CN116970291A - 一种酞菁类纳米颜料的制备方法及应用 - Google Patents
一种酞菁类纳米颜料的制备方法及应用 Download PDFInfo
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- 239000000049 pigment Substances 0.000 title claims abstract description 126
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 44
- 229920005989 resin Polymers 0.000 claims abstract description 44
- 238000004898 kneading Methods 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 235000002639 sodium chloride Nutrition 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 3
- XLLIQLLCWZCATF-UHFFFAOYSA-N 2-methoxyethyl acetate Chemical compound COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 125000002947 alkylene group Chemical group 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 235000011148 calcium chloride Nutrition 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 125000005543 phthalimide group Chemical group 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 125000001273 sulfonato group Chemical class [O-]S(*)(=O)=O 0.000 claims description 2
- 150000003458 sulfonic acid derivatives Chemical class 0.000 claims description 2
- 229920003169 water-soluble polymer Polymers 0.000 claims description 2
- HFFXLYHRNRKAPM-UHFFFAOYSA-N 2,4,5-trichloro-n-(5-methyl-1,2-oxazol-3-yl)benzenesulfonamide Chemical compound O1C(C)=CC(NS(=O)(=O)C=2C(=CC(Cl)=C(Cl)C=2)Cl)=N1 HFFXLYHRNRKAPM-UHFFFAOYSA-N 0.000 claims 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 35
- 239000006185 dispersion Substances 0.000 abstract description 13
- 230000009471 action Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012860 organic pigment Substances 0.000 abstract description 3
- 239000012043 crude product Substances 0.000 abstract description 2
- 239000010419 fine particle Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 13
- 238000003756 stirring Methods 0.000 description 10
- 230000004580 weight loss Effects 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- -1 dichloro-completed Chemical compound 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000019612 pigmentation Effects 0.000 description 1
- 230000000485 pigmenting effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
- G02B5/223—Absorbing filters containing organic substances, e.g. dyes, inks or pigments
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0002—Grinding; Milling with solid grinding or milling assistants
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
- C09B67/0008—Coated particulate pigments or dyes with organic coatings
- C09B67/0009—Coated particulate pigments or dyes with organic coatings containing organic acid derivatives
- C09B67/001—Coated particulate pigments or dyes with organic coatings containing organic acid derivatives containing resinic acid derivatives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
- C09B67/0008—Coated particulate pigments or dyes with organic coatings
- C09B67/0011—Coated particulate pigments or dyes with organic coatings containing amine derivatives, e.g. polyamines
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
- C09B67/0008—Coated particulate pigments or dyes with organic coatings
- C09B67/0013—Coated particulate pigments or dyes with organic coatings with polymeric coatings
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0014—Influencing the physical properties by treatment with a liquid, e.g. solvents
- C09B67/0016—Influencing the physical properties by treatment with a liquid, e.g. solvents of phthalocyanines
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0021—Flushing of pigments
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0032—Treatment of phthalocyanine pigments
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Abstract
本发明属于纳米颜料技术领域,涉及一种酞菁类纳米颜料的制备方法及应用,酞菁类纳米颜料的制备方法包括如下步骤:(1)预包覆;(2)捏合;(3)后处理。本发明在颜料化工序之前,将颜料粗品与水溶性树脂在溶剂中混合预包覆,使水溶性树脂在溶剂的作用下充分扩散到颜料表面,能进一步增强捏合时树脂与颜料颗粒的作用效果,减少大颗粒聚集体存在,能够得到对比度高的细微粒子,尤其对于酞菁类有机颜料,效果更为明显;而且水溶性树脂在洗涤时能被洗去,不会残留在颜料中,因此不会影响颜料的色纯度及分散稳定性。
Description
技术领域
本发明属于纳米颜料技术领域,尤其涉及一种酞菁类纳米颜料的制备方法及应用。
背景技术
滤色器是使白光透过并转换为红、绿、蓝三色的器件,被广泛应用于彩色个体摄像元件,液晶显示等彩色显示。近年来,出于对滤色器画质高清晰度的迫切需求,尤其是对绿色像素部,要求滤色器具有高亮度和高对比度。
滤色器的绿色像素部一般用卤代酞菁颜料,为了实现高亮度和高对比度,需要使用一次粒子尺寸在100nm以下的微细颜料。而用于有机颜料的有机化合物在合成后颜料分子以无规凝聚的状态存在,这种凝聚体被称之为粗颜料,不能直接用作颜料使用,需要调整粒子尺寸,得到微细化的颜料。这种调整粒子尺寸的工序被称为颜料化过程。
常用的颜料化工序是将粗颜料、无机盐、有机溶剂一起置于混炼机中进行混炼捏合,使颜料粒子在有机溶剂和无机盐的作用下进行尺寸调整和微细化。在混炼时,粗颜料的微细化及微细颜料的结晶化同时进行,若颜料不能充分微细化则存在大的凝聚颗粒会导致对比度降低,若微细颜料过分结晶化也会导致对比度降低。
专利CN113227260A公开了在捏合混炼时加入干冰能增强溶剂对粗大凝聚颗粒的渗透性,提高颜料化效果。专利CN113272389A公开了混炼捏合时,投入到混炼机中的能量过大会使微细颜料结晶化占优势,导致对比度降低。专利CN112601790A公开了在颜料化时加入树脂,通过树脂与颜料粒子生长面的相互作用,减轻粒子生长方向上的失衡,从而能够得到平均纵横比小的颜料,使像素部的对比度提高,但是所用树脂会存在于颜料中,通常这种颜料被称为颜料组合物,颜料组合物中由于树脂的存在会降低颜料的有效含量,降低颜料的色纯度;另外,若树脂选择不合适,颜料后期应用时会导致颜料与分散液中其他组分不配伍,使分散液的稳定性降低,即颜料组合物使颜料的应用范围受限。
发明内容
本发明针对上述现有技术存在的不足,提一种酞菁类纳米颜料的制备方法及应用,具体的技术方案如下:
本发明的第一个目的在于提供一种酞菁类纳米颜料的制备方法,包括如下步骤:
(1)预包覆:将水溶性树脂溶解于溶剂中,将酞菁颜料加入到水溶性树脂的溶液中,使酞菁颜料充分分散,蒸干溶剂,得到树脂预包覆颜料;
(2)捏合:将树脂预包覆颜料与无机盐、有机溶剂放于捏合机中,进行研磨捏合,得到捏合物料;
(3)后处理:将捏合物料倒入水中,洗涤至电导率与所用水的电导率相同,然后过滤,烘干,得酞菁类纳米颜料。
本发明制备的酞菁类纳米颜料具有颗粒规整,颗粒尺寸小,易分散等优点,提高了所制备的滤色片的对比度。
本发明经过研究发现,在颜料化工序之前,将颜料粗品与水溶性树脂在溶剂中混合预包覆,使水溶性树脂在溶剂的作用下充分扩散到颜料表面,能进一步增强捏合时树脂与颜料颗粒的作用效果,减少大颗粒聚集体存在,能够得到对比度高的细微粒子,尤其对于酞菁类有机颜料,效果更为明显。而且水溶性树脂在洗涤时能被洗去,不会残留在颜料中,因此不会影响颜料的色纯度及分散稳定性。
进一步地,所述酞菁颜料包括金属酞菁及溴氯代金属酞菁。
进一步地,所述金属酞菁及所述溴氯代金属酞菁的中心原子金属包括铝、硅、铜、锌、钴或镍金属元素,优选铜和锌。
进一步地,所述水溶性树脂是指能溶于水形成澄清透明溶液的水溶性聚合物,包括聚乙烯基吡咯烷酮,聚丙烯酸或聚丙胺。
进一步地,酞菁颜料与水溶性树脂的重量比为100:(0.1~100),优选100:(1~10)。
进一步地,预包覆的压力为0~40MPa,优选0.1~20MPa;预包覆的温度为-80~200℃,优选20~150℃;预包覆的时间为0.1~72h,优选2~12h。实现包覆效果最大化。
进一步地,所述分散的方法为机械搅拌、超声分散、乳化、高速剪切、球磨或高压均质中的一种或两种及以上组合。
进一步地,所述步骤(1)中,所述溶剂为甲醇、乙醇、异丙醇、甲苯、二甲苯、丙酮、四氢呋喃、N,N-二甲基甲酰胺、二氯甲烷、氯仿、二氧六环、石油醚、正己烷、环己烷、乙酸乙酯、乙酸丁酯、乙二醇、二乙二醇、二乙二醇甲醚或二乙二醇甲醚醋酸酯中的一种或两种及以上。
进一步地,所述步骤(2)中,所述无机盐包括但不限于氯化钠、氯化钾、氯化钙或硫酸钠,优选氯化钠。
进一步地,所述步骤(2)中,捏合温度范围为-20~200℃,优选30~100℃;捏合压力为0~1MPa,优选0.1~0.8MPa;捏合时间为0.5~72h,优选8~24h。
进一步地,所述步骤(2)中,所述有机溶剂为甲醇、乙醇、异丙醇、甲苯、二甲苯、丙酮、四氢呋喃、N,N-二甲基甲酰胺、二氯加完、氯仿、二氧六环、石油醚、正己烷、环己烷、乙酸乙酯、乙酸丁酯、乙二醇、二乙二醇、二乙二醇甲醚或二乙二醇甲醚醋酸酯中的一种或两种及以上。
进一步地,所述步骤(2)中,树脂预包覆颜料、有机溶剂与无机盐的质量比为1:(0.5~10):(5~20)。
进一步地,所述步骤(2)中,还包括颜料衍生物,所述颜料衍生物为酞菁衍生物,包括但不限于酞菁或卤代酞菁的磺酸衍生物、磺酸盐衍生物、磺酰胺衍生物,以及通过亚烷基与邻苯二甲酰亚胺骨架结合的酞菁衍生物等。
本发明的第二个目的在于提供上述酞菁类纳米颜料的制备方法所制得的酞菁类纳米颜料制备滤色器中的应用。
本发明的有益效果为:
本发明采用水溶性树脂将酞菁颜料进行预包覆,再进行捏合,增强树脂与颜料颗粒的作用效果,更能抑制颜料结晶,减少大颗粒聚集体存在,促进颜料整形,制备的酞菁类纳米颜料具有颗粒规整,颗粒尺寸小,易分散等优点,提高了所制备的滤色片的对比度,而且水溶性树脂在洗涤时能被洗去,不会残留在颜料中,因此不会影响颜料的色纯度及分散稳定性。
附图说明
图1为本发明实施例1制备的酞菁类纳米颜料一、树脂预包覆颜料一和聚乙烯吡咯烷酮K29的热失重图;
图2为本发明实施例2制备的酞菁类纳米颜料二、树脂预包覆颜料二和聚乙烯吡咯烷酮K29的热失重图;
图3为本发明实施例1酞菁类纳米颜料一的TEM图像;
图4为本发明对比例1颜料的TEM图像;
图5为本发明实施例2酞菁类纳米颜料二的TEM图像;
图6为本发明对比例2颜料的TEM图像。
具体实施方式
以下结合实例对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
实施例1:
一种酞菁类纳米颜料的制备方法,包括如下步骤:
(1)预包覆:500mL三口烧瓶内加入300mL丙酮,加入8g聚乙烯吡咯烷酮(分子量K29-32),搅拌溶解,加入100g颜料绿G58继续搅拌分散,然后将反应体系升温至80℃回流6h,用蒸馏的方法除去丙酮,得到树脂预包覆颜料一;
(2)捏合:将树脂预包覆颜料一70g、氯化钠500g、二乙二醇70g加入1L捏合机中,80℃捏合24h,得到捏合物料;
(3)后处理:将捏合物料倒入80℃水中搅拌2h后,洗涤至电导率与所用水的电导率相同,然后过滤,烘干,得酞菁类纳米颜料一。
实施例2:
一种酞菁类纳米颜料的制备方法,包括如下步骤:
(1)预包覆:500mL高压瓶内加入300mL乙醇,加入14g聚乙烯吡咯烷酮(分子量K29-32),搅拌溶解,加入100g颜料绿G36继续搅拌分散,然后将反应体系升温至100℃保压6h,降温,降压后,用蒸馏的方法除去乙醇,得到树脂预包覆颜料二;
(2)捏合:将树脂预包覆颜料二70g,氯化钠500g,二乙二醇70g加入1L捏合机中,80℃捏合24h,得到捏合物料;
(3)后处理:将捏合物料倒入80℃水中搅拌2h后,洗涤至电导率与所用水的电导率相同,然后过滤,烘干,得酞菁类纳米颜料二。
对比例1:
(1)预处理:500mL三口烧瓶内加入300mL丙酮,加入100g颜料绿G58继续搅拌分散,然后将反应体系升温至80℃回流6h,用蒸馏的方法除去丙酮,得到预处理颜料一;
(2)捏合:将预处理颜料一70g,氯化钠500g,二乙二醇70g加入1L捏合机中,80℃捏合24h,得到捏合物料;
(3)后处理:将捏合物料倒入80℃水中搅拌2h后,洗涤至电导率与所用水的电导率相同,然后过滤,烘干,得对比例1颜料。
对比例2
(1)预处理:500mL高压瓶内加入300mL乙醇,加入100g颜料绿G36继续搅拌分散,然后将反应体系升温至100℃保压6h,降温,降压后,用蒸馏的方法除去乙醇,得到预处理颜料二;
(2)捏合:将预处理颜料二70g,氯化钠500g,二乙二醇70g加入1L捏合机中,80℃捏合24h,得到捏合物料;
(3)后处理:将捏合物料倒入80℃水中搅拌2h后,洗涤至电导率与所用水的电导率相同,然后过滤,烘干,得对比例2颜料。
实施例评价:
1.热重性能测试:
图1为本发明实施例1制备的酞菁类纳米颜料一、树脂预包覆颜料一和聚乙烯吡咯烷酮K29的热失重图,由图1可见,聚乙烯吡咯烷酮K29在500℃时完全分解。树脂预包覆颜料一在250~500℃区间失重为7.32%,与预包覆添加的聚乙烯吡咯烷酮比例(7.41%)接近,说明其失重是由聚乙烯吡咯烷酮K29的分解产生的。但实施例1酞菁类纳米颜料一在300~400℃区间几乎无失重,说明经后处理聚乙烯吡咯烷酮可被全部洗去,几乎没有残留,因此不会影响颜料的色纯度及分散稳定性。
图2为本发明实施例2制备的酞菁类纳米颜料二、树脂预包覆颜料二和聚乙烯吡咯烷酮K29的热失重图,同样由图2可见,聚乙烯吡咯烷酮K29在500℃时完全分解,树脂预包覆颜料二在250~500℃区间失重为11.52%,与预包覆添加的聚乙烯吡咯烷酮比例(12.28%)接近,说明其失重是由聚乙烯吡咯烷酮K29的分解产生的。实施例2酞菁类纳米颜料二在300~400℃区间几乎无失重,说明经后处理聚乙烯吡咯烷酮也被全部洗去,几乎没有残留,不会影响颜料的色纯度及分散稳定性。
2.TEM测试:
用透射电镜测试实施例1酞菁类纳米颜料一和对比例1颜料的颗粒形貌,如图3和图4所示,可以看出,实施例1制备的酞菁类纳米颜料一颗粒轮廓清晰,大小均匀,颜料颗粒平均粒径为25.49nm。对比例1颜料颗粒轮廓不清晰,有较多团聚体存在,统计测得对比例1的平均粒径为32.19nm。
用透射电镜测试实施例2酞菁类纳米颜料二和对比例2颜料的颗粒形貌,如图5和图6所示,可以看出,实施例2制备酞菁类纳米颜料二纳米颗粒规整,尺寸均一,颜料平均粒径为25.25nm;对比例2颜料的颗粒较大,颗粒形状不规整,有较多细长颗粒,平均粒径为41.35nm。
通过以上TEM的测试结果可以发现,本发明使用的方法更容易制备颗粒规整,尺寸均匀的纳米颜料。这是因为,通过预包覆树脂与颜料表面的相互作用,颜料颗粒晶面的不规则生长受到限制。另外,通过预包覆工序,树脂充分扩散到了颜料表面,使团聚的颜料颗粒在捏合时更容易分散。
3.应用性能测试
(1)物料配比
按如下配比制备评价组合物色浆:
酞菁类纳米颜料一/酞菁类纳米颜料二/对比例1颜料/对比例2颜料13g;BYK2001分散剂15g;丙烯酸树脂分散液(PMA溶液,30%固含量)15g;PMA溶剂(丙二醇甲醚醋酸酯)65g。
(2)色浆制备
将上述配比物料按顺序加入玻璃瓶内,加入0.5mm锆球150g,在油漆调配器上分散2h,滤去锆球,得到评价组合物色浆。
(3)色浆评价
用粒度仪测试色浆中纳米颜料粒径,结果如表1所示;
取色浆1mL,以1000rpm的速度旋涂于玻璃片上,将涂膜后的玻璃片置于90℃的热台上加热3min后置于230℃烘箱内继续烘烤30min。用色度仪和对比度仪测试色坐标和对比度,结果如表1所示。
表1.实施例和对比例的色浆评价数据
样品名称 | D50 | D90 | 亮度 | 对比度 |
实施例1 | 53.62 | 77.27 | 60.16 | 19631 |
对比例1 | 56.16 | 90.76 | 59.61 | 18872 |
实施例2 | 51.65 | 70.57 | 54.61 | 17749 |
对比例2 | 69.61 | 107.93 | 52.53 | 16136 |
由表1可见,实施例1,实施例2的纳米颜料粒径D50,D90相对于对比例1和对比例2的数值变小,亮度和对比度变大,说明本发明所制备的纳米颜料较处理前粒径变得小且规整,亮度和对比度得到提升。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种酞菁类纳米颜料的制备方法,其特征在于,包括如下步骤:
(1)预包覆:将水溶性树脂溶解于溶剂中,将酞菁颜料加入到水溶性树脂的溶液中,使酞菁颜料充分分散,蒸干溶剂,得到树脂预包覆颜料;
(2)捏合:将树脂预包覆颜料与无机盐、有机溶剂放于捏合机中,进行研磨捏合,得到捏合物料;
(3)后处理:将捏合物料倒入水中,洗涤至电导率与所用水的电导率相同,然后过滤,烘干,得酞菁类纳米颜料。
2.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,所述酞菁颜料包括金属酞菁及溴氯代金属酞菁;所述水溶性树脂是指能溶于水形成澄清透明溶液的水溶性聚合物,包括聚乙烯基吡咯烷酮,聚丙烯酸或聚丙胺。
3.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,酞菁颜料与水溶性树脂的重量比为100:(0.1~100)。
4.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,预包覆的压力为0~40MPa,预包覆的温度为-80~200℃,预包覆的时间为0.1~72h。
5.根据权利要求4所述的酞菁类纳米颜料的制备方法,其特征在于,所述步骤(1)中,所述溶剂为甲醇、乙醇、异丙醇、甲苯、二甲苯、丙酮、四氢呋喃、N,N-二甲基甲酰胺、二氯甲烷、氯仿、二氧六环、石油醚、正己烷、环己烷、乙酸乙酯、乙酸丁酯、乙二醇、二乙二醇、二乙二醇甲醚或二乙二醇甲醚醋酸酯中的一种或两种及以上。
6.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,所述步骤(2)中,捏合温度范围为-20~200℃,捏合压力为0~1MPa,捏合时间为0.5~72h。
7.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,所述步骤(2)中,树脂预包覆颜料、有机溶剂与无机盐的质量比为1:(0.5~10):(5~20)。
8.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,所述步骤(2)中,所述无机盐包括氯化钠、氯化钾、氯化钙或硫酸钠。
9.根据权利要求1所述的酞菁类纳米颜料的制备方法,其特征在于,所述步骤(2)中,还包括颜料衍生物,所述颜料衍生物为酞菁衍生物,包括酞菁或卤代酞菁的磺酸衍生物、磺酸盐衍生物、磺酰胺衍生物,以及通过亚烷基与邻苯二甲酰亚胺骨架结合的酞菁衍生物。
10.如权利要求1~9任一项所述的酞菁类纳米颜料的制备方法所制得的酞菁类纳米颜料在制备滤色器中的应用。
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