CN102227479A - 颜料颗粒、其生产方法及其用途 - Google Patents
颜料颗粒、其生产方法及其用途 Download PDFInfo
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- CN102227479A CN102227479A CN2009801477975A CN200980147797A CN102227479A CN 102227479 A CN102227479 A CN 102227479A CN 2009801477975 A CN2009801477975 A CN 2009801477975A CN 200980147797 A CN200980147797 A CN 200980147797A CN 102227479 A CN102227479 A CN 102227479A
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- pigment
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- 239000000049 pigment Substances 0.000 title claims abstract description 143
- 239000008187 granular material Substances 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 40
- 238000000576 coating method Methods 0.000 claims abstract description 40
- 150000001875 compounds Chemical class 0.000 claims abstract description 38
- 239000006185 dispersion Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000003973 paint Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000006229 carbon black Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- 239000004964 aerogel Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000976 ink Substances 0.000 abstract 2
- 239000004922 lacquer Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 16
- 238000005507 spraying Methods 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 235000019241 carbon black Nutrition 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 239000000080 wetting agent Substances 0.000 description 9
- 239000013530 defoamer Substances 0.000 description 7
- 230000003115 biocidal effect Effects 0.000 description 6
- 239000003139 biocide Substances 0.000 description 6
- 239000006231 channel black Substances 0.000 description 5
- 239000003610 charcoal Substances 0.000 description 5
- 239000011164 primary particle Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000001055 blue pigment Substances 0.000 description 4
- 239000006232 furnace black Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000005357 flat glass Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- -1 alkylbenzene sulfonate Chemical class 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000012785 packaging film Substances 0.000 description 2
- 229920006280 packaging film Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- LJCJRRKKAKAKRV-UHFFFAOYSA-N (2-amino-2-methylpropyl) 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(N)COC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 LJCJRRKKAKAKRV-UHFFFAOYSA-N 0.000 description 1
- 240000002989 Euphorbia neriifolia Species 0.000 description 1
- 239000004435 Oxo alcohol Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- RFAFBXGYHBOUMV-UHFFFAOYSA-N calcium chromate Chemical compound [Ca+2].[O-][Cr]([O-])(=O)=O RFAFBXGYHBOUMV-UHFFFAOYSA-N 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
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000001056 green pigment Substances 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- UHOKSCJSTAHBSO-UHFFFAOYSA-N indanthrone blue Chemical compound C1=CC=C2C(=O)C3=CC=C4NC5=C6C(=O)C7=CC=CC=C7C(=O)C6=CC=C5NC4=C3C(=O)C2=C1 UHOKSCJSTAHBSO-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001053 orange pigment Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 229920003009 polyurethane dispersion Polymers 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical class OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 description 1
- 235000013799 ultramarine blue Nutrition 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0084—Dispersions of dyes
- C09B67/0085—Non common dispersing agents
- C09B67/0089—Non common dispersing agents non ionic dispersing agent, e.g. EO or PO addition products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- 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
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0092—Dyes in solid form
- C09B67/0095—Process features in the making of granulates
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
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- C09C1/50—Furnace black ; Preparation thereof
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
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- C09C1/58—Agglomerating, pelleting, or the like by wet methods
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
本发明涉及一种颜料颗粒,其含有40-65重量%的颜料和至少10重量%的通式I:CH3-(CH2)n-CH2-O-[(CH2)p-O]m-H的化合物,其中n=8-18,p=1-4和m=35-100;所述通式I的化合物与颜料的重量比≥该颜料以m2/g计的STSA表面积乘以0.0021g/m2;和所述颜料颗粒的质量加权平均粒径是<20μm。该颜料颗粒可以通过将所述颜料和通式I的化合物分散于溶剂中,然后干燥获得的分散体来生产。根据本发明的颜料可以在水性漆和清漆体系、分散色漆、印刷油墨、油墨体系和涂料体系中用于着色和/或抗静电处理。
Description
本发明涉及颜料颗粒、其生产方法及其用途。
粉末颜料用于热塑性塑料和热固性塑料的着色。粉末颜料的优势在于它们不依赖于载体材料。但是,通常这个优势的实现是以损害可分散性为代价的。
为了改善可分散性,用树脂(DE 2540355)或用聚合物(US 3133893)涂覆颜料。
由EP 0036520可获知具体的干燥方法,其涉及将高度分散的颜料和临界温度低于颜料的分解温度的液体在加压下加热至该液体的临界温度之上,然后释放压力,将温度稳定保持在液体露点线(dew line)之上。
而且,EP 0282855公开了颜料制剂,其包含有机颜料和/或炭黑和选自烷基苯磺酸盐系列或特定的磺基丁二酸酯的表面活性剂,并且,如果合适,在湿粉碎后,通过喷雾干燥或冷冻干燥从水性介质中干燥该颜料制剂。
EP 1103173公开了用于染色种子的颜料制剂,其包含颜料和聚醚多元醇。
EP 857764公开了无机颜料颗粒,其包含无机颜料和基于颜料含量为0.1-10重量%的水溶性亲水助剂或疏水/亲水助剂,并且该无机颜料颗粒的平均粒径为50-1500μm。
此外,EP 1090081公开了水分散体,其包含颜料和式为[CH3(CH2)n][CH3(CH2)m]CH[(CH2)pO(AO)qH]的分散剂。
而且,由US 6063182和DE 19731572获知颜料制剂,以及由US 5837044获知喷墨油墨。
WO 2003055959公开了固体粒子制剂,其包括固体粒子和0.05-9重量%的化合物,所述化合物选自具有至少一个非氢端基的聚乙二醇或二醇、或者烷基磺酸酯。
此外,US 2005090609公开了平均粒径为50-5000μm和BET表面积为<=15m2/g的颜料颗粒,其尤其包含,基于聚醚为10-40重量%的至少一种非离子表面活性添加剂。
现有的颜料制剂的缺点在于在不加入添加剂的情况下其在水或水性表面涂料体系中的分散性能很差。
DE 102007026551公开一种颜料制剂,其包含至少一种颜料和至少一种通式为CH3-(CH2)n-CH2-O-[(CH2)p-O]m-H的化合物,其中n=8-18,p=1-4,和m=15-25。
本发明的一个目的是提供颜料颗粒,其在水中或水性表面涂料体系中呈现出良好的分散性能,同时具有很好的表面涂层色彩,而且,由此,在交联涂膜中该颜料颗粒的任何组分不产生浮色(迁移到涂膜的表面)。
本发明提供颜料颗粒,其特征在于,所述颜料颗粒包含基于颜料颗粒40-65重量%,优选43-63重量%,更优选45-60重量%,非常优选45-56重量%的颜料和基于颜料颗粒至少10重量%,优选至少12重量%,更优选至少15重量%,非常优选至少20重量%的通式I的化合物:
CH3-(CH2)n-CH2-O-[(CH2)p-O]m-H I,
其中n=8-18,优选n=10-18,更优选n=12-17,非常优选n=14-16;p=1-4,优选p=2;和m=35-100,优选m=35-90,更优选m=40-80,非常优选m=45-70;通式I的化合物与颜料的重量比大于或等于该颜料以m2/g计的STSA表面积乘以0.0021g/m2;而且该颜料颗粒的质量加权平均粒径是<20μm,优选<15μm,更优选<12μm,非常优选<9μm。
确定通式I的化合物与颜料重量比的下限可以确保通式I化合物对颜料表面(STSA表面积)的最小涂层。
该颜料的STSA表面积可以小于或等于385m2/g,优选小于或等于380m2/g。
除了颜料黑之外,根据ASTM D 6556(2004)测量该颜料的STSA表面积。对于颜料黑,与ASTM D 6556(2004)不符的是,在105℃下干燥样品。
用根据ISO 133201的激光衍射光谱法测定颜料颗粒的质量加权平均粒径。在购自Sympatec的HELOS激光衍射光谱仪中进行测定。在1巴的分散气压下分散颜料颗粒。根据Fraunhofer理论评估粒径分布。
使用的颜料可以是炭黑、炭气凝胶或彩色颜料。
可以使用的彩色颜料的实例包括黄色颜料、橙色颜料、红色颜料、洋红色颜料、紫色颜料、蓝色颜料、青色颜料、绿色颜料或棕色颜料。可以使用的彩色颜料包括无机蓝色颜料,例如铁蓝、群青蓝、钴蓝或混合相蓝色颜料,或者有机蓝色颜料,例如酞菁蓝或阴丹士林蓝。
使用的炭黑可以是炉黑、气黑、灯黑、乙炔黑、由WO 98/45361或DE 19613796已知的含硅炭黑、由DE 19521565获知的反性炭黑(inversion black)、和由WO 98/42778获知的含金属炭黑。作为炭黑,可以优选使用平均原生粒径为8-80nm,优选10-35nm和OAN值为40-200ml/100g,优选60-150ml/100g的颜料黑。
气黑具有的平均原生粒径可以为8-30nm,优选10-25nm。气黑具有的pH可以为2-5,优选3.5-4.5。
炉黑具有的平均原生粒径可以为8-80nm,优选10-50nm和OAN值可以为40-200ml/100g,优选50-180ml/100g。
使用根据ASTM D 2414的方法测量炭黑颜料的吸油值(OAN)。与ASTM D 2414(2000)不符的是,将炭黑颜料在105℃下干燥到恒重并且以ml/100g炭黑颜料记录吸油值。
使用根据DIN ISO 787/9(1995)的方法测量颜料黑的pH。与DIN ISO 787/9(1995)不符的是,使用去离子水(在使用前不经煮沸排气),操作的炭黑颜料的浓度是10%,将该炭黑颜料悬浮液搅拌1分钟,一直不断地添加5滴乙醇以便增湿,当显示恒定时读出pH。
根据DIN 53206测量平均原生粒径。根据校准TEM显微照片使用TGZ3粒径计数器直接测量平均原生粒径。
用作颜料的炭气凝胶可以具有20-1500m2/g,优选100-1200m2/g,更优选400-900m2/g的BET值。
根据DIN ISO 9277(1995)在购自Quantachrome的NOVA e2000吸附测量仪器中测量BET表面积。
用作颜料的炭气凝胶可以具有0.005-5cm3/g,优选0.05-3cm3/g,更优选0.2-2cm3/g的中孔体积。
用作颜料的炭气凝胶可以具有1.8-50nm,优选5-45nm,更优选10-35nm的平均中孔孔径。
根据DIN 66134(1998)通过BJH方法由在0.99-0.34的相对压力范围p/p0下记录的等温线解吸数据来测定中孔体积和孔径分布。
另外,用作颜料的炭气凝胶可以具有0.01-1.0cm3/g,优选0.05-0.5cm3/g,更优选0.1-0.35cm3/g的微孔体积。
根据DIN 66135-1、66135-2、66135-3(2001)用t-plot法测量微孔体积。根据de Boer等式评估t-plot。
用作颜料的炭气凝胶可以具有小于1μm,优选0.05-1μm,更优选0.1-1μm,非常优选0.5-0.95μm的平均粒径。
所述颜料可以是多种颜料的混合物。
通式I的化合物可以优选是CH3-(CH2)n-CH2-O-[(CH2)2-O]m-H,其中n=10、12、14、16或18和m=35-100。
通式I的化合物可以是例如CH3-(CH2)10-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)12-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)14-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)16-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)18-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)10-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)12-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)14-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)16-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)18-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)10-CH2-O-[(CH2)2-O]90-H、CH3-(CH2)12-CH2-O-[(CH2)2-O]90-H、CH3-(CH2)14-CH2-O-[(CH2)2-O]90-H、CH3-(CH2)16-CH2-O-[(CH2)2-O]90-H或CH3-(CH2)18-CH2-O-[(CH2)2-O]90-H。
颜料颗粒可以包括杀生物剂、pH调节剂、润湿剂、粘合剂、流动助剂或消泡剂。
该颜料颗粒可以包含沉淀法白炭黑和/或气相法白炭黑。
本发明的颜料颗粒可以包含分散剂。所述分散剂可以是非离子、阳离子、阴离子或两性润湿剂。除了通式I的化合物之外,本发明的颜料颗粒可以是不含分散剂的。
该颜料颗粒可以由基于该颜料颗粒40-65重量%,优选43-63重量%,更优选45-60重量%,非常优选45-56重量%的颜料;基于该颜料颗粒至少10重量%,优选至少12重量%,更优选至少15重量%,非常优选至少20重量%的通式I的化合物;任选存在的pH调节剂;任选存在的润湿剂;任选存在的粘合剂;任选存在的消泡剂;任选存在的流动助剂;和任选存在的杀生物剂组成:
CH3-(CH2)n-CH2-O-[(CH2)p-O]m-H I,
其中n=8-18,优选n=10-18,更优选n=12-17,非常优选n=14-16;p=1-4,优选p=2;和m=35-100,优选m=35-90,更优选m=40-80,很优选m=45-70,所述通式I的化合物与颜料的重量比可以大于或等于该颜料以m2/g计的STSA表面积乘以0.0021g/m2;以及该颜料颗粒的质量加权平均粒径可以为<20μm,优选<15μm,更优选<12μm,非常优选<9μm。
根据DIN ISO 787-2测量,该颜料颗粒可以具有0-20重量%,优选0.1-5重量%的残留含水量。
该颜料颗粒可以包含0-5重量%,优选0.1-3重量%的pH调节剂。
该颜料颗粒可以包含0-5重量%,优选0.1-3重量%的润湿剂。
该颜料颗粒可以包含0-5重量%,优选0.1-3重量%的粘合剂。
该颜料颗粒可以包含0-5重量%,优选0.1-3重量%的消泡剂。
该颜料颗粒可以包含0-5重量%,优选0.1-3重量%的流动助剂。
该颜料颗粒可以包含0-5重量%,优选0.1-3重量%的杀生物剂。
在本发明的一个实施方案中,该颜料颗粒可以由基于颜料颗粒40-65重量%,优选43-63重量%,更优选45-60重量%,非常优选45-56重量%的选自气黑、炉黑、颜料黄74、颜料蓝15:3和颜料红122的颜料;基于颜料颗粒至少10重量%,优选至少12重量%,更优选至少15重量%,非常优选至少20重量%的通式I的化合物;任选存在的pH调节剂;任选存在的润湿剂;任选存在的粘合剂;任选存在的消泡剂;任选存在的流动助剂;和任选存在的杀生物剂组成:
CH3-(CH2)n-CH2-O-[(CH2)p-O]m-H I,
其中n=8-18,优选n=10-18,更优选n=12-17,非常优选n=14-16;p=1-4,优选p=2;和m=35-100,优选m=35-90,更优选m=40-80,非常优选m=45-70,所述通式I的化合物与颜料的重量比可以大于或等于该颜料以m2/g计的STSA表面积乘以0.0021g/m2;以及该颜料颗粒的质量加权平均粒径可以为<20μm,优选<15μm,更优选<12μm,非常优选<9μm。
本发明另外提供一种生产本发明的颜料颗粒的方法,其特征在于:将基于颜料颗粒40-65重量%,优选43-63重量%,更优选45-60重量%,非常优选45-56重量%的颜料和基于颜料颗粒至少10重量%,优选至少12重量%,更优选至少15重量%,非常优选至少20重量%的通式I的化合物分散于溶剂中,其中所述通式I的化合物与颜料的重量比大于或等于该颜料以m2/g计的STSA表面积乘以0.0021g/m2;和随后干燥所得的分散体。
使用的溶剂可以是水、乙二醇、甘油、醇、酮或上述化合物的混合物。
可以用玻珠研磨机、行星式磨机、超声波、搅拌和混合元件、溶解器、振动混合器例如Skandex、转子-定子分散组件例如Ultra-Turrax、或高压均质器来进行分散。
可以通过冷冻干燥、红外线干燥、微波干燥或喷雾干燥来干燥所述分散体。
可以在喷雾干燥器中进行喷雾干燥,所述喷雾干燥器具有喷嘴雾化和并流、半逆流(喷射雾化)或逆流气体通道。
在喷雾干燥器中的雾化可以通过单流体或多流体喷嘴来进行。喷嘴孔径可以是0.01-3mm,优选0.05-2mm,更优选0.1-1.5mm。使用的雾化介质可以是气态物质例如空气、氮、CO2和氩。使用的喷嘴可以是完全圆锥体、空心圆锥体、平面喷射和直线喷射喷嘴。
可以用外场来辅助分散体进入到喷雾干燥器实现喷雾。所述外场可以是电场或声场,例如超声波。
可以通过旋转雾化器、加压雾化器、振动雾化器或文丘里喷嘴实现分散体进入到喷雾干燥器喷雾。
在喷雾干燥器中通过喷雾而产生的液滴尺寸可以是50nm-3mm,优选100nm-1mm,更优选200nm-0.5mm。
喷雾干燥可以在80-500℃,优选80-250℃的进口温度下进行。出口温度可以是10-150℃,优选15-90℃。
喷雾干燥可以在喷嘴下游0.03-1.2巴的压力水平下进行。
喷雾干燥可以在喷嘴处0.8-8巴的压力水平下进行。
分散体的干燥可以优选通过在进口温度为80-500℃,优选80-250℃,在喷嘴处压力水平为0.8-8巴和喷嘴孔径为0.01-3mm,优选0.05-2mm,更优选0.1-1.5mm下喷雾干燥来进行。
本发明的颜料颗粒可以在水性漆和表面涂料体系、乳胶漆、印刷油墨、液体油墨体系和涂料体系中用于着色和/或抗静电处理。
本发明另外提供一种表面涂料,其至少包含本发明的颜料颗粒。
本发明的颜料颗粒有利地在水或水性涂料体系中呈现出很好的搅拌分散性能,同时具有很好的表面涂层色彩,而且,在交联涂膜中该颜料颗粒的任何组分不产生浮色(迁移到涂膜的表面)。
实施例
实施例1-8
实施例1-8的颜料颗粒的生产
在表1中列出了颜料水分散体的组成。
表1
烷醇S 20是购自Tego的通式I的化合物(类别:脂肪醇乙氧基化物),其中p=2,m=20和n=16。
烷醇S 60是购自Tego的通式I的化合物(类别:脂肪醇乙氧基化物),其中p=2,m=60和n=16。
Lutensol AO 30是购自BASF AG的通式I的化合物(类别:羰基醇乙氧基化物),其中p=2,m=30和n=11-13。
着色用炭黑S 160是购自Evonik Degussa GmbH的气黑,其具有123m2/g的平均STSA。
着色用炭黑FW 171是购自Evonik Degussa GmbH的炉黑,其具有380m2/g的平均STSA。
AMP 90是购自Angus Chemie的2-氨基-2甲基-丙醇。
2-二甲基氨基乙醇是购自Merck KGaA的胺。
TEGO消泡剂XP 7001是购自Evonik Tego的消泡剂。
Acticide MBS是购自Thor Chemie的杀生物剂。
1.实施例1-8的润湿剂溶液的制备
首先将通式I的化合物熔融并且将待使用的水加热到约45℃。随后,使用溶解器将这两个组分按照表1的比例混合60分钟。随后如表1所述向该润湿剂溶液中加入pH调节剂、任选存在的消泡剂、异丙醇和杀生物剂。
2.将颜料加入/预分散到制备的润湿剂溶液中
为了制备不同的颜料分散体1-8,将相应的颜料在缓慢搅拌下加入到制备的润湿剂溶液中。
3.分散
用购自FrymaKoruma的CoBall-Mill MS 12环形隙玻珠研磨机(AGBM)利用氧化锆磨料(0.75-1.0mm,钇稳定的)将在2中制备的颜料分散体1-8分散。磨料的装载量是60%以及圆周速度是12m/s。在每个情况下运行9遍。分散之后的颜料分散体1-8为高度流动的均质分散体。
4.喷雾干燥
随后将颜料分散体1-8喷雾干燥(Büchi 190Mini喷雾干燥器,喷嘴孔径0.5mm,喷嘴处压力水平2巴)。用蠕动泵将分散体传输到喷雾喷嘴,并在200℃的进口温度和80℃的出口温度下进行干燥。通过旋流器将颗粒沉积。这得到如表2所计算的颜料颗粒组成。为了计算,假定在喷雾干燥之后不再考虑助剂AMP 90、2-二甲基氨基乙醇、消泡剂XP 7001、Acticide MBS和异丙醇,由于它们低的比例和低沸点。此外,测量颜料颗粒的残留含水量并且从100%之中减去该残留含水量,因此剩余的在颜料和通式I的化合物之间分配。
表2
涂料试验
用传统的分散法根据相应的颜料黑S160和FW 171产生的涂料作为相对于本发明涂料的对照涂料A-C。
a.生产对照涂料A-C
颜料黑S160和FW 171的对照涂料的漆浆组成如下:
Tego Dispers 760W,35%是购自Tego的润湿和分散助剂。
Tego Foamex 830是购自Tego的消泡剂。
将物质1-4称重到Skandex分散烧杯(180ml,直径5.3cm,高度12.5cm)内并且用抹刀均质化。将预先在105℃下干燥的颜料黑称重并且在抹刀搅拌下加入,直到润湿全部量。
用实验室溶解器(Pendraulik,LR 34)将该漆浆用直径为40mm的分散圆盘以4000rpm预分散5分钟。
随后测量初步分散体的pH。通过添加AMP 90将pH调节到8.5-9.0的数值。
然后将直径为3mm的540g Chromanit钢珠加入到该漆浆中。
利用实验室震动器(Skandex分散器BA S 20)研磨颜料黑。分散时间是60分钟。将该实验室震动器的冷却设置为2级。
在分散操作之后,利用VA不锈钢筛筛选该漆浆并且将其收集在350ml的塑料烧杯中。然后,再次检测pH并且如果合适通过添加AMP 90将pH调节到8.2-8.7的数值。
使用的稀释粘合剂是购自Alberdingk & Boley,Alberdingk U710的聚氨酯分散体(30%)。
如上所述产生的漆浆是如下的调漆:
用于相对于实施例1-3的对照涂料A和B的调漆:
1.漆浆 5.6g
2.Alberdingk U710,30% 24.4g
总计 30g
炭黑浓度,总计 2.4%
用于相对于实施例4-8的对照涂料C的调漆:
1.漆浆 5.6g
2.Alberdingk U710,30% 42.9g
总计 48.5g
炭黑浓度,总计 1.5%
以所述的顺序将漆浆和粘合剂的量称重到180ml的混合烧杯,然后用抹刀强烈均质化10分钟。在1小时之后,根据DIN EN ISO 1524用Erichsen细度计元件测量细度值(研磨细度)。
b.基于颜料颗粒1-8的涂料的生产(表2)
在Skandex分散烧杯(180ml,直径5.3cm,高度12.5cm)中装入完全软化的水,在所有情况下,借助于抹刀在搅拌下加入一组颗粒1-8。然后使用溶解器在3000rpm下分散10分钟,所述溶解器具有直径为40mm的溶解器圆盘。
选择完全软化的水与颗粒的比值以便产生15重量%浓度的颜料。将该浆料静置过夜。
利用购自Alberdingk & Boley的稀释粘合剂Alberdingk U710(30%)调稀由此产生的浓浆料。
对于实施例1-3的涂料,调漆的炭黑浓度是2.4%;对于实施例4-8的涂料,调漆的炭黑浓度是1.5%。
将浆料和粘合剂的量称重到180ml的混合烧杯中,然后用抹刀强烈均质化10分钟。在1小时之后,根据DIN EN ISO 1524用Erichsen细度计元件测量细度值(研磨细度)。
c.施涂来自a的对照涂料A-C和来自b的涂料,并且测量色彩
将完成的涂料用狭缝高度为200μm的薄膜牵引棒在均一的张力和压力下拉伸到玻璃板上(130×90×1mm)。为了这个目的,利用塑料吸管吸出2ml完成的涂料以便拉伸,并且将其以5cm长和约1cm宽的条施涂到玻璃板上。应该注意确保在涂层条中没有产生气泡。将薄膜牵引棒置于涂层条的上方并且均匀拉伸过该板。产生的拉伸是大约10cm长和6cm宽。
在拉伸工序之后,将在玻璃板上的湿涂层在室温下通风30分钟,然后在80℃下将涂层玻璃板强制干燥30分钟。
利用Pausch Q-Color 35仪器和WinQC+软件测量色彩。从后面通过涂层玻璃来进行所有的测量。
计算色彩的数据:
与色彩无关的黑色值My和由色彩决定的黑色值Mc:
首先,由测量的三色Y(光源D65/10)计算与色彩无关的黑色值My(等式1):
随后,计算由色彩决定的黑色值(等式2):
Xn/Zn/Yn(DIN 6174)=根据光源和观察者,坐标原点的三色值(DIN5033/部分7,光源D65/10°)。
Xn=94.81 Zn=107.34 Yn=100.0
X/Y/Z=由样品的测量计算的三色值。
绝对色彩贡献(Absolute hue contribution)dM:
由黑色值Mc和My测量绝对色彩贡献dM(等式3):
(3)dM=Mc-My
表3比较了颜料颗粒1-8的涂料测试的结果与对照涂料的涂料测试的结果。色深My的值越大,相应涂膜的颜色越深(“越黑”)。底色dM的值越大,颜料在涂膜中的分布越稳定,黑色涂膜的外表越蓝。为了肯定的评估,基于相应颜料颗粒的涂膜的色深My和底色dM的值必须至少为相应对照涂膜的色深值My和底色dM的水平。此外,研磨细度应该具有小于10μm的值,表面应该是视觉良好的、没有不均匀性和聚集的颜料颗粒,以及在48小时的存储时间之后通式I的化合物一定不能迁移到涂膜的表面(浮色)。
表3
对照涂料1与对照涂料A的色彩不相符。没有实现色深My和蓝底色dM。表面不是令人满意的,并且m=20的通式I的化合物产生浮色。
对照涂料2与对照涂料B的色彩不相符。没有实现色深My。表面粗糙并且具有看得见的颜料结块。通式I的化合物与颜料黑的比值过低。m=30的化合物I产生浮色。
对照涂料3与对照涂料B的色彩几乎相符。研磨细度是令人满意的。通式I的化合物与颜料黑的比值是令人满意的。然而,m=30的通式I的化合物如前所述产生浮色。
含有m=60的通式I的化合物的对照涂料4不再产生浮色。然而,通式I的化合物与颜料黑FW 171的比值过低。涂层的表面是破碎的,研磨细度是令人不满意的,而且没有获得对照涂料C的色彩数据。
本发明的涂料5-8优于对照涂料C的色彩数据。研磨细度<10μm,而且涂膜的表面没有破碎,是令人满意的。通式I的化合物没有产生浮色。
Claims (7)
1.颜料颗粒,其特征在于,所述颜料颗粒包含基于颜料颗粒40-65重量%的颜料和基于颜料颗粒至少10重量%的通式I的化合物:
CH3-(CH2)n-CH2-O-[(CH2)p-O]m-H I,
其中n=8-18,p=1-4和m=35-100;所述通式I的化合物与颜料的重量比大于或等于该颜料以m2/g计的STSA表面积乘以0.0021g/m2;以及所述颜料颗粒的质量加权平均粒径是<20μm。
2.根据权利要求1的颜料颗粒,其特征在于,所述颜料是彩色颜料、炭气凝胶或炭黑。
3.根据权利要求1或2的颜料颗粒,其特征在于,所述通式I的化合物是CH3-(CH2)10-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)12-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)14-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)16-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)18-CH2-O-[(CH2)2-O]35-H、CH3-(CH2)10-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)12-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)14-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)16-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)18-CH2-O-[(CH2)2-O]60-H、CH3-(CH2)10-CH2-O-[(CH2)2-O]90-H、CH3-(CH2)12-CH2-O-[(CH2)2-O]90-H、CH3-(CH2)14-CH2-O-[(CH2)2-O]90-H、CH3-(CH2)16-CH2-O-[(CH2)2-O]90-H或CH3-(CH2)18-CH2-O-[(CH2)2-O]90-H。
4.根据权利要求1的颜料颗粒,其特征在于,其残留含水量是0-20重量%。
5.生产根据权利要求1-4之一的颜料颗粒的方法,其特征在于,将基于颜料颗粒40-65重量%的颜料和基于颜料颗粒至少10重量%的通式I的化合物分散于溶剂中,其中所述通式I的化合物与颜料的重量比大于或等于该颜料以m2/g计的STSA表面积乘以0.0021g/m2;以及随后干燥所产生的分散体。
6.根据权利要求1-4之一的颜料颗粒在水性漆和表面涂料体系、乳胶漆、印刷油墨、液体油墨体系和涂料体系中用于着色和/或抗静电处理的用途。
7.表面涂料,其特征在于,所述表面涂料至少包含根据权利要求1-4之一的颜料颗粒。
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2008
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- 2009-11-19 JP JP2011537941A patent/JP5583138B2/ja active Active
- 2009-11-19 ES ES09763908.2T patent/ES2533482T3/es active Active
- 2009-11-19 EP EP20090763908 patent/EP2350210B9/de active Active
- 2009-11-19 BR BRPI0921960A patent/BRPI0921960A2/pt not_active IP Right Cessation
- 2009-11-19 CA CA2744421A patent/CA2744421C/en active Active
- 2009-11-19 WO PCT/EP2009/065500 patent/WO2010060858A2/de active Application Filing
- 2009-11-19 PL PL09763908T patent/PL2350210T3/pl unknown
- 2009-11-19 AU AU2009319060A patent/AU2009319060A1/en not_active Abandoned
- 2009-11-19 CN CN200980147797.5A patent/CN102227479B/zh active Active
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- 2009-11-19 MX MX2011005443A patent/MX2011005443A/es not_active Application Discontinuation
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110343407A (zh) * | 2018-04-03 | 2019-10-18 | M/s科尔颜料私人有限公司 | 防尘且易于分散的颜料 |
Also Published As
Publication number | Publication date |
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KR101676505B1 (ko) | 2016-11-15 |
EP2350210B9 (de) | 2015-05-20 |
WO2010060858A2 (de) | 2010-06-03 |
AU2009319060A1 (en) | 2010-06-03 |
ZA201103879B (en) | 2012-01-25 |
IL212004A0 (en) | 2011-06-30 |
PL2350210T3 (pl) | 2015-06-30 |
JP5583138B2 (ja) | 2014-09-03 |
DE102008044116A1 (de) | 2010-06-02 |
US20110232531A1 (en) | 2011-09-29 |
MX2011005443A (es) | 2011-06-09 |
KR20110098717A (ko) | 2011-09-01 |
US8915998B2 (en) | 2014-12-23 |
JP2012509969A (ja) | 2012-04-26 |
ES2533482T3 (es) | 2015-04-10 |
WO2010060858A3 (de) | 2010-08-05 |
CN102227479B (zh) | 2014-03-05 |
EP2350210B1 (de) | 2015-01-07 |
BRPI0921960A2 (pt) | 2016-01-05 |
MA32897B1 (fr) | 2011-12-01 |
CA2744421A1 (en) | 2010-06-03 |
EP2350210A2 (de) | 2011-08-03 |
CA2744421C (en) | 2016-11-29 |
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