOOSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 2
- UWKAYLJWKGQEPM-LBPRGKRZSA-N linalyl acetate Chemical compound CC(C)=CCC[C@](C)(C=C)OC(C)=O UWKAYLJWKGQEPM-LBPRGKRZSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 229940041616 menthol Drugs 0.000 description 2
- KVWWIYGFBYDJQC-UHFFFAOYSA-N methyl dihydrojasmonate Chemical compound CCCCCC1C(CC(=O)OC)CCC1=O KVWWIYGFBYDJQC-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 2
- 235000011007 phosphoric acid Nutrition 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- CZCBTSFUTPZVKJ-UHFFFAOYSA-N rose oxide Chemical compound CC1CCOC(C=C(C)C)C1 CZCBTSFUTPZVKJ-UHFFFAOYSA-N 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000003352 sequestering agent Substances 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- PHXATPHONSXBIL-UHFFFAOYSA-N xi-gamma-Undecalactone Chemical compound CCCCCCCC1CCC(=O)O1 PHXATPHONSXBIL-UHFFFAOYSA-N 0.000 description 2
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 2
- NPNUFJAVOOONJE-ZIAGYGMSSA-N β-(E)-Caryophyllene Chemical compound C1CC(C)=CCCC(=C)[C@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-ZIAGYGMSSA-N 0.000 description 2
- PSQYTAPXSHCGMF-BQYQJAHWSA-N β-ionone Chemical compound CC(=O)\C=C\C1=C(C)CCCC1(C)C PSQYTAPXSHCGMF-BQYQJAHWSA-N 0.000 description 2
- WGVKWNUPNGFDFJ-DQCZWYHMSA-N β-tocopherol Chemical compound OC1=CC(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C WGVKWNUPNGFDFJ-DQCZWYHMSA-N 0.000 description 2
- SFEOKXHPFMOVRM-UHFFFAOYSA-N (+)-(S)-gamma-ionone Natural products CC(=O)C=CC1C(=C)CCCC1(C)C SFEOKXHPFMOVRM-UHFFFAOYSA-N 0.000 description 1
- YBJHBAHKTGYVGT-ZKWXMUAHSA-N (+)-Biotin Chemical compound N1C(=O)N[C@@H]2[C@H](CCCCC(=O)O)SC[C@@H]21 YBJHBAHKTGYVGT-ZKWXMUAHSA-N 0.000 description 1
- GEWDNTWNSAZUDX-WQMVXFAESA-N (-)-methyl jasmonate Chemical compound CC\C=C/C[C@@H]1[C@@H](CC(=O)OC)CCC1=O GEWDNTWNSAZUDX-WQMVXFAESA-N 0.000 description 1
- HZYHMHHBBBSGHB-UHFFFAOYSA-N (2E,6E)-2,6-Nonadienal Natural products CCC=CCCC=CC=O HZYHMHHBBBSGHB-UHFFFAOYSA-N 0.000 description 1
- HZYHMHHBBBSGHB-DYWGDJMRSA-N (2e,6e)-nona-2,6-dienal Chemical compound CC\C=C\CC\C=C\C=O HZYHMHHBBBSGHB-DYWGDJMRSA-N 0.000 description 1
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
- RBCOYOYDYNXAFA-UHFFFAOYSA-L (5-hydroxy-4,6-dimethylpyridin-3-yl)methyl phosphate Chemical compound CC1=NC=C(COP([O-])([O-])=O)C(C)=C1O RBCOYOYDYNXAFA-UHFFFAOYSA-L 0.000 description 1
- 239000001306 (7E,9E,11E,13E)-pentadeca-7,9,11,13-tetraen-1-ol Substances 0.000 description 1
- QMVPMAAFGQKVCJ-SNVBAGLBSA-N (R)-(+)-citronellol Natural products OCC[C@H](C)CCC=C(C)C QMVPMAAFGQKVCJ-SNVBAGLBSA-N 0.000 description 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 1
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- UFLHIIWVXFIJGU-ARJAWSKDSA-N (Z)-hex-3-en-1-ol Chemical compound CC\C=C/CCO UFLHIIWVXFIJGU-ARJAWSKDSA-N 0.000 description 1
- 229940058015 1,3-butylene glycol Drugs 0.000 description 1
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- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- NFIDBGJMFKNGGQ-UHFFFAOYSA-N isopropylmethylphenol Natural products CC(C)CC1=CC=CC=C1O NFIDBGJMFKNGGQ-UHFFFAOYSA-N 0.000 description 1
- 239000010656 jasmine oil Substances 0.000 description 1
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- 229910052744 lithium Inorganic materials 0.000 description 1
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
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- ZUFQODAHGAHPFQ-UHFFFAOYSA-N pyridoxine hydrochloride Chemical compound Cl.CC1=NC=C(CO)C(CO)=C1O ZUFQODAHGAHPFQ-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
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Description
【０００１】
【発明の属する技術分野】
本発明は、被覆酸化亜鉛粉体、その製造方法およびそれを用いた化粧料に関し、さらに詳しくは、酸化亜鉛粉体の表面被覆工程の効率がよく、化粧料として配合された時に、水素発生や未表面被覆部分による酸化亜鉛粉体を配合された化粧料のゲル化や粘度上昇の懸念がなく、安定で、さらに酸化亜鉛粉体それ自体が持つ耐皮脂性に優れた化粧持続性の向上した化粧料を製造できる被覆酸化亜鉛粉体、その製造方法およびそれを配合してなる化粧料に関する。
【０００２】
【従来の技術】
従来から、化粧料に配合される粉体の多くは、二次凝集を防止し、撥水性や撥油性を付与するために、メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体で表面被覆されている。
その際、粉体として用いられる酸化亜鉛粉体は、顔の皮脂と反応して皮脂をゲル化して固定し、皮脂の広がりを押さえ、脂っぽさを抑制し、化粧の持続性を向上させるのに役立っている。
【０００３】
メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体は、一般的にいえば、次の一般式（２）で示される構造を有する。
【０００４】
【化２】
こうしたメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体は、酸化亜鉛粉体の表面に被覆された後、加熱処理されると、下記の式（３）で示される反応が起こり、酸化亜鉛表面で重合され、あるいは、式（４）で示される反応により酸化亜鉛表面に存在する水酸基とも結合して被覆皮膜を形成し、二次凝集を防止しながら、撥水性や撥油性を付与し、耐皮脂性を増強するすることが知られている。
【０００６】
【化３】
【化４】
例えば、特開平８−４１３７９号には、特定の比表面積を持つ酸化亜鉛粉体を特定の繰返し単位数を持つメチルハイドロジェンシロキサン・ジメチルシロキサン共重合体で表面被覆した耐皮脂粉体が開示されている。
【０００９】
しかしながら、同公報に記載の特定の繰返し単位数を持つメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体では、酸化亜鉛粉体との結合が不十分であったり、あるいは、化粧料に配合した後で未反応のＳｉＨ基から水素を発生し、これが被覆酸化亜鉛粉体の貯蔵時、または最終製品である化粧料での容器の変形・破壊につながる危険性が起こるといった問題があった。
【００１０】
また、別の問題としては、酸化亜鉛粉体は、化粧料の他の成分に対して活性であり、化学結合を起こすことが認められ、完全に表面被覆されていないと化粧料をゲル化させることがあり、これは化粧料がファンデーション等の固形形状のものでは影響が少ないが、ローション等液状形状のものでは粘度が上昇し、大きな問題を引き起こすことがあった。
【００１１】
こうした状況下、酸化亜鉛粉体の表面被覆工程の効率がよく、化粧料として配合された時に、水素発生や未表面被覆部分による酸化亜鉛粉体を配合された化粧料のゲル化や粘度上昇の懸念がなく、安定で、さらに酸化亜鉛粉体それ自体が持つ耐皮脂性に優れた化粧持続性の向上した化粧料を製造できる被覆酸化亜鉛粉体の研究・開発が求められていた。
【００１２】
【発明が解決しようとする課題】
本発明の課題は、こうした従来技術の問題点に鑑み、酸化亜鉛粉体の表面をメルハイドロジェンシロキサン−ジメチルシロキサン共重合体で被覆したとき、より高い重合や酸化亜鉛との結合力（以下、これを単に「重合結合能」という。）を持ち、且つ、酸化亜鉛粉体表面を、より十分に表面被覆（以下、これを単に「表面被覆能」という。）し、この結果として、酸化亜鉛粉体の表面被覆工程の効率がよく、化粧料として配合された時に、水素発生や未表面被覆部分による酸化亜鉛粉体を配合された化粧料のゲル化や粘度上昇の懸念がなく、安定で、さらに酸化亜鉛粉体それ自体が持つ耐皮脂性に優れた化粧持続性の向上した化粧料を製造できる被覆酸化亜鉛粉体、その製造方法、およびそれを用いた化粧料を提供することにある。
【００１３】
【課題を解決するための手段】
本発明者等は、上記課題を解決すべく、鋭意研究を重ねた結果、種々のメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体を検討したところ、特定のメチルハイドロジェンシロキサンの繰返し単位数（ｎ）とジメチルシロキサンの繰返し単位数（ｍ）とを有する共重合体を合成し、それを特定の比表面積の酸化亜鉛粉体に表面被覆すると、高い重合結合能を持ち、且つより十分な表面被覆能を持つ被覆酸化亜鉛粉体が得られ、上記課題が達成されることを見出し、本発明を完成するに至った。
【００１４】
すなわち、本発明の第１の発明によれば、比表面積が１５〜１００ｍ２／ｇの酸化亜鉛粉体（Ａ）の表面を、次の化学式（１）で表されるメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）で被覆することを特徴とする被覆酸化亜鉛粉体が提供される。
【００１５】
【化５】
【００１６】
また、本発明の第２の発明によれば、第１の発明において、酸化亜鉛粉体（Ａ）の平均一次粒子径が、０．０１〜０．１μｍであることを特徴とする被覆酸化亜鉛粉体が提供される。
【００１７】
さらに、本発明の第３の発明によれば、第１あるいは２の発明において、メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）の被覆量が、酸化亜鉛粉体（Ａ）に対して２〜１０重量％であることを特徴とする被覆酸化亜鉛粉体が提供される。
【００１８】
一方、本発明の第４の発明によれば、酸化亜鉛粉体（Ａ）とハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）とを溶媒の存在下又は非存在下に混合し、表面被覆された酸化亜鉛粉体を得る第１の工程と、引き続いて、該表面被覆された酸化亜鉛粉体を５０〜２００℃で０．５〜５時間加熱処理する第２の工程とからなることを特徴とする第１〜３のいずれかの発明に記載の被覆酸化亜鉛粉体の製造方法が提供される。
【００１９】
また、本発明の第５の発明によれば、第１〜３のいずれかの発明に記載の被覆酸化亜鉛粉体を配合することを特徴とする化粧料が提供される。
【００２０】
【発明の実施の形態】
以下、本発明の被覆酸化亜鉛粉体、その製造方法およびそれを配合してなる化粧料について、各項目毎に詳細に説明する。
【００２１】
１．酸化亜鉛粉体（Ａ）
本発明で使用される酸化亜鉛粉体（Ａ）は、比表面積が１５〜１００ｍ２／ｇ好ましくは２０〜１００ｍ２／ｇのものである。
比表面積が１５ｍ２／ｇ未満では、皮脂をゲル化し固定する能力が劣り、一方、比表面積が１００ｍ２／ｇを超えると、粉体の表面活性が高くなり、二次凝集が起こったり、均一な表面被覆を得ることが困難になり、安定な被覆酸化亜鉛粉体の製造が困難になるので望ましくない。
【００２２】
また、酸化亜鉛粉体（Ａ）の平均一次粒子径は、特に限定されないが、通常は０．０１〜０．１μｍ、好ましくは０．０１５〜０．０５μｍ程度であることが望ましい。
平均一次粒子径が０．０１μｍ未満では、粉体の表面活性が高くなり、二次凝集が起こり、一方、０．１μｍを超えると、皮脂をゲル化し固定する能力が劣り、また化粧表面の平滑性が劣り望ましくない。
【００２３】
本発明に使用する市販の酸化亜鉛粉体（Ａ）としては、例えば、テイカ社製のＭＺ−３００、ＭＺ−５００、ＭＺ−７００、堺化学社製のＦＩＮＥＸ２５、ＦＩＮＥＸ５０、ＦＩＮＥＸ７５、ＦＩＮＥＸ９０等が好適に使用することができる。
【００２４】
２．メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）
本発明で使用されるメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）は、下記の一般式（１）で表されるものである。
【００２５】
【化６】
ここで、ｍとｎは正数であり、以下のイ、ロの要件を満たす。
イ．ｍ：ｎ＝４．０〜１．５：１
ロ．ｍ＋ｎ＝４〜６０
【００２７】
その際、ｍ＋ｎが４未満で、且つｍ：ｎが１．５未満：１あると、表面被覆の際、良好な重合結合能は得られるが、十分な表面被覆能が得られないので望ましくない。ｍ＋ｎが１５〜６０であっても、ｍ：ｍが１．５未満：１であると、十分な表面被覆能は得られるが、重合結合能が不十分となるので好ましくない。
一方、ｍ＋ｎが６０を超えると、重合結合能が不十分となり、且つ十分な表面被覆能が得られなくなるので好ましくない。
【００２８】
メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）としては、好ましくは、ｍ：ｎが３．５〜１．５：１で、且つｍ＋ｎが５〜５５、さらに好ましくは、ｍ：ｎが３．５〜２．０：１で、且つｍ＋ｎが５〜５０であるものが好適に使用される。
【００２９】
本発明で使用されるメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）は、例えば、ヘキサメチルジシロキサン等の低分子量シロキサン化合物、オクタメチルシクロテトラシロキサン等の環状ジメチルシロキサン化合物、ポリメチルハイドロジェンシロキサンあるいはテトラメチルテトラハイドロジェンシクロテトラシロキサン等のメチルハイドロジェンシロキサン化合物を原料とし、触媒として硫酸、塩酸、リン酸、活性白土、塩化鉄、ホウ酸、トリフルオロ酢酸等の酸触媒を用いた平衡反応などの公知の方法で調製することができる。
【００３０】
メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）の使用量は、酸化亜鉛粉体（Ａ）に対して２〜１０重量％、好ましくは４〜８重量％であることが望ましい。
【００３１】
３．被覆酸化亜鉛粉体の製法
本発明の製造方法は、前述の酸化亜鉛粉体（Ａ）とハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）とを溶媒の存在下又は非存在下に混合し、表面被覆された酸化亜鉛粉体を得る第１の工程と、引き続いて、該表面被覆された酸化亜鉛粉体を５０〜２００℃で０．５〜５時間加熱処理する第２の工程とからなる。
【００３２】
本発明の第１の工程において、表面被覆とは、酸化亜鉛粉体（Ａ）の表面を、メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）で被覆することを意味し、メチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）の被覆量として、酸化亜鉛粉体（Ａ）に対して２〜１０重量％、好ましくは４〜８重量％であることが望ましい。
【００３３】
本発明の第１の工程は、上記の表面被覆を達成できるものであれば、特に限定されず、公知の方法を用いればよい。
【００３４】
具体的な表面被覆法としては、以下の混合方法を挙げることができる。
▲１▼酸化亜鉛粉体（Ａ）とメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）を、公知の混合装置で混合する。
▲２▼酸化亜鉛粉体（Ａ）と少量の溶剤に溶解させたメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）を、公知の混合装置で混合する。
▲３▼酸化亜鉛粉体（Ａ）と相当量の溶剤に溶解させたメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）を、公知の混合装置で混合し、スラリーを調製する。
▲４▼スプレードライヤー、エアーブレンダーを用いて、酸化亜鉛粉体（Ａ）をメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）で被覆する。
【００３５】
公知の混合装置としては、サンドグラインダーミル、タワーミル、アトライター、ボールミル、ホジャーサイトボールミル、振動式ボールミル、回転式ボールミル、振動式ロッドミル、振動式ミル、ポットミル、ロッドミル、パソミル、ヘンシェルミキサー、スーパーミキサー、オングミル、乳鉢、ハイブリダイザー等を挙げることができる。
【００３６】
第１の工程を溶剤の存在下で行う場合には、溶剤としては、留去効率の点から低沸点のものが好ましく、具体的には、トルエン、ジクロロメタン、ｎ−へキサン、シクロヘキサン、石油エーテル、アセトン、イソプロピルアルコール、メチルエチルケトン、ヘプタン等を挙げることができる。
【００３７】
本発明の第２の工程では、前述の第１の工程に引き続き、酸化亜鉛粉体（Ａ）に表面被覆したメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（Ｂ）同士の重合や、さらには酸化亜鉛粉体（Ａ）との結合反応を起こさせるために、加熱処理が行われる。その際、加熱処理条件としては、５０〜２００℃で０．５〜５時間、好ましくは７０〜１５０℃で１〜４時間が望ましい。
加熱装置としては、送風乾燥機、真空乾燥機、スプレードライヤー、エバポレーター等を挙げることができるが、溶剤を使用した場合にあっては、真空乾燥機が好ましい。また、２回以上に分けて加熱処理を行ってもよい。
【００３８】
第１の工程で溶剤を使用した場合には、加熱後、これを減圧留去し、留去後さらに必要ならば、１００℃で１時間程度加熱処理をし、冷却後常圧に戻し、ハンマーミル等で粉砕し、目的とする被覆酸化亜鉛粉体が調製される。
これらの中で、溶剤を用いてスラリーを調製し、７０〜１５０℃で１〜４時間加熱処理し、溶剤留去後粉砕機で粉砕する表面被覆法が好ましい。
【００３９】
４．被覆酸化亜鉛粉体
上記のようにして得られた本発明の被覆酸化亜鉛粉体は、従来のものと比べて、表面被覆が高度に重合結合しており、またより優れた表面被覆をしているので、優れた二次凝集防止性、撥水性、撥油性を持つとともに、残存ＳｉＨ基がより少なく、また、よく全体に被覆されているので、酸化亜鉛粉体の持つ皮脂を固定する効果をより持続あるものとするばかりでなく、酸化亜鉛粉体及びこれを含む化粧料の増粘や容器の破壊がなく、優れた安定性を持ち、非常に有用なものである。
【００４０】
５．化粧料
本発明の化粧料は、前述の被覆酸化亜鉛粉体に、必要に応じて通常化粧料に添加される他の公知の原料を配合して調製されるが、溶液状、乳液状、クリーム状、油状、油状固形状、粉状など所望の剤型にすることができる。
化粧料としては、化粧水、スキンケア乳液、サンスクリーン乳液、パウダーファンデーション、粉白粉、頬紅、化粧下地クリーム等を例示できる。
【００４１】
なお、本発明の化粧料には、本発明の特徴を損なわない範囲で、以下に述べる通常化粧料の配合剤として使用される、例えば、有機変性粘土鉱物、抗菌防腐剤、酸化防止剤、紫外線吸収剤、有機酸、ビタミン類、無機塩類、香料、金属イオン封鎖剤、抗炎症剤、収斂剤、清涼化剤、鎮痒剤、顔料などの原料を添加してもよい。
【００４２】
有機変性粘土鉱物としては、モンモリロナイト、サポナイト、ヘクトライト等の天然または合成のモンモリロナイト群（市販品ではビーガム、クニピア、ラポナイトなどがある）、ナトリウムシリシックマイカやナトリウムまたはリチウムテニオライトの名で知られる合成雲母（市販品ではダイモナイト トピー工業（株）製等がある）等の粘土鉱物をドデシルトリメチルアンモニウムクロリド、ミリスチルトリメチルアンモニウムクロリド、ステアリルトリメチルアンモニウムクロリド等の第四級アンモニウム塩型カチオン界面活性剤で処理して得られるもの等が挙げられる。この際、非イオン性界面活性剤を併用してもよい。
【００４３】
抗菌防腐剤としては、パラオキシ安息香酸アルキルエステル（エチルパラペン、ブチルパラペン等）、安息香酸、サリチル酸、ソルビン酸、石炭酸、デヒドロ酢酸及びその塩類、パラクロロメタクレゾール、ホウ酸、ヘキサクロロフェン、トリブロムサラン、イソプロピルメチルフェノール、オルトフェニルフェノール、塩化ベンザルコニウム、塩酸クロルヘキシジン、臭化アルキルイソキノリニウム、トリクロロカルバニリド、ハロカルバン、チラム、フェノキシエタノール、トリクロサン等が挙げられる。
【００４４】
酸化防止剤としては、トコフェノール、フィチン酸、ブチルヒドロキシトルエン等が挙げられる。
【００４５】
紫外線吸収剤としては、オクチルシンナメート、２，４−ジヒドロキシベンゾフェノン、パラアミノ安息香酸、ホモメチル−７Ｎ−アセチルアラントイラニレート、ブチルメトキシベンゾイルメタン、ジ−パラメトキシケイヒ酸−モノ−２−エチルヘキサン酸グリセリル、アミルサリシレート等が挙げられる。
【００４６】
有機酸としては、乳酸、酒石酸、リンゴ酸、クエン酸、グルタチオン、アルコサルコシン酸、ラウロイルコシンナトリウム等が挙げられる。
【００４７】
ビタミン類としては、ビタミンＡ及びその誘導体、ビタミンＢ６塩酸塩、ビタミンＢ６トリパルミテート、ビタミンＢ６ジオクタノエート、ビタミンＢ２及びその誘導体、ビタミンＢ１２、ビタミンＢ１５及びその誘導体等のビタミンＢ類、アスコルビン酸、アスコルビン酸硫酸エステル（塩）、アスコルビン酸リン酸エステル、アスコルビン酸ジパルミテート等のビタミンＣ類、α−トコフェロール、β−トコフェロール、γ−トコフェロール、ビタミンＥ−アセテート、ビタミンＥ−ニコチネート等のビタミンＥ類、ビタミンＤ類、ビタミンＨ類、パントテン酸、パントテチン等が挙げられる。
【００４８】
無機塩類としては、硫酸ナトリウム、硫酸ナトリウム、硫酸マグネシウム、硫酸カリウム、硝酸ナトリウム、硝酸アルミニウム、硝酸カリウム、硝酸マグネシウム、塩化マグネシウム、塩化カリウム、塩化ナトリウム、塩化アルミニウム等があげられ、油中水型エマルジョン組成物に配合する場合は、０．１〜３．０重量％、好ましくは０．５〜２．０重量％配合する。
【００４９】
香料としては、バラ油、ジャスミン油、ラベンダー油、ペパーミント油、ゼラニウム油、シンナモン油、オレンジ油、ムスク油等の天然香料、リモネン、β−カリオフィレン、シス−３−ヘキセノール、リナロール、β−フェニルエチルアルコール、２，６−ノナジエナール、シトラール、α−ヘキシルシンナシックアルデヒド、β−イオノン、シクロペンタデカノン、リナリルアセテート、ベンジルベンゾエート、γ−ウンデカラクトン、オイゲノール、ローズオキサイド、インドール、フェニルアセトアルデヒド、オーランチオール、ゲラニオール、シトロネロール、タービネオール、サンタロール、リラール、リリアール、ダマスコン、メチルイオノン、アセチルセドレン、ムスコン、ベンジルアセテート、メチルジヒドロジャスモネート、メチルジャスモネート、ジャスミンラクトン、シクロペンタデカノリット等の合成香料が挙げられる。
【００５０】
金属イオン封鎖剤としては、エチレンジアミン四酢酸ナトリウム塩、リン酸、クエン酸、アスコルピン酸、コハク酸、グルコン酸、ポリリン酸ナトリウム、メタリン酸ナトリウム等が挙げられる。
【００５１】
抗炎症剤としては、β−グリチルレチン酸、アラントイン、アズレン、ε−アミノカプロン酸、ヒドロコーチゾン（Ｖ）、酢酸ヒドロコーチゾン、プレドニゾロン等が挙げられる。
【００５２】
収斂剤としては、硫酸亜鉛、アラントインヒドロキシアルミニウム、塩化アルミニウム、硫酸アルミニウム、スルホ石炭酸亜鉛、タンニン酸、クエン酸等が挙げられる。
【００５３】
清涼化剤としては、メントール、カンフル等が挙げられる。
【００５４】
鎮痒剤としては、塩酸ジフェニルヒドラミン、マレイン酸クロルフェラミン、カンファー、メントール等が挙げられる。
【００５５】
顔料としては、ベンガラ、黄酸化鉄、黒酸化鉄、グンジョウ、コンジョウ、酸化クロム等の無機顔料、タール色素、コチニール、カーサシン、β−カロチン等の有機顔料、酸化チタン、酸化亜鉛等の白色顔料、タルク、マイカ、セリサイト、カオリン、硫酸バリウム、無水ケイ酸、炭酸カルシウム、ケイ酸マグネシウム等の体質顔料、雲母チタン、魚鱗箔、オキシ塩化ビスマス等のパール顔料、ナイロンパウダー、ポリエチレン末等の高分子粉末等が挙げられる。
【００５６】
【実施例】
次に実施例に基づいて本発明をさら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、本実施例、比較例中で用いられたメチルハイドロジェンシロキサン−ジメチルシロキサン共重合体（以下、単に「共重合体」と略称する。）及び評価法は、それぞれ以下の方法によるものである。
【００５７】
１．メチルハイドロジェン・ジメチルシロキサン共重合体の製造
１−１．共重合体（１）の製造
ヘキサメチルジシロキサン４１重量部、オクタメチルシクロテトラシロキサン７３８重量部、ポリメチルハイドロジェンシロキサン（平均重合度３７）２２２重量部、および濃硫酸２５重量部を室温で５時間攪拌して平衡反応を行った。その後、重曹１２５重量部を加えて硫酸を中和し、更に５時間攪拌を続けた。加圧濾過器で重曹を濾別し、共重合体（１）を得た。得られた共重合体（１）は、前述の一般式（１）における繰り返し単位数はｍが２９、ｎが１０であった。
【００５８】
１−２．共重合体（２）〜（８）の製造
ヘキサメチルジシロキサン、オクタメチルシクロテトラシロキサン、およびポリメチルハイドロジェンシロキサンの重量部数を変更して、共重合体（１）と同様な製造法で、共重合体（２）〜（８）を製造した。
なお、共重合体（１）〜（８）の繰返し単位数、ｍ：ｎ、ｍ＋ｎをまとめて表１に示す。
【００５９】
【表１】
２．評価法
２−１．重合結合能
上記で製造された共重合体を使用して得られた被覆酸化亜鉛粉体１００ｇを水：水酸化カリウム：エタノール＝３：２：２からなる検出液に投入し、発生した水素ガスの体積を湿式ガスメーターにより測定し、温度、圧力を標準状態に換算することにより、該粉体中に含まれる未反応のＳｉＨ基を定量した。処理前の共重合体中の総ＳｉＨ基を１００％と換算し、これから未反応のＳｉＨ定量値を百分率で表示し、これを１００％から差し引いた百分率の数値を重合結合能として評価した。重合結合能は、９５％以上を合格とした。
【００６１】
２−２．表面被覆能
得られた被覆酸化亜鉛粉体１５重量％、水２０重量％、１，３−ブチレングリコール１０重量％、デカメチルシクロペンタシロキサン（ＶＳ−７１５８、日本ユニカー品）５０重量％、及びポリエーテル変性ポリジメチルシロキサン（ＦＺ−２１９１、日本ユニカー品、粘度１２００ｃＳｔ、ＨＬＢ＝５）５重量％をホモジナイザーに投入し、３０００ｒｐｍで１０分間攪拌混合し、Ｗ／Ｏエマルジョンを得た。これをＢ型粘度計で、温度２５℃、回転数６０ｒｐｍ及び６ｒｐｍで粘度を測定した。
粘度は、このＷ／Ｏエマルジョンの場合、６０ｒｐｍにおいて４００ｍＰａｓ以下を合格とした。
【００６２】
実施例１
５重量部の共重合体（１）および１００重量部のトルエンをボールミルで混合し、１００重量部の酸化亜鉛粉体（テイカ品、ＭＺ−５００、平均一次粒子径０．０２〜０．０３μｍ、比表面積４５ｍ２／ｇ）をさらに投入し、５分間混合してスラリーを調製した。処理後のスラリーをニーダーに投入して減圧加熱し、温度を徐々に上げて１００℃に到達してから３時間加熱攪拌を行った。次いで、１５０ｔｏｒｒに減圧し、約１時間維持してトルエンを留去した。その後さらに１２０℃で１時間加熱し、冷却後得られた粗被覆酸化亜鉛粉体をハンマーミルで粉砕して、被覆酸化亜鉛粉体を得た。
得られた被覆酸化亜鉛粉体について、その重合結合能及び表面被覆能を評価した。評価結果は、表２に示した。
重合結合能は９６％、表面被覆能は６０ｒｐｍの粘度で２３０ｍＰａｓ、６ｒｐｍの粘度で３００ｒｐｍを示し、すぐれた表面被覆皮膜が形成されていることが確認された。
【００６３】
実施例２、比較例１〜６
実施例２では、共重合体（２）を用い、一方、比較例１〜６では、共重合体（３）〜（８）を用いて実施例１と同様の試験を行ない、同様に評価した。結果は、表２に示した。
実施例２は、実施例１と同様の優れた表面被覆被膜が確認されたが、比較例１、２では、表面被覆能が不十分であり、比較例３では重合結合能及び表面被覆能が不十分であり、比較例４では、重合結合能が不十分であった。さらに、比較例５では、重合結合能及び表面被覆能が不十分であり、比較例６では、重合結合能が不十分であった。結局、比較例１〜６では、いずれも実施例１、２のように重合結合能及び表面被覆能の両方を満たすものはなかった。
【００６４】
【表２】
実施例３
精製水７０重量％、エタノール１５重量％、およびグリセリン１０重量％を攪拌混合し、さらに実施例１で得られた被覆酸化亜鉛粉体５重量％を攪拌混合して、モデル化粧水を調製した。この粘度を２５℃、６ｒｐｍの条件でＢ型粘度計で測定した。一方、これを３００ｍｌのポリエチレン製密閉容器に入れ、５０℃で１週間保存後、同様に粘度を測定したところ、粘度変化は有意に観測されなかった。また、容器の膨張も認められず、安定な化粧水であった。
【００６６】
比較例７
被覆酸化亜鉛粉体を比較例１で得られたものに変更した以外は、実施例３と同様に試験した。これを３００ｍｌのポリエチレン製密閉容器に入れ、５０℃で１週間保存した後、室温に冷却しても密閉容器に膨れがみとめられ、また有意な粘度上昇が確認された。
【００６７】
【発明の効果】
以上詳細に説明したように、本発明の被覆酸化亜鉛粉体は、重合結合能及び表面被覆能の両方に優れた特定のハイドロジェンシロキサン−ジメチルシロキサン共重合体で表面被覆されているので、優れた二次凝集防止性、撥水性、撥油性を持つとともに、残存ＳｉＨ基がより少なく、また、未被覆部分も実質的にないので、酸化亜鉛粉体の持つ皮脂を固定する効果をより持続あるものとする安定化効果を有する。従って、これを含む本発明の化粧料は、例え液状形状であっても、増粘や容器の破壊の懸念がなく、化粧料としても優れた持続効果を持ち、安定性をもつ。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a coated zinc oxide powder, a method for producing the same, and a cosmetic using the coated zinc oxide powder. More specifically, the surface coating process of the zinc oxide powder is efficient, and when it is formulated as a cosmetic, There is no concern about the gelation and viscosity increase of cosmetics containing zinc oxide powder by uncoated parts, and it is stable, and the durability of makeup with excellent sebum resistance that zinc oxide powder itself has has been improved. The present invention relates to a coated zinc oxide powder capable of producing a cosmetic, a production method thereof, and a cosmetic comprising the same.
[0002]
[Prior art]
Conventionally, many powders blended in cosmetics have been surface-coated with a methylhydrogensiloxane-dimethylsiloxane copolymer in order to prevent secondary aggregation and impart water repellency and oil repellency.
At that time, the zinc oxide powder used as a powder reacts with the sebum of the face to gel and fix the sebum, suppresses the spread of the sebum, suppresses the greasy, and improves the sustainability of the makeup It is useful for.
[0003]
Generally speaking, the methylhydrogensiloxane-dimethylsiloxane copolymer has a structure represented by the following general formula (2).
[0004]
[Chemical formula 2]
When such a methylhydrogensiloxane-dimethylsiloxane copolymer is coated on the surface of the zinc oxide powder and then heat-treated, a reaction represented by the following formula (3) occurs and is polymerized on the surface of the zinc oxide. Alternatively, the reaction represented by the formula (4) is combined with a hydroxyl group present on the surface of zinc oxide to form a coating film, while preventing secondary aggregation and imparting water repellency and oil repellency, and having sebum resistance. It is known to enhance.
[0006]
[Chemical 3]
[Formula 4]
For example, JP-A-8-41379 discloses a sebum-resistant powder obtained by coating a surface of zinc oxide powder having a specific specific surface area with a methylhydrogensiloxane / dimethylsiloxane copolymer having a specific number of repeating units. ing.
[0009]
However, in the methylhydrogensiloxane-dimethylsiloxane copolymer having a specific number of repeating units described in the same publication, the bond with the zinc oxide powder is insufficient, or it has not been blended in cosmetics. There is a problem that hydrogen is generated from the SiH group of the reaction, which may cause a risk of deformation or destruction of the container when the coated zinc oxide powder is stored or in the final product cosmetic.
[0010]
Another problem is that zinc oxide powder is active against other components of cosmetics, and is known to cause chemical bonding. If it is not completely surface-coated, it will gel the cosmetics. In some cases, the cosmetic is less affected when the cosmetic is in a solid form such as a foundation, but when the cosmetic is in a liquid form such as a lotion, the viscosity increases, which may cause a serious problem.
[0011]
Under these circumstances, the surface coating process of zinc oxide powder is efficient, and when it is formulated as cosmetics, the gelation and viscosity increase of cosmetics formulated with zinc oxide powder due to the generation of hydrogen and non-surface coated parts. There has been a need for research and development of coated zinc oxide powder that can produce cosmetics that are stable, stable, and have excellent makeup resistance with excellent sebum resistance that the zinc oxide powder itself has.
[0012]
[Problems to be solved by the invention]
In view of the problems of the prior art, the problem of the present invention is that when the surface of the zinc oxide powder is coated with a merhydrogensiloxane-dimethylsiloxane copolymer, higher polymerization and bonding strength with zinc oxide (hereinafter, This is simply referred to as “polymerization binding ability”), and the surface of the zinc oxide powder is more fully surface-coated (hereinafter simply referred to as “surface coverage ability”), and as a result, zinc oxide The efficiency of the powder surface coating process is stable, and when formulated as a cosmetic, there is no concern about hydrogen generation or gelation or viscosity increase of the cosmetic containing zinc oxide powder due to the uncoated surface. Furthermore, the object is to provide a coated zinc oxide powder capable of producing a cosmetic with excellent sebum resistance and improved cosmetic durability, and a method for producing the same, and a cosmetic using the same. .
[0013]
[Means for Solving the Problems]
As a result of intensive studies to solve the above-mentioned problems, the present inventors have studied various methylhydrogensiloxane-dimethylsiloxane copolymers. As a result, the number of repeating units of a specific methylhydrogensiloxane (n) And a copolymer having a repeating unit of dimethylsiloxane (m), and surface-coating it on zinc oxide powder having a specific surface area, it has high polymerization bonding ability and more sufficient surface covering ability The present inventors have found that the above-mentioned problems can be achieved by obtaining a coated zinc oxide powder having the following characteristics.
[0014]
That is, according to the first aspect of the present invention, the surface of the zinc oxide powder (A) having a specific surface area of 15 to 100 m 2 / g is treated with methylhydrogensiloxane-dimethyl represented by the following chemical formula (1). A coated zinc oxide powder characterized by coating with a siloxane copolymer (B) is provided.
[0015]
[Chemical formula 5]
[0016]
According to the second invention of the present invention, the coated zinc oxide according to the first invention, wherein the zinc oxide powder (A) has an average primary particle diameter of 0.01 to 0.1 μm. Powder is provided.
[0017]
Furthermore, according to the third aspect of the present invention, in the first or second aspect, the coating amount of the methylhydrogensiloxane-dimethylsiloxane copolymer (B) is 2 with respect to the zinc oxide powder (A). A coated zinc oxide powder characterized in that it is 10 to 10% by weight is provided.
[0018]
On the other hand, according to the fourth aspect of the present invention, the zinc oxide powder (A) and the hydrogensiloxane-dimethylsiloxane copolymer (B) are mixed in the presence or absence of a solvent, and the surface coating is performed. A first step of obtaining a zinc oxide powder and a second step of subsequently heat-treating the surface-coated zinc oxide powder at 50 to 200 ° C. for 0.5 to 5 hours. A method for producing a coated zinc oxide powder according to any one of the first to third inventions is provided.
[0019]
Moreover, according to 5th invention of this invention, the cosmetics characterized by mix | blending the covering zinc oxide powder as described in any one of 1st-3rd invention are provided.
[0020]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the coated zinc oxide powder of the present invention, its production method, and a cosmetic obtained by blending it will be described in detail for each item.
[0021]
1. Zinc oxide powder (A)
The zinc oxide powder (A) used in the present invention has a specific surface area of 15 to 100 m 2 / g, preferably 20 to 100 m 2 / g.
When the specific surface area is less than 15 m 2 / g, the ability to gel and fix sebum is inferior. On the other hand, when the specific surface area exceeds 100 m 2 / g, the surface activity of the powder increases, secondary agglomeration occurs, and it is uniform. It is difficult to obtain a stable surface coating, and it is difficult to produce a stable coated zinc oxide powder.
[0022]
Moreover, the average primary particle diameter of the zinc oxide powder (A) is not particularly limited, but is usually 0.01 to 0.1 μm, preferably about 0.015 to 0.05 μm.
When the average primary particle size is less than 0.01 μm, the surface activity of the powder becomes high and secondary agglomeration occurs. On the other hand, when the average primary particle size exceeds 0.1 μm, the ability to gel and fix sebum is inferior, and the cosmetic surface is smooth. Unsatisfactory due to poor properties
[0023]
As the commercially available zinc oxide powder (A) used in the present invention, for example, MZ-300, MZ-500, MZ-700 manufactured by Teika, and FINEX25, FINEX50, FINEX75, FINEX90 manufactured by Sakai Chemical Co., Ltd. are preferable. Can be used for
[0024]
2. Methylhydrogensiloxane-dimethylsiloxane copolymer (B)
The methylhydrogensiloxane-dimethylsiloxane copolymer (B) used in the present invention is represented by the following general formula (1).
[0025]
[Chemical 6]
Here, m and n are positive numbers and satisfy the following requirements (a) and (b).
A. m: n = 4.0 to 1.5: 1
B. m + n = 4-60
[0027]
At that time, when m + n is less than 4 and m: n is less than 1.5: 1, a good polymerization bonding ability can be obtained during surface coating, but it is not desirable because sufficient surface covering ability cannot be obtained. . Even if m + n is 15 to 60, if m: m is less than 1.5, sufficient surface covering ability can be obtained, but the polymerization bonding ability becomes insufficient.
On the other hand, when m + n exceeds 60, the polymerization bonding ability becomes insufficient, and a sufficient surface covering ability cannot be obtained.
[0028]
The methylhydrogensiloxane-dimethylsiloxane copolymer (B) is preferably m: n of 3.5 to 1.5: 1 and m + n of 5 to 55, more preferably m: n of 3. One having a thickness of 5 to 2.0: 1 and m + n of 5 to 50 is preferably used.
[0029]
Examples of the methylhydrogensiloxane-dimethylsiloxane copolymer (B) used in the present invention include low molecular weight siloxane compounds such as hexamethyldisiloxane, cyclic dimethylsiloxane compounds such as octamethylcyclotetrasiloxane, and polymethylhydrogen. Equilibrium using methylhydrogensiloxane compounds such as siloxane or tetramethyltetrahydrogencyclotetrasiloxane as raw materials and using an acid catalyst such as sulfuric acid, hydrochloric acid, phosphoric acid, activated clay, iron chloride, boric acid, trifluoroacetic acid as a catalyst It can be prepared by a known method such as reaction.
[0030]
The amount of the methylhydrogensiloxane-dimethylsiloxane copolymer (B) used is 2 to 10% by weight, preferably 4 to 8% by weight, based on the zinc oxide powder (A).
[0031]
3. Production method of coated zinc oxide powder The production method of the present invention comprises mixing the aforementioned zinc oxide powder (A) and hydrogensiloxane-dimethylsiloxane copolymer (B) in the presence or absence of a solvent, It consists of a first step of obtaining a surface-coated zinc oxide powder and a second step of subsequently heat-treating the surface-coated zinc oxide powder at 50 to 200 ° C. for 0.5 to 5 hours. .
[0032]
In the first step of the present invention, the surface coating means that the surface of the zinc oxide powder (A) is coated with a methyl hydrogen siloxane-dimethyl siloxane copolymer (B), and methyl hydrogen siloxane. -The coating amount of the dimethylsiloxane copolymer (B) is 2 to 10% by weight, preferably 4 to 8% by weight, based on the zinc oxide powder (A).
[0033]
The first step of the present invention is not particularly limited as long as the above surface coating can be achieved, and a known method may be used.
[0034]
Specific surface coating methods include the following mixing methods.
(1) The zinc oxide powder (A) and the methylhydrogensiloxane-dimethylsiloxane copolymer (B) are mixed with a known mixing device.
(2) The zinc oxide powder (A) and the methylhydrogensiloxane-dimethylsiloxane copolymer (B) dissolved in a small amount of solvent are mixed with a known mixing apparatus.
(3) Zinc oxide powder (A) and methylhydrogensiloxane-dimethylsiloxane copolymer (B) dissolved in an appropriate amount of solvent are mixed with a known mixing device to prepare a slurry.
(4) The zinc oxide powder (A) is coated with the methylhydrogensiloxane-dimethylsiloxane copolymer (B) using a spray dryer and an air blender.
[0035]
Known mixers include sand grinder mills, tower mills, attritors, ball mills, hoger sight ball mills, vibratory ball mills, rotary ball mills, vibratory rod mills, vibratory mills, pot mills, rod mills, paso mills, Henschel mixers, super mixers, An ang mill, a mortar, a hybridizer, etc. can be mentioned.
[0036]
When the first step is performed in the presence of a solvent, the solvent preferably has a low boiling point from the viewpoint of distillation efficiency. Specifically, toluene, dichloromethane, n-hexane, cyclohexane, petroleum ether , Acetone, isopropyl alcohol, methyl ethyl ketone, heptane and the like.
[0037]
In the second step of the present invention, subsequent to the first step described above, polymerization of the methylhydrogensiloxane-dimethylsiloxane copolymer (B) surface-coated on the zinc oxide powder (A), and further oxidation Heat treatment is performed to cause a binding reaction with the zinc powder (A). In that case, as heat processing conditions, it is 0.5 to 5 hours at 50-200 degreeC, Preferably it is 1-4 hours at 70-150 degreeC.
Examples of the heating device include a blower dryer, a vacuum dryer, a spray dryer, and an evaporator. When a solvent is used, a vacuum dryer is preferable. Further, the heat treatment may be performed in two or more times.
[0038]
When a solvent is used in the first step, after heating, the solvent is distilled off under reduced pressure. After the distillation, if necessary, heat treatment is performed at 100 ° C. for about 1 hour, and after cooling, the pressure is returned to normal pressure. The desired coated zinc oxide powder is prepared by grinding with a mill or the like.
Among these, a surface coating method is preferred in which a slurry is prepared using a solvent, heat-treated at 70 to 150 ° C. for 1 to 4 hours, and pulverized with a pulverizer after the solvent is distilled off.
[0039]
4). Coated zinc oxide powder The coated zinc oxide powder of the present invention obtained as described above has a surface coating that is highly polymerized and has a superior surface coating compared to the conventional one. As a result, it has excellent secondary aggregation prevention, water repellency, oil repellency, fewer residual SiH groups, and is well coated throughout, so it has the effect of fixing the sebum of zinc oxide powder. In addition to making it more durable, there is no thickening of zinc oxide powder and cosmetics containing it and destruction of containers, and it has excellent stability and is very useful.
[0040]
5. Cosmetics The cosmetics of the present invention are prepared by blending the above-described coated zinc oxide powder with other known raw materials that are usually added to cosmetics as necessary. , Oily, oily solid, powder, etc.
Examples of cosmetics include skin lotion, skin care emulsion, sunscreen emulsion, powder foundation, powdered white powder, blusher, makeup base cream and the like.
[0041]
In addition, the cosmetics of the present invention are used as a usual cosmetic compounding agent described below, as long as the characteristics of the present invention are not impaired. For example, organically modified clay minerals, antibacterial preservatives, antioxidants, ultraviolet rays You may add raw materials, such as an absorber, organic acid, vitamins, inorganic salts, a fragrance | flavor, a sequestering agent, an anti-inflammatory agent, an astringent agent, a refreshing agent, an antipruritic agent, and a pigment.
[0042]
Organically modified clay minerals are known as natural or synthetic montmorillonite groups such as montmorillonite, saponite and hectorite (commercially available products include bee gum, kunipia and laponite), sodium silicic mica and sodium or lithium teniolite. Treating clay minerals such as synthetic mica (commercially available from Daimonite Topy Industries, Ltd.) with quaternary ammonium salt type cationic surfactants such as dodecyltrimethylammonium chloride, myristyltrimethylammonium chloride, stearyltrimethylammonium chloride Can be obtained. At this time, a nonionic surfactant may be used in combination.
[0043]
Antibacterial preservatives include paraoxybenzoic acid alkyl esters (ethyl parapen, butyl parapen, etc.), benzoic acid, salicylic acid, sorbic acid, carboxylic acid, dehydroacetic acid and its salts, parachlorometacresol, boric acid, hexachlorophene, tribromosaran , Isopropylmethylphenol, orthophenylphenol, benzalkonium chloride, chlorhexidine hydrochloride, alkylisoquinolinium bromide, trichlorocarbanilide, halocarban, thiram, phenoxyethanol, triclosan and the like.
[0044]
Examples of the antioxidant include tocophenol, phytic acid, butylhydroxytoluene and the like.
[0045]
Examples of ultraviolet absorbers include octyl cinnamate, 2,4-dihydroxybenzophenone, paraaminobenzoic acid, homomethyl-7N-acetyl allanilanilate, butylmethoxybenzoylmethane, di-paramethoxycinnamic acid-mono-2-ethylhexanoic acid Examples thereof include glyceryl and amyl salicylate.
[0046]
Examples of the organic acid include lactic acid, tartaric acid, malic acid, citric acid, glutathione, arcosarcosic acid, and lauroylcosin sodium.
[0047]
Vitamins such as vitamin A and its derivatives, vitamin B 6 hydrochloride, vitamin B 6 tripalmitate, vitamin B 6 dioctanoate, vitamin B 2 and its derivatives, vitamin B 12 , vitamin B 15 and its derivatives, etc. , Ascorbic acid, ascorbic acid sulfate (salt), vitamin C such as ascorbic acid phosphate, ascorbic acid dipalmitate, α-tocopherol, β-tocopherol, γ-tocopherol, vitamin E-acetate, vitamin E-nicotinate, etc. Vitamin E, vitamin D, vitamin H, pantothenic acid, pantothetin and the like.
[0048]
Examples of inorganic salts include sodium sulfate, sodium sulfate, magnesium sulfate, potassium sulfate, sodium nitrate, aluminum nitrate, potassium nitrate, magnesium nitrate, magnesium chloride, potassium chloride, sodium chloride, and aluminum chloride. Water-in-oil emulsion composition When blended into a product, it is blended in an amount of 0.1 to 3.0% by weight, preferably 0.5 to 2.0% by weight.
[0049]
As perfumes, natural perfumes such as rose oil, jasmine oil, lavender oil, peppermint oil, geranium oil, cinnamon oil, orange oil, musk oil, limonene, β-caryophyllene, cis-3-hexenol, linalool, β-phenylethyl Alcohol, 2,6-nonadienal, citral, α-hexylcinnasic aldehyde, β-ionone, cyclopentadecanone, linalyl acetate, benzyl benzoate, γ-undecalactone, eugenol, rose oxide, indole, phenylacetaldehyde, auranchi All, Geraniol, Citronellol, Turbineol, Santalol, Lilal, Lilianar, Damascon, Methylionone, Acetyl Cedrene, Muscone, Benzyl Acetate, Methyldihydrojasmonate And synthetic fragrances such as methyl jasmonate, jasmine lactone, and cyclopentadecanolite.
[0050]
Examples of the sequestering agent include sodium ethylenediaminetetraacetate, phosphoric acid, citric acid, ascorbic acid, succinic acid, gluconic acid, sodium polyphosphate, sodium metaphosphate, and the like.
[0051]
Examples of anti-inflammatory agents include β-glycyrrhetinic acid, allantoin, azulene, ε-aminocaproic acid, hydrocortisone (V), hydrocortisone acetate, prednisolone, and the like.
[0052]
Examples of the astringent include zinc sulfate, allantoin hydroxyaluminum, aluminum chloride, aluminum sulfate, zinc sulfocolate, tannic acid, citric acid and the like.
[0053]
Examples of the refreshing agent include menthol and camphor.
[0054]
Examples of the antipruritic agent include diphenylhydramine hydrochloride, chlorferamine maleate, camphor, and menthol.
[0055]
Examples of the pigment include inorganic pigments such as bengara, yellow iron oxide, black iron oxide, gunjo, kongyou, and chromium oxide, tar pigments, organic pigments such as cochineal, Casasin, β-carotene, white pigments such as titanium oxide and zinc oxide, Body pigments such as talc, mica, sericite, kaolin, barium sulfate, silicic anhydride, calcium carbonate, magnesium silicate, pearl pigments such as mica titanium, fish scale foil, bismuth oxychloride, polymers such as nylon powder and polyethylene powder A powder etc. are mentioned.
[0056]
【Example】
EXAMPLES Next, although this invention is demonstrated further in detail based on an Example, this invention is not limited to these Examples. The methylhydrogensiloxane-dimethylsiloxane copolymer (hereinafter simply referred to as “copolymer”) and the evaluation method used in the examples and comparative examples are based on the following methods, respectively. .
[0057]
1. 1. Production of methylhydrogen / dimethylsiloxane copolymer 1-1. Production of Copolymer (1) 41 parts by weight of hexamethyldisiloxane, 738 parts by weight of octamethylcyclotetrasiloxane, 222 parts by weight of polymethylhydrogensiloxane (average polymerization degree 37), and 25 parts by weight of concentrated sulfuric acid at room temperature The equilibration reaction was carried out with stirring for a period of time. Thereafter, 125 parts by weight of sodium bicarbonate was added to neutralize the sulfuric acid, and stirring was further continued for 5 hours. Sodium bicarbonate was filtered off with a pressure filter to obtain a copolymer (1). As for the obtained copolymer (1), m was 29 and n was 10 in the above-mentioned general formula (1).
[0058]
1-2. Production of copolymers (2) to (8) By changing the number of parts by weight of hexamethyldisiloxane, octamethylcyclotetrasiloxane, and polymethylhydrogensiloxane, the same production method as for copolymer (1), Copolymers (2) to (8) were produced.
The number of repeating units, m: n, and m + n of the copolymers (1) to (8) are collectively shown in Table 1.
[0059]
[Table 1]
2. Evaluation method 2-1. Polymer binding ability 100 g of coated zinc oxide powder obtained by using the above-produced copolymer is put into a detection solution consisting of water: potassium hydroxide: ethanol = 3: 2: 2, and hydrogen gas generated is generated. The unreacted SiH group contained in the powder was quantified by measuring the volume of the sample with a wet gas meter and converting the temperature and pressure to the standard state. The total SiH group in the copolymer before the treatment was converted to 100%, the unreacted SiH quantitative value was displayed as a percentage from this, and the numerical value of the percentage obtained by subtracting this from 100% was evaluated as the polymerization binding ability. The polymerization bonding ability was determined to be 95% or more.
[0061]
2-2. Surface covering ability 15% by weight of coated zinc oxide powder, 20% by weight of water, 10% by weight of 1,3-butylene glycol, 50% by weight of decamethylcyclopentasiloxane (VS-7158, Nippon Unicar), and poly 5% by weight of ether-modified polydimethylsiloxane (FZ-2191, Nippon Unicar Co., Ltd., viscosity 1200 cSt, HLB = 5) was added to a homogenizer and stirred and mixed at 3000 rpm for 10 minutes to obtain a W / O emulsion. This was measured with a B-type viscometer at a temperature of 25 ° C. and a rotation speed of 60 rpm and 6 rpm.
In the case of this W / O emulsion, the viscosity was determined to be 400 mPas or less at 60 rpm.
[0062]
Example 1
5 parts by weight of copolymer (1) and 100 parts by weight of toluene were mixed with a ball mill, and 100 parts by weight of zinc oxide powder (Taika product, MZ-500, average primary particle size 0.02 to 0.03 μm, A specific surface area of 45 m 2 / g) was further added and mixed for 5 minutes to prepare a slurry. The treated slurry was put into a kneader and heated under reduced pressure, and the temperature was gradually raised to reach 100 ° C., followed by stirring with heating for 3 hours. Subsequently, the pressure was reduced to 150 torr and maintained for about 1 hour to distill off toluene. Thereafter, it was further heated at 120 ° C. for 1 hour, and the coarsely coated zinc oxide powder obtained after cooling was pulverized with a hammer mill to obtain a coated zinc oxide powder.
The resulting coated zinc oxide powder was evaluated for its ability to bond to polymerization and surface coverage. The evaluation results are shown in Table 2.
The polymerization bonding ability was 96%, the surface covering ability was 230 mPas at a viscosity of 60 rpm, and 300 rpm at a viscosity of 6 rpm, and it was confirmed that an excellent surface coating film was formed.
[0063]
Example 2, Comparative Examples 1-6
In Example 2, the copolymer (2) was used, while in Comparative Examples 1 to 6, the same tests as in Example 1 were performed using the copolymers (3) to (8) and evaluated in the same manner. . The results are shown in Table 2.
In Example 2, the same excellent surface coating film as in Example 1 was confirmed. However, in Comparative Examples 1 and 2, the surface covering ability was insufficient, and in Comparative Example 3, the polymerization bonding ability and the surface covering ability were low. Insufficient, and in Comparative Example 4, the polymerization bonding ability was insufficient. Further, in Comparative Example 5, the polymerization bonding ability and the surface covering ability were insufficient, and in Comparative Example 6, the polymerization bonding ability was insufficient. As a result, none of Comparative Examples 1 to 6 satisfied both the polymerization bonding ability and the surface covering ability as in Examples 1 and 2.
[0064]
[Table 2]
Example 3
70% by weight of purified water, 15% by weight of ethanol, and 10% by weight of glycerin were stirred and mixed, and 5% by weight of the coated zinc oxide powder obtained in Example 1 was further stirred and mixed to prepare a model lotion. This viscosity was measured with a B-type viscometer at 25 ° C. and 6 rpm. On the other hand, when this was put into a 300 ml polyethylene sealed container and stored at 50 ° C. for 1 week, the viscosity was measured in the same manner, and no significant change in viscosity was observed. Further, no swelling of the container was observed and the skin lotion was stable.
[0066]
Comparative Example 7
The test was performed in the same manner as in Example 3 except that the coated zinc oxide powder was changed to that obtained in Comparative Example 1. This was placed in a 300 ml polyethylene sealed container and stored at 50 ° C. for 1 week. After cooling to room temperature, the sealed container swelled and a significant increase in viscosity was confirmed.
[0067]
【Effect of the invention】
As described above in detail, the coated zinc oxide powder of the present invention is surface-coated with a specific hydrogensiloxane-dimethylsiloxane copolymer that is excellent in both the polymer bonding ability and the surface covering ability. In addition, it has secondary aggregation prevention properties, water repellency, oil repellency, fewer residual SiH groups, and substantially no uncoated portion, so the effect of fixing the sebum of zinc oxide powder is more sustained. It has a stabilizing effect. Therefore, the cosmetics of the present invention including this have no fear of thickening or destruction of the container, even in a liquid form, and have an excellent sustaining effect and stability as a cosmetic.
Claims (5)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015005490A1 (en) | 2013-07-09 | 2015-01-15 | L'oreal | Long-wear cosmetic composition |
| WO2015005488A1 (en) | 2013-07-09 | 2015-01-15 | L'oreal | Long- wear cosmetic composition |
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| JP5239122B2 (en) * | 2006-03-03 | 2013-07-17 | 信越化学工業株式会社 | Organopolysiloxane powder treating agent, powder treated with the treating agent, and cosmetic containing the powder |
| KR101146067B1 (en) | 2009-08-24 | 2012-05-14 | 애경산업(주) | Inorganic powder for cosmetics and manufacturing method thereof and cosmetic composition containing thereof |
| JP5637514B2 (en) * | 2011-02-15 | 2014-12-10 | 住友金属鉱山シポレックス株式会社 | Lightweight cellular concrete |
| CN119326672B (en) * | 2024-12-23 | 2025-06-03 | 宁波御坊堂生物科技有限公司 | Preparation method and application of comfort-assisting composition |
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| JP3567335B2 (en) * | 1993-12-28 | 2004-09-22 | 三好化成株式会社 | Organosilicon compound-treated pigment or extender, method for producing the same and cosmetics |
| JP3942767B2 (en) * | 1999-04-06 | 2007-07-11 | 花王株式会社 | Ultraviolet shielding ultrafine particle dispersion |
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| WO2015005488A1 (en) | 2013-07-09 | 2015-01-15 | L'oreal | Long- wear cosmetic composition |
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