CN1703466A - 还原颜料 - Google Patents
还原颜料 Download PDFInfo
- Publication number
- CN1703466A CN1703466A CNA2003801013047A CN200380101304A CN1703466A CN 1703466 A CN1703466 A CN 1703466A CN A2003801013047 A CNA2003801013047 A CN A2003801013047A CN 200380101304 A CN200380101304 A CN 200380101304A CN 1703466 A CN1703466 A CN 1703466A
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- CN
- China
- Prior art keywords
- ltoreq
- sio
- layer
- tio
- pigment
- Prior art date
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- 239000000049 pigment Substances 0.000 title claims abstract description 128
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 238000000576 coating method Methods 0.000 claims abstract description 42
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 39
- 239000002537 cosmetic Substances 0.000 claims abstract description 26
- -1 ink-jet printing Substances 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 238000007639 printing Methods 0.000 claims abstract description 17
- 239000000976 ink Substances 0.000 claims abstract description 13
- 229920003023 plastic Polymers 0.000 claims abstract description 9
- 239000004033 plastic Substances 0.000 claims abstract description 9
- 239000003973 paint Substances 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 6
- 238000007641 inkjet printing Methods 0.000 claims abstract description 5
- 239000004753 textile Substances 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 210
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 57
- 229910052782 aluminium Inorganic materials 0.000 claims description 54
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 45
- 239000000758 substrate Substances 0.000 claims description 40
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 32
- 239000011248 coating agent Substances 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 26
- 239000012298 atmosphere Substances 0.000 claims description 23
- 230000001590 oxidative effect Effects 0.000 claims description 23
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- 239000010936 titanium Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 17
- 239000004411 aluminium Substances 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000003086 colorant Substances 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 239000011229 interlayer Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 description 45
- 239000000203 mixture Substances 0.000 description 43
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 33
- 230000000694 effects Effects 0.000 description 31
- 229910052710 silicon Inorganic materials 0.000 description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 23
- 239000010703 silicon Substances 0.000 description 23
- 239000000126 substance Substances 0.000 description 22
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 21
- 239000002904 solvent Substances 0.000 description 19
- 238000000151 deposition Methods 0.000 description 16
- 239000002245 particle Substances 0.000 description 16
- 239000003921 oil Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 15
- 235000019198 oils Nutrition 0.000 description 14
- 239000011368 organic material Substances 0.000 description 14
- 239000000377 silicon dioxide Substances 0.000 description 14
- 210000003491 skin Anatomy 0.000 description 14
- 239000004408 titanium dioxide Substances 0.000 description 14
- 238000006722 reduction reaction Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 239000004480 active ingredient Substances 0.000 description 12
- 239000003638 chemical reducing agent Substances 0.000 description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 230000009467 reduction Effects 0.000 description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- 150000002148 esters Chemical class 0.000 description 9
- 150000004706 metal oxides Chemical class 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000000725 suspension Substances 0.000 description 9
- 239000004166 Lanolin Substances 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 8
- 235000019388 lanolin Nutrition 0.000 description 8
- 229940039717 lanolin Drugs 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 238000007740 vapor deposition Methods 0.000 description 8
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 7
- 238000009472 formulation Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical class OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 239000010445 mica Substances 0.000 description 6
- 229910052618 mica group Inorganic materials 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 239000001993 wax Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000006071 cream Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 150000003608 titanium Chemical class 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- DFPAKSUCGFBDDF-UHFFFAOYSA-N Nicotinamide Chemical compound NC(=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-UHFFFAOYSA-N 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004040 coloring Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 239000002674 ointment Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 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 3
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 3
- 241001237961 Amanita rubescens Species 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 241000238631 Hexapoda Species 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 239000000020 Nitrocellulose Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910010282 TiON Inorganic materials 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 3
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- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 3
- 239000008168 almond oil Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
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- 239000007864 aqueous solution Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000002781 deodorant agent Substances 0.000 description 3
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
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- 230000002940 repellent Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 239000006200 vaporizer Substances 0.000 description 3
- 239000002966 varnish Substances 0.000 description 3
- 229940088594 vitamin Drugs 0.000 description 3
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- 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
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- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 2
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 2
- IJFXRHURBJZNAO-UHFFFAOYSA-N 3-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC(O)=C1 IJFXRHURBJZNAO-UHFFFAOYSA-N 0.000 description 2
- VXIXUWQIVKSKSA-UHFFFAOYSA-N 4-hydroxycoumarin Chemical compound C1=CC=CC2=C1OC(=O)C=C2O VXIXUWQIVKSKSA-UHFFFAOYSA-N 0.000 description 2
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
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- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 description 2
- 239000004904 UV filter Substances 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 229940081735 acetylcellulose Drugs 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 230000001166 anti-perspirative effect Effects 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 239000003213 antiperspirant Substances 0.000 description 2
- 235000021302 avocado oil Nutrition 0.000 description 2
- 239000008163 avocado oil Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
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- 239000012876 carrier material Substances 0.000 description 2
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Abstract
本发明涉及片状颜料,所述片状颜料包含通过煅烧TiO2/SiOy或TiO2/金属,特别是TiO2/铝(其中0.03≤y≤1.95,特别是0.03≤y≤1.8,更特别是0.7≤y≤1.8)得到的层,本发明还涉及这些颜料在油漆、纺织品、喷墨印刷、化妆品、涂料、塑料、印刷油墨、陶瓷和玻璃的釉料以及保密印刷中的用途。本发明的颜料的独特之处在于高光泽和非常均匀的厚度,因此色纯度和色强度非常高。
Description
本发明涉及包含通过煅烧TiO2/SiOy(0.03≤y≤1.95)或TiO2/金属(特别是钛、锆、铬或锌,更特别是铝)得到的层的片状颜料,以及该片状颜料在油漆、纺织品、喷墨印刷、化妆品、涂料、塑料、印刷油墨、陶瓷和玻璃的釉料以及保密印刷中的用途。
本发明的颜料的不同之处在于高光泽和非常均匀的厚度,因此色纯度和色强度非常高。
已知的二氧化钛还原颜料基于使用云母或二氧化钛片作为底材。将二氧化钛沉淀于带涂层或不带涂层的底材上,随后还原为钛的低价氧化物。通常用气态还原剂(例如氢气或氨)或金属(例如硅或钛)作为还原剂。
US-B-4,948,631公开了通过在750-850℃下用氨还原涂有二氧化钛的云母颜料特别制备蓝色珠光颜料的方法。
JP H4-20031描述了通过将涂有二氧化钛的云母颜料与钛混合,然后在500-1000℃、真空下将得到的混合物还原,制备有色云母颜料的方法。
DE-A-19618562公开了由二氧化钛、钛的低价氧化物以及其他适当的金属二氧化物或氮氧化钛组成的二氧化钛还原颜料。该颜料可通过下面的方法得到:在环形带上固化可加热水解的钛化合物的水溶液,移除得到的层,再用二氧化钛湿法涂覆得到的二氧化钛片,干燥并适当时在非氧化气氛中煅烧和处理。
但是已知颜料的一个缺点在于遮盖力不足和/或无随角异色效应(color flop)。
DE-A-19843014中描述了基于SiO2片的高光泽、片状的钛还原颜料。该钛还原颜料通过涂有TiO2以及在适当的情况下至少一种其他金属氧化物的SiO2片与至少一种固体还原剂以100∶1-5∶1的比率混合制备,然后在高于600℃下、非氧化性气氛中煅烧该混合物得到。
令人惊奇的是,现已发现具有高光泽和随角异色效应的基于SiOy或金属片(特别是钛、锆、铬或锌片,更特别是铝片)的颜料可通过下面的方法得到:首先在高于600℃、非氧化性气氛中将涂有TiO2的SiOy片(其中0.03≤y≤1.95)或涂有TiO2的金属片(特别是铝片)煅烧,特别对于涂有TiO2的SiOy片而言,然后在适当的情况下在高于200℃,优选高于400℃,特别是500-1000℃下用空气或其他含氧气体处理。
因此本发明涉及包含通过煅烧TiO2/SiOy(其中0.03≤y≤1.95,特别是0.03≤y≤1.80,更特别是0.70≤y≤1.80)或TiO2/金属(特别是TiO2/铝)得到的层的片状颜料,
通常所述片状颜料的颗粒的长度为1μm-5mm,宽度为1μm-2mm,厚度为20nm-2μm,长度与厚度的比率至少为2∶1,该颗粒具有两个基本平行的面,两个面之间的距离为该中心的最短的轴。
本发明的薄片形状不均匀。然而,为了简化起见,认为该薄片具有“直径”。该薄片具有非常好的平行性,并且规定的厚度为平均厚度±30%,特别是±10%最优选±5%该薄片的厚度为20-2000nm,特别是100-350nm。目前优选该薄片的直径的优选范围为大约1-60μm,更优选大约5-40μm。
术语“0.03≤y≤1.95的SiOy”是指氧化硅层上的氧与硅的平均摩尔比率为0.03-1.95。氧化硅层的组成可由ESCA(化学分析用电子能谱法)确定。SiOx、SiOx1、SiOx2、SiOy1、SiOz同此定义。
根据本发明,术语“铝”包含铝和铝合金。铝合金例如G.Wassermann描述于Ullmanns Enzyklopdie der Industriellen Chemie,4.Auflage,Verlag Chemie,Weinheim,Band 7,S.281-292页中的那些。特别适合的为WO00/12634中第10-12页中描述的耐腐蚀的铝合金,所述铝合金除了铝外,还包含小于20%重量,优选小于10%重量的硅、镁、锰、铜、锌、镍、钒、铅、锑、锡、镉、铋、钛、铬和/或铁。
优选所述颜料包含:
(a)SiOz底材层,其中0.03≤z≤2.0,
(b)通过在非氧化性气氛中煅烧TiO2/SiOy,其中0.03≤y≤1.8,得到的中间层,和
(c)TiO2层,或
所述颜料包含:
(a)铝底材层,
(b)通过在非氧化性气氛中煅烧TiO2/铝得到的中间层,和
(c)TiO2层,
特别优选基于SiOz片或铝片的颜料,所述SiOz片或铝片的整个表面涂有TiO2,然后在非氧化性气氛中煅烧。
根据TiO2和SiOy层的厚度以及煅烧工艺选择的工艺参数,整个TiO2或SiOy层可掺入中间层,在这种情况下得到仅有底材层(a)和中间层(b)或者中间层(b)以及TiO2层(c)的片状颜料。
因此在本发明的实施方案中,本发明涉及片状颜料,该颜料颗粒的长度通常为2μm-5mm,宽度为2μm-2mm,厚度为20nm-1.5μm,并且长度与厚度的比率至少为2∶1,该颗粒具有SiOz或铝中心,该SiOz或铝中心具有两个基本平行的平面,两个平行面之间的距离为该中心的最短的轴,并且TiO2层涂覆于该中心的平行面,优选整个表面上,位于SiOz或铝底材和TiO2层之间为通过煅烧TiO2/SiOy(其中0.03≤y≤1.8)得到的中间层。所述颜料在TiO2层上在适当的情况下还可具有其他层。
通常SiOz层的厚度为20-1000nm,优选50-500nm,通常TiO2层的厚度为1-200nm,特别是10-100nm,更特别是20-50nm。
本发明还涉及本发明的颜料在油漆、纺织品(EP02405889.3)、喷墨印刷(EP02405888.5)、化妆品(WO/03076520)、印刷油墨、塑料、涂料(WO03/068868)(特别是汽车罩面漆)、陶瓷和玻璃釉料以及保密印刷中的用途。
基于SiOz或铝片的颜料通过在高于600℃(如果为铝,则低于600℃),优选700-1100℃下,在非氧化性气氛中将涂有TiO2的SiOy片(其中0.03≤y≤1.95,特别是0.03≤y≤1.80,更特别是0.70≤y≤1.80)或涂有TiO2的铝片煅烧10分钟以上,优选15-120分钟得到。特别是基于SiOy片的颜料可随后在高于200℃,优选高于400℃,特别是500-1000℃下用空气或其他含氧气体处理。
涂有TiO2的SiOy片或金属片(特别是铝片)基本上可通过包含以下步骤的方法制得(WO03/068868):
a)在载体上蒸气淀积TiO2层,
b)在由步骤a)得到的TiO2层上蒸气淀积SiOy层或金属层(特别是铝层),以及
c)在由步骤b)中得到的SiOy层或金属层上蒸气淀积TiO2层。
优选在步骤a)之前,将分离剂蒸气淀积在载体上,以制备便于将薄片从载体分离的分离剂层。
但是优选首先制备SiOy或铝薄片,然后通过湿化学涂布将TiO2涂覆在SiOy或铝薄片上。
下面将用铝作为金属层的例子来更详细地说明本发明,而不是对本发明的范围加以限制。
可使用由铝箔冲压得到的铝片或者由已知的雾化和研磨技术制备的铝颜料作为底材。优选使用通过物理蒸气淀积制备的铝薄片(例如参见US-B-4,321,087、WO00/24946)。这种方法包括以下步骤:
a)在载体上蒸气淀积分离剂以制备分离剂层,
b)在分离剂层上蒸气淀积铝层,
c)将分离剂层溶解在溶剂中,并
d)从溶剂中分离铝薄片。
然后可例如根据EP-A-338428,采用化学蒸气淀积(CVD)工艺,用二氧化钛涂覆该铝颜料。在该方法中,在热的流动的铝颗粒存在下,使流化床中的低浓度的TiCl4蒸气与水蒸汽反应。
然后在低于600℃、非氧化性气氛中将涂有TiO2的铝薄片煅烧10分钟以上,优选15-120分钟。
在非氧化性气氛(例如N2、Ar、He、CO2、H2或NH3,优选N2或Ar)中发生还原反应。在使用N2或NH3的情况下,除了生成TiO2-x外,还生成了TiN或TiON。
然后可用其他无机涂料(例如Fe2O3、Cr2O3、CrOOH、SiO2、Al2O3或ZrO2)涂覆涂有TiO2的还原颜料。
特别有利的是使用SiOy薄片作原料。片状SiOy底材(其中0.95≤y≤1.95,优选其中1.0≤y≤1.80)可通过包含以下步骤的方法制得(参见WO03/068868):
a)在载体上蒸气淀积分离剂以制备分离剂层,
b)在分离剂层上蒸气淀积SiOy层,
c)将分离剂层溶解在溶剂中,并
d)从溶剂中分离SiOy薄片。
与天然云母片以及湿法制备的片比较,用上述方法得到的可用的SiOz底材具有非常好的平行性,并且厚度为平均厚度±30%,特别是±10%,最优选±5%。
优选通过在高于1300℃下蒸发硅含量最高可达20%重量的一氧化硅来形成SiOy底材或层(其中0.70≤y≤0.99)。如果在几个10-2帕的工业用真空下,硅(而不是Si/SiO2或SiO/Si)被气化,可得到氧含量小于0.95的硅的氧化物,即SiOx(其中0.03≤x≤0.95,特别是0.05≤x≤0.50,非常特别是0.10≤x≤0.30)(WO03/076520)。
优选步骤b)中的SiOy层(其中0.95≤y≤1.95,优选1.0≤y≤1.80)从含有包含Si和SiO2的混合物、SiOy或其混合物的物料的气化器中蒸气淀积。优选通过在高真空,在如DE-C-4342574和US-B-6,202,591中所述的气化器中将化学计量的细微的硅和石英(SiO2)粉的混合物加热至高于1300℃得到SiOy层。反应产物为一氧化硅气体,在真空下该气体被直接引导至移动载体(passing carrier)上而冷凝为SiO。也可使用非化学计量的混合物。该气化器中的物料包含Si和SiO2的混合物、SiOy或其混合物,这些相互反应的物质(Si和SiO2)的粒径最好小于0.3mm。最好Si与SiO2的重量比为0.15∶1-0.75∶1(以重量份计),优选使用化学计量的混合物。
直接将在气化器中的SiOy汽化。在高于1300℃下Si与SiO2反应生成一氧化硅蒸气。冷凝于载体上的分离剂可为天然漆、聚合物(例如US-B-6,398,999中所述的那些聚合物(热塑性聚合物),特别是丙烯酸或苯乙烯聚合物或其混合物)、可溶于有机溶剂或水并且在真空下可蒸发的有机物(例如蒽、蒽醌、乙酰氨基苯酚、乙酰水杨酸、樟脑酸酐、苯并咪唑、1,2,4-苯三甲酸、2,2-联苯二甲酸、双(4-羟苯基)砜、二羟基蒽醌、己内酰脲、3-羟基苯甲酸、8-羟基喹啉-5-磺酸一水合物、4-羟基香豆素、7-羟基香豆素、3-羟基-2-萘甲酸、间苯二甲酸、4,4-亚甲基-双-3-羟基-2-萘甲酸、1,8-萘二甲酸酐、邻苯二甲酰亚胺及其钾盐、酚酞、吩噻嗪、糖精及其盐、四苯基甲烷、苯并[9,10]菲、三苯基甲醇或至少两种这些物质的混合物)。优选分离剂为可溶于水并且在真空下可蒸发的无机盐(例如参见DE-A-19844357),例如氯化钠、氯化钾、氯化锂、氟化钠、氟化钾、氟化锂、氟化钙、氟化铝钠和四硼酸二钠。
步骤c)通常在高于步骤a)和b)的压力并小于大气压的压力下进行。
优选可移动的载体包含一条或多条带有或不带聚合物涂层的连续的金属带、一条或多条聚酰亚胺或聚对苯二甲酸乙二醇酯带。可移动的载体还可包含一个或多个绕轴旋转的盘、圆筒或其他旋转对称体。
在通过溶解冷凝的分离剂层移走分离剂层和硅的低价氧化物层之前,可在真空下将多个分离剂层和硅的低价氧化物层连续交替蒸气淀积于可移动的载体上。优选通过洗涤并随后过滤、沉淀、离心、倾析或蒸发将SiOy组成的平面平行结构从分离剂的溶剂中分离。此外,还可在洗涤溶剂中溶解的分离剂之后,将硅的低价氧化物(SiOy)组成的平面平行结构(片或薄片)与溶剂一起冷冻,随后冷冻干燥,在低于三相点下将溶剂升华分离,残留的干的硅的低价氧化物为独立的平面平行结构。
冷凝于可移动载体上的硅的低价氧化物对应于式SiOy(其中0.95≤y≤1.8,优选1.0≤y≤1.8),通过在气化器物料中加入过量的硅得到小于1的y值。除了在特别高的真空下,在几个10-2帕的工业用真空下,气化的SiO通常冷凝为SiOy(其中1≤y≤1.8,特别是其中1.1≤y≤1.5),因为高真空设备由于从其表面排放气体而通常包含痕量的水蒸汽,在气化温度下水蒸汽与易反应的SiO反应。
具体地讲,依次将盐(例如NaCl)和硅的低价氧化物(SiOy)蒸气淀积在载体上,该载体可为经过真空度小于0.5Pa的气化器的连续的金属带。蒸气淀积的盐的厚度大约为20-100nm,优选30-60nm,根据产物预期的用途,蒸气淀积的SiO的厚度为20-1000nm,优选50-500nm。下一步,使闭合成环的带状载体通过已知结构的动态真空锁室(参见US-B-6,270,840)进入压力为1-5×104Pa,优选600至109Pa,特别是103至5×103Pa的区域,在该区域中带状载体浸入分离浴中。应当选择溶剂的温度以便其蒸气压在指定的压力范围内。在机械的辅助下,分离剂层快速溶解,产品层破碎成薄片,该薄片随后在溶剂中形成悬浮液。下一步,干燥该带,没有任何污染物粘附于其上。使该带通过的第二组动态真空锁室,回到气化室,在此重复涂覆分离剂和SiOy产物层的过程。
采用已知的技术,然后将两步得到的含有产物结构和溶有分离剂的溶剂的悬浮液进一步分离。为此,首先将所述产物结构在液体中浓缩,并用新鲜的溶剂冲洗多次以洗去溶解的分离剂。然后通过过滤、沉淀、离心、倾析或蒸发来分离仍为湿固体形式的产物并干燥。
可在汽化区中带的前进方向上顺次排列多个分离剂汽化器和产物汽化器。通过这种方法,无需额外添加设备,就可以得到顺序为S+P+S+P的层,其中S为分离剂层,P为产物层。
在大气压下洗涤之后,可通过下面的方法来分离平面平行结构:在温和的条件下冷冻已经将固含量浓缩至大约50%的悬浮液,然后在大约-10℃和50Pa下用已知的方法冷冻干燥该悬浮液。残留的干物质为产物,可将该产物通过涂覆或化学转化进行下一加工步骤。
除了使用连续带,也可根据WO01/25500在带有旋转体的装置中通过分离剂和SiO的蒸气沉积、分离以及干燥载体这些步骤来制备产物。所述旋转体可为一个或多个盘、圆筒或其他旋转对称体。
所述底材也可为多层底材,例如:具有SiOx1中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx2层或SiOy1层;具有SiOx2中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx1层或SiOy1层;具有SiOy1中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx1层或SiOx2层;或具有金属中心(特别是铝)的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx1层、SiOx2层或SiOy1层;其中:0.03≤x1<0.70,特别是0.05≤x1≤0.50,非常特别是0.10≤x1≤0.30,0.70≤x2≤0.99和1.00≤y1≤1.95,特别是1.0≤y1≤1.8,非常特别是1.1≤y1≤1.8(PCT/EP03/50229)。
所述底材还可为具有SiOy/金属反射材料的层结构的底材,优选金属的熔点高于1000℃,例如通过在分离剂上依次蒸气淀积SiOy、金属反射材料和SiOy得到的钛/SiOy。
因此由所述多层底材形成的颜料包含:
(a)多层片状底材层,
(b)通过在非氧化性气氛中煅烧TiO2/SiOx1、TiO2/SiOx2或TiO2/SiOy1得到的中间层,以及
(c)TiO2层,
其中0.03≤x1<0.70,特别是0.05≤x1≤0.50,非常特别是0.10≤x1≤0.30,0.70≤x2≤0.99和1.00≤y1≤1.95,特别是1.0≤y1≤1.8,非常特别是1.1≤y1≤1.8。
SiOy片的涂覆可如WO93/08237中所述用湿法化学法,或者用溶胶-凝胶法,或者如DE-A-19614637中所述用CVD法进行。优选用湿法化学法涂覆SiOy片,可使用例如下列文献中描述的研制珠光颜料的步骤进行:DE-A-1467468、DE-A-1959988、DE-A-2009566、DE-A-2214545、DE-A-2215191、DE-A-2244298、DE-A-2313331、DE-A-2522572、DE-A-3137808、DE-A-3137809、DE-A-3151343、DE-A-3151354、DE-A-3151355、DE-A-3211602、DE-A-3235017、DE-A-1959988、WO93/08237、WO98/53001和WO03/6558。
为了涂覆,将SiOy颗粒悬浮于水中,并在适合水解的pH值下加入一种或多种可水解的钛盐,选择pH值使得钛氧化物或水合钛氧化物直接沉淀在颗粒上,而不会发生二次沉淀。通常通过同时计量地加入碱保持pH值稳定。然后将该颜料分离、洗涤并干燥,并在适当的情况下进行煅烧。如果需要,为了再次悬浮以沉淀其他层,可在已涂覆各个涂层以后,将该颜料分离、干燥并在适当的情况下进行煅烧。
采用类似于例如DE-A-19501307中描述的方法,通过溶胶-凝胶方法,在适当的有机溶剂和碱性催化剂存在下,通过控制一种或多种金属酸酯的水解制备TiO2层。适合的碱性催化剂例如为胺(例如三乙胺、乙二胺、三丁胺、二甲基乙醇胺和甲氧基丙胺)。所述有机溶剂为与水溶混的有机溶剂,例如C1-4醇,特别是异丙醇。
适合的钛酸酯选自钛的烷基和芳基醇化物;羧基化物;羧基、烷基或芳基取代的烷基醇化物或羧基化物。优选钛酸四异丙酯。此外可使用钛的乙酰丙酮化物和乙酰乙酰丙酮化物。优选这种类型的金属酸酯的实例为乙酰丙酮络钛。
根据本发明的一个优选的实施方案,使用US-A-3,553,001中描述的方法涂覆二氧化钛层。将钛盐的水溶液缓慢加入已预加热至大约50-100℃,特别是70-80℃的待涂覆材料的悬浮液中,通过同时计量地加入碱(例如氨水溶液或碱金属氢氧化物水溶液)保持pH值基本稳定为大约0.5-5,特别是大约1.2-2.5。一旦达到了所需厚度的TiO2沉淀层,则停止加入钛盐溶液和碱。
该方法(也称作“滴定”方法)的不同之处在于避免钛盐过量。这一点通过单位时间内向水解液中仅加入用水合TiO2均匀涂覆所需的钛盐量以及单位时间内可被待涂覆颗粒的有效表面所吸附的量。
按照常规工艺得到的基于SiOy片(其中0.03≤y≤1.95,特别是0.03≤x1≤0.70,0.70≤x2≤0.99和1.0<y1≤1.95,特别是1.10≤y1≤1.80)并且包含(a)SiOy底材层和(b)TiO2层的颗粒为新型的颗粒,并且本发明也涉及这些颗粒。如果TiO2层通过湿法化学法沉积在SiOy片上,则TiO2存在于SiOy片的整个表面,包括SiOy片的下表面、上表面以及侧面。
随后在高于600℃,优选700-1100℃下、非氧化性气氛中将涂有TiO2的SiOy片煅烧10分钟以上,优选15-120分钟。在非氧化性气氛(例如N2、Ar和/或He,优选N2或Ar)中或者在真空小于13Pa(10-1托)下发生还原反应。在使用N2或NH3的情况下,除了生成TiO2-x外,还生成了TiN或TiON。
任选将涂有TiO2的SiOy片进行氧化性热处理。例如在高于200℃,优选高于400℃,特别是500-1000℃下将空气或某些其他含氧的气体通过松散材料形式的或者在流化床中的涂有TiO2的SiOy片。然后通过研磨、超声波处理、空气分级或筛分,得到所需粒径的产物,并交付下一步使用。
用上述方法得到的基于SiOy片并且包含(a)SiOz底材层,其中0.03≤z≤2.0,特别是0.10≤z≤2.0,更特别是0.70≤z≤2.0,和(b)通过煅烧TiO2/SiOy得到的中间层,其中0.03≤y≤1.95,特别是0.03≤y≤1.80,更特别是0.70≤y≤1.80,和(c)TiO2层的颜料也为新型颜料,并且本发明也同样涉及这些颜料。
原则上,在起始颜料的表面形成的为锐钛矿形式的TiO2。但是通过加入少量SnO2,在800-900℃下煅烧可转化为金红石结构(参见WO93/08237和US-A-4,086,100)。
在另一个优选的实施方案中,所述底材包含以下顺序的层:
(a1)SiOx1层或SiOx2层,特别是SiOy1层,
(b1)反射层,特别是金属层,和
(c1)SiOx1层或SiOx2层,特别是SiOy1层,其中0.03≤x1<0.70,特别是0.05≤x1≤0.50,非常特别是0.10≤x1≤0.30,0.70≤x2≤0.99和1.00≤y1≤1.95,特别是1.0≤y1≤1.8,非常特别是1.1≤y1≤1.8。
制备包含层(a1)、(b1)、(c1)的底材的方法包括以下步骤:
a)在可移动的载体上蒸气淀积分离剂以制备分离剂层,
b1)在分离剂层上蒸气淀积SiOx1层、SiOx2层或SiOy1层,
b2)在由步骤(b1)得到的层上蒸气淀积反射材料,特别是钛或铝,
b3)在所述金属层上蒸气淀积SiOx1层、SiOx2层或SiOy1层,
c)将分离剂层溶解在溶剂中,和
d)从溶剂中分离氧化硅/反射材料/氧化硅颗粒。
如果省略了(b3)步骤,则得到包含层(a1)和(b1)的不对称颜料。
优选所述反射层由金属反射材料组成,特别是Ag、Al、Au、Cu、Cr、Ge、Mo、Ni、Si、Ti以及这些金属的合金、石墨、Fe2O3或MoS2,特别优选Al或MoS2。如果用铝形成反射层,为了防止铝与相邻层中含有的硅和/或氧化硅反应,则应当避免温度超过600℃,以保留该反射层。如果用铝形成反射层,并将该薄片加热至高于600℃,则铝与相邻层中含有的硅和/或氧化硅反应,反射层转化为透明的硅酸铝层。
如果用铝作为层(b1)的金属,则层(b1)的厚度通常为20-100nm,特别是40-60nm。铝在高于1000℃下气化。
层(a1)和(c1)的厚度通常为2-500nm,特别是50-300nm。
在另一个优选的实施方案中,所述底材包含以下顺序的层:
(a2)SiO0.70-0.99层,
(b2)SiO1.00-1.8层,和
(c2)SiO0.70-0.99层。
制备包含层(a2)、(b2)和(c2)的底材的方法包括以下步骤:
a)在可移动的载体上蒸气淀积分离剂以制备分离剂层,
b1)在分离剂层上蒸气淀积SiOy层,其中0.70≤y≤0.99,
b2)在由步骤(b1)得到的层上蒸气淀积SiOy层,其中1.0≤y≤1.8,
b3)在由步骤(b2)得到的层上蒸气淀积SiOy层,其中0.70≤y≤0.99,
c)将分离剂层溶解在溶剂中,和
d)从溶剂中分离SiO0.70-0.99/SiO1.0-1.8/SiO0.70-0.99颗粒。
如果省略了(b3)步骤,则得到包含层(a2)和(b2)的不对称颜料。
优选步骤b)中的SiO1.00-1.8层通过在高于1300℃下由硅和二氧化硅的混合物在气化器中反应制得的一氧化硅蒸气形成。
优选步骤b)中的SiO0.70-0.99层通过在高于1300℃下蒸发硅含量最高可达20%重量的一氧化硅形成。
在另一个优选的实施方案中,所述底材包含以下顺序的层:
(a3)SiO1.00-1.8层,
(b3)SiO0.70-0.99层,和
(c3)SiO1.00-1.8层。
制备包含(a3)、(b3)和(c3)层的底材的方法包括以下步骤:
a)在可移动的载体上蒸气淀积分离剂以制备分离剂层,
b1)在分离剂层上蒸气淀积SiOy层,其中1.0≤y≤1.8,
b2)在由步骤(b1)得到的层上蒸气淀积SiOy层,其中0.70≤y≤0.99,
b3)在由步骤(b2)得到的层上蒸气淀积SiOy层,其中1.0≤y≤1.8,
c)将分离剂层溶解在溶剂中,
d)从溶剂中分离SiO1.0-1.8/SiO0.70-0.99/SiO1.0-1.8颗粒。
优选步骤b1)和b3)中的SiO1.00-1.8层通过在高于1300℃下由硅和二氧化硅的混合物在气化器中反应制得的一氧化硅蒸气形成。
优选步骤b2)中的SiO0.70-0.99层通过在高于1300℃下蒸发硅含量最高可达20%重量的一氧化硅形成。
如果在几个10-2帕的工业用真空下,硅(而不是Si/SiO2或SiO/Si)被气化,可得到氧含量小于0.95的氧化硅,即SiOx(其中0.03≤x≤0.95)(WO03/076520)。
如果省略了(b3)步骤,得到包含层(a3)和(b3)的不对称颜料。
通常层(b3)的厚度为50-400nm,特别是100-300nm。
通常层(a3)和(c3)的厚度为50-200nm,特别是50-100nm。
通常调节所述颜料的色彩效果的方法有:
-调节TiO2层的厚度,
-调节中间层的厚度,和
-调节中间层的组成。
假设在非氧化性气氛中煅烧TiO2/SiOy产生了引起折光指数改变的中间层。但是,还应考虑所述中间层可能不是连续的层,可能只是TiO2与SiOy界面的个别区域发生了转化,这种转化使得折光指数发生变化。还假设折光指数的变化是由于TiO2被SiOy还原。因此本发明的原理是基于用SiOy(或铝)还原TiO2制备引起折光指数发生变化的中间层。
目前尚不能排除在高于400℃,特别是400-1100℃下,在不含氧的气氛中(即氩气或氦气气氛中)或者小于13Pa(10-1托)的真空中加热TiO2/SiOy颗粒时,除了TiO2被SiOy还原外,SiOy歧化为SiO2和Si(PCT/EP03/50229):
SiOy→(y/y+a)SiOy+a+(1-(y/y+a))Si
在该歧化反应中,生成包含(1-(y/y+a))Si的歧化的SiOy+a薄片,其中0.03≤y≤1.95,特别是0.70≤y≤0.99或1≤y≤1.8,0.05≤a≤1.97,特别是0.05≤a≤1.30,并且y和a的总和等于或小于2,SiOy+a为富氧的硅的低价氧化物。
可采用各种形成附加涂层的涂覆方法。形成涂层的适合方法包括真空蒸气淀积、溶胶-凝胶水解、流化床中的CVD(US-A-5,364,467和US-A-5,763,086)以及电化学沉积。另一种沉积方法是化学物质通过等离子体活化的等离子加强化学蒸气沉积(PECVD)。这种方法的详细描述见WO02/31058。
原则上,所述平面平行颜料还可包含具有“低”折光指数(本文规定的低折光指数是指折光指数大约为1.65或低于1.65)的材料和/或具有“高”折光指数(本文规定的高折光指数是指折光指数大于大约1.65)的材料和/或半透明金属层。可用的各种材料(电介体)包括无机材料(例如金属氧化物、金属氟化物、金属硫化物、金属氮化物、金属碳化物及其组合等)和有机电介体。这些材料易于得到并且可采用物理或化学蒸气淀积工艺涂覆。
可用的适合的低折光指数的电介体包括但不限于二氧化硅(SiO2)、氧化铝(Al2O3)、金属氟化物(例如氟化镁(MgF2)、氟化铝(AlF3)、氟化铈(CeF3)、氟化镧(LaF3)、氟化铝钠(例如Na3AlF6或Na5Al3F14)、氟化钕(NdF3)、氟化钐(SmF3)、氟化钡(BaF2)、氟化钙(CaF2)、氟化锂(LiF)及其混合物)或者折光指数大约为1.65或小于1.65的任何其他低折光指数的材料。可用作低折光指数材料的有机单体和聚合物例如有二烯或链烯(例如丙烯酸酯(例如甲基丙烯酸酯))、全氟链烯烃的聚合物、聚四氟乙烯(TEFLON)、氟化乙烯丙烯的聚合物(FEP)、聚对亚苯基二甲基、对二甲苯及其组合等。上述材料还包括可通过US-B-5,877,895中描述的方法沉积的蒸发的、冷凝的和交联的透明丙烯酸酯层。
适合用作半透明金属层的金属的例子有Cr、Ti、Mo、W、Al、Cu、Ag、Au或Ni。
具有“高”折光指数(即折光指数大于大约1.65,优选大于大约2.0,最优选大于大约2.2)的电介体的实例有硫化锌(ZnS)、氧化锌(ZnO)、氧化锆(ZrO2)、二氧化钛(TiO2)、碳、氧化铟(In2O3)、氧化铟锡(ITO)、五氧化二钽(Ta2O5)、三氧化二铬(Cr2O3)、氧化铈(CeO2)、氧化钇(Y2O3)、氧化铕(Eu2O3)、铁的氧化物如铁(II)/铁(III)的氧化物(Fe3O4)和铁(III)的氧化物(Fe2O3)、氮化铪(HfN)、碳化铪(HfC)、二氧化铪(HfO2)、氧化镧(La2O3)、氧化镁(MgO)、氧化钕(Nd2O3)、氧化镨(Pr6O11)、氧化亚钐(Sm2O3)、三氧化锑(Sb2O3)、一氧化硅(SiO)、三氧化硒(Se2O3)、氧化锡(SnO2)、三氧化钨(WO3)或其组合。优选所述电介体为金属氧化物,该金属氧化物可为具有或不具吸收特性的单一的氧化物或氧化物的混合物,例如TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,特别优选TiO2。
可通过CVD(化学蒸气淀积)或湿法化学涂布法涂覆金属氧化物层。可通过在水蒸汽存在下(对于使用较低分子量的金属氧化物,例如磁铁矿)或氧以及在适当情况下水蒸汽存在下(对于使用例如氧化镍和氧化钴)分解金属羰基化合物得到金属氧化物层。特别可通过以下方法涂覆金属氧化物层:金属羰基化合物(例如五羰基合铁、六羰基合铬;EP-A-45851)的氧化气相分解,或者金属醇化物(例如四正丙醇/四异丙醇钛/锆;DE-A-4140900)或金属卤化物(例如四氯化钛;EP-A-338428)的水解气相分解,或者有机锡化合物(特别是烷基锡化合物,例如四丁基锡和四甲基锡;DE-A-4403678)的氧化分解,或者EP-A-668329中所述的有机硅化合物(特别是二叔丁氧基乙酰氧基硅烷)的气相水解。所述涂覆操作可在流化床反应器(EP-A-045851和EP-A-106235)中进行。最好在涂有铝的颜料的冷却过程中通过控制氧化反应(该反应可在惰性气体中进行)得到Al2O3层(B)(DE-A-19516181)。
可通过在TiO2层上涂覆低折光指数的金属氧化物(例如SiO2、Al2O3、AlOOH、B2O3或其混合物,优选SiO2),然后在金属氧化物层上再涂覆一层TiO2层,得到色彩更强烈并且更透明的颜料(EP-A-892832、EP-A-753545、WO93/08237、WO98/53011、WO98/12266、WO98/38254、WO99/20695、WO00/42111和EP-A-1 213 330)。
可适当地使用下面的方法在TiO2层上涂覆SiO2层(保护层):将计量的苏打水玻璃(soda water glass)溶液加入已加热至大约50-100℃,优选70-80℃的待涂覆材料的悬浮液中,通过同时加入10%的盐酸保持pH为4-10,优选6.5-8.5,加完水玻璃溶液后,再搅拌30分钟。
还可将成品颜料后涂覆或后处理,以进一步提高耐光性、耐候性和耐化学品性或者便于对颜料的操作,特别是加到各种介质中。例如DE-A-2215191、DE-A-3151354、DE-A-3235017、DE-A-3334598、DE-A-4030727、EP-A-649886、WO97/29059、WO99/57204和US-A-5,759,255中描述的方法适用于后涂覆或后处理。
也可采用DE-A-19502231、WO97/39065、WO00/17277以及特别是DE-A-19843014中描述的方法还原存在于颜料表面的TiO2,从而形成钛的低价氧化物、金属氧化物、非金属氧化物、钛的氮化物和/或钛的氧氮化物。
使用的还原剂为气态还原剂(例如氢)或金属粉末、金属合金、金属溴化物、金属碳化物或金属硅化物形式的固体还原剂。优选使用金属/非金属粉末(例如硼、铝、硅、锌或铁),特别是硅或其组合。
也可使用液相或气相的常规还原剂(例如碱金属)。可提及的其他还原剂有氢化物(例如LiH或CaH2)。这些还原剂相互的组合也是合适的还原剂。
将涂有二氧化钛的片与上述固体还原剂以100∶1-5∶1的比率剧烈混合,并在高于600℃,优选700-1100℃下,在非氧化性气氛中处理10分钟以上,优选15-60分钟。
在卤化物(优选氯化物)存在下,还原反应速度增加。特别优选所述卤化物为LiCl、NaCl、KCl、MgCl2、CaCl2、CuCl2、CrCl3、MnCl2、FeCl2、FeCl3、CoCl2、NiCl2或CeCl3。在氯化物(例如CaCl2)存在下,反应温度可降低150-300℃。优选无水氯化物。卤化物的量为涂有TiO2的SiO2片重量的0.1-40%,优选0.5-10%。此外,本发明的颜料还可涂有微溶的附着牢固的无机或有机着色剂。优选使用色淀,特别是铝色淀。为了沉淀氢氧化铝色淀层,在第二步中,使用色淀进行沉淀(DE-A-2429762和DE-A-2928287)。
此外,本发明的颜料还可具有涂有络合物盐颜料,特别是氰基高铁酸盐络合物的附加涂层(EP-A-141173和DE-A-2313332)。
根据DE-A-4009567,本发明的颜料还可涂有有机染料,特别是酞菁染料或金属酞菁染料和/或阴丹酮染料。
有色颜料的制备方法如下:将涂有TiO2的SiOz片与至少一种固体还原剂(优选碱土金属、B、Al、Si、Zn、Fe、LiH、CaH2、Al4C3、Mg2Si、MgSi2、Ca2Si或CaSi2)混合,随后在高于600℃下、非氧化性气氛中将该混合物煅烧10分钟以上。还原反应发生在非氧化性气氛中(例如N2、Ar、He、CO2、H2或NH3,优选N2或Ar)。优选还可使用氢含量优选为3%体积的氢/氮混合物。在使用N2或NH3的情况下,除了生成TiO2-x外,还生成了TiN或TiON。
本发明的颜料的不同之处在于高光泽和非常均匀的厚度,因此色纯度和色强度非常高。
本发明的颜料可用于所有常规的用途,例如着色纺织品、聚合物料、涂料(包括效果涂料、用于汽车的效果涂料)、陶瓷和玻璃的釉料以及印刷油墨(包括用于保密印刷的油墨),并可例如用于化妆品和喷墨印刷中。这类用途可参见参考文献例如“Industrielle OrganischePigmente”(W.Herbst和K.Hunger,VCH Verlagsgesellschaft mbHWeinheim/New York,第2次完全修订版,1995)。
本发明的颜料为效果颜料(金属效果颜料和干涉颜料),也就是说该颜料除了赋予涂覆介质颜色之外,还赋予其他特性,例如随角度不同颜色的变化(随角异色)、闪光(而不是表面光泽)或纹理。对于金属效果颜料,在定向取向的颜料颗粒上发生基本直接的反射。对于干涉颜料,色彩效果由薄的高折射层中的光干涉现象产生。本发明的颜料为角等色的明亮的颜料,并且产生高饱和(明亮)的颜色。因此本发明的颜料特别适合与常规的透明颜料,例如有机颜料(比如二酮基吡咯并吡咯、喹吖啶酮、二噁嗪、苝、异吲哚啉酮等)结合使用。所述透明颜料可具有和所述效果颜料相似的颜色。但是,类似于例如EP-A-388932或EP-A-402943,当透明颜料的颜色与效果颜料的颜色互补时,得到特别令人感兴趣的组合效果。
可用本发明的颜料效果出色地给高分子量有机材料着色。
可用本发明的颜料或颜料组合物着色的高分子量有机材料可为天然或合成来源的高分子量有机材料。通常高分子量有机材料的分子量为大约103-108g/mol或更高。高分子量有机材料可为例如天然树脂、干性油、橡胶、酪蛋白或改性的天然物质(例如氯化橡胶、油改性醇酸树脂、纤维胶、纤维素醚或纤维素酯(例如乙基纤维素、乙酸纤维素、丙酸纤维素、乙酰丁酸纤维素或硝酸纤维素)),但是特别是通过聚合反应、缩聚反应或加成聚合反应得到的全合成有机聚合物(热固性塑料和热塑性塑料)。从聚合树脂的种类上,特别可提及的有聚烯烃(如聚乙烯、聚丙烯或聚异丁烯)、取代的聚烯烃(如氯乙烯、乙酸乙烯酯、苯乙烯、丙烯腈、丙烯酸酯、甲基丙烯酸酯或丁二烯的聚合产物)以及所述单体的共聚产物,特别是ABS或EVA。
在多种加聚树脂和缩聚树脂中,可提及的是甲醛与苯酚的缩合产物(被称作“酚醛塑料”)以及甲醛与脲、硫脲或三聚氰胺的缩合产物(被称作“氨基塑料”)以及用作表面涂料树脂的饱和聚酯(例如醇酸树脂)或不饱和聚酯(例如马来酸酯树脂),还有直链聚酯、聚酰胺、聚氨酯或聚硅氧烷。
所述高分子量化合物可单独存在或以塑性物料或熔融物形式的混合物存在。还可以溶解的单体或聚合状态的形式作为涂料或印刷油墨的成膜剂或粘合剂,例如熟亚麻仁油、硝基纤维素、醇酸树脂、三聚氰胺树脂、脲-甲醛树脂或丙烯酸树脂。
根据目的用途,已证明最好将本发明的效果颜料或效果颜料组合物作为调色剂或者以制剂形式使用。根据调理方法或目的用途,最好在调理工艺之前或之后,往效果颜料中加入一定量的立体花纹改进剂,条件是这样不会对效果颜料在高分子量有机材料(特别是聚乙烯)中的使用产生负面影响。适合的立体花纹改进剂特别为包含至少18个碳原子的脂肪酸(例如硬脂酸或山嵛酸)或其酰胺或其金属盐(特别是镁盐)以及增塑剂、蜡、树脂酸(例如松香酸)、松香皂、烷基苯酚或脂肪醇(例如硬脂醇)或包含8-22个碳原子的脂族1,2-二羟基化合物(例如1,2-十二烷二醇)以及改性的松香马来酸酯树脂或富马酸松香树脂。优选立体花纹改进剂的加入量为最终产物重量的0.1-30%,特别是2-15%。
可以任意染色有效量将本发明的效果颜料加入待染色的高分子量有机材料中。最好已着色的组合物包含高分子量有机材料和占高分子量有机材料的重量的0.01-80%,优选0.1-30%的本发明的效果颜料。实践上通常使用的浓度为1-20%重量,特别是大约10%重量。
高浓度(例如大于30%重量)的着色的组合物通常为浓缩物(“母料”)形式,该浓缩物可用作制备较低颜料含量的着色材料的着色剂,本发明的颜料在常规制剂中具有非常低的粘度,因而该常规制剂仍具有良好的加工性。
可单独加入本发明的效果颜料将有机材料着色。但是为了得到不同的色调或色彩效果,也可除了本发明的效果颜料外,将任意需要量的其他色彩赋予组分(例如白色、有色、黑色或效果颜料)加入到高分子有机物质中。当有色颜料与本发明的效果颜料混合使用时,优选总量为高分子量有机材料重量的0.1-10%。本发明的效果颜料与其他颜色(特别是互补色)的有色颜料的优选的组合物具有特别高的角等色性,在测量角度为10°下,使用所述效果颜料和使用所述有色颜料得到的色彩的色差(ΔH*)为20-340,特别是150-210。
优选本发明的效果颜料与透明有色颜料一起使用,该透明有色颜料可存在于与本发明的效果颜料相同的介质中,也可存在于相邻的介质中。所述效果颜料与所述有色颜料有利地存在于相邻的介质中的分配方式的一个实例为多层效果罩面漆。
用本发明的颜料将高分子量有机材料物质着色的方法如下:使用辊式轧墨机或混合装置或研磨装置将这种颜料(可以适当的母料形式)与所述基质混合;然后使用已知的方法(例如压延、压模、挤出、涂覆、倾倒或注塑),将着色的材料制备成最终需要的形式。可在掺入所述颜料之前或者之后,以常规的量往聚合物中加入塑料工业中的任何常规添加剂(例如增塑剂、填料或稳定剂)。特别是为了制备非刚性的成型物品或者为了降低成型物品的脆性,需要在成型之前往高分子量化合物中加入增塑剂(例如磷酸、邻苯二甲酸或癸二酸的酯)。
为了将涂料和印刷油墨着色,将高分子量有机材料和本发明的效果颜料以及在适当的情况下与常规添加剂(例如填料、其他颜料、干燥剂或增塑剂)一起细微分散于或溶解于相同的有机溶剂或溶剂混合物中,也可将各个组分分别分散或溶解,或者将多种组分一同分散或溶解,然后将所有的组分混合在一起。
在将本发明的效果颜料分散于待染色的高分子量有机材料的过程中,以及在本发明的颜料组合物的加工过程中,优选保持仅产生较低剪切力的条件,以便不会将该效果颜料打碎成更小的片。
本发明的颜料在塑料中的用量为0.1-50%重量,特别是0.5-7%重量。本发明的颜料在涂料中的用量为0.1-10%重量。在粘合剂体系的染色中,例如油漆和用于凹版印刷、胶版印刷或丝网印刷的印刷油墨,颜料在印刷油墨中的掺入量为0.1-50%重量,优选5-30%重量,特别是8-15%重量。在例如塑料、涂料或印刷油墨中,特别是涂料或印刷油墨中、更特别是涂料中得到的色彩的独特之处在于非常良好的特性,特别是非常高的饱和度、突出的牢固性和高的角等色性。当被染色的高分子材料为涂料时,该涂料优选为特殊涂料,最优选为汽车罩面漆。
本发明的颜料还适用于嘴唇或皮肤化妆,或者用于染发或染指甲。
因此本发明还涉及化妆品制剂,所述化妆品制剂包含占其总重量的0.0001-90%的硅/二氧化硅薄片和/或本发明的颜料以及10-99.9999%的化妆品适用的载体物质。
这种化妆品制剂例如为唇膏、胭脂、粉底、指甲油和洗发香波。
可单独或以混合物形式使用本发明的颜料,还可将其与如上所述或化妆品制剂中熟知的其他颜料和/或着色剂结合使用。
优选本发明的化妆品制剂包含占其总重量的0.005-50%的本发明的颜料。
用于本发明的化妆品制剂的适合载体物质包括用于这类组合物的常规材料。
本发明的化妆品制剂可为以下形式:例如棒、软膏、乳膏、乳剂、悬浮液、分散液、粉末或溶液。例如该化妆品制剂为唇膏、睫毛油制剂、胭脂、眼影、粉底、眼线膏、粉或指甲油。
如果制剂为棒状(例如唇膏、眼影、胭脂或粉底),则该制剂包含相当多的脂肪成分,该组分可由一种或多种蜡组成,例如地蜡;羊毛脂;羊毛脂醇;氢化羊毛脂;乙酰化羊毛脂;羊毛脂蜡;蜂蜡;小烛树蜡;微晶蜡;巴西棕榈蜡;鲸蜡醇;硬脂醇;可可脂;羊毛脂脂肪酸;凡士林;矿脂;单、双或三甘油酯或其在25℃下为固体的脂肪酸酯;硅酮蜡(例如甲基十八烷羟基聚硅氧烷和聚(二甲基硅氧基)硬脂氧基硅烷);硬脂酸单乙醇胺;松香及其衍生物(例如乙二醇的松香酯和甘油的松香酯);在25℃下固化的氢化油;蔗糖的甘油酯以及油酸、豆蔻酸、羊毛脂酸、硬脂酸、二羟基硬脂酸的钙盐、镁盐、锆盐和铝盐。
所述脂肪成分还可由至少一种蜡和至少一种油组成,在这种情况下,适合的油例如有:石蜡油、purcelline oil、全氢化角鲨烯、甜杏仁油、鳄梨油、海棠果油、蓖麻油、芝麻油、霍霍巴油、沸点为大约310-140℃的矿物油、硅油(例如二甲基聚硅氧烷)、linoleylalcohol、linolenyl alcohol、油醇、谷物杂醇油(例如小麦胚芽油)、羊毛脂酸异丙酯、棕榈酸异丙酯、豆蔻酸异丙酯、豆蔻酸丁酯、豆蔻酸十六烷酯、硬脂酸十六烷酯、硬脂酸丁酯、油酸癸酯、乙酰甘油酯、醇和多元醇(例如乙二醇和甘油)的辛酸酯和癸酸酯、醇和多元醇(例如鲸蜡醇、异硬脂醇)的蓖麻油酸酯、羊毛醇酸异鲸蜡酯、己二酸异丙酯、月桂酸己酯和辛基十二烷醇。
在这类棒状制剂中脂肪成分的含量通常最高可达该制剂总重量的99.91%。
本发明的化妆品制剂还可包含其他组分,例如有二元醇、聚乙二醇、聚丙二醇、单链烷醇酰胺、无色的填料(聚合的、无机的或有机的)、防腐剂、紫外线滤除剂或化妆品中常规使用的其他助剂和添加剂(例如有天然的或合成的或部分合成的二甘油酯或三甘油酯、矿物油、硅油、蜡、脂肪醇、格尔伯特(Guerbet)醇或其酯)、亲油的功能性化妆品活性成分(包括防日光过滤剂或这类物质的混合物))。
适用于皮肤化妆品的亲油的功能性化妆品活性成分、活性成分组合物或活性组分提取物为可用于皮肤或局部使用的一种组分或多种组分的混合物。可提及的例如有下列物质:
-对皮肤表面和毛发具有清洁作用的活性成分,这些活性成分包括所有可用于清洁皮肤的物质,例如油、皂、合成洗涤剂和固体物质;
-具有祛臭和抑汗作用的活性成分,这些活性成分包括基于铝盐或锌盐的防汗剂、包含杀菌或抑菌祛臭物质的祛臭剂(例如玉洁纯、六氯酚、醇或阳离子物质(如季铵盐))和气味吸收剂(例如Grillocin(蓖麻油酸锌与各种添加剂的组合)或柠檬酸三乙酯(任选与抗氧化剂如丁基羟基甲苯结合)或离子交换树脂);
-防日晒的活性成分(紫外线滤除剂),适合的活性成分为能从阳光中吸收紫外光辐射并将其转化为热的过滤物质(防晒剂),根据需要的作用,优选以下防日光老化剂:选择性地吸收引起晒黑的、波长范围为大约280-315nm的高能量的紫外光辐射并透射较长波长范围(例如315-400nm,即UV-A范围)的防日光老化剂(UV-B吸收剂)和仅吸收315-400nm的UV-A范围的较长波长的紫外光辐射的防日光老化剂(UV-A吸收剂),适合的防日光老化剂例如有以下类型的紫外线吸收剂:对氨基苯甲酸衍生物、水杨酸衍生物、二苯甲酮衍生物、二苯甲酰甲烷衍生物、二苯基丙烯酸酯(diphenyl acrylate)衍生物、苯并呋喃衍生物、包含一个或多个有机硅基团的聚合的紫外光吸收剂、肉桂酸衍生物、樟脑衍生物、三苯胺基-s-三嗪衍生物、苯基苯并咪唑磺酸及其盐、邻氨基苯甲酸酯、苯并三唑衍生物和/或选自涂有氧化铝或二氧化硅的二氧化钛、氧化锌或云母的无机微细颜料;
-防止昆虫的活性组分(驱虫剂),该组分为防止昆虫接触皮肤并在皮肤上活动的试剂,它们将昆虫驱走,并且蒸发缓慢,最常用的驱虫剂为二乙基甲苯甲酰胺(避蚊胺),其他常见的驱虫剂例如可参见“Pflegekosmetik”(W.Raab和U.Kindl,Gustav-Fischer-VerlagStuttgart/New York,1991)第161页;
-保护免受化学和物理影响的活性组分,这些活性组分包括在皮肤与外界有害物质之间形成屏障的所有物质,例如用来保护皮肤以防水溶液的石蜡油、硅油、植物油、PCL产物和羊毛脂,保护皮肤以防有机溶剂作用的成膜剂(例如海藻酸钠、海藻酸三乙醇胺、聚丙烯酸酯、聚乙烯醇或纤维素醚)或保护皮肤以抵抗皮肤上强烈的机械应力的作为“润滑剂”的基于矿物油、植物油或硅油的物质;
-润湿剂,例如以下物质可用作湿度调节剂(润湿剂):乳酸钠、尿素、醇、山梨醇、甘油、丙二醇、胶原蛋白、弹性蛋白和透明质酸;
-具有角质增生作用的活性成分:过氧化苯甲酰、视黄酸、胶体硫和间苯二酚;
-抗微生物剂,例如玉洁纯或季铵化合物;
-可用于皮肤的油性或油溶性维生素或维生素衍生物,例如维生素A(游离酸或其衍生物形式的视黄醇)、泛醇、泛酸、叶酸及其混合物、维生素E(生育酚)、维生素F、必需脂肪酸或烟酰胺(烟酸酰胺);
-维生素基胎盘提取物,其活性成分组合物特别包含维生素A、C、E、B1、B2、B6、B12、叶酸、维生素H、氨基酸和酶以及微量元素镁、硅、磷、钙、锰、铁或铜的化合物;
-皮肤修复复合物,得自双歧乳杆菌细菌的非活性培养物和分解培养物;
-植物和植物提取物,例如山金车、芦荟、须地衣、常春藤、荨麻、人参、指甲花、洋甘菊、万寿菊、迷迭香、鼠尾草、问荆或百里香;
-动物提取物,例如蜂王浆、蜂胶、蛋白质或胸腺提取物;
-可用于皮肤的化妆品用油,例如有:Miglyol 812型中性油、杏仁油、鳄梨油、巴巴苏油、棉籽油、琉璃苣油、蓟油、花生油、γ-米谷酚、玫瑰籽油、大麻油、榛实油、黑醋栗籽油、霍霍巴油、樱桃核油、鲑鱼油、亚麻籽油、玉米油、夏威夷果油、杏仁油、月见草油、貂油、橄榄油、山核桃油、桃仁油、开心果油、菜油、rice-seedoil、蓖麻油、红花油、芝麻油、大豆油、葵花籽油、茶树油、葡萄籽油或小麦胚芽油。
优选所述棒状制剂为无水的,但是在某些情况下可包含通常不超过化妆品制剂总重量的40%的水。
如果本发明的化妆品制剂为半固体形式的产品,也就是说以软膏或乳膏形式,则同样也可无水或含水。这类制剂例如有睫毛油、眼线膏、粉底、胭脂、眼影或治疗眼袋(ring under the eyes)的组合物。
另一方面,如果这种油膏或乳膏含水,则特别是油包水或水包油类型的乳液,该乳液除了颜料外,还包含1-98.8%重量的脂肪相,1-98.8%重量的水相和0.2-30%重量的乳化剂。
这种软膏和乳膏还可包含其他常规的添加剂,例如有香料、抗氧化剂、防腐剂、胶凝剂、紫外线滤除剂、着色剂、颜料、珠光剂、无色聚合物以及无机或有机填料。
如果所述制剂为粉末形式,则该制剂主要由矿物、无机或有机填料(例如滑石粉、高岭土、淀粉、聚乙烯粉末或聚酰胺粉末)以及助剂(例如粘合剂、着色剂)等组成。
这种制剂还可包含各种常规用于化妆品中的助剂,例如香料、抗氧化剂、防腐剂等。
如果本发明的化妆品制剂为指甲油,则该制剂主要由硝酸纤维素和以溶剂体系中的溶液形式的天然的或合成的聚合物组成,该溶液可包含其他助剂(例如珠光剂)。
在本发明的实施方案中,所述有色聚合物的量为大约0.1-5%重量。
本发明的化妆品制剂还可用于染发,在这种情况下,可使用由常规用于化妆品工业的基础物质和本发明的颜料组成的香波、乳膏或凝胶形式的制剂。
可使用常规方法制备本发明的化妆品制剂,例如将各组分混合或搅拌在一起,任选加热以熔化该混合物。
下面的实施例举例说明了本发明,但不限制本发明的范围。除非特别说明,否则百分数和份数均以重量计。
实施例
实施例1
在高真空下,将一层TiO2(100nm)、一层SiO(100nm)和一层TiO2(100nm)按顺序升华在一块玻璃板上。一个试样(试样1)用作对照样品,另一个试样(试样2)在550℃、氮气气氛下加热2小时。
试样1和试样2在10度和65度的反射光谱见图1。从图1明显看出煅烧使反射最大值发生了变化,但反射最小值没有变化,表明在TiO2/SiO界面的折光指数发生了变化,推测这种变化是因为TiO2被SiO还原所致。
试样1和试样2的L*、a*、b*、c*和h值(CIE LAB体系)见下表:
试样 | 是否煅烧 | 观察角度(度) | L* | a* | b* | c* | h |
1 | 否 | 10 | 44.2 | 10.3 | 9.9 | 14.3 | 44.1 |
2 | 是 | 10 | 45.5 | 16 | 14.6 | 21.7 | 42.3 |
1 | 否 | 65 | 65.7 | 11.6 | 15.4 | 19.3 | 52.9 |
2 | 是 | 65 | 67.3 | 12 | 19.8 | 23.1 | 58.8 |
实施例2
在小于0.1Pa的真空下,通过SiO的升华制备SiOy薄片。所述底材预先涂覆100nm厚的NaCl分离层。用去离子水洗涤该底材,得到的薄片用去离子水洗涤以除去NaCl并干燥。得到厚度为245nm±5%的白色SiOy薄片。在用反射光工作的显微镜下,观察到该SiOy薄片为蓝色。在空气中最大反射系数小于10%。
将190mg所述SiOy薄片加入44ml去离子水中,并在超声波浴中搅拌10分钟。用65%的硝酸将该悬浮液的pH值调节为1.4。然后将该悬浮液加热至75℃,并在60分钟内、快速搅拌下加入总量为1ml的TiOCl2。通过连续加入NaOH保持pH值为1.4。
然后将该悬浮液在75℃下再搅拌2小时,接着冷却并过滤。在50℃下干燥得到薄片。在用背光模式工作的显微镜下,观察到该涂有TiO2的SiOy薄片为黄绿色。观察到在透明瓶子中的相同的涂有TiO2的SiOy薄片为白绿色。随在小于10Pa的真空、700℃下将该粉末加热2小时。加热后,观察到在透明瓶子中的该涂有TiO2的SiOy薄片为明亮的绿色。在显微镜下(用反射光工作)观察到该涂有TiO2的SiOy薄片的颗粒为明亮的黄绿色,并且最大反射系数高于20%。
Claims (11)
1.一种片状颜料,所述片状颜料包含在非氧化性气氛中通过煅烧TiO2/SiOy或TiO2/金属得到的层,其中0.03≤y≤1.95,特别是0.03≤y≤1.8,更特别是0.70≤y≤1.8,且所述金属特别是钛、锆、铬或锌,更特别是铝。
2.权利要求1的颜料,所述颜料包含:
(a)SiOz底材层,其中0.03≤z≤2.0,特别是0.10≤z≤2.0,更特别是0.70≤z≤2.0,
(b)在非氧化性气氛中通过煅烧TiO2/SiOy得到的中间层,其中0.03≤y≤1.8,和
(c)TiO2层。
3.权利要求1的颜料,所述颜料包含:
(a)铝底材层,
(b)在非氧化性气氛中通过煅烧TiO2/铝得到的中间层,和
(c)TiO2层。
4.权利要求1的颜料,所述颜料包含:
(a)具有SiOx1中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx2层或SiOy1层;具有SiOx2中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx1层或SiOy1层;具有SiOy1中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx1层或SiOx2层;或具有金属、特别是铝中心的多层片状底材层,在该中心的上下表面,但不是侧面有SiOx1层、SiOx2层或SiOy1层,
(b)在非氧化性气氛中通过煅烧TiO2/SiOx1、TiO2/SiOx2或TiO2/SiOy1得到的中间层,以及
(c)TiO2层,其中0.03≤x1<0.70,特别是0.05≤x1≤0.50,非常特别是0.10≤x1≤0.30,0.70≤x2≤0.99和1.00≤y1≤1.95,特别是1.0≤y1≤1.8,非常特别是1.1≤y1≤1.8。
5.权利要求2的颜料,其中所述底材层的厚度为20-1000nm,优选为50-500nm。
6.权利要求2或5中任一项的颜料,其中所述中间层的厚度为1-500nm,优选为10-50nm。
7.权利要求2、5和6中任一项的颜料,其中所述TiO2层的厚度为1-200nm,特别是10-100nm,更特别是20-50nm。
8.一种制备权利要求1的颜料的方法,所述方法包括:
(a)在高于600℃下、非氧化性气氛中煅烧涂有TiO2的SiOy片或涂有TiO2的金属片,其中0.03≤y≤1.95,特别是0.03≤y≤1.8,更特别是0.7≤y≤1.8,所述金属片特别是铝片,和
(b)任选在高于200℃,优选高于400℃,特别是500-1000℃下用空气或其他含氧气体处理所述涂有TiO2的SiOy片。
9.一种通过权利要求8的方法得到的颜料。
10.权利要求1-7中任一项或权利要求9的颜料单独或其与常规商品颜料的组合在油漆、纺织品、喷墨印刷、化妆品、涂料、印刷油墨、塑料、陶瓷和玻璃的釉料以及保密印刷中的用途。
11.一种包含权利要求1-7中任一项或权利要求9的颜料的化妆品制剂、着色剂、涂料、印刷油墨、塑料或陶瓷和玻璃的釉料。
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2003
- 2003-10-06 CN CNA2003801013047A patent/CN1703466A/zh active Pending
- 2003-10-06 EP EP03808738A patent/EP1554352B1/en not_active Expired - Lifetime
- 2003-10-06 CA CA002494902A patent/CA2494902A1/en not_active Abandoned
- 2003-10-06 US US10/530,098 patent/US7510765B2/en not_active Expired - Fee Related
- 2003-10-06 KR KR1020057006600A patent/KR101015030B1/ko not_active IP Right Cessation
- 2003-10-06 WO PCT/EP2003/050690 patent/WO2004035694A1/en active Application Filing
- 2003-10-06 AU AU2003301270A patent/AU2003301270A1/en not_active Abandoned
- 2003-10-06 RU RU2005115067/15A patent/RU2005115067A/ru not_active Application Discontinuation
- 2003-10-06 JP JP2004544297A patent/JP4820549B2/ja not_active Expired - Fee Related
- 2003-10-06 MX MXPA05001941A patent/MXPA05001941A/es not_active Application Discontinuation
- 2003-10-07 CN CNB2003801015517A patent/CN100352865C/zh not_active Expired - Fee Related
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110724396A (zh) * | 2019-09-24 | 2020-01-24 | 河北欧克新型材料股份有限公司 | 耐温黑色珠光颜料及其制备方法 |
CN110724396B (zh) * | 2019-09-24 | 2021-10-01 | 河北欧克新型材料股份有限公司 | 耐温黑色珠光颜料及其制备方法 |
Also Published As
Publication number | Publication date |
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JP4820549B2 (ja) | 2011-11-24 |
RU2005115067A (ru) | 2006-01-27 |
CA2494902A1 (en) | 2004-04-29 |
AU2003301270A1 (en) | 2004-05-04 |
EP1554352A1 (en) | 2005-07-20 |
CN100352865C (zh) | 2007-12-05 |
MXPA05001941A (es) | 2005-04-28 |
JP2006503146A (ja) | 2006-01-26 |
KR101015030B1 (ko) | 2011-02-16 |
CN1705720A (zh) | 2005-12-07 |
KR20050048690A (ko) | 2005-05-24 |
WO2004035694A1 (en) | 2004-04-29 |
EP1554352B1 (en) | 2012-08-01 |
US20050287090A1 (en) | 2005-12-29 |
US7510765B2 (en) | 2009-03-31 |
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