TWI395794B - 干涉顏料 - Google Patents
干涉顏料 Download PDFInfo
- Publication number
- TWI395794B TWI395794B TW092135451A TW92135451A TWI395794B TW I395794 B TWI395794 B TW I395794B TW 092135451 A TW092135451 A TW 092135451A TW 92135451 A TW92135451 A TW 92135451A TW I395794 B TWI395794 B TW I395794B
- Authority
- TW
- Taiwan
- Prior art keywords
- layer
- flakes
- pigment
- sio
- glass
- Prior art date
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- 239000000049 pigment Substances 0.000 title claims abstract description 165
- 239000010410 layer Substances 0.000 claims abstract description 110
- 239000011521 glass Substances 0.000 claims abstract description 78
- 238000000576 coating method Methods 0.000 claims abstract description 73
- 239000000203 mixture Substances 0.000 claims abstract description 52
- 239000011248 coating agent Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 239000002537 cosmetic Substances 0.000 claims abstract description 20
- 239000000976 ink Substances 0.000 claims abstract description 16
- 238000009472 formulation Methods 0.000 claims abstract description 14
- 239000004033 plastic Substances 0.000 claims abstract description 13
- 229920003023 plastic Polymers 0.000 claims abstract description 13
- 238000007639 printing Methods 0.000 claims abstract description 11
- 239000000123 paper Substances 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000010330 laser marking Methods 0.000 claims abstract description 5
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000011241 protective layer Substances 0.000 claims abstract description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 73
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 239000010445 mica Substances 0.000 claims description 11
- 229910052618 mica group Inorganic materials 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 239000002250 absorbent Substances 0.000 claims description 6
- 230000002745 absorbent Effects 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 230000002829 reductive effect Effects 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 claims description 4
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims 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 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000000454 talc Substances 0.000 claims description 3
- 229910052623 talc Inorganic materials 0.000 claims description 3
- 239000003021 water soluble solvent Substances 0.000 claims description 3
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- IAOQICOCWPKKMH-UHFFFAOYSA-N dithieno[3,2-a:3',2'-d]thiophene Chemical compound C1=CSC2=C1C(C=CS1)=C1S2 IAOQICOCWPKKMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 claims description 2
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 claims description 2
- 239000002923 metal particle Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000012736 aqueous medium Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 claims 1
- 230000003301 hydrolyzing effect Effects 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 16
- 239000006096 absorbing agent Substances 0.000 abstract description 2
- 239000003125 aqueous solvent Substances 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 58
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 57
- 229910044991 metal oxide Inorganic materials 0.000 description 21
- 150000004706 metal oxides Chemical class 0.000 description 21
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 21
- 239000008367 deionised water Substances 0.000 description 20
- 229910021641 deionized water Inorganic materials 0.000 description 20
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 17
- 239000000725 suspension Substances 0.000 description 15
- 239000011651 chromium Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 10
- 239000003086 colorant Substances 0.000 description 9
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000004922 lacquer Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 8
- 235000019353 potassium silicate Nutrition 0.000 description 7
- 239000012463 white pigment Substances 0.000 description 7
- 239000000020 Nitrocellulose Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 6
- 238000001354 calcination Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 229920001220 nitrocellulos Polymers 0.000 description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- -1 TiO 2 Chemical class 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 4
- 239000002671 adjuvant Substances 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 235000012730 carminic acid Nutrition 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910017089 AlO(OH) Inorganic materials 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229920000106 Liquid crystal polymer Polymers 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- POJWUDADGALRAB-UHFFFAOYSA-N allantoin Chemical compound NC(=O)NC1NC(=O)NC1=O POJWUDADGALRAB-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 2
- 229940063656 aluminum chloride Drugs 0.000 description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 239000012860 organic pigment Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000006072 paste Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- XMTQQYYKAHVGBJ-UHFFFAOYSA-N 3-(3,4-DICHLOROPHENYL)-1,1-DIMETHYLUREA Chemical compound CN(C)C(=O)NC1=CC=C(Cl)C(Cl)=C1 XMTQQYYKAHVGBJ-UHFFFAOYSA-N 0.000 description 1
- POJWUDADGALRAB-PVQJCKRUSA-N Allantoin Natural products NC(=O)N[C@@H]1NC(=O)NC1=O POJWUDADGALRAB-PVQJCKRUSA-N 0.000 description 1
- 241001076973 Aroma Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000258937 Hemiptera Species 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910017639 MgSi Inorganic materials 0.000 description 1
- 229910017625 MgSiO Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 235000013838 Osmorhiza longistylis Nutrition 0.000 description 1
- 244000223081 Osmorhiza longistylis Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009418 agronomic effect Effects 0.000 description 1
- 229960000458 allantoin Drugs 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000005293 duran Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- WQXNXVUDBPYKBA-YFKPBYRVSA-N ectoine Chemical compound CC1=[NH+][C@H](C([O-])=O)CCN1 WQXNXVUDBPYKBA-YFKPBYRVSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- UQPHVQVXLPRNCX-UHFFFAOYSA-N erythrulose Chemical compound OCC(O)C(=O)CO UQPHVQVXLPRNCX-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 1
- 229910000271 hectorite Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000006115 industrial coating Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000077 insect repellent Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
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- 238000000691 measurement method Methods 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000006254 rheological additive Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0051—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating low and high refractive indices, wherein the first coating layer on the core surface has the low refractive index
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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Description
本發明係關於以經塗覆的薄片形式基材為主的干涉顏料及應用,尤其是使用於塗料、塗層、油墨、塑膠及使用於化妝品配方。
干涉顏料在工業上許多領域可用作為光澤或金屬效果顏料,尤其是用於裝飾性塗層,用於塑膠,用於塗料、塗層、油墨及用於化妝品配方。介於複數的干涉顏色之間可展現角度依存性顏色表現的顏料,由於其顏色展現,特別可用於汽車塗料,防偽保全及用於裝飾性化妝品。
干涉顏料一般由薄片形式擔體組成,在其上塗以薄的金屬氧化物層。此類顏料之光學效應係基於由主要平行排列薄片對光的定向反射。具有不同折射率之各層界面上對光的反射,導致形成干涉顏色(G. Pfaff,在High Performance Pigments,Wiley-VCH Verlag,Weinheim,2002年,第七章,特殊效果顏料)。
U.S.3,331,699敘述珍珠光彩顏料,其具有明亮干涉顏色及強的閃亮效應。此顏料主要由玻璃薄片所組成,在其上塗覆有半透明的高折射率金屬氧化物層。適合的金屬氧化物有ZrO2
、TiO2
及Cr2
O3
。在此顏料的顏色係取決於所選擇的金屬氧化物,且取決於金屬氧化物之層厚。經由不同層厚可造成許多干涉顏色,從銀色至金色、紫色、藍
及綠色。針對帶有金屬氧化物的塗層,在此玻璃組成物不具有定性的影響。然而,為了達成完全塗覆,絕對必須在玻璃表面上存在成核劑,例如二氧化錫或薄水鋁石。
WO 97/46624敘述珍珠光彩顏料,其係以玻璃薄片為主的,且塗以TiO2
或Fe2
O3
。
若在擔體上薄的金屬層非常光滑且均勻,僅能得到光輝顏料。WO 97/46624敘述塗層必須強力黏附在擔體上,以使得在加工期間塗層不會斷裂及/或分離。使用者感知不充分的金屬氧化物層對擔體之黏合,而呈現不良的顏料之機械穩定性,因為於施加機械應力期間光澤會大幅地下降,例如在下列各項期間的摩擦中之剪力:化妝品製劑中的顏料在皮膚上、在印刷方法中、在製作顏料顆粒中,或於塗料廠圓形環線生產期間。甚至小比例之受損顏料微粒將會導致顯著的施用顏料之顏色性質受損。
由於所使用的玻璃型態,來自U.S.3,331,639及WO 97/46624的顏料,僅可在低於600℃的溫度鍛燒。然而,在此600℃之溫度不代表嚴格的限制,但卻成為一項技術須求妥協而難於統合。
帶有已在低溫下鍛燒的TiO2
層之顏料,可展現增加的光活性,尤其是加入塑膠系統中,且不適用於強曝光或長期持續曝光的物品。其原因為沈澱金屬氧化物層的孔隙度及大的活化表面積,其僅在700℃的鍛燒溫度硬化。此硬化可造成金屬氧化物層孔隙度的降低,且同時提高折射率且如此可改良顏料的光學性質。然而,在較高的溫度下
,經由玻璃核大量的軟化,且因此薄片變形與塗層的斷裂及/或分離,將破壞顏料。甚至在600℃或更低之鍛燒溫度,可能發生黏合至擔體上之層的降低,削弱顏料之機械穩定性。在實用上該顏料只能以有限程度使用。
EP 0 753 545 B1揭示基於高折射率、透明的、非金屬的、薄片形式基材之角度變色光澤顏料,其至少包含一層包裝層,該包裝層內含射率n≦1.8的無色的塗層與選擇或非選擇反射吸收劑塗層。適合的基材,例如有薄片形式氧化鐵、BiOCl、TiO2
或ZrO2
塗覆的雲母,其折射率n為≧2。角度變色光澤顏料展現介於複數的強干涉顏色之間的角度依存的顏色展現,且如此有顯著的顏色變化,在許多工業應用上這是有利的,在裝飾性應用上頻繁地需要它,但在珍珠光彩顏料的主要應用上卻不希望發生。
WO 01/30920揭示有高遮蔽率金色及橙色的色彩干涉顏料,其優越性在於在薄片形式基材上塗覆至少二層,此二層中包含低折射率層與高折射率層,其中包含下列Fe2
O3
與TiO2
之金屬氧化物混合物。針對低折射率塗層,可提及下列材料:SiO2
、Al2
O3
、AlO(OH)、B2
O3
、MgF2
、MgSiO3
或此類之混合物氧化物。然而,作為WO 01/30920中顏料主要特色,在於主體色彩與遮蔽率高,且由於混合氧化物層與生俱來的吸收。如此,僅可得到高遮蔽率的金色與橙色彩色顏料。其僅可得到具有高光澤的銀白色顏料,作為具有明亮干涉顏色及高透明度的高光澤顏料。在下列產業中有需求印刷技藝:塑膠,用於化
妝品的表面塗層及,尤其是用於具有改良光澤的銀白色顏料。
本發明之目的在提供銀白色干涉顏料,其具有高光澤及高光澤干涉顏料,該顏料具有明亮干涉顏色,其在機械上係穩定的,且可簡單地製備,且優越性在於其進一步有利的技術性質。
出人意外地,目前已發現,若將薄片塗覆以第一層的SiO2
,然後再於其上施用高折射率層,例如二氧化鈦、低氧化鈦、氧化鋯、氧化錫、氧化鉻、Fe2
O3
或Fe3
O4
,以透明的薄片形式基材為主的干涉顏料具有改良的光澤,且展現更強顏色。
除了其較高的光澤之外,具有玻璃薄片作為擔體的本發明顏料,優於先前技藝中經塗覆的玻璃薄片者,在於顯著改良的鍛燒行為。以玻璃薄片為主的本發明干涉顏料,可在>700℃溫度鍛燒而未發生變形或薄片結構破壞。
如此,本發明干涉顏料清楚地優於先前技藝的顏料,不僅在於其光學性質,如光澤及色強度,同時也在於其技術性質,例如機械穩定性及光穩定性。
因本發明係關於以薄片形式基材為主的干涉顏料,其優越之處在於其包含(A)一層的SiO2
,其層厚為5-350 nm,(B)一高折射率塗層,折射率n>1.8及/或
(C)由高與低折射率層交替組成的干涉系統及視需要的(D)外保護層。
此外本發明係關於將本發明干涉顏料使用於塗料、塗層,尤其是汽車塗料、粉末塗層、油墨、保全油墨、塑膠、陶瓷材料、玻璃、紙,使用於電子照相印刷方法的調色劑,使用於種子,使用於溫室薄板及帳篷布篷,作為在雷射標誌的紙及塑膠上吸收劑,及使用於化妝品配方。此外,本發明顏料亦適用於與水、有機及/或水溶性溶劑製備顏料糊狀物,及用於製備顏料製劑及乾燥製劑,例如顆粒、碎片、顆粒、磚狀物等。乾燥製劑特別適用於油墨及化妝品中。
針對本發明干涉顏料中適合的基本基材為無色的或選擇或非選擇性吸收劑薄片形式基材。適合的基材尤其有葉狀矽酸鹽,如天然的及/或合成的雲母、滑石粉、高嶺土、薄片形式的氧化鐵或氧化鋁、玻璃薄片、SiO2
薄片、TiO2
薄片、石墨薄片、合成的無支撐薄片、氮化鈦、矽化鈦、液晶聚合物(LCPs)、全像顏料、BiOCl及薄片形式混合氧化物、或其混合物。特別較佳的基材為玻璃薄片、雲母薄片及Al2
O3
薄片。
特別優先者為玻璃薄片,這是由於其特別光滑的表面且有非常高反射性。
基礎基材本身尺寸並不具有定性。且可被與特定的應用相配合。一般而言,薄片形式基材的厚度在介於0.005
與10μm之間,尤其是在0.1與5μm之間。另二個其它範圍尺寸一般在1-500μm,較佳為2-300μm且尤其是20-200μm。較佳的較小的粒徑範圍在1-100μm,尤其是5-60μm及1-15μm。
特別優先者為平均厚度在<2μm的玻璃薄片。較厚的薄片一般不能使用於一般的印刷方法且不能使用於嚴苛要求的最終塗飾。玻璃薄片之厚度宜在<1μm,尤其是<0.9μm,非常特別較佳為<0.7μm。特別優先者為厚度在0.25-0.7μm的玻璃薄片。玻璃薄片直徑宜在5-300μm,特別宜為10-100μm,更佳為5-60μm。具有此類尺寸的玻璃薄片,可經由例如敘述於EP 0 289 240的方法製備。
在此的玻璃薄片可包含已知於熟悉此技藝的專業人士的所有玻璃型態,例如窗戶玻璃、C玻璃、E玻璃、ECR玻璃、Duran®
玻璃、實驗室設備玻璃或光學玻璃。特別優先者為E玻璃或ECR玻璃。玻璃薄片的折射率宜在1.45-1.80,尤其是1.50-1.70。
然而,由於此塗層帶有SiO2
層(層(A)),針對進一步塗層與生成的顏料之技術性質,玻璃薄片之化學組成為第二重要的。此SiO2
塗層可保護玻璃表面對抗化學的改良,如膨潤、玻璃組分的溶出或溶解在強性的酸性塗層溶液中。
於鍛燒加工期間,針對在介於玻璃主體與沈澱在其上的SiO2
之間界面的玻璃薄片,介於化學上相關的材料之
間的緊密鍵結將會提高。由於高的軟化溫度,沈澱在其上的SiO2
鞘將賦予基材必需的機械穩定性,甚至當鍛燒至700℃以上。在SiO2
層之後的高折射率塗層之黏合亦非常良好,甚至在700℃以上。
取決於所需要之效應,在基材上層(A)之厚度可在寬廣範圍中變化。層(A)之厚度在5-350 nm,較佳為5-150 nm。為控制光澤及色強度,層厚在30-100 nm為較佳的。
此SiO2
層亦可用碳黑微粒、無機彩色顏料及/或金屬微粒作攙添,若此攙添可在空氣中或於惰性氣體之下在>700℃的溫度呈穩定的。在SiO2
基質中摻雜物之比例為1-30重量%,較佳為2-20重量%,尤其是5-20重量%。
此高折射率塗層(B)宜含有金屬氧化物及/或低氧化物。
層(B)宜含有金屬氧化物,例如TiO2
、ZrO2
、SnO2
、ZnO、Ce2
O3
、Fe2
O3
、Fe3
O4
、Cr2
O3
、CoO、Co3
O4
、VO2
、V2
O3
、NiO,此外鈦的低氧化物(帶有局部降低氧化態在<4至2的TiO2
,如較低的氧化物Ti3
O5
、Ti2
O3
至TiO)、氧氮化鈦、FeO(OH);薄的半透明金屬層,例如其中包含Al、Fe、Cr、Ag、Au、Pt或Pd、或其組合物。此TiO2
層可呈金紅石或銳鈦礦改良,優先者為金紅石層。金紅石宜經由BP 0 271 767的方法製備。
層(B)較佳為金屬氧化物層,尤其是TiO2
、Fe2
O3
、Fe3
O4
、SnO2
、ZrO2
或Cr2
O3
,特別優先者為二氧化鈦。
層(B)當然亦可由複數的高折射率層組成。層(B)較佳僅包含一層,此外可包含二層。
高折射率之層厚取決於所需要之干涉顏色。層(B)之厚度宜在60-300 nm。結合薄的SiO2
層與高折射率金屬氧化物層,將使能夠得到例如干涉顏色由純銀白色經金色到深綠色。
可將另外的高及/或低折射率層(層C)供選擇地施用層(B)上。層數目較佳為二,此外可為三、四、五、六或七層。
尤其,在層(B)上的內含高與低折射率層之干涉包裝,將造成具有增加光澤的顏料,且進一步的增加干涉顏色。
取代層(B),亦可將內含交替高與低折射率層(層C)的干涉系統直接施用在SiO2
層上。
高或低折射率之各層的厚度依次對光學之性質顏料有重要影響。針對本發明干涉顏料,必須相互精確地設定個別層厚。層(C)之厚度為40-800 nm,較佳為60-600 nm,尤其是100-400 nm。
作為高折射率層的適合材料為所有那些針對層(B)所提及者。
用於塗層(C)適合的無色低折射率材料,較佳為金屬氧化物或對應的氧化物水合物,例如SiO2
、Al2
O3
、
AlO(OH)、B2
O3
,化合物如MgF2
、MgSi3
、或該金屬氧化物之混合物。層(C)之干涉系統尤其為TiO2
-SiO2
-TiO2
層序列。
此外,本發明干涉顏料亦可帶有半透明金屬層作為外層。此類型的塗層係已知的,例如見於DE 38 25 702 A1。金屬層較佳為鉻或鋁層,其層厚為5-25 nm。
所使用的高折射率層(B)及/或(C)當然亦可為無色的高折射率材料,例如金屬氧化物,尤其是TiO2
及ZrO2
,其已使用隨溫度穩定的吸收劑著色劑上色,例如紅色氧化鐵或提納德藍(Thenard's Blue)。此吸收劑著色劑亦可呈膜的形式而施用於高折射率塗層上。柏林藍(Berlin Blue)與胭脂紅(Carmine Red)宜施用於預鍛燒的TiO2
及ZrO2
層。此類型塗層之實施例例如揭示於DE 23 13 332。
可提出特別較佳的干涉顏料如下:玻璃薄片+SiO2
+TiO2
玻璃薄片+SiO2
+Fe2
O3
玻璃薄片+SiO2
+Fe3
O4
玻璃薄片+SiO2
+Cr2
O3
玻璃薄片+SiO2
+TiO2
+柏林藍
玻璃薄片+SiO2
+TiO2
+胭脂紅
玻璃薄片+SiO2
+TiO2
+SiO2
+TiO2
玻璃薄片+SiO2
+TiO2
+Cr
雲母薄片+SiO2
+TiO2
雲母薄片+SiO2
+Fe2
O3
雲母薄片+SiO2
+Fe3
O4
雲母薄片+SiO2
+Cr2
O3
雲母薄片+SiO2
+TiO2
+柏林藍
雲母薄片+SiO2
+TiO2
+胭脂紅
雲母薄片+SiO2
+TiO2
+SiO2
+TiO2
雲母薄片+SiO2
+TiO2
+Cr
Al2
O3
薄片+SiO2
+TiO2
Al2
O3
薄片+SiO2
+Fe2
O3
Al2
O3
薄片+SiO2
+Fe3
O4
Al2
O3
薄片+SiO2
+Cr2
O3
Al2
O3
薄片+SiO2
+TiO2
+柏林藍
Al2
O3
薄片+SiO2
+TiO2
+胭脂紅
Al2
O3
薄片+SiO2
+SnO2
+TiO2
+胭脂紅
Al2
O3
薄片+SiO2
+TiO2
+SiO2
+TiO2
Al2
O3
薄片+SiO2
+TiO2
+Cr
在特別較佳的干涉顏料中,經塗覆的玻璃薄片係特別較佳的,更佳為經塗覆的Al2
O3
薄片。
術語高折射率塗層意指折射率>1.8的各層,且術語低折射率意指那些n≦1.8的各層。
本發明干涉顏料一般可相對地容易地製備。
金屬氧化物層宜採用溼化學方法施用,可使用製備珍珠光彩顏料所發展的溼化學塗覆方法。此類方法例如記述於DE 14 67 468、DE 19 59 988、LSE 20 09 566、
DE 22 14 545、DE 22 15 191、DE 22 44 298、DE 23 13 331、DE 15 22 572、DE 31 37 808、DE 31 37 809、DE 31 51 343、DE 31 51 354、DE 31 51 355、DE 32 11 602、DE 32 35 017或其它專利文件,以及已知於熟悉此技藝的專業人士之其它刊物。
當使用溼塗覆法,將基材微粒懸浮於水中,且將一或更多可水解的金屬鹽類或水玻璃溶液加入,這是在其適合於水解的pH之下,此選擇的pH係使金屬氧化物或金屬氧化物水合物直接沈澱到薄片上而未發生二次沉澱。一般經由同時計量加入鹼及/或酸而使pH保持固定。接著分離顏料,清洗且於50-150℃乾燥6-18小時,且視需要鍛燒0.5-3小時,存在於各案例中的塗層,有可能將鍛燒溫度作最佳化考量。一般而言,鍛燒溫度介於700與1000℃之間,較佳介於700與900℃之間。若有需求,可將顏料分離,於施用個別塗層之後乾燥且視需要鍛燒且然後再懸浮再一次以沈澱另一層。
在基材上沈澱SiO2
層,一般是經由在適合的pH之下加入鉀或鈉水玻璃溶液而進行。
此外,亦可在流化床反應器中經由氣相塗覆而進行塗層,有可能對應地使用所提出的方法,例如在EP 0 045 851及EP 0 106 235中用於製備珍珠光彩顏料所提出的方法。
經由塗層量或其生成的層厚之不同選擇,可在非常寬廣範圍內變化干涉顏料的色調。經由於肉眼之下或測量技
藝控制之下調控所需要之色彩,可達成針對超出單純選擇量之外特定色調的微調。
為了增加對於光、水與天氣的穩定性,取決於應用區域,頻繁地建意言將最終顏料作後塗覆或後處理。適合的後塗層或後處理例如有敘述於德國專利22 15 191 DE-A 31 51 354、DE-A 32 35 017或DE-A 33 34 598的方法。此後塗層(層D)可進一步增加化學與光化學穩定性或簡化顏料的操作,尤其是加入各種介質。為改良溼化性、分散性及/或與使用介質的相容性,有可能將例如Al2
O3
或ZrO2
的功能性塗層或其混合物施用於顏料表面上。此外,有機後塗層可能例如帶有矽烷,如例如記述於EP 0090259,EP 0 634 459、WO 99/57204、WO 96/32446、WO 99/57204、U.S.5,759,255、U.S.5,571,851、WO 01/92425或在J.J. Ponjeé,Philips Technical Review, Vol. 44, No.3,81 ff.及P. H. Harding J.C. Berg, J. Adhesion Sci. Technol. Vol. 11 No.4, pp. 471-493。
相較於先前技藝中在基材上沒有SiO2
層的顏料,本發明顏料優越性在於其較高的色度(色強度C*),其較高的光澤(L值)及顯著的閃光效應,尤其是針對以玻璃或Al2
O3
薄片為主的顏料。相較於EP 0 753 545 B1的角度變色顏料,本發明干涉顏料未展現或僅展現低的顏色角度從屬性。
相較於WO 01/30920的教示,本發明顏料針對光澤
及機械穩定性的決定性優點,僅發生針對SiO2
作為第一塗覆擔體的之材料。在WO 01/30920的揭示內容之外,本發明可得到具有明亮干涉顏色如紅、藍或綠色的銀白色顏料及高光澤干涉顏料。由於其透明度,本發明顏料可有利地與吸收顏料或顏色劑摻合。此類型之組成物將可採用特別簡單方法,而能夠達成不平常的色彩印象。
本發明顏料相容於多重顏色系統,較佳領域在塗料、塗層及油墨及化妝品配方。針對製備油墨,例如用於凹版印刷、橡膠版輪轉印刷、平版印刷及平版再塗印刷(offset overvanishing)、多重黏著,尤其是水溶性等級,適合者例如由下列各廠家銷售者:BASF、Marabu、Proll、Sericol、Hartmann、Gebr. Schmidt、Sicpa、Aarberg、Siegberg、GSB-Wahl、Follmann、Ruco或Coates Screen INKS GmbH的。此油墨可水性的或溶劑性的。此外此顏料亦適用於雷射標誌的紙及塑膠及在農藝部門的應用,例如用於溫室薄板,而且,例如用於帳篷布篷的著色劑。
因為本發明干涉顏料結合了高光澤與強干涉顏色,且有高度顯著的閃光效應,經由將其加入各種用途介質中可達成特別有效的效應,例如加入化妝品配方中,例如指甲油、唇膏、粉餠、凝膠、乳液、肥皂、牙膏,加入塗料中,例如汽車塗料、工業塗層及粉末塗層,及加入塑膠與陶瓷中。
由於良好的皮膚感覺及非常良好的皮膚黏合,本發明顏料適合於個人保養應用,例如身體乳液、乳化液、洗髮
精、肥皂等等。而且,尤其是適合於裝飾性化妝品。
所未提及者,針對各種用途,本發明多層化顏料亦可有利地使用於與有機染料、有機顏料或其它顏料的摻合,例如透明與不透明的白色,彩色及黑色顏料,及與下列各項摻合:薄片形式氧化鐵、有機顏料、全像顏料、LCP(液晶聚合物)及慣常的由金屬氧化物塗覆的雲母及SiO2薄片等為主的透明的、彩色及黑色光澤顏料。本發明顏料可以任何比例而與商購之顏料及填料混合。
可提及的填料例如有天然的及合成的雲母、尼龍粉末、純或裝入三聚氰胺樹脂、滑石粉、SiO2、玻璃、高嶺土、氧化物或氫之氧化物鋁、鎂、鈣或鋅、BiOCl、硫酸鋇、硫酸鈣、碳酸鈣、碳酸鎂、碳、及此類物質的物理或化學之組成物。
針對填料的顆粒形狀沒有限制。依據須求,例如可為薄片形式、球形的或針狀的。
當然也可能的將本發明顏料為與帶有化妝品原料及任何類型輔助劑的配方合併。此類輔助劑尤其是包含油、脂肪、薄膜成形劑、防腐劑及一般測定用於技術性質的輔助劑,例如黏稠劑及流變添加劑,例如皂土、水輝石、二氧化矽、Ca的矽酸鹽、膠質、高分子量碳水化合物及/或表面活化的輔助劑等
包含本發明顏料的配方可屬於親油性、親水性或疏水性類型。在具有不連接的水相與非水相的異質的配方中,本發明顏料在各案例中僅可存在於二個相之一或供選擇地
分佈在兩相中。
配方中的pH值在可介於1與14之間,較佳介於2與11之間,且特別較佳介於5與8之間。
本發明顏料在配方中之濃度沒有限制。其可取決於應用,而介於0.001(沖去型產物,例如沐浴凝膠)與100%(例如針對特別應用的光澤效應物品)之間。
此外,本發明顏料亦可與化妝品的有效成分合併。適合的有效成分例如有昆蟲驅蟲劑、UV A/BC保護濾膜(例如OMC、B3或MBC)、抗老化有效成分、維生素及其衍生物(例如維生素A、C、E等)、自身曬黑試藥(例如DHA,尤其是赤蘚酮糖)及其它化妝品的有效成分,例如甜沒藥帖醇、LPO、茶樹葉精華(ectoin)、油柑子(emblica)、尿囊素、生物-類黃酮及其衍生物。
此外本發明顏料也適用於製備可流動的顏料製劑與乾燥製劑,尤其是針對油墨及化妝品的應用,其中包含一或更多本發明顏料、黏著劑與視需要的一或更多添加劑。
本發明如此亦關於將顏料使用各種配方中,如塗料、塗層、汽車塗料、粉末塗層、油墨、保全油墨、塑膠、陶瓷材料、玻璃、紙,使用於電子照相印刷方法的調色劑,使用於種子,使用於溫室薄板及帳篷布篷,作為在雷射標誌的紙及塑膠上吸收劑,使用於化妝品的配方,用於與水、有機及/或水溶性溶劑製備顏料糊狀物,及用於製備顏料製劑及乾燥製劑,例如顆粒。
以下實施例係用以詳細地說明本發明,但而未加以限
制。
於攪拌下在1.9公升的去離子水之中,將150 g的平均層厚為700 nm的玻璃薄片(表1中的玻璃A),加熱至75℃。然後使用5%鹽酸將懸浮液之pH調至7.5。接著逐滴加入鈉水玻璃溶液(112 g的鈉水玻璃溶液,其中包含26.8%的SiO2溶於112 g的去離子水),於此期間經由同時計量加入5%鹽酸而將其pH值保持固定在7.5。當完成加入後,將混合物進一步攪拌0.5小時。然後將懸浮液之pH調至1.8,將此懸浮液進一步攪拌15分鐘,且逐滴加入四氯化錫在鹽酸中的溶液(3 g的SnCl4*5 H2O,溶於15毫升的25%鹽酸及85毫升的去離子水中),於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當完成加入後,將混合物進一步攪拌15分鐘。
接著計量加入30%四氯化鈦溶液,於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。於製程期間經由顏色測量而監測在顏料製備中的顏色性質,且依據色調(色調角度為弧正切b*/a*)而控制沈澱程序。當已達到所需要之銀終點,將混合物進一步攪拌15分鐘。此顏料包含20%的沈澱SiO2,此係基於玻璃薄片
重量而計算。
將產物過濾、清洗,於150℃乾燥且在>700℃鍛燒。
將此最終顏料加入商購之硝化纖維素亮漆中,且製備塗料卡片。此塗料卡片展現非常純的銀白色而帶有高光澤。
經由實施例1敘述之方法製備銀白色顏料。使用具有相同厚度及尺寸分佈(20-200μm)的組成物B玻璃薄片,替代表1中組分A的玻璃薄片。如在實施例1中相同終點進行二氧化鈦塗覆。所得到的顏料由目視無法與實施例1中的顏料區分。
經由在實施例中1相同步驟製備具有如下SiO2
重量比例的銀白色顏料,其中SiO2
重量比例係基於玻璃薄片重量而計算:
2% SiO2
,經由計量加入溶於11:5 g水中之11.5 g水玻璃溶液
59% SiO2
,經由計量加入溶於28 g水中之28 g水玻璃溶液
10% SiO2
,經由計量加入溶於56 g水中之56 g水玻璃溶液
進行二氧化鈦塗層使達到如在實驗1及2之中相同色調。
於攪拌下在1.9公升的去離子水之中,將150 g的平均層厚為700 nm的表1中玻璃A玻璃薄片加熱至75℃。然後使用5%鹽酸將懸浮液之pH調至1.8。接著逐滴加入在鹽酸中的四氯化錫溶液(4,5 g的SnCl4
* 5 H2
O溶於
22.5毫升的25%鹽酸與128毫升的去離子水中),於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當完成加入後,將混合物進一步攪拌15分鐘。接著計量加入30%四氯化鈦溶液,於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當已達到所需要之銀終點,將混合物進一步攪拌15分鐘。
將產物過濾、清洗且於150□乾燥。在600℃鍛燒一個試樣顏料(實施例6),且將另一試樣顏料(實施例7)在700℃鍛燒,在兩個案例中均鍛燒60分鐘。
將此最終顏料加入商購之硝基纖維素亮漆中,且使用此亮漆製備塗料卡片。針對在600℃鍛燒的顏料,塗料卡片展現純銀白色且具有良好的光澤,而針對在700℃鍛燒的顏料,其光澤顯著地降低。
於攪拌下在1.9公升的去離子水之中,將150 g的平均層厚為700 nm的表1中玻璃A玻璃薄片加熱至75℃。將pH調至5.5。在75℃於攪拌下逐滴加入180毫升的在鹽酸中的氯化鋁溶液(18 g的氯化鋁六水合物),於此期間使用氫氧化鈉溶液將其pH值保持在5。當完成加入,於75℃將混合物進一步攪拌2小時。將此經塗層的玻璃薄片過濾、清洗,於150℃乾燥且在400℃脫水30分鐘。於冷卻之後,經過氧化鋁塗覆的(約5% Al2
O3
)玻璃薄片使用鈦,經由在實施例6中指出的步驟作進一步加工,
以生成銀白色顏料。
相較於依據實施例6中先前技藝的顏料,實施例8的顏料顯示絕對沒有光澤改良,且相較於具有SiO2
層的顏料,此顏料展現顯著較低的光澤。
可在一實用測試之中測試化妝品製劑中顏料之磨耗穩定性。在此可測定顏料之機械穩定性在實用上是否能充分,例如在粉餠或乳膏中。作為快速測試,顏料試樣與手掌上手指的摩擦已證明可成功地應用。當經由摩擦而造成層顏料微粒的分離或斷裂,磨擦試樣的光澤將會降低或完全
地失去。光澤降低之目視評估分為1至5段,其中1段意指於摩擦期間光澤沒有改變或增加,且步驟5意指有強的暗澹。步驟3視為實用上可用的限制程度,4與5視為不可用的。
將實施例1-7中的顏料作此類型的磨耗測試。其結果展示於表3中,且顯示僅本發明具有SiO2
層的顏料,具有足夠的針對化妝品應用之機械穩定性。
在5公升的實驗室反應器之中,將100 g的氧化鋁薄片(如敘述於EP 0 763 573 B1,實施例2所製備)懸浮於2公升的去離子水中。在75℃,於攪拌下採用3毫升/分鐘的速率逐滴加入200毫升的水溶性SnCl4
溶液(36 g的SnCl4
每公升的溶液)。懸浮液之pH保持在1.8經由計
量加入氫氧化鈉溶液。將混合物進一步攪拌10分鐘,且然後採用3毫升/分鐘之速率計量加入水溶性四氯化鈦溶液(125 g的TiCl4
/公升的溶液),於此期間經由加入氫氧化鈉溶液將其pH值保持在1.7-1.9。以此方式,將氧化鋁薄片塗覆以二氧化鈦層,其中,隨著增加二氧化鈦層之層厚,首先形成銀白色且然後形成第一至第三順序的色彩干涉顏色。於塗層方法期間,借助於間隙形式測量腔室而測量干涉顏料之顏色性質,該間隙形式測量腔室係連接至反應器,且於塗層期間經由此腔室將反應混合物連續地抽送。於流經測量腔室的間隙期間,顏料薄片實質上排列平行於流動方向,且相對加於黑色背景而作測量。使用商購之Minolta CR 300色彩測量腔室,於閃光之後在某一角度測量反射光。依據DIN 5033部分3將測量數據轉化成CIELAB值且顯示。以此方式,在塗層的任何階段可測定顏料之顏色性質。圖1顯示塗層之顏色性質,呈a*/b*示圖的形式。在此系統中,+a值代表紅色,-a值代表綠色,+b值代表黃色且-b值代表藍色。在座標起始處開始測量曲線,且顯示對應於二氧化鈦塗層的干涉顏色。顏色位置愈自座標分離,顏料的色度愈大。
在實施例10的實驗室反應器中,將100 g的氧化鋁薄片(如敘述於EP 0 763 573 131,實施例2而製備)懸浮於1.6公升的去離子水中。將懸浮液之pH設定在8,
且接著逐滴加入鈉水玻璃溶液(190 g的鈉水玻璃溶液,其中包含26.8% SiO2
溶於190 g的去離子水中),於此期間經由同時計量加入5%鹽酸將其pH值保持固定在8。當完成加入後,將混合物進一步攪拌0.5小時。然後使用5%鹽酸將懸浮液之pH調至1.8,將混合物進一步攪拌15分鐘,且逐滴加入四氯化錫在鹽酸中的溶液(4.5 g的SnCl4
* 5 H2
O溶於22.5毫升的25%鹽酸及128毫升的去離子水中),於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當完成加入後,將混合物進一步攪拌15分鐘,且然後採用3毫升/分鐘之速率計量加入水溶性四氯化鈦溶液(125 g的TiCl4
/公升的溶液),於此期間經由加入氫氧化鈉溶液將其pH值保持在1.7-1.9。於TiO2
塗覆期間,如在實施例10中測量顏料之顏色性質。此比較顯示,相較於先前技藝顏料,本發明顏料具有顯著較佳的色度(〝色強度〞)(圖2)。此外,本發明顏料展現顯著較高的光澤。
於攪拌下在1.9公升的離子水之中,將150 g的平均層厚為900 nm的玻璃薄片(表4中的玻璃C)加熱至75℃。然後使用5%鹽酸將懸浮液之pH調至7.5。接著逐滴加入鈉水玻璃溶液(112 g的鈉水玻璃溶液,其中包含26.8% SiO2
溶於112 g的去離子水),於此期間經由同時計量加入5%鹽酸而將其pH值保持固定在7.5。當完成加
入後,將混合物進一步攪拌0.5小時。然後將懸浮液之pH調至1.8,將混合物進一步攪拌15分鐘,且逐滴加入四氯化錫在鹽酸中的溶液(3 g的SnCl4
* 5 H2
O溶於15毫升的25%鹽酸及85毫升的去離子水中),於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當完成加入後,將混合物進一步攪拌15分鐘。
接著計量加入30%四氯化鈦溶液,於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。於製備顏料期間,經由於製程期間的顏色測量而監測顏色性質,且依據色調(色調角度arc tan b*/a*)而控制沈澱方法。當已達到所需要之銀終點,將混合物進一步攪拌15分鐘。此顏料包含20%的沈澱SiO2
,此係基於玻璃薄片重量而計算。
將產物過濾、清洗,於150℃乾燥且在>700℃鍛燒。
將此最終顏料加入商購之硝基纖維素亮漆中,且製備塗料卡片。此塗料卡片展現非常純的銀白色而帶有高光澤。
經由實施例12敘述之方法製備銀白色顏料。使用具有相同厚度及尺寸分佈(20-200μm)的表4中組成D的玻璃薄片,取代表4中組成C的玻璃薄片。如在實施例12中進行二氧化鈦塗覆至相同終點。所得到的顏料由目視無法與實施例12中的顏料區分。
經由在實施例12中指出的步驟製備銀白色顏料,其具有以下重量比例的SiO2
,此係基於玻璃薄片重量而計算,
2% SiO2
,經由計量加入11.5 g的水玻璃溶液溶於11.5 g的水中
5% SiO2
,經由計量加入28 g的水玻璃溶液溶於28 g的水中
10% SiO2
,經由計量加入56 g的水玻璃溶液溶於56 g的水中
進行二氧化鈦塗層到如在實施例12與13中相同色調。
於攪拌下在1.9公升的去離子水之中,將150 g的平均層厚為900 nm的表4中組成C的玻璃薄片,加熱至75℃。使用鹽酸將懸浮液之pH調至pH 1.8。接著逐滴加入四氯化錫在鹽酸中的溶液(4.5 g的SnCl4
* 5 H2
O溶於225毫升的25%鹽酸及128毫升的去離子水中),於此期間經由同時逐滴加入32%氫氧化鈉溶液將其pH保持固定。當完成加入後,將混合物進一步攪拌15分鐘。接著計量加入30%四氯化鈦溶液,於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當已達到所需要之銀終點,將混合物進一步攪拌15分鐘。
將產物過濾、清洗且於150℃乾燥。在600℃鍛燒一項試樣顏料(實施例17),且將另一項試樣顏料在700℃鍛燒(實施例18),在各案例中鍛燒60分鐘。
將此最終顏料加入商購之硝化纖維素亮漆中,且使用此亮漆製備塗料卡片。針對在600℃鍛燒的顏料,塗料卡片展現純銀白色且具有良好的光澤,而針對在700℃鍛燒的顏料,其光澤顯著地降低。
於攪拌下在1.9公升的離子水之中,將150 g的平均層厚為900 nm的表4中組成C的玻璃薄片加熱至75℃。pH調至5.5。在75℃,於攪拌下,逐滴加入180毫升的在鹽酸中的氯化鋁溶液(18 g的氯化鋁六水合物),於此期間使用氫氧化鈉溶液將其pH值保持在5。當完成加入,於75℃將混合物進一步攪拌2小時。將此經塗層的玻璃薄片過濾、清洗,於150℃乾燥且在400℃脫水30分鐘。於冷卻之後,經由在實施例17中指出的步驟,使用二氧化鈦將經過氧化鋁塗覆的(約5% Al2
O3
)玻璃薄片進一步加工,以生成銀白色顏料。
相較於依據實施例17的先前技藝之顏料,實施例19的顏料顯示絕對沒有光澤改良,且相較於具有SiO2
層的顏料,此顏料展現顯著較低的光澤。
採用類似於實施例9的方法進行機械穩定性的測試。
將實施例12-18的顏料作此類型的磨耗測試。其結果展示於表5,且顯示僅本發明具有SiO2
層的顏料具有足夠的針對化妝品應用之機械穩定性。
在1.75公升的去離子水中,將125 g的平均層厚為500 nm的玻璃薄片(表4中的玻璃D)加熱至75℃於攪拌下。然後使用5%鹽酸將懸浮液之pH調至8。接著逐滴加入鈉水玻璃溶液(67 g的鈉水玻璃溶液,其中包含26.8% SiO2
溶於67 g的去離子水中),於此期間經由同時計量加入5%鹽酸而將其pH值保持固定在7.5。當完成加入後,將混合物進一步攪拌15分鐘。然後將懸浮液之pH調至2.8,將混合物進一步攪拌15分鐘,且逐滴加入
約320毫升的15%的溶液在鹽酸中的氯化鐵,於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。於塗層期間,如在實施例10中測量顏料之顏色性質。當完成加入後,將混合物進一步攪拌15分鐘。此顏料包含10%的沈澱SiO2
,此係基於玻璃薄片重量而計算。
將產物過濾、清洗,於150℃乾燥且在>700℃鍛燒。
將此最終顏料加入商購之硝化纖維素亮漆中,且製備塗料卡片。此塗料卡片展現非常純的具有高光澤的氧化鐵紅色。
在1.75公升的去離子水中,於攪拌下,將125 g的平均層厚為500 nm的玻璃薄片(表4中的玻璃Q,粒徑10-60 pm)加熱至75℃。然後使用5%鹽酸將懸浮液之pH調至7.5。接著逐滴加入鈉水玻璃溶液(67 g的鈉水玻璃溶液,其中包含26.8% SiO2
溶於67 g的去離子水中),於此期間經由同時計量加入5%鹽酸而將其pH值保持固定在7.5。當完成加入後,將混合物進一步攪拌15分鐘。然後將懸浮液之pH調至1.8,將混合物進一步攪拌15分鐘,且逐滴加入四氯化錫在鹽酸中的溶液(2.5 g的SnCl4
* 5 H2
O溶於12.5毫升的25%鹽酸及70毫升的去離子水中),於此期間經由同時逐滴加入32%氫氧化鈉溶液而將其pH值保持固定。當完成加入後,將混合物進
一步攪拌15分鐘。將懸浮液之pH接著保持在1.8,且採用2毫升/分鐘之速率計量加入水溶性四氯化鈦溶液(400 g的TiCl4
/每公升的溶液),於此期間經由加入氫氧化鈉溶液將其pH值保持在1.7-1.9。於TiO2
塗覆期間,採用如在實施例10中測量顏料之顏色性質。當已達到所必需的色調角度,經由加入32% NaOH使pH值緩慢調整至pH 8,且再一次逐滴加入鈉水玻璃溶液(9.8 g的鈉水玻璃溶液,其中包含26.8% SiO2
溶於9.8 g的去離子水中),於此期間經由同時計量加入5%鹽酸而將其pH值保持固定在7.5。當完成加入後,將混合物進一步攪拌15分鐘。必須準確地計算鈉水玻璃溶液之體積,因為於塗層期間不可能以顏色術語監測顏色形成。
使用5%鹽酸然後再一次將pH調至1.8,且採用2毫升/分鐘之速率計量加入水溶性四氯化鈦溶液(400 g的TiCi4
/公升的溶液),於此期間經由加入氫氧化鈉溶液將其pH值保持在1.7-1.9。由色調角度測定滴定終點。
此顏料包含10%的沈澱SiO2
,此係基於玻璃薄片重量而計算。
將產物過濾、清洗,於150℃乾燥且在>700℃鍛燒。
將此最終顏料加入商購之硝化纖維素亮漆中,且製備塗料卡。此塗料卡片展現非常純的且明亮的干涉顏色而帶有高光澤。
Claims (12)
- 一種以經塗覆的薄片形式基材為主的干涉顏料,其中包含於該基材上之依順序存在的以下組份:(A)一層的SiO2 ,其層厚為5-350 nm,(B)一高折射率塗層,其折射率n>1.8,且其係含有TiO2 、ZrO2 、SnO2 、ZnO、Ce2 O3 、Fe2 O3 、Fe3 O4 、Cr2 O3 、CoO、Co3 O4 、VO2 、V2 O3 、NiO、鈦的低氧化物(帶有局部降低氧化態在<4至2的TiO2 )、氧氮化鈦、FeO(OH)及/或薄的半透明金屬層(其包含Al、Fe、Cr、Ag、Au、Pt或Pd),及/或(C)一種具有層序列為TiO2 -SiO2 -TiO2 之干涉系統,及視需要的(D)外保護層。
- 如申請專利範圍第1項之干涉顏料,其中其包含於該基質上之依順序存在的以下組份:(A)層-(B)層。
- 如申請專利範圍第1項之干涉顏料,其中其包含於該基質上之依順序存在的以下組份:(A)層-(C)層。
- 如申請專利範圍第1項之干涉顏料,其中其包含於該基質上之依順序存在的以下組份:(A)層-(B)層-(C)層。
- 如申請專利範圍第1項之干涉顏料,其中薄片形式基材為天然的及/或合成的雲母、滑石粉、高嶺土、薄片形式的鐵或氧化鋁、玻璃薄片、SiO2 薄片、TiO2 薄片、石墨薄片、合成的無支撐薄片、氮化鈦、矽化鈦、液晶聚合物(LCPs)、全像顏料、BiOCl或薄片形式混合氧化物、或其混合物。
- 如申請專利範圍第5項之干涉顏料,其中薄片形式基材為玻 璃薄片、雲母薄片或氧化鋁薄片。
- 如申請專利範圍第1項之干涉顏料,其中層(A)之厚度為30-100 nm。
- 如申請專利範圍第1項之干涉顏料,其中層(A)中攙添有碳黑微粒、金屬微粒及/或彩色顏料。
- 如申請專利範圍第1項之干涉顏料,其中層(B)為二氧化鈦。
- 如申請專利範圍第1至9項中任一項之干涉顏料,其中帶有外保護層(D),可增加對光、溫度與天候的穩定性。
- 一種製備如申請專利範圍第1項之干涉顏料之方法,其中基材的塗層係由溼化學方法進行,採用金屬鹽類在水溶性介質中的水解降解,或採用在流化床反應器中氣相塗覆。
- 如申請專利範圍第1項之干涉顏料在用於塗料、塗層、汽車塗料、粉末塗層、油墨、保全油墨、塑膠、陶瓷材料、玻璃、紙,使用於電子照相印刷方法的調色劑,使用於種子,使用於溫室薄板及帳篷布篷,作為在雷射標誌的紙及塑膠上吸收劑,使用於化妝品配方,用於與水、有機及/或水溶性溶劑製備顏料糊狀物,及用於製備顏料製劑及乾燥製劑中之用途。
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DE2002159301 DE10259301A1 (de) | 2002-12-17 | 2002-12-17 | Interferenzpigmente |
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EP (1) | EP1572812B1 (zh) |
JP (2) | JP5431632B2 (zh) |
AU (1) | AU2003292216A1 (zh) |
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- 2003-12-09 JP JP2005502428A patent/JP5431632B2/ja not_active Expired - Fee Related
- 2003-12-09 US US10/539,592 patent/US20060225609A1/en not_active Abandoned
- 2003-12-09 EP EP03767774.7A patent/EP1572812B1/de not_active Expired - Lifetime
- 2003-12-09 AU AU2003292216A patent/AU2003292216A1/en not_active Abandoned
- 2003-12-15 TW TW092135451A patent/TWI395794B/zh not_active IP Right Cessation
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2010
- 2010-03-22 US US12/728,790 patent/US8500901B2/en not_active Expired - Lifetime
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JP2000239559A (ja) * | 1999-02-15 | 2000-09-05 | Merck Patent Gmbh | 強力な干渉顔料 |
WO2001030920A1 (de) * | 1999-10-28 | 2001-05-03 | Merck Patent Gmbh | Farbstarke interferenzpigmente |
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Also Published As
Publication number | Publication date |
---|---|
US20100175587A1 (en) | 2010-07-15 |
JP2006510797A (ja) | 2006-03-30 |
TW200422355A (en) | 2004-11-01 |
US20060225609A1 (en) | 2006-10-12 |
WO2004055119A1 (de) | 2004-07-01 |
JP5431632B2 (ja) | 2014-03-05 |
AU2003292216A1 (en) | 2004-07-09 |
JP2012224858A (ja) | 2012-11-15 |
EP1572812B1 (de) | 2019-05-15 |
US8500901B2 (en) | 2013-08-06 |
EP1572812A1 (de) | 2005-09-14 |
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