JP3495296B2 - Oil-based dispersion of titanium oxide, lipophilic titanium oxide powder, method for producing these, and cosmetics containing these - Google Patents
Oil-based dispersion of titanium oxide, lipophilic titanium oxide powder, method for producing these, and cosmetics containing theseInfo
- Publication number
- JP3495296B2 JP3495296B2 JP21007399A JP21007399A JP3495296B2 JP 3495296 B2 JP3495296 B2 JP 3495296B2 JP 21007399 A JP21007399 A JP 21007399A JP 21007399 A JP21007399 A JP 21007399A JP 3495296 B2 JP3495296 B2 JP 3495296B2
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- dispersion
- oily
- oil
- titanium
- 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 - Fee Related
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 100
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 95
- 239000006185 dispersion Substances 0.000 title claims description 50
- 239000002537 cosmetic Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000000843 powder Substances 0.000 title description 38
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 claims description 59
- -1 titanium alkoxide Chemical class 0.000 claims description 42
- 239000010936 titanium Substances 0.000 claims description 35
- 229910052719 titanium Inorganic materials 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000003921 oil Substances 0.000 claims description 25
- 235000019198 oils Nutrition 0.000 claims description 25
- 150000002894 organic compounds Chemical class 0.000 claims description 25
- 239000002904 solvent Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 17
- 239000004533 oil dispersion Substances 0.000 claims description 15
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 14
- 229960003540 oxyquinoline Drugs 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 239000010775 animal oil Substances 0.000 claims description 3
- 150000001735 carboxylic acids Chemical class 0.000 claims description 3
- 239000010696 ester oil Substances 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 241000894007 species Species 0.000 claims description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 3
- 239000008158 vegetable oil Substances 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N squalane Chemical compound CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 40
- 239000002253 acid Substances 0.000 description 29
- 239000002585 base Substances 0.000 description 26
- 239000000463 material Substances 0.000 description 24
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 description 20
- 229940032094 squalane Drugs 0.000 description 20
- 239000000203 mixture Substances 0.000 description 18
- 238000006460 hydrolysis reaction Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- 230000000694 effects Effects 0.000 description 15
- 230000007062 hydrolysis Effects 0.000 description 15
- 239000002245 particle Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 12
- 230000006750 UV protection Effects 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 9
- 239000002304 perfume Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 239000000049 pigment Substances 0.000 description 9
- 229920001296 polysiloxane Polymers 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 235000021355 Stearic acid Nutrition 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- 239000003112 inhibitor Substances 0.000 description 7
- 229940057995 liquid paraffin Drugs 0.000 description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 7
- 239000008117 stearic acid Substances 0.000 description 7
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 6
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 6
- 239000008213 purified water Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000003973 paint Substances 0.000 description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 239000001099 ammonium carbonate Substances 0.000 description 4
- 229940121375 antifungal agent Drugs 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 239000006071 cream Substances 0.000 description 4
- 239000002612 dispersion medium Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- 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 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 239000000454 talc Substances 0.000 description 4
- 229910052623 talc Inorganic materials 0.000 description 4
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 4
- 229940099259 vaseline Drugs 0.000 description 4
- 229940058015 1,3-butylene glycol Drugs 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 3
- ZAKOWWREFLAJOT-CEFNRUSXSA-N D-alpha-tocopherylacetate Chemical compound CC(=O)OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-CEFNRUSXSA-N 0.000 description 3
- 239000004166 Lanolin Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 235000012211 aluminium silicate Nutrition 0.000 description 3
- 230000000843 anti-fungal effect Effects 0.000 description 3
- 235000019437 butane-1,3-diol Nutrition 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 239000007863 gel particle Substances 0.000 description 3
- 229940075507 glyceryl monostearate Drugs 0.000 description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- 235000019388 lanolin Nutrition 0.000 description 3
- 229940039717 lanolin Drugs 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 239000006210 lotion Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 3
- 229940042585 tocopherol acetate Drugs 0.000 description 3
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 2
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 description 2
- OAOABCKPVCUNKO-UHFFFAOYSA-N 8-methyl Nonanoic acid Chemical compound CC(C)CCCCCCC(O)=O OAOABCKPVCUNKO-UHFFFAOYSA-N 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- 239000005695 Ammonium acetate Substances 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 235000019257 ammonium acetate Nutrition 0.000 description 2
- 229940043376 ammonium acetate Drugs 0.000 description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 2
- 235000012501 ammonium carbonate Nutrition 0.000 description 2
- 235000013871 bee wax Nutrition 0.000 description 2
- 239000012166 beeswax Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 229960000541 cetyl alcohol Drugs 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- YYVJAABUJYRQJO-UHFFFAOYSA-N isomyristic acid Chemical compound CC(C)CCCCCCCCCCC(O)=O YYVJAABUJYRQJO-UHFFFAOYSA-N 0.000 description 2
- XUGNVMKQXJXZCD-UHFFFAOYSA-N isopropyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC(C)C XUGNVMKQXJXZCD-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 239000004200 microcrystalline wax Substances 0.000 description 2
- 235000019808 microcrystalline wax Nutrition 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- 239000007764 o/w emulsion Substances 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 239000002674 ointment Substances 0.000 description 2
- 229960005235 piperonyl butoxide Drugs 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- XOJVVFBFDXDTEG-UHFFFAOYSA-N pristane Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- 239000000516 sunscreening agent Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- CUNWUEBNSZSNRX-RKGWDQTMSA-N (2r,3r,4r,5s)-hexane-1,2,3,4,5,6-hexol;(z)-octadec-9-enoic acid Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.CCCCCCCC\C=C/CCCCCCCC(O)=O.CCCCCCCC\C=C/CCCCCCCC(O)=O.CCCCCCCC\C=C/CCCCCCCC(O)=O CUNWUEBNSZSNRX-RKGWDQTMSA-N 0.000 description 1
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 description 1
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- UOFGSWVZMUXXIY-UHFFFAOYSA-N 1,5-Diphenyl-3-thiocarbazone Chemical compound C=1C=CC=CC=1N=NC(=S)NNC1=CC=CC=C1 UOFGSWVZMUXXIY-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 description 1
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 1
- ZONJATNKKGGVSU-UHFFFAOYSA-N 14-methylpentadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCC(O)=O ZONJATNKKGGVSU-UHFFFAOYSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-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
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- IEDKVDCIEARIIU-UHFFFAOYSA-N 2-Nonadecanone Chemical compound CCCCCCCCCCCCCCCCCC(C)=O IEDKVDCIEARIIU-UHFFFAOYSA-N 0.000 description 1
- UMHYVXGZRGOICM-AUYXYSRISA-N 2-[(z)-octadec-9-enoyl]oxypropyl (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(C)OC(=O)CCCCCCC\C=C/CCCCCCCC UMHYVXGZRGOICM-AUYXYSRISA-N 0.000 description 1
- GTAKOUPXIUWZIA-UHFFFAOYSA-N 2-[2-[2-(2-ethoxyethoxy)ethoxy]ethoxy]ethanol Chemical compound CCOCCOCCOCCOCCO GTAKOUPXIUWZIA-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- XULHFMYCBKQGEE-UHFFFAOYSA-N 2-hexyl-1-Decanol Chemical compound CCCCCCCCC(CO)CCCCCC XULHFMYCBKQGEE-UHFFFAOYSA-N 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、油性材料への分散
性に優れ、紫外線吸収性，光触媒活性，フォトクロミッ
ク性等種々の性状を有する酸化チタンの油性分散体及び
親油性酸化チタン粉体、及びこれらの製造方法に関す
る。本発明に係る酸化チタンの油性分散体及び親油性酸
化チタン粉体は、医薬品，化粧品，油性塗料，樹脂，吸
着剤，イオン交換剤，複合酸化物前駆体，光学材料，フ
ォトクロミック材料，電子・電気材料，記録・記憶材
料，繊維，光触媒，抗菌・抗黴性材料，環境汚染物分解
除去剤等、幅広い分野で応用し得るものである。また特
に、紫外線防御効果を有する化粧料への応用に適するも
のである。TECHNICAL FIELD The present invention relates to an oily dispersion of titanium oxide and a lipophilic titanium oxide powder, which are excellent in dispersibility in oily materials and have various properties such as ultraviolet absorption, photocatalytic activity, and photochromic property, and It relates to these manufacturing methods. The oil dispersion of titanium oxide and the lipophilic titanium oxide powder according to the present invention are used for pharmaceuticals, cosmetics, oil paints, resins, adsorbents, ion exchange agents, complex oxide precursors, optical materials, photochromic materials, electronic / electrical materials. It can be applied in a wide range of fields such as materials, recording / memory materials, fibers, photocatalysts, antibacterial and antifungal materials, and environmental pollutant decomposition and removal agents. Further, it is particularly suitable for application to cosmetics having an ultraviolet protection effect.
【０００２】 さらに詳しくは、チタンアルコキシド又
はその油性溶液もしくは分散液に、分子内に孤立電子対
を有する原子及び／又は極性基を有する有機化合物を添
加し、次いで水を添加し加水分解して得られる酸化チタ
ンの油性分散体、及びこれより分散媒を除去し、乾燥し
て得られる親油性酸化チタン粉体とこれらの製造方法、
並びにこれらを含有して成る化粧料に関する。More specifically, it is obtained by adding an organic compound having an atom having a lone electron pair and / or a polar group in a molecule to a titanium alkoxide or an oily solution or dispersion thereof, and then adding water for hydrolysis. An oily dispersion of titanium oxide obtained, and a lipophilic titanium oxide powder obtained by removing the dispersion medium therefrom and drying, and a method for producing these,
It also relates to cosmetics containing these.
【０００３】[0003]
【従来の技術】酸化チタンは高い紫外線遮蔽効果を有
し、塗料等の紫外線による退色防止や、紫外線による炎
症を防止するための化粧料等に顔料としてよく用いられ
る。かかる目的に適する薄片状或いは微粒子状の酸化チ
タンを得るには、形状や粒子径の制御の容易なゾル−ゲ
ル法が広く用いられている。しかしながらこの方法で
は、チタンアルコキシドを加水分解させるため水の添加
が不可欠であり、分散媒としてブタノール等の低級アル
コールを用いる。それゆえ、ゾル−ゲル法により得られ
た酸化チタンは親油性に乏しく、油性材料に対する分散
性の悪いものであった。また親水性を有するため耐水性
に乏しく、油性材料への配合に際し分散性を向上させた
り、或いは耐水性を持たせるためには、疎水化処理を行
う必要があった。2. Description of the Related Art Titanium oxide has a high UV shielding effect and is often used as a pigment in cosmetics and the like for preventing discoloration of paints due to UV rays and for preventing inflammation due to UV rays. To obtain titanium oxide in the form of flakes or fine particles suitable for this purpose, the sol-gel method, whose shape and particle size are easily controlled, is widely used. However, in this method, the addition of water is indispensable for hydrolyzing the titanium alkoxide, and a lower alcohol such as butanol is used as the dispersion medium. Therefore, titanium oxide obtained by the sol-gel method was poor in lipophilicity and poor in dispersibility in oily materials. Further, since it has hydrophilicity, it is poor in water resistance, and it has been necessary to perform a hydrophobic treatment in order to improve dispersibility in compounding into an oily material or to impart water resistance.
【０００４】[0004]
【発明が解決しようとする課題】そこで本発明において
は、油性材料への分散性に優れ、幅広い分野で応用可能
な酸化チタンの油性分散体及び親油性酸化チタン粉体を
得ること、並びに種々の目的に適する形状及び性状の制
御の容易な前記油性分散体及び親油性酸化チタン粉体の
製造方法を提供することを目的とした。さらには使用感
及び透明感に優れ、且つ良好な仕上がり感が得られて、
紫外線防御効果にも優れる化粧料を得ることをも目的と
した。Therefore, in the present invention, it is possible to obtain an oily dispersion of titanium oxide and a lipophilic titanium oxide powder which are excellent in dispersibility in an oily material and can be applied in a wide variety of fields, and various It is an object of the present invention to provide a method for producing the above-mentioned oily dispersion and lipophilic titanium oxide powder whose shape and properties are suitable for the purpose and which can be easily controlled. Furthermore, it has excellent feeling of use and transparency, and a good finished feeling is obtained,
It was also intended to obtain a cosmetic material having an excellent UV protection effect.
【０００５】[0005]
【課題を解決するための手段】上記課題を解決するべく
種々検討を行った結果、チタンアルコキシド又はその油
性溶液もしくは分散液において、加水分解反応を進行さ
せる際、チタンアルコキシドからチタン酸化物の粒子が
成長する過程で、分子内に孤立電子対を有する原子及び
／又は極性基を有する有機化合物を適量加えることによ
り、油性分散媒中に良好に分散した酸化チタン粒子が得
られることを見いだし、さらにこの酸化チタンの油性分
散体より、分散媒を除去した後乾燥することによって、
親油性の酸化チタン粉体を得ることに成功し、本発明を
完成するに至った。[Means for Solving the Problems] As a result of various studies to solve the above problems, when titanium alkoxide or an oily solution or dispersion thereof is allowed to undergo a hydrolysis reaction, particles of titanium oxide are converted from titanium alkoxide. It was found that titanium oxide particles well dispersed in an oil dispersion medium can be obtained by adding an appropriate amount of an organic compound having an atom having a lone electron pair and / or a polar group in the growth process. From the oil dispersion of titanium oxide, by removing the dispersion medium and then drying,
We succeeded in obtaining a lipophilic titanium oxide powder and completed the present invention.
【０００６】すなわち本発明においては、チタンアルコ
キシド又はその油性溶液もしくは分散液に、分子内に孤
立電子対を有する原子及び／又は極性基を有する有機化
合物の１種又は２種以上と水を添加して加水分解し、酸
化チタンの油性分散体を得、さらにこの油性分散体より
分散媒を除去した後乾燥して、親油性の酸化チタン粉体
を得る。なお、チタンアルコキシドの加水分解を行う際
に、加水分解抑制剤の１種又は２種以上を共存させるこ
とにより、選択的に薄片状や針状のゲル粒子を得ること
ができる。また必要に応じ、酸又は塩基、或いは弱酸と
弱塩基，強酸と弱塩基及び弱酸と強塩基の中和により得
られる塩を触媒として用いることができる。That is, in the present invention, one or more organic compounds having an atom and / or a polar group having a lone electron pair in the molecule and water are added to a titanium alkoxide or an oily solution or dispersion thereof. And hydrolyzed to obtain an oily dispersion of titanium oxide. Further, the dispersion medium is removed from the oily dispersion and then dried to obtain a lipophilic titanium oxide powder. When the titanium alkoxide is hydrolyzed, flakes or needle-like gel particles can be selectively obtained by coexisting one or more of the hydrolysis inhibitors. If necessary, an acid or a base, a salt obtained by neutralizing a weak acid and a weak base, a strong acid and a weak base, or a weak acid and a strong base can be used as a catalyst.
【０００７】[0007]
【発明の実施の形態】本発明において用い得るチタンア
ルコキシドとしては、チタンテトラメトキシド，チタン
テトラエトキシド，チタンテトラノルマルプロポキシ
ド，チタンテトライソプロポキシド，チタンテトラノル
マルブトキシド，チタンテトライソブトキシド，チタン
テトラターシャルブトキシド等が挙げられ、これらより
１種又は２種以上を選択して用いる。かかるチタンアル
コキシドは、分子内に孤立電子対を有する原子及び／又
は極性基を有する有機化合物が液状の場合には、直接そ
れらに溶解又は分散することができる。また油性溶媒に
溶解又は分散して、分子内に孤立電子対を有する原子及
び／又は極性基を有する有機化合物を添加し、作用させ
る。かかるチタンアルコキシドの溶液又は分散液の濃度
としては０．０００１Ｍ〜１０．０Ｍであることが好ま
しく、０．０１Ｍ〜６．０Ｍの範囲とすることが特に好
ましい。BEST MODE FOR CARRYING OUT THE INVENTION Titanium alkoxides usable in the present invention include titanium tetramethoxide, titanium tetraethoxide, titanium tetranormal propoxide, titanium tetraisopropoxide, titanium tetranormal butoxide, titanium tetraisobutoxide, and titanium. Examples thereof include tetratertial butoxide, and one or more selected from these are used. Such a titanium alkoxide can be directly dissolved or dispersed in an organic compound having an atom having a lone electron pair and / or a polar group in the molecule in a liquid state. Further, the compound is dissolved or dispersed in an oily solvent, and an organic compound having an atom having a lone electron pair and / or a polar group in the molecule is added to act. The concentration of the titanium alkoxide solution or dispersion is preferably 0.0001 M to 10.0 M, and particularly preferably 0.01 M to 6.0 M.
【０００８】 上記チタンアルコキシドを溶解又は分散
する油性溶媒としては、アボカド油，アルモンド油，オ
リーブ油，ゴマ油，サザンカ油，サフラワー油，大豆
油，ツバキ油，トウモロコシ油，ナタネ油，パーシック
油，ヒマシ油，綿実油，落花生油，ホホバ油等の液状植
物油類、ミンク油，卵黄油，液状ラノリン等の液状動物
油類、流動パラフィン，イソパラフィン，スクワラン，
プリスタン等の炭化水素油類、オレイルアルコール，2-
ヘキシルデカノール，イソステアリルアルコール，2-オ
クチルドデカノール等の液状高級アルコール類、オクタ
ン酸セチル，ミリスチン酸イソプロピル，パルミチン酸
イソプロピル，ラウリン酸ヘキシル，オレイン酸オレイ
ル，オレイン酸デシル，ミリスチン酸オクチルドデシ
ル，ジメチルオクタン酸ヘキシルデシル，フタル酸ジエ
チル，フタル酸ジブチル，ジオイレイン酸プロピレング
リコール，トリ2-エチルヘキサン酸グリセリル，トリ2-
エチルヘキサン酸トリメチロールプロパン等の液状エス
テル油類、ジメチルポリシロキサン，メチルフェニルポ
リシロキサン，オクタメチルシクロテトラシロキサン，
デカメチルシクロペンタシロキサン等のシリコーン油な
ど、一般に化粧料用或いは塗料用として用いられる油性
物質を用いることができる。本発明にはこれらより１種
又は２種以上を選択して用いる。[0008] as an oily solvent for dissolving or dispersing the titanium alkoxide, A Bokado oil, almond oil, olive oil, sesame oil, sasanqua oil, safflower oil, soybean oil, camellia oil, corn oil, rapeseed oil, persic oil, castor Liquid vegetable oils such as oil, cottonseed oil, peanut oil, jojoba oil, mink oil, egg yolk oil, liquid animal oils such as liquid lanolin, liquid paraffin, isoparaffin, squalane,
Hydrocarbon oils such as pristane, oleyl alcohol, 2-
Hexyldecanol, isostearyl alcohol, 2-octyldodecanol liquid higher alcohols such as, OH Kuta <br/> phosphate cetyl, isopropyl myristate, isopropyl palmitate, hexyl laurate, oleyl oleate, decyl oleate, myristate Octyldodecyl, hexyldecyl dimethyloctanoate, diethyl phthalate, dibutyl phthalate, propylene glycol dioleate, glyceryl tri-2-ethylhexanoate, tri 2-
Liquid ester oils such as trimethylolpropane ethylhexanoate, dimethylpolysiloxane, methylphenylpolysiloxane, octamethylcyclotetrasiloxane,
An oily substance generally used for cosmetics or paints such as silicone oil such as decamethylcyclopentasiloxane can be used. In the present invention, one kind or two or more kinds are selected from these and used.
【０００９】 本発明においては、チタンアルコキシド
に有機化合物を作用させ、それによりチタンアルコキシ
ドの加水分解を制御するが、本発明において使用し得る
有機化合物としては、分子内に孤立電子対を有する原子
や極性基を有する有機化合物で、液状であるか、油性溶
媒に溶解又は分散させ得るものであれば、特に限定され
ない。たとえば、ミリスチン酸，パルミチン酸，ステア
リン酸，イソオクタン酸，イソミリスチン酸，イソパル
ミチン酸，イソステアリン酸，ヒドロキシパルミチン
酸，ヒドロキシステアリン酸，安息香酸，ヒドロキシ安
息香酸等のカルボン酸類、アセチルアセトン，エチレン
グリコール，ジエチレングリコール，プロピレングリコ
ール，ジプロピレングリコール，エチレンジアミン，エ
チレンジアミン四酢酸，ジチゾン，ジメチルグリオキシ
ム，8-キノリノール，フタロシアニン，1,10-フェナン
トロリン，2,2'-ビピリジル，インジゴ等のキレート作
用を有する化合物などが挙げられ、これらより１種又は
２種以上を選択して用いる。チタンアルコキシドに対す
る添加量としては、チタンアルコキシド１モルに対して
０．００１モル〜４モル程度とするのが好ましい。In the present invention, an organic compound is allowed to act on the titanium alkoxide to control the hydrolysis of the titanium alkoxide, but as the organic compound usable in the present invention, an atom having a lone electron pair in the molecule or The organic compound having a polar group is not particularly limited as long as it is liquid or can be dissolved or dispersed in an oily solvent. For example, Mi Risuchin acid, palmitic acid, stearic acid, isooctanoic acid, isomyristic acid, isopalmitic acid, isostearic acid, hydroxypalmitic acid, hydroxystearic acid, benzoic acid, carboxylic acids such as hydroxy benzoic acid, A cetyl acetone, ethylene Compounds with chelating action such as glycol, diethylene glycol, propylene glycol, dipropylene glycol, ethylenediamine, ethylenediaminetetraacetic acid, dithizone, dimethylglyoxime, 8-quinolinol, phthalocyanine, 1,10-phenanthroline, 2,2'-bipyridyl, indigo etc. things include, selected and used one or more from these. The addition amount to the titanium alkoxide is preferably about 0.001 to 4 mol per 1 mol of the titanium alkoxide.
【００１０】また本発明においては、チタンアルコキシ
ドから酸化チタンへの重縮合に際し、加水分解を制御す
る加水分解抑制剤を添加することもできる。加水分解抑
制剤を添加することにより、チタンアルコキシドの加水
分解の進行を制御し、選択的に薄片状や針状のゲル粒子
を得ることができる。In the present invention, it is also possible to add a hydrolysis inhibitor for controlling the hydrolysis during the polycondensation of titanium alkoxide to titanium oxide. By adding a hydrolysis inhibitor, it is possible to control the progress of hydrolysis of the titanium alkoxide and selectively obtain flaky or acicular gel particles.
【００１１】上記加水分解抑制剤はキレート試薬及び電
子供与性試薬より選択され、ジエチレングリコール，ト
リエチレングリコール，ポリエチレングリコール，ポリ
プロピレングリコール等のアルキレングリコール類、エ
チレングリコールモノメチルエーテル，エチレングリコ
ールモノエチルエーテル，エチレングリコールモノブチ
ルエーテル，ジエチレングリコールモノメチルエーテ
ル，ジエチレングリコールモノエチルエーテル，テトラ
エチレングリコールモノメチルエーテル，テトラエチレ
ングリコールモノエチルエーテル，プロピレングリコー
ルモノメチルエーテル，プロピレングリコールモノエチ
ルエーテル等のアルキレングリコールのアルキルエーテ
ル類、エチレングリコールモノフェニルエーテル，エチ
レングリコールモノベンジルエーテル等のアルキレング
リコールのアリールエーテル類、アセチルアセトン等の
β-ジケトン類、エチレンジアミン，トリエタノールア
ミン等のアミン類などが挙げられ、これらより１種又は
２種以上を選択して用いる。前記の中でも、特にアルキ
レングリコール類が好ましく使用できる。The above-mentioned hydrolysis inhibitor is selected from chelating agents and electron-donating reagents, and includes alkylene glycols such as diethylene glycol, triethylene glycol, polyethylene glycol, polypropylene glycol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol. Alkyl ethers of alkylene glycols such as monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, tetraethylene glycol monomethyl ether, tetraethylene glycol monoethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, ethylene glycol monophenyl ether, Ethylene glycol mono Aryl ethers of alkylene glycols such Nji ether, beta-diketones such as acetylacetone, ethylene diamine, include such amines such as triethanolamine, it is used to select one or more from these. Among the above, alkylene glycols are particularly preferably used.
【００１２】上記の加水分解抑制剤は、チタンアルコキ
シド１モルに対し１モル〜２０モルの割合で添加するこ
とが好ましく、２モル〜１０モルとするのがより好まし
い。加水分解抑制剤の添加量が１モル未満であると、チ
タンアルコキシドの加水分解の制御効果が十分に得られ
ず、また２０モルを超えると、チタンアルコキシドの加
水分解が十分に進行しないので好ましくない。The above hydrolysis inhibitor is preferably added in a ratio of 1 mol to 20 mol per 1 mol of titanium alkoxide, more preferably 2 mol to 10 mol. When the addition amount of the hydrolysis inhibitor is less than 1 mol, the effect of controlling the hydrolysis of titanium alkoxide cannot be sufficiently obtained, and when it exceeds 20 mol, the hydrolysis of titanium alkoxide does not proceed sufficiently, which is not preferable. .
【００１３】さらに本発明においては、必要に応じ酸又
は塩基、或いは弱酸と弱塩基，強酸と弱塩基，弱酸と強
塩基の中和により得られる塩を触媒として添加すること
ができる。かかる酸又は塩基としては、塩酸，硫酸等の
強酸、炭酸，ギ酸，酢酸，ミリスチン酸，パルミチン
酸，ステアリン酸等の弱酸、水酸化ナトリウム，水酸化
カリウム等の強塩基、ヒドロキシアンモニウム，アセト
アミジン，ヒドラジン等の弱塩基が用いられる。これら
酸又は塩基の添加量としては、チタン１モルに対し１０
-3〜１０-4モルの範囲とするのが適切である。Further, in the present invention, if necessary, an acid or a base, a weak acid and a weak base, a strong acid and a weak base, or a salt obtained by neutralizing a weak acid and a strong base can be added as a catalyst. Examples of the acid or base include strong acids such as hydrochloric acid and sulfuric acid, weak acids such as carbonic acid, formic acid, acetic acid, myristic acid, palmitic acid and stearic acid, strong bases such as sodium hydroxide and potassium hydroxide, hydroxyammonium, acetamidine, Weak bases such as hydrazine are used. The addition amount of these acids or bases is 10 with respect to 1 mol of titanium.
It is suitable to be in the range of -3 to 10 -4 mol.
【００１４】また、弱酸と弱塩基，強酸と弱塩基，弱酸
と強塩基の中和により得られる塩としては、炭酸，カル
ボン酸及びその誘導体、並びにフェノキシド及びその誘
導体より成る群から選ばれる１種以上と、アルカリ金
属，アルカリ土類金属，アミン類，アンモニウム化合
物，ヒドラジニウム化合物，ピリジニウム化合物及びヒ
ドロキシアルミニウム化合物から成る群から選ばれる１
種以上との塩が好ましく用いられ、炭酸リチウム，炭酸
ナトリウム，炭酸カリウム，炭酸ルビジウム，炭酸セシ
ウム，炭酸アンモニウム，炭酸水素リチウム，炭酸水素
ナトリウム，炭酸水素カリウム，炭酸水素ルビジウム，
炭酸水素セシウム，炭酸水素アンモニウム，ギ酸リチウ
ム，ギ酸ナトリウム，ギ酸カリウム，ギ酸ルビジウム，
ギ酸セシウム，ギ酸カルシウム，ギ酸アンモニウム，酢
酸リチウム，酢酸ナトリウム，酢酸カリウム，酢酸ルビ
ジウム，酢酸セシウム，酢酸カルシウム，酢酸アンモニ
ウム，ミリスチン酸ナトリウム，パルミチン酸ナトリウ
ム，ステアリン酸ナトリウム，ヒドロキシアンモニウム
塩酸塩，アセトアミジン塩酸塩，ヒドラジン塩酸塩等が
例示される。これらのうち、炭酸ナトリウム，炭酸アン
モニウム，炭酸水素ナトリウム，炭酸水素アンモニウ
ム，酢酸ナトリウム，酢酸アンモニウム，ステアリン酸
ナトリウムが特に好ましい。前記より１種又は２種以上
を選択して用いるが、用いる塩により、生成するチタン
アルコキシドゲルの状態を制御することができる。な
お、これらの塩は中和反応を行わせて塩を形成させてか
ら添加してもよいが、塩を形成し得る酸と塩基をそれぞ
れ別々にチタンアルコキシドの油性溶液又は分散液に添
加し、前記溶液又は分散液中で塩を形成させてもよい。
これらの塩の添加量としては、チタンアルコキシド１モ
ルに対して０．００１モル〜２モルとするのが好まし
い。The salt obtained by neutralizing a weak acid and a weak base, a strong acid and a weak base, and a weak acid and a strong base is one selected from the group consisting of carbonic acid, carboxylic acid and its derivatives, and phenoxide and its derivatives. 1 selected from the group consisting of the above, an alkali metal, an alkaline earth metal, an amine, an ammonium compound, a hydrazinium compound, a pyridinium compound and a hydroxyaluminum compound.
Salts with one or more species are preferably used and include lithium carbonate, sodium carbonate, potassium carbonate, rubidium carbonate, cesium carbonate, ammonium carbonate, lithium hydrogen carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, rubidium hydrogen carbonate,
Cesium hydrogen carbonate, ammonium hydrogen carbonate, lithium formate, sodium formate, potassium formate, rubidium formate,
Cesium formate, calcium formate, ammonium formate, lithium acetate, sodium acetate, potassium acetate, rubidium acetate, cesium acetate, calcium acetate, ammonium acetate, sodium myristate, sodium palmitate, sodium stearate, hydroxyammonium hydrochloride, acetamidine hydrochloride Examples thereof include salts and hydrazine hydrochloride. Of these, sodium carbonate, ammonium carbonate, sodium hydrogen carbonate, ammonium hydrogen carbonate, sodium acetate, ammonium acetate, and sodium stearate are particularly preferable. Although one or more selected from the above are used, the state of the titanium alkoxide gel produced can be controlled by the salt used. Incidentally, these salts may be added after the salt is formed by performing a neutralization reaction, but an acid and a base capable of forming a salt are separately added to an oily solution or dispersion of titanium alkoxide, Salts may be formed in the solution or dispersion.
The amount of these salts added is preferably 0.001 to 2 mol per 1 mol of titanium alkoxide.
【００１５】本発明における酸化チタンの油性分散体の
製造方法としては、まずチタンアルコキシドを油性溶媒
の１種又は２種以上に溶解又は分散し、この油性溶液又
は分散液を撹拌しながら、分子内に孤立電子対を有する
原子及び／又は極性基を有する有機化合物の１種又は２
種以上を油性溶媒に溶解又は分散して添加した後、水を
添加し、加水分解する。水の添加量はチタンアルコキシ
ド１モルに対し０．００１モル〜４モル程度とするのが
適切である。分子内に孤立電子対を有する原子及び／又
は極性基を有する有機化合物が液状である場合には、チ
タンアルコキシドに直接かかる有機化合物を添加しても
よい。分子内に孤立電子対を有する原子及び／又は極性
基を有する有機化合物の種類やチタンアルコキシドに対
する添加量を調整することにより、生成される酸化チタ
ンの形状を制御することができる。また、水の添加量比
を増加させるにつれて、得られる酸化チタンの油性分散
体は、透明〜微白濁〜白濁と変化し、その透明性を制御
することができる。As a method for producing an oily dispersion of titanium oxide in the present invention, first, a titanium alkoxide is dissolved or dispersed in one or more oily solvents, and the oily solution or dispersion is stirred to form an intramolecular compound. One or two of the organic compounds having an atom having a lone pair of electrons and / or having a polar group
After dissolving or dispersing one or more species in an oily solvent and adding them, water is added to hydrolyze them. It is appropriate that the amount of water added is about 0.001 to 4 mol per 1 mol of titanium alkoxide. When the organic compound having an atom having a lone electron pair and / or a polar group in the molecule is liquid, the organic compound may be added directly to the titanium alkoxide. The shape of titanium oxide produced can be controlled by adjusting the type of organic compound having an atom having a lone electron pair and / or a polar group in the molecule and the amount added to the titanium alkoxide. Moreover, as the addition ratio of water is increased, the obtained titanium oxide oil dispersion changes from transparent to slightly cloudy to cloudy, and the transparency can be controlled.
【００１６】さらに本発明においては、加水分解抑制剤
を油性溶媒の１種又は２種以上に溶解又は分散して添加
することにより、選択的に薄片状や針状のゲルを得るこ
とができる。また触媒として酸又は塩基、或いは弱酸と
弱塩基，強酸と弱塩基及び弱酸と強塩基との中和により
得られる塩を添加する場合は、これらの油性溶液又は分
散液は水と同時に添加してもよいが、ある程度加水分解
を進行させた後に添加してもよく、添加時期によりゲル
粒子の形状を制御することが可能である。また、油性溶
媒又は配位能を有する有機化合物として、加水分解抑制
作用を有するものを用いてもよい。Further, in the present invention, a flaky or acicular gel can be selectively obtained by dissolving or dispersing the hydrolysis inhibitor in one or more oily solvents and adding it. When a salt obtained by neutralizing an acid or a base, a weak acid and a weak base, a strong acid and a weak base, or a weak acid and a strong base is added as a catalyst, these oily solutions or dispersions should be added simultaneously with water. However, it may be added after the hydrolysis has proceeded to some extent, and the shape of the gel particles can be controlled by the time of addition. Further, as the oily solvent or the organic compound having a coordinating ability, one having a hydrolysis suppressing action may be used.
【００１７】上記反応系については、撹拌を停止して２
〜１２０時間程度静置し、反応を継続させる。必要に応
じてチタンに対し５〜７倍モル量の酸を添加して反応を
停止し、過剰量の水を添加して未反応のチタンアルコキ
シドが残留しないことを確認し、残留する場合には過剰
量の水により洗浄，除去する。反応を停止するのに添加
する酸については特に限定されない。With respect to the above reaction system, the stirring was stopped and 2
Let stand for about 120 hours to continue the reaction. If necessary, 5 to 7 times the molar amount of acid is added to the titanium to stop the reaction, and excess water is added to confirm that unreacted titanium alkoxide does not remain. Wash and remove with excess water. The acid added to stop the reaction is not particularly limited.
【００１８】本発明に係る酸化チタンの油性分散体が、
揮発性の油性溶媒又は有機化合物に分散されている場合
には、風乾，減圧蒸留等によりこれらを揮発させて乾燥
することによって、親油性の酸化チタン粉体を得ること
ができる。油性溶媒又は有機化合物として不揮発性のも
のを用いた場合には、シクロヘキサン等の揮発性の油性
溶媒を添加して共沸させて乾燥する。The oily dispersion of titanium oxide according to the present invention comprises
When dispersed in a volatile oily solvent or organic compound, a lipophilic titanium oxide powder can be obtained by evaporating these by air-drying, vacuum distillation or the like and drying. When a non-volatile oily solvent or organic compound is used, a volatile oily solvent such as cyclohexane is added and azeotropically dried.
【００１９】本発明に係る酸化チタンの油性分散体及び
親油性酸化チタン粉体は、油性材料への分散性及び耐水
性に優れ、紫外線吸収性，光触媒活性，フォトクロミッ
ク性，抗菌活性等種々の性状を有し、形状の制御も容易
で、薄片状，針状，繊維状等とすることができる。さら
に、高い透明性を有するものを得ることもできる。従っ
て、本発明に係る酸化チタンの油性分散体等は、医薬
品，化粧品，油性塗料，樹脂，吸着剤，イオン交換剤，
複合酸化物前駆体，光学材料，フォトクロミック材料，
電子・電気材料，記録・記憶材料，繊維，光触媒，抗菌
・抗黴性材料，環境汚染物分解除去剤等として、幅広い
分野で応用することができる。なかでも特に、紫外線防
御効果を有する化粧料への応用に適する。The oil dispersion of titanium oxide and the lipophilic titanium oxide powder according to the present invention are excellent in dispersibility in oily materials and water resistance, and have various properties such as ultraviolet absorption, photocatalytic activity, photochromic activity and antibacterial activity. It is easy to control the shape, and can be in the shape of flakes, needles, fibers or the like. Further, it is possible to obtain a material having high transparency. Therefore, the oily dispersion of titanium oxide according to the present invention can be used for pharmaceuticals, cosmetics, oil paints, resins, adsorbents, ion exchange agents,
Complex oxide precursor, optical material, photochromic material,
It can be applied in a wide range of fields such as electronic / electrical materials, recording / memory materials, fibers, photocatalysts, antibacterial / antifungal materials, agents for decomposing and removing environmental pollutants. Among them, it is particularly suitable for application to cosmetics having an ultraviolet protection effect.
【００２０】すなわち本発明においては、化粧料用油性
原料として、上記酸化チタンの油性分散体の１種又は２
種以上を含有させ、及び／又は化粧料用粉体として、上
記親油性酸化チタン粉体の１種又は２種以上を含有させ
ることにより、紫外線による皮膚への悪影響を防止する
のに有効な化粧料を得ることができる。かかる化粧料
は、二層ないし三層状の化粧水，乳液，クリーム，ゲ
ル，パック等の皮膚用化粧料、メイクアップベースロー
ション，メイクアップベースクリーム等の下地化粧料、
乳液状，クリーム状，油性軟膏型，油性スティック状，
粉末状等のファンデーション類，アイカラー類，チーク
カラー類といったメイクアップ化粧料、リップクリー
ム，リップスティック等の口唇用化粧料などとして提供
し得る。That is, in the present invention, as the oily raw material for cosmetics, one or two of the above-mentioned oily dispersions of titanium oxide are used.
One or more of the above lipophilic titanium oxide powders as a powder for cosmetics, and / or two or more of the above lipophilic titanium oxide powders, thereby making it effective to prevent the harmful effects of ultraviolet rays on the skin. You can get a fee. Such cosmetics include skin cosmetics such as two- or three-layered lotions, emulsions, creams, gels and packs, base cosmetics such as makeup base lotions and makeup base creams,
Emulsion, cream, oily ointment, oily stick,
It can be provided as makeup cosmetics such as powdery foundations, eye colors and cheek colors, and lip cosmetics such as lip balms and lipsticks.
【００２１】本発明に係る化粧料には、上記の酸化チタ
ンの油性分散体及び／又は親油性酸化チタン粉体の他、
油脂類，ロウ類，炭化水素類，脂肪酸類，高級アルコー
ル類，エステル類，低級アルコール類，多価アルコール
類，保湿剤，細胞賦活剤，抗炎症剤，界面活性剤，水溶
性高分子化合物，防菌防黴剤，色素類，香料等、一般的
に化粧料に配合される原料を含有させることができる。
また本発明に係る親油性酸化チタン粉体以外に、体質顔
料，着色顔料，真珠光沢顔料等の粉体類を含有させるこ
とができる。特に紫外線防御を目的とした日焼け止め化
粧料においては、従来より用いられている微粒子酸化チ
タンや酸化亜鉛といった紫外線散乱効果を有する粉体
や、紫外線吸収剤を併用し得る。In the cosmetics according to the present invention, in addition to the above-mentioned oily dispersion of titanium oxide and / or lipophilic titanium oxide powder,
Fats, waxes, hydrocarbons, fatty acids, higher alcohols, esters, lower alcohols, polyhydric alcohols, humectants, cell activating agents, anti-inflammatory agents, surfactants, water-soluble polymer compounds, Ingredients generally contained in cosmetics such as antibacterial and antifungal agents, pigments, and fragrances can be contained.
In addition to the lipophilic titanium oxide powder according to the present invention, powders such as extender pigments, coloring pigments and pearlescent pigments can be contained. Particularly in sunscreen cosmetics for the purpose of protecting against ultraviolet rays, powders having an ultraviolet scattering effect such as fine particle titanium oxide and zinc oxide which have been conventionally used, and an ultraviolet absorber can be used in combination.
【００２２】[0022]
【実施例】さらに実施例により、本発明について詳細に
説明する。The present invention will be described in more detail with reference to examples.
【００２３】［実施例１〜実施例３］ イソステアリン
酸を作用させた酸化チタンのスクワラン分散体
チタンテトラエトキシドをスクワランに溶解して０．２
Ｍの溶液とした。この溶液１リットルを撹拌しながら、
表１に示す量のイソステアリン酸をスクワラン溶液とし
て添加し、次いで表１に示す量の水を添加した。撹拌を
停止して室温で２４時間静置した後、ステアリン酸１．
４モルを添加して反応を停止し、水を添加して洗浄し
た。Examples 1 to 3 Squalane dispersion of titanium oxide treated with isostearic acid Titanium tetraethoxide was dissolved in squalane to 0.2.
M solution. While stirring 1 liter of this solution,
The amount of isostearic acid shown in Table 1 was added as a squalane solution, followed by the amount of water shown in Table 1. After stirring was stopped and the mixture was allowed to stand at room temperature for 24 hours, stearic acid 1.
The reaction was stopped by adding 4 mol, and water was added for washing.
【００２４】[0024]
【表１】 [Table 1]
【００２５】［実施例４〜実施例６］ イソステアリン
酸を作用させて成る親油性酸化チタン粉体
実施例１〜実施例３の酸化チタンのスクワラン分散体に
シクロヘキサンを加え、共沸させて乾燥して酸化チタン
粉体を得、それぞれ実施例４〜実施例６とした。[Examples 4 to 6] Lipophilic titanium oxide powder prepared by the action of isostearic acid Cyclohexane was added to the squalane dispersion of titanium oxide of Examples 1 to 3, and the mixture was azeotropically dried. Then, titanium oxide powder was obtained, which were referred to as Example 4 to Example 6, respectively.
【００２６】［実施例７］ 8-キノリノールを作用させ
た酸化チタンのスクワラン分散体
チタンテトラエトキシドをスクワランに溶解して０．２
Ｍの溶液とした。この溶液１リットルを撹拌しながら、
０．００１モルの8-キノリノールをスクワラン溶液とし
て添加し、次いで０．１モルの水を添加した。撹拌を停
止して室温で２４時間静置した後、ステアリン酸１．４
モルを添加して反応を停止し、水を添加して洗浄した。[Example 7] Squalane dispersion of titanium oxide treated with 8-quinolinol Titanium tetraethoxide was dissolved in squalane to 0.2.
M solution. While stirring 1 liter of this solution,
0.001 mol of 8-quinolinol was added as a squalane solution, followed by 0.1 mol of water. After stirring was stopped and the mixture was allowed to stand at room temperature for 24 hours, stearic acid 1.4 was added.
The reaction was stopped by adding mol and water was added for washing.
【００２７】［実施例８］ 8-キノリノールを作用させ
て成る親油性酸化チタン粉体
実施例７の8-キノリノールを作用させた酸化チタンのス
クワラン分散体に、シクロヘキサンを加えて共沸させて
乾燥し、実施例８とした。[Example 8] Lipophilic titanium oxide powder formed by reacting with 8-quinolinol [0027] Cyclohexane was added to the squalane dispersion of titanium oxide treated with 8-quinolinol of Example 7 and azeotroped to dry. Then, it is referred to as Example 8.
【００２８】本発明の実施例１〜実施例３及び実施例７
について粒子形状を観察したところ、薄片状粒子の生成
が認められた。次いでこれらの粒子径，Ｘ線回折及び紫
外部吸収スペクトルの測定を行った。粒子径は島津製作
所製島津レーザー回折式粒度分布測定装置ＳＡＬＤ-２
０００Ｊにより、薄片状酸化チタン粒子の長径及び短径
の平均値を求めて算出した。紫外部吸収スペクトル及び
Ｘ線回折はそれぞれ日立製スペクトロフォトメータＵ-
３０００及びリガク社製ＲＩＮＴ２０００縦型ゴニオメ
ータにより測定した。また、ＳＰＦアナライザーにより
ＳＰＦ値をも求めた。以上の結果を表２にまとめて示し
た。なお、チタンエトキシドとイソステアリン酸又は8-
キノリノールとの作用については、赤外吸収スペクトル
により確認した。Examples 1 to 3 and 7 of the present invention
As a result of observing the shape of the particles, it was confirmed that flaky particles were generated. Next, the particle size, X-ray diffraction and ultraviolet absorption spectrum of these particles were measured. The particle size is Shimadzu Shimadzu laser diffraction particle size distribution analyzer SALD-2.
The average value of the major axis and the minor axis of the flaky titanium oxide particles was determined and calculated at 000 J. Ultraviolet absorption spectrum and X-ray diffraction are Hitachi spectrophotometer U-
It was measured with a 3000 and RINT2000 vertical type goniometer manufactured by Rigaku Corporation. Moreover, the SPF value was also obtained by the SPF analyzer. The above results are summarized in Table 2. In addition, titanium ethoxide and isostearic acid or 8-
The action with quinolinol was confirmed by infrared absorption spectrum.
【００２９】[0029]
【表２】 [Table 2]
【００３０】表２より明らかなように、本発明の実施例
１〜実施例３及び実施例７は、粒子径が３〜１１６μｍ
とかなり大きな薄片状酸化チタンの分散体であるが、非
常に優れた透明性を有していた。Ｘ線回折の結果から
は、いずれにおいてもアモルファス状の結晶状態を呈す
ることが示された。また、実施例１〜実施例３について
は、２６４〜２７１ｎｍにおいて吸収極大を有してお
り、実施例７については、さらに長波長側に8-キノリノ
ールに起因する吸収が認められた。いずれの分散体につ
いても粘度は低く、ＳＰＦアナライザーによる測定では
７付近のＳＰＦ値を示していた。As is clear from Table 2, in Examples 1 to 3 and 7 of the present invention, the particle size is 3 to 116 μm.
Although it was a fairly large dispersion of flaky titanium oxide, it had very excellent transparency. From the results of X-ray diffraction, it was shown that each exhibited an amorphous crystalline state. Further, Examples 1 to 3 have absorption maximums at 264 to 271 nm, and in Example 7, absorption due to 8-quinolinol was observed on the longer wavelength side. The viscosity of all the dispersions was low, and the SPF value was around 7 as measured by the SPF analyzer.
【００３１】続いて、実施例３に係る酸化チタンの油性
分散体において、溶媒を流動パラフィンに代替し、他は
同様に調製した後、温浴にて２０時間静置して流動パラ
フィンを蒸散させて濃縮したものを実施例９とし、これ
についてフォトクロミック性の評価を行った。実施例９
の酸化チタンの油性分散体に対し、ＳＣＨＯＴＴ社製Ｗ
Ｇ320フィルターを装着したキセノンランプを光源とし
て、４０ｍＪ／ｃｍ2〜３００ｍＪ／ｃｍ2の紫外線を照
射し、その際の色調の変化（ΔＥ）を、ＳＨＩＭＡＤＺ
Ｕ ＵＶ-1600にて測定した３８０〜７２０ｎｍの透過率
をもとに算出した。その結果を図１に示す。また、紫外
線照射を停止した後の色調の変化についても同様に算出
し、図２に示した。Subsequently, in the titanium oxide oil dispersion according to Example 3, liquid paraffin was used as a solvent instead of the solvent, and the same procedure was followed except that the liquid paraffin was evaporated by leaving it in a warm bath for 20 hours. The concentrated product was used as Example 9 and its photochromic property was evaluated. Example 9
To the oil dispersion of titanium oxide of W, manufactured by SCHOTT Co.
Using a xenon lamp equipped with a G320 filter as a light source and irradiating ultraviolet rays of 40 mJ / cm 2 to 300 mJ / cm 2 , the change in color tone (ΔE) at that time is calculated by SHIMADZ.
It was calculated based on the transmittance of 380 to 720 nm measured by U UV-1600. The result is shown in FIG. Further, the change in color tone after stopping the irradiation of ultraviolet rays was calculated in the same manner and is shown in FIG.
【００３２】図１より明らかなように、本発明の実施例
９に係る酸化チタンの油性分散体においては紫外線照射
量の増大に伴って色調変化（ΔＥ）が大きくなってお
り、さらに図２に示すごとく、紫外線照射を停止する
と、速やかに色調が元に戻ることが認められ、フォトク
ロミック材料としても有用であることが示唆される。As is apparent from FIG. 1, in the titanium oxide oil dispersion according to Example 9 of the present invention, the change in color tone (ΔE) increased with the increase of the ultraviolet ray irradiation amount, and further in FIG. As shown, it is confirmed that the color tone is quickly restored to the original color when the irradiation of ultraviolet rays is stopped, which suggests that it is also useful as a photochromic material.
【００３３】さらに、本発明に係る透明な酸化チタンの
油性分散体について、他の実施例を示す。表３に示す油
性溶媒を用いて、チタンテトラエトキシドの１．５Ｍ溶
液を調製し、その溶液各１リットルを撹拌しながら、イ
ソステアリン酸０．７５モルを各油性溶媒に溶解して添
加し、次いで水０．７５モル及びジエチレングリコール
７．５モルをそれぞれ添加した。撹拌を停止して室温で
５日間静置した後、ステアリン酸９．０モルを添加して
反応を停止し、水を加えて洗浄し、実施例１０〜実施例
１４を得た。Further, other examples of the transparent titanium oxide oil dispersion according to the present invention will be shown. Using the oily solvent shown in Table 3, a 1.5M solution of titanium tetraethoxide was prepared, and 0.75 mol of isostearic acid was dissolved in each oily solvent and added while stirring 1 liter of each solution, Then 0.75 mol of water and 7.5 mol of diethylene glycol were added respectively. After stirring was stopped and the mixture was allowed to stand at room temperature for 5 days, 9.0 mol of stearic acid was added to stop the reaction, and water was added to wash the mixture to obtain Examples 10 to 14.
【００３４】[0034]
【表３】 [Table 3]
【００３５】［実施例１５］ 針状酸化チタン油性分散
体
チタンテトラエトキシド４０ｍｍｏｌをイソパラフィン
５ｍｌに溶解し、イソデカン酸４０ｍｍｏｌ，精製水２
０ｍｍｏｌ及びステアリン酸ナトリウム０．０２５ｍｍ
ｏｌを撹拌しながら添加した。撹拌を停止した後、室温
で２４時間静置し、針状の形状を有する酸化チタンの分
散体を得た。Example 15 A needle-shaped titanium oxide oil dispersion of titanium tetraethoxide (40 mmol) was dissolved in isoparaffin (5 ml), and isodecanoic acid (40 mmol) and purified water (2) were added.
0 mmol and sodium stearate 0.025 mm
was added with stirring. After the stirring was stopped, the mixture was allowed to stand at room temperature for 24 hours to obtain a titanium oxide dispersion having a needle shape.
【００３６】［実施例１６］ 針状親油性酸化チタン粉
体
実施例１５に係る針状酸化チタン油性分散体より温浴に
て溶媒を揮発させて乾燥し、針状の親油性酸化チタン粉
体を回収した。[Example 16] Needle-shaped lipophilic titanium oxide powder A needle-shaped lipophilic titanium oxide powder was dried from the needle-shaped titanium oxide oil dispersion according to Example 15 by evaporating the solvent in a warm bath and dried. Recovered.
【００３７】続いて、本発明に係る化粧料の実施例の処
方を示す。Next, the formulations of the examples of the cosmetics according to the present invention will be shown.
【００３８】
［実施例１７］ 二層状化粧水
(1)イソステアリン酸を作用させた酸化チタンの ８．００（重量％）
スクワラン分散体（実施例１）
(2)β-カロチン ０．０２
(3)エタノール １０．００
(4)ポリオキシエチレン(20E.O.)ソルビタン ０．２０
テトラオレイン酸エステル
(5)パラオキシ安息香酸メチル ０．１０
(6)香料 ０．１０
(7)ソルビトール １．００
(8)グリセリン １．００
(9)精製水 ７９．５８
製法：(1)に(2)を添加，溶解し、さらにこれに(4)〜(6)
を(3)に溶解したアルコール部を加えて油層とする。(9)
に(7)，(8)を溶解したものを水層とし、この水層部に油
層部を室温下に加え、撹拌，混合する。[Example 17] Two-layered lotion (1) 8.00 (wt%) of titanium oxide treated with isostearic acid Squalane dispersion (Example 1) (2) β-carotene 0.02 (3) ) Ethanol 10.00 (4) Polyoxyethylene (20E.O.) sorbitan 0.20 Tetraoleic acid ester (5) Methyl paraoxybenzoate 0.10 (6) Perfume 0.10 (7) Sorbitol 1.00 ( 8) Glycerin 1.00 (9) Purified water 79.58 Manufacturing method: (2) was added to (1) and dissolved, and then (4) to (6)
Add the dissolved alcohol part to (3) to make an oil layer. (9)
An aqueous layer is prepared by dissolving (7) and (8) in (1), and an oil layer is added to this aqueous layer at room temperature, followed by stirring and mixing.
【００３９】
［実施例１８］ 水中油型乳液
(1)セタノール １．０（重量％）
(2)ミツロウ ０．５
(3)ワセリン ２．０
(4)イソステアリン酸を作用させた酸化チタンの ６．０
スクワラン分散体（実施例２）
(5)イソステアリン酸を作用させた酸化チタンの ２．０
トリ2-エチルヘキサン酸グリセリル分散体（実施例１１）
(6)ポリオキシエチレン(10E.O.)モノオレイン酸 １．０
エステル
(7)グリセリルモノステアリン酸エステル １．０
(8)グリセリン ４．０
(9)1,3-ブチレングリコール ４．０
(10)パラオキシ安息香酸メチル ０．１
(11)精製水 ５８．２
(12)カルボキシビニルポリマー（１．０重量％ １５．０
水溶液）
(13)水酸化カリウム ０．１
(14)香料 ０．１
(15)エタノール ５．０
製法：(1)〜(7)の油相成分を混合，加熱溶解し、７０℃
とする。一方、(8)〜(10)を(11)に添加して溶解し、７
０℃に加熱する。この水相に前記油相を添加して予備乳
化し、次いで(12)を添加して撹拌後、(13)を添加して増
粘させ、ホモミキサーにて均一に乳化する。続いて冷却
し、４０℃にて(14)を(15)に溶解して添加，混合する。[Example 18] Oil-in-water emulsion (1) Cetanol 1.0 (wt%) (2) Beeswax 0.5 (3) Vaseline 2.0 (4) Titanium oxide treated with isostearic acid 6 0.0 Squalane dispersion (Example 2) (5) Titanium oxide treated with isostearic acid 2.0 Glyceryl tri-2-ethylhexanoate dispersion (Example 11) (6) Polyoxyethylene (10E.O. ) Monooleic acid 1.0 ester (7) Glyceryl monostearate 1.0 (8) Glycerin 4.0 (9) 1,3-butylene glycol 4.0 (10) Methyl paraoxybenzoate 0.1 (11 ) Purified water 58.2 (12) Carboxyvinyl polymer (1.0 wt% 15.0 aqueous solution) (13) Potassium hydroxide 0.1 (14) Perfume 0.1 (15) Ethanol 5.0 Manufacturing method: (1 ) ~ (7) oil phase components are mixed, heated and dissolved, 70 ℃
And Meanwhile, add (8) to (10) to (11) and dissolve,
Heat to 0 ° C. The above oil phase is added to this aqueous phase for preliminary emulsification, then (12) is added and stirred, and then (13) is added to increase the viscosity and uniformly emulsified with a homomixer. Then, the mixture is cooled, and (14) is dissolved in (15) at 40 ° C., and the mixture is added and mixed.
【００４０】
［実施例１９］ 水中油型クリーム
(1)イソステアリン酸を作用させた酸化チタンの １０．０（重量％）
スクワラン分散体（実施例３）
(2)ワセリン ５．０
(3)ステアリルアルコール ３．０
(4)ステアリン酸 ３．０
(5)グリセリルモノステアリン酸エステル ３．０
(6)ポリアクリル酸エチル １．０
(7)酢酸トコフェロール ０．２
(8)イソステアリン酸を作用させて成る親油性 ６．０
酸化チタン粉体（実施例４）
(9)1,3-ブチレングリコール ７．０
(10)水酸化カリウム ０．２
(11)パラオキシ安息香酸メチル ０．１
(12)精製水 ６１．４
(13)香料 ０．１
製法：(1)〜(7)の油相成分を混合し、加熱溶解したもの
に(8)を分散した後７０℃とする。一方、(9)〜(11)を(1
2)に加えて溶解して加熱し、７０℃とする。この水相に
前記油相を撹拌しながら添加し、ホモジナイザーにより
乳化した後冷却し、４０℃にて(13)を添加，混合する。[Example 19] Oil-in-water cream (1) 10.0 (wt%) of titanium oxide treated with isostearic acid Squalane dispersion (Example 3) (2) Vaseline 5.0 (3) Stearyl Alcohol 3.0 (4) Stearic acid 3.0 (5) Glyceryl monostearate 3.0 (6) Polyethyl acrylate 1.0 (7) Tocopherol acetate 0.2 (8) Apply isostearic acid Lipophilic 6.0 titanium oxide powder (Example 4) (9) 1,3-butylene glycol 7.0 (10) potassium hydroxide 0.2 (11) methyl paraoxybenzoate 0.1 (12) purified Water 61.4 (13) Perfume 0.1 Manufacturing method: The oil phase components of (1) to (7) are mixed and heated to dissolve (8), and then the mixture is heated to 70 ° C. On the other hand, (9) to (11) are changed to (1
In addition to 2), dissolve and heat to 70 ° C. The oil phase is added to this aqueous phase with stirring, emulsified by a homogenizer and then cooled, and (13) is added and mixed at 40 ° C.
【００４１】
［実施例２０］ 日焼け止め用油中水型クリーム
(1)イソステアリン酸を作用させた酸化チタンの ２０．０（重量％）
流動パラフィン分散体（実施例９）
(2)スクワラン ２０．０
(3)グリセリルジイソステアリン酸エステル ３．０
(4)有機変性モンモリロナイト １．５
(5)パラメトキシ桂皮酸2-エチルヘキシル ５．０
(6)オキシベンゾン ３．０
(7)4-ターシャルブチル-4'-メトキシジベンゾイル １．０
メタン
(8)イソステアリン酸を作用させて成る親油性 ３．０
酸化チタン粉体（実施例５）
(9)1,3-ブチレングリコール ５．０
(10)パラオキシ安息香酸メチル ０．１
(11)精製水 ３８．３
(12)香料 ０．１
製法：(1)〜(7)の油相成分を混合，加熱溶解し、(8)を
分散させた後７０℃とする。一方、(9)〜(11)を混合，
溶解して加熱し、７０℃とする。この水相を前記油相に
撹拌しながら添加し、ホモジナイザーにより乳化した後
冷却し、４０℃にて(12)を添加，混合する。[Example 20] Sunscreen water-in-oil cream (1) 20.0% by weight of titanium oxide treated with isostearic acid Liquid paraffin dispersion (Example 9) (2) Squalane 20. 0 (3) Glyceryl diisostearate 3.0 (4) Organically modified montmorillonite 1.5 (5) 2-Ethylhexyl paramethoxycinnamate 5.0 (6) Oxybenzone 3.0 (7) 4-tert-Butyl-4 ' -Methoxydibenzoyl 1.0 Methane (8) Lipophilicity obtained by the action of isostearic acid 3.0 Titanium oxide powder (Example 5) (9) 1,3-butylene glycol 5.0 (10) paraoxybenzoic acid Methyl 0.1 (11) Purified water 38.3 (12) Perfume 0.1 Manufacturing method: The oil phase components of (1) to (7) are mixed and dissolved by heating, and (8) is dispersed and then at 70 ° C. To do. On the other hand, mix (9)-(11),
Melt and heat to 70 ° C. This aqueous phase is added to the oil phase while stirring, emulsified by a homogenizer, then cooled, and (12) is added and mixed at 40 ° C.
【００４２】
［実施例２１］ メイクアップベースクリーム
(1)ステアリン酸 １０．００（重量％）
(2)8-キノリノールを作用させた酸化チタンの ５．８５
スクワラン分散体（実施例７）
(3)セタノール １．５０
(4)イソステアリン酸を作用させた酸化チタンの ２．００
オクタン酸セチル分散体（実施例１０）
(5)自己乳化型グリセリルモノステアリン酸エステル ２．００
(6)プロピレングリコール ８．００
(7)水酸化カリウム ０．２０
(8)パラオキシ安息香酸メチル ０．１０
(9)精製水 ６９．００
(10)酸化チタン １．００
(11)ベンガラ ０．０５
(12)黄酸化鉄 ０．２０
(13)香料 ０．１０
製法：(1)〜(5)の油相成分を混合，加熱溶解し、７５℃
とする。一方、(6)〜(9)の水相成分を混合，溶解し、７
５℃に加熱したものに(10)〜(12)の顔料を添加して、ホ
モミキサーにて分散する。この水相成分に前記油相成分
を添加し、ホモミキサーにて均一に乳化した後冷却し、
４０℃にて(13)を添加，混合する。Example 21 Makeup Base Cream (1) Stearic Acid 10.00 (wt%) (2) 8.85 Squalane Dispersion of Titanium Dioxide Treated with 8-Quinolinol (Example 7) (3) ) Cetanol 1.50 (4) 2.00 Cetyl octoate dispersion of titanium oxide treated with isostearic acid (Example 10) (5) Self-emulsifying glyceryl monostearate 2.00 (6) Propylene glycol 8 0.000 (7) Potassium hydroxide 0.20 (8) Methyl paraoxybenzoate 0.10 (9) Purified water 69.00 (10) Titanium oxide 1.00 (11) Red iron oxide 0.05 (12) Yellow iron oxide 0.20 (13) Perfume 0.10 Manufacturing method: The oil phase components (1) to (5) are mixed, dissolved by heating, and heated to 75 ° C.
And On the other hand, the water phase components (6) to (9) are mixed and dissolved, and
The pigments (10) to (12) are added to the mixture heated to 5 ° C. and dispersed by a homomixer. The oil phase component was added to this aqueous phase component, and the mixture was uniformly emulsified with a homomixer and then cooled,
Add (13) at 40 ° C. and mix.
【００４３】
［実施例２２］ 油性軟膏型ファンデーション
(1)固形パラフィン ３．００（重量％）
(2)マイクロクリスタリンワックス ６．００
(3)ミツロウ ２．００
(4)ワセリン １２．００
(5)酢酸ラノリン １．００
(6)イソステアリン酸を作用させた酸化チタンの ６．００
スクワラン分散体（実施例１）
(7)パルミチン酸イソプロピル １８．００
(8)酢酸トコフェロール ０．２０
(9)パラオキシ安息香酸ブチル ０．０２
(10)8-キノリノールを作用させて成る親油性 １５．５０
酸化チタン粉体（実施例８）
(11)タルク １７．４８
(12)カオリン １５．００
(13)ベンガラ １．００
(14)黄酸化鉄 ２．５０
(15)黒酸化鉄 ０．２０
(16)香料 ０．１０
製法：(1)〜(9)を混合し、８５℃に加熱して溶解し、こ
れにまず(10)を添加して分散し、次いで(11)〜(15)を十
分混合し粉砕した後、撹拌しながら添加し、コロイドミ
ルで磨砕分散する。(16)を加え、脱気後７０℃で容器に
流し込み、冷却する。[Example 22] Oil-based ointment type foundation (1) Solid paraffin 3.00 (% by weight) (2) Microcrystalline wax 6.00 (3) Beeswax 2.00 (4) Vaseline 12.00 (5) Lanolin acetate 1.00 (6) 6.00 squalane dispersion of titanium oxide treated with isostearic acid (Example 1) (7) Isopropyl palmitate 18.00 (8) Tocopherol acetate 0.20 (9) Paraoxybenzoic acid Butyl acid 0.02 (10) 8-Quinolinol lipophilic 15.50 titanium oxide powder (Example 8) (11) Talc 17.48 (12) Kaolin 15.00 (13) Red iron oxide 1. 00 (14) Yellow iron oxide 2.50 (15) Black iron oxide 0.20 (16) Perfume 0.10 Manufacturing method: (1) to (9) are mixed and heated to 85 ° C. to be dissolved. First, add (10) and disperse, then mix (11) to (15) thoroughly. After crushed, it was added with stirring and grinding the dispersion in a colloid mill. After adding (16) and degassing, pour into a container at 70 ° C. and cool.
【００４４】
［実施例２３］ 油性スティック状ファンデーション
(1)イソステアリン酸を作用させた酸化チタンの １８．０８（重量％）
流動パラフィン分散体（実施例１２）
(2)ミリスチン酸イソプロピル １５．００
(3)液状ラノリン ４．５０
(4)マイクロクリスタリンワックス ４．５０
(5)セレシン １０．００
(6)カルナウバロウ ２．００
(7)ソルビタンセスキオレイン酸エステル １．００
(8)酢酸トコフェロール ０．２０
(9)パラオキシ安息香酸ブチル ０．０２
(10)イソステアリン酸を作用させて成る親油性 １０．００
酸化チタン粉体（実施例４）
(11)イソステアリン酸を作用させて成る親油性 １０．００
酸化チタン粉体（実施例５）
(12)カオリン １４．６０
(13)タルク ２．８０
(14)マイカ ３．００
(15)ベンガラ １．００
(16)黄酸化鉄 ３．００
(17)黒酸化鉄 ０．２０
(18)香料 ０．１０
製法：(1)〜(9)の基剤成分を混合し、７０℃〜８０℃で
加熱融解し、(10)，(11)を添加して分散する。一方、(1
2)〜(17)の顔料成分を混合して前記基剤に加え、ロール
ミルで練る。混練物を加熱融解し、調色した後脱泡し、
(18)を添加して型に充填して冷却固化する。[Example 23] Oily stick-shaped foundation (1) 18.08 (wt%) of titanium oxide treated with isostearic acid Liquid paraffin dispersion (Example 12) (2) Isopropyl myristate 15.00 ( 3) Liquid lanolin 4.50 (4) Microcrystalline wax 4.50 (5) Ceresin 10.00 (6) Carnauba wax 2.00 (7) Sorbitan sesquioleate 1.00 (8) Tocopherol acetate 0.20 ( 9) Butyl paraoxybenzoate 0.02 (10) Lipophilic 10.00 titanium oxide powder formed by acting isostearic acid (Example 4) (11) Lipophilic 10.00 formed by acting isostearic acid 10.00 Titanium oxide Powder (Example 5) (12) Kaolin 14.60 (13) Talc 2.80 (14) Mica 3.00 (15) Red iron oxide 1.00 (16) Yellow iron oxide 3.0 0 (17) Black iron oxide 0.20 (18) Perfume 0.10 Production method: Mix the base components of (1) to (9), heat and melt at 70 ° C to 80 ° C, and then (10), (11 ) Is added and dispersed. On the other hand, (1
The pigment components of 2) to (17) are mixed, added to the above base, and kneaded by a roll mill. The kneaded product is heated and melted, toned and then defoamed,
(18) is added and the mixture is filled in a mold and cooled and solidified.
【００４５】
［実施例２４］ パウダーファンデーション
(1)イソステアリン酸を作用させた酸化チタンの ５．０（重量％）
流動パラフィン分散体（実施例１２）
(2)ミリスチン酸オクチルドデシル ２．５
(3)ワセリン ２．５
(4)パラオキシ安息香酸メチル ０．１
(5)香料 ０．１
(6)針状親油性酸化チタン（実施例１６） ６．０
(7)8-キノリノールを作用させて成る親油性酸化チタン ６．０
粉体（実施例８）
(8)ナイロンパウダー １０．０
(9)マイカ ２０．０
(10)タルク ４２．３
(11)ベンガラ ３．０
(12)黄酸化鉄 ２．０
(13)黒酸化鉄 ０．５
製法：(6)〜(13)の顔料成分を混合し、粉砕機を通して
粉砕する。これを高速ブレンダーに移し、(1)〜(5)を混
合して加え、均一に混合する。これを粉砕機で処理し、
ふるいを通し粒度をそろえた後、金皿に充填して圧縮成
形する。[Example 24] Powder foundation (1) 5.0 (wt%) of titanium oxide treated with isostearic acid Liquid paraffin dispersion (Example 12) (2) Octyldodecyl myristate 2.5 (3) ) Vaseline 2.5 (4) Methyl paraoxybenzoate 0.1 (5) Perfume 0.1 (6) Needle-like lipophilic titanium oxide (Example 16) 6.0 (7) 8-quinolinol Lipophilic titanium oxide 6.0 powder (Example 8) (8) Nylon powder 10.0 (9) Mica 20.0 (10) Talc 42.3 (11) Red iron oxide 3.0 (12) Yellow iron oxide 2 0.0 (13) Black iron oxide 0.5 Manufacturing method: The pigment components of (6) to (13) are mixed and pulverized through a pulverizer. This is moved to a high speed blender, (1) to (5) are mixed and added, and they are mixed uniformly. This is processed with a crusher,
After adjusting the particle size through a sieve, it is filled in a gold plate and compression molded.
【００４６】
［実施例２５］ ツーウェイファンデーション
(1)流動パラフィン ４．０（重量％）
(2)スクワラン ２．０
(3)イソステアリン酸を作用させた酸化チタンの ４．０
メチルフェニルポリシロキサン分散体（実施例１４）
(4)パラオキシ安息香酸メチル ０．１
(5)香料 ０．１
(6)イソステアリン酸を作用させて成る親油性 １０．０
酸化チタン粉体（実施例４）
(7)イソステアリン酸を作用させて成る親油性 ５．０
酸化チタン粉体（実施例６）
(8)シリコーン処理セリサイト ２５．０
(9)シリコーン処理タルク ３０．２
(10)シリコーン処理カオリン ５．０
(11)シリコーン処理ベンガラ ２．５
(12)シリコーン処理黄酸化鉄 ２．０
(13)シリコーン処理黒酸化鉄 ０．１
(14)ポリエチレン末 １０．０
製法：(6)〜(14)の顔料成分を混合し、粉砕機を通して
粉砕する。これを高速ブレンダーに移し、(1)〜(5)を混
合して加え、均一に混合する。これを粉砕機で処理し、
ふるいを通し粒度をそろえた後、金皿に充填して圧縮成
形する。[Example 25] Two-way foundation (1) Liquid paraffin 4.0 (wt%) (2) Squalane 2.0 (3) Titanium oxide 4.0 methylphenylpolysiloxane dispersion treated with isostearic acid (Example 14) (4) Methyl paraoxybenzoate 0.1 (5) Perfume 0.1 (6) Lipophilicity obtained by the action of isostearic acid 10.0 Titanium oxide powder (Example 4) (7) Isostearin Lipophilic 5.0 titanium dioxide powder (Example 6) formed by the action of acid (8) Silicone-treated sericite 25.0 (9) Silicone-treated talc 30.2 (10) Silicone-treated kaolin 5.0 (11) ) Silicone-treated red iron oxide 2.5 (12) Silicone-treated yellow iron oxide 2.0 (13) Silicone-treated black iron oxide 0.1 (14) Polyethylene powder 10.0 Manufacturing method: The pigment components of (6) to (14) are added. Mix and pass through a crusher Grinding. This is moved to a high speed blender, (1) to (5) are mixed and added, and they are mixed uniformly. This is processed with a crusher,
After adjusting the particle size through a sieve, it is filled in a gold plate and compression molded.
【００４７】上記の本発明の実施例１７〜実施例２５に
ついて、使用試験を行った。その際、前記各実施例にお
いて配合した本発明の実施例１〜実施例３，実施例７に
係る酸化チタンのスクワラン分散体をスクワランに、実
施例４〜実施例６に係るイソステアリン酸を作用させて
成る親油性酸化チタン粉体，及び実施例８に係る8-キノ
リノールを作用させて成る親油性酸化チタン粉体をシリ
コーン処理酸化チタンに、実施例９〜実施例１４に係る
酸化チタンの油性溶媒分散体をそれぞれの調製に用いた
油性溶媒に、実施例１６に係る針状親油性酸化チタン粉
体をシリコーン処理針状酸化チタン粉体に代替したもの
を、それぞれ比較例１〜比較例９とした。使用試験は、
２０才代〜５０才代の女性パネラー２０名を１群として
用い、各群に実施例及び比較例のそれぞれをブラインド
にて２週間使用させて行った。使用試験終了後、化粧料
の付き，伸び、透明感、紫外線防御効果、仕上がり感及
び化粧持ちについて官能評価させ、評価結果を以下に示
す評価基準に従って点数化させて２０名の平均値を算出
し、表４に示した。Usage tests were carried out on Examples 17 to 25 of the present invention described above. At this time, the squalane of the titanium oxide squalane according to Examples 1 to 3 and 7 of the present invention blended in each of the above Examples was allowed to act on squalane and the isostearic acid according to Examples 4 to 6 was allowed to act on the squalane. And a lipophilic titanium oxide powder obtained by reacting 8-quinolinol according to Example 8 with silicone-treated titanium oxide, and an oily solvent for titanium oxide according to Examples 9 to 14 Comparative examples 1 to 9 were obtained by replacing the needle-shaped lipophilic titanium oxide powder according to Example 16 with a silicone-treated needle-shaped titanium oxide powder in the oil solvent used for each preparation of the dispersion. did. The usage test is
Twenty female panelists in their twenties to fifties were used as one group, and each group was allowed to use each of the examples and comparative examples for 2 weeks in the blind. After the end of the use test, sensory evaluation was performed on the amount of cosmetics, elongation, transparency, UV protection effect, finish feeling and makeup retention, and the evaluation results were scored according to the following evaluation criteria to calculate the average value of 20 persons. , Shown in Table 4.
【００４８】［化粧料の付き］ 良好 ５点 やや良好 ４点 普通 ３点 やや悪い ２点 悪い １点[With cosmetics] Good 5 points Good 4 points Normally 3 points Two bad points 1 bad point
【００４９】［化粧料の伸び］ 良好 ５点 やや良好 ４点 普通 ３点 やや悪い ２点 悪い １点[Growth of cosmetics] Good 5 points Good 4 points Normally 3 points Two bad points 1 bad point
【００５０】［透明感］ ある ５点 ややある ４点 どちらともいえない ３点 ややない ２点 ない １点[Transparency] There are 5 points There are 4 points 3 points that can not be said 2 points Not 1 point
【００５１】［紫外線防御効果］ 高い ５点 やや高い ４点 普通 ３点 やや低い ２点 低い １点[UV protection effect] 5 points high 4 points which are slightly high Normally 3 points 2 points that are a little low 1 point low
【００５２】［仕上がり感］ 自然である ５点 やや自然である ４点 どちらともいえない ３点 やや不自然である ２点 不自然である １点[Finishing feeling] 5 points that are natural 4 points that are a little natural 3 points that can not be said 2 points that are a little unnatural One point that is unnatural
【００５３】［化粧持ち］ 良好 ５点 やや良好 ４点 普通 ３点 やや悪い ２点 悪い １点[Makeup lasting] Good 5 points Good 4 points Normally 3 points Two bad points 1 bad point
【００５４】[0054]
【表４】 [Table 4]
【００５５】表４より明らかなように、本発明の実施例
使用群では、化粧料の付き及び伸びについて、いずれに
おいてもおおむね良好な評価を得ていた。また、いずれ
においてもほぼ良好な透明感が得られており、普通程度
以上の紫外線防御効果が認められていた。特に実施例２
０使用群では、紫外線防御効果の相乗的な向上が認めら
れた。また、いずれにおいても自然な仕上がり感が得ら
れており、水系や水中油型乳化系の化粧料についても、
ほぼ良好な化粧持ちが得られていた。As is clear from Table 4, in the groups used in the examples of the present invention, generally good evaluation was obtained regarding the sticking and elongation of the cosmetics. In addition, in all cases, almost good transparency was obtained, and a UV protection effect higher than normal was recognized. Especially Example 2
In the 0 use group, a synergistic improvement in the ultraviolet protection effect was observed. Further, in each case, a natural finish feeling is obtained, and also for water-based and oil-in-water emulsion cosmetics,
Almost good makeup lasting was obtained.
【００５６】これに対し比較例使用群では、シリコーン
処理酸化チタン粉体を含有するものを使用した群で化粧
料の付きや伸びに対する評価が低下していた。また、透
明感及び仕上がり感についての評価も悪くなっていた。
比較例１〜比較例３及び比較例５使用群では、有意な紫
外線防御効果は見られなかった。さらに各比較例使用群
において、化粧持ちについての評価が低下していた。On the other hand, in the group using the comparative example, the evaluation of the stickiness and elongation of the cosmetics was lower in the group using the silicone-treated titanium oxide powder. In addition, the evaluations of transparency and finish were also poor.
No significant ultraviolet protection effect was observed in the groups using Comparative Examples 1 to 3 and Comparative Example 5. Furthermore, in each of the groups used in Comparative Examples, the evaluation of makeup retention was decreased.
【００５７】すなわち、本発明の実施例１７〜実施例２
５については、皮膚への付き，伸びが良好で、優れた透
明感と自然な仕上がりが得られ、化粧持ちも良好であっ
た。さらに、有機系紫外線吸収剤や微粒子酸化チタン等
の無機紫外線遮断剤を含有していなくても、ある程度の
紫外線防御効果を有しており、日常生活で曝露する紫外
線の防御に有効であることが示された。また紫外線吸収
剤と併用することにより、紫外線防御効果が相乗的に向
上することが示された。That is, Example 17 to Example 2 of the present invention
Regarding No. 5, the adhesion to the skin and the elongation were good, an excellent transparency and a natural finish were obtained, and the makeup lasting was also good. Furthermore, even if it does not contain an inorganic UV blocking agent such as an organic UV absorber or particulate titanium oxide, it has some UV protection effects and is effective in protecting UV exposure to daily life. Was shown. It was also shown that the UV protection effect was synergistically improved by using it together with the UV absorber.
【００５８】なお本発明の実施例１７〜実施例２５につ
いては、室温で６カ月間保存した場合に、状態の変化は
全く認められなかった。また上記使用試験において、皮
膚刺激性反応や皮膚感作性反応の見られたパネラーは存
在しなかった。Regarding Examples 17 to 25 of the present invention, no change in state was observed when the sample was stored at room temperature for 6 months. In the use test, no panelists showed skin irritation reaction or skin sensitization reaction.
【００５９】[0059]
【発明の効果】以上詳述したように、本発明により、油
性材料への分散性に優れ、紫外線吸収性，光触媒活性，
フォトクロミック性等種々の性状を有し、医薬品，化粧
品，油性塗料，樹脂，吸着剤，イオン交換剤，複合酸化
物前駆体，光学材料，フォトクロミック材料，電子・電
気材料，記録・記憶材料，繊維，光触媒，抗菌・抗黴性
材料，環境汚染物分解除去剤等、幅広い分野で応用し得
る酸化チタンの油性分散体及び親油性酸化チタン粉体を
得ることができ、また特に、紫外線防御効果を有する化
粧料を提供することができた。As described above in detail, according to the present invention, excellent dispersibility in oily materials, ultraviolet absorption, photocatalytic activity,
Having various properties such as photochromic properties, pharmaceuticals, cosmetics, oil paints, resins, adsorbents, ion exchangers, complex oxide precursors, optical materials, photochromic materials, electronic / electric materials, recording / memory materials, fibers, Photocatalysts, antibacterial / antifungal materials, agents for decomposing / removing environmental pollutants, etc., which can be applied in a wide range of fields, to obtain oil dispersions of titanium oxide and lipophilic titanium oxide powders, and especially to have an ultraviolet protection effect. I was able to provide cosmetics.
【図１】本発明の実施例９に係る酸化チタンの油性分散
体について、紫外線照射による色調変化を示す図であ
る。FIG. 1 is a diagram showing a change in color tone of an oil dispersion of titanium oxide according to Example 9 of the present invention when irradiated with ultraviolet rays.
【図２】本発明の実施例９に係る酸化チタンの油性分散
体について、紫外線照射を停止した際の色調変化の消失
を示す図である。FIG. 2 is a diagram showing disappearance of change in color tone when the irradiation of ultraviolet rays is stopped in the oil dispersion of titanium oxide according to Example 9 of the present invention.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平７−25617（ＪＰ，Ａ) 特開 平３−103324（ＪＰ，Ａ) 特開 平３−184905（ＪＰ，Ａ) 特開 平１−230407（ＪＰ，Ａ) 特開 平９−100124（ＪＰ，Ａ) 特開 平６−157648（ＪＰ，Ａ) 特開 平11−171543（ＪＰ，Ａ) 特開 平９−239269（ＪＰ，Ａ) 特開 平11−199230（ＪＰ，Ａ) 特開 平10−265223（ＪＰ，Ａ) 特開 昭63−30706（ＪＰ，Ａ) 特開2000−44242（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) A61K 7/00 - 7/50 C01G 23/053 C09C 1/36 ─────────────────────────────────────────────────── --- Continuation of the front page (56) References JP-A-7-25617 (JP, A) JP-A-3-103324 (JP, A) JP-A-3-184905 (JP, A) JP-A-1- 230407 (JP, A) JP 9-100124 (JP, A) JP 6-157648 (JP, A) JP 11-171543 (JP, A) JP 9-239269 (JP, A) JP-A-11-199230 (JP, A) JP-A-10-265223 (JP, A) JP-A-63-30706 (JP, A) JP-A-2000-44242 (JP, A) (58) Fields investigated ( Int.Cl. 7 , DB name) A61K 7/ 00-7/50 C01G 23/053 C09C 1/36
Claims (7)
液に、分子内に孤立電子対を有する原子及び／又は極性
基を有する有機化合物の１種又は２種以上と、水を添加
して加水分解して得られる酸化チタンの油性分散体であ
って、以下のＡ〜Ｃを満たすことを特徴とする酸化チタ
ンの油性分散体。Ａ：前記油性溶液又は分散液に用いら
れる油性溶媒は、液状植物油類、液状動物油類、炭化水
素油類、液状高級アルコール類、液状エステル油類及び
シリコーン油からなる群より選択される１種又は２種以
上を含む油性溶媒である。Ｂ：前記有機化合物は、カル
ボン酸類又はキレート作用を有する化合物である。Ｃ：
前記酸化チタンは、前記有機化合物が作用している薄片
状又は針状の酸化チタンである。1. An oily solution or dispersion of titanium alkoxide is hydrolyzed by adding one or more organic compounds having an atom having a lone electron pair and / or a polar group in the molecule and water. An oily dispersion of titanium oxide obtained by satisfying the following requirements A to C: A: The oily solvent used in the oily solution or dispersion is one selected from the group consisting of liquid vegetable oils, liquid animal oils, hydrocarbon oils, liquid higher alcohols, liquid ester oils and silicone oils, or It is an oily solvent containing two or more kinds. B: The organic compound is a carboxylic acid or a compound having a chelating action. C:
The titanium oxide is flaky or acicular titanium oxide on which the organic compound acts.
請求項１に記載の酸化チタンの油性分散体。2. The organic compound is isostearic acid,
An oily dispersion of titanium oxide according to claim 1.
請求項１に記載の酸化チタンの油性分散体。3. The organic compound is 8-quinolinol,
An oily dispersion of titanium oxide according to claim 1.
液に、分子内に孤立電子対を有する原子及び／又は極性
基を有する有機化合物の１種又は２種以上と水を添加
し、加水分解する酸化チタンの油性分散体の製造方法で
あって、以下のＡ〜Ｃを満たすことを特徴とする酸化チ
タンの油性分散体の製造方法。Ａ：前記油性溶液又は分
散液に用いられる油性溶媒は、液状植物油類、液状動物
油類、炭化水素油類、液状高級アルコール類、液状エス
テル油類及びシリコーン油からなる群より選択される１
種又は２種以上を含む油性溶媒である。Ｂ：前記有機化
合物がカルボン酸類又はキレート作用を有する化合物で
ある。Ｃ：前記酸化チタンは、前記有機化合物が作用し
ている薄片状又は針状の酸化チタンである。4. Oxidation by hydrolyzing an oily solution or dispersion of titanium alkoxide with one or more organic compounds having an atom having a lone electron pair and / or a polar group in the molecule and water. A method for producing an oily dispersion of titanium, wherein the following A to C are satisfied, the method for producing an oily dispersion of titanium oxide. A: The oily solvent used in the oily solution or dispersion is selected from the group consisting of liquid vegetable oils, liquid animal oils, hydrocarbon oils, liquid higher alcohols, liquid ester oils and silicone oils 1
It is an oily solvent containing two or more species. B: The organic compound is a carboxylic acid or a compound having a chelating action. C: The titanium oxide is flaky or acicular titanium oxide on which the organic compound acts.
請求項４に記載の酸化チタンの油性分散体の製造方法。5. The organic compound is isostearic acid,
The method for producing the oil dispersion of titanium oxide according to claim 4.
請求項４に記載の酸化チタンの油性分散体の製造方法。6. The organic compound is 8-quinolinol,
The method for producing the oil dispersion of titanium oxide according to claim 4.
の油性分散体より選択される１種又は２種以上を含有し
て成る、化粧料。7. A cosmetic comprising one or more selected from the oil dispersions of titanium oxide according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21007399A JP3495296B2 (en) | 1998-07-27 | 1999-07-26 | Oil-based dispersion of titanium oxide, lipophilic titanium oxide powder, method for producing these, and cosmetics containing these |
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22758498 | 1998-07-27 | ||
| JP10-227584 | 1998-07-27 | ||
| JP10-256513 | 1998-09-10 | ||
| JP25651398 | 1998-09-10 | ||
| JP21007399A JP3495296B2 (en) | 1998-07-27 | 1999-07-26 | Oil-based dispersion of titanium oxide, lipophilic titanium oxide powder, method for producing these, and cosmetics containing these |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000143433A JP2000143433A (en) | 2000-05-23 |
| JP3495296B2 true JP3495296B2 (en) | 2004-02-09 |
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ID=27329090
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|---|---|---|---|
| JP21007399A Expired - Fee Related JP3495296B2 (en) | 1998-07-27 | 1999-07-26 | Oil-based dispersion of titanium oxide, lipophilic titanium oxide powder, method for producing these, and cosmetics containing these |
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| JP (1) | JP3495296B2 (en) |
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| Publication number | Publication date |
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