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    • 6. 发明授权
    • Process for preparing N,N′-dimethylperylene-3,4,9,10-tetracarboxylic diimide in transparent pigment form
    • 制备透明颜料形式的N,N'-二甲基亚丙基-3,4,9,10-四羧酸二酰亚胺的方法
    • US06174361B1
    • 2001-01-16
    • US09373805
    • 1999-08-13
    • Manfred UrbanMartin BoehmerJoachim Weber
    • Manfred UrbanMartin BoehmerJoachim Weber
    • C09B562
    • C09B67/0033C09B5/62C09B67/0022
    • The invention relates to a process for preparing N,N′-dimethylperylene-3,4,9,10-tetracarboxylic diimide, utilizing the reaction of perylene-3,4,9,10-tetracarboxylic dianhydride with monomethylamine, which comprises employing at least 2 times the molar amount of monomethylamine per mole of perylene-3,4,9,10-tetracarboxylic dianhydride and at least 3 times the amount by weight of water based on the weight of the dianhydride, conducting the reaction at a temperature from 50 to 200° C., removing unreacted monomethylamine by distillation, subjecting the resulting crude pigment to wet grinding in a liquid, aqueous or aqueous-organic medium in a stirred ballmill which is operated with a power density of more than 1.5 kW per liter of milling space and a stirrer tip speed of more than 12 m/s under the action of grinding media having a diameter of less than or equal to 0.9 mm, and isolating the pigment obtained, with the proviso that at any desired point during the process, but no later than during wet grinding, one or more additives from the group consisting of pigment dispersants and surfactants are added.
    • 本发明涉及一种利用苝-3,4,9,10-四羧酸二酐与一甲胺的反应制备N,N'-二甲基亚丙基-3,4,9,10-四羧酸二酰亚胺的方法,该方法包括至少使用 每摩尔苝-3,4,9,10-四羧酸二酐的摩尔量为1摩尔的2倍,并且是基于二酐重量的水的重量的至少3倍,在50至50℃的温度下进行反应 通过蒸馏除去未反应的一甲胺,使得到的粗颜料在搅拌式球磨机中的液态水溶液或水性有机介质中进行湿法研磨,所述搅拌式球磨机的功率密度大于1.5kW /升研磨空间 并且在直径小于或等于0.9mm的研磨介质的作用下,搅拌器尖端速度大于12m / s,并且分离所获得的颜料,条件是在该过程中的任何期望点,但是没有 比du晚 加入环状湿法研磨,添加一种或多种由颜料分散剂和表面活性剂组成的组中的添加剂。
    • 7. 发明授权
    • Process for preparing linear unsubstituted .beta.-phase quinacridone
pigments
    • 线性无取代β相喹吖啶酮颜料的制备方法
    • US5755874A
    • 1998-05-26
    • US834725
    • 1997-04-01
    • Manfred UrbanDieter Schnaitmann
    • Manfred UrbanDieter Schnaitmann
    • C09B67/20C09B67/52C09B48/00
    • C09B67/0027
    • Process for preparing linear unsubstituted .beta.-phase quinacridone pigments A process for preparing linear unsubstituted .beta.-phase quinacridone pigments or pigment preparations, which comprises a) cyclizing 2,5-dianilinoterephthalic acid in polyphosphoric acid or polyphosphoric ester with a phosphorus pentoxide content of at least 84% by weight to form the quinacridone, b) subsequently hydrolyzing this quinacridone with water or with an aqueous mineral acid solution, preferably orthophosphoric acid solution, at a temperature of at least 40.degree. C., preferably from 60.degree. to 105.degree. C., to form the crude quinacridone pigment which is predominantly in the .alpha.-phase, c) then heating the crude .alpha.-phase quinacridone pigment to a temperature between 120.degree. and 200.degree. C. in the presence of a from 0.1 to 3% strength by weight, preferably from 0.2 to 2% strength by weight, inorganic base in water and alkali-stable organic solvents, for the change of phase into coarsely crystalline crude .beta.-phase pigment, and d) subjecting the coarsely crystalline crude .beta.-phase quinacridone pigment, for the fine division to form a pigment or prepigment, to dry or wet milling; and then isolating the resulting finely divided .beta.-phase pigment; e) or subjecting the finely divided .beta.-phase prepigment obtained in d) to a finish treatment in the presence of solvents, and then isolating the pigment.
    • 制备线性未取代的β-相喹吖啶酮颜料的方法制备线型未取代的β-相喹吖啶酮颜料或颜料制剂的方法,其包括:a)使多磷酸或多磷酸中的2,5-二苯胺基对苯二甲酸至少在五氧化二磷含量至少 84重量%以形成喹吖啶酮,b)随后用水或无机酸水溶液(优选正磷酸溶液)在至少40℃,优选60℃至105℃的温度下水解该喹吖啶酮。 ,以形成主要在α相中的粗喹吖啶酮颜料,c)然后在0.1至3%的强度存在下,将粗α-相喹吖啶酮颜料加热至120至200℃的温度, 重量,优选0.2-2%重量,无机碱在水和碱稳定的有机溶剂中,用于将相变为粗结晶的Cr udeβ相色素,和d)将粗结晶粗β相喹吖啶酮颜料进行细分,形成颜料或指色剂进行干或湿磨; 然后分离得到的细碎的β-相色素; e)或在d)中得到的细碎的β-相指示剂在溶剂存在下进行最终处理,然后分离颜料。
    • 8. 发明授权
    • Surface-treated quinacridone and dioxazine pigments
    • 表面处理的喹吖啶酮和二恶嗪颜料
    • US5746820A
    • 1998-05-05
    • US837720
    • 1997-04-22
    • Manfred UrbanDieter Schnaitmann
    • Manfred UrbanDieter Schnaitmann
    • C09B67/14C09B67/08C09B67/20C09C3/08C09D7/12C09C1/02C08K5/00C08K5/34C09B48/00
    • C09B67/0009C09B67/0065
    • The use of sulfuric monoesters of the formulae (I) and (II) R.sup.1 --O--(CH.sub.2 O).sub.n --SO.sub.3 .sup.- M.sup.+ (I) R.sup.1 --CO--NR.sup.2 --(CH.sub.2 O)(.sub.n+1)--SO.sub.3 .sup.- M.sup.+ (II) in which R.sup.1 is a straight-chain or branched alkyl group of 10 to 24 carbon atoms, R.sup.2 is a hydrogen atom or a C.sub.1 -C.sub.6 -alkyl group, M.sup.+ is a hydrogen ion, an alkali metal ion, 1/2 an alkaline earth metal ion, or an ammonium ion of the formula N.sup.+ R.sup.3 R.sup.4 R.sup.5 R.sup.6, where the substituents R.sup.3, R.sup.4, R.sup.5 and R.sup.6 independently of one another are each hydrogen atoms or C.sub.1 -C.sub.6 -alkyl groups, which alkyl groups can be substituted by 1 to 3 hydroxyl groups, and n is a number from 0 to 4; or of a mixture of at least two sulfuric monoesters of the formulae (I) and/or (II), for preparing surface-treated pigments from the classes of the quinacridones and dioxazines.
    • 式(I)和(II)的硫酸单酯使用R 1 -O-(CH 2 O)n -SO 3 -M +(I)R 1 -CO-NR 2 - (CH 2 O)(n + 1)-SO 3 -M + ),其中R 1是10-24个碳原子的直链或支链烷基,R2是氢原子或C1-C6烷基,M +是氢离子,碱金属离子,+ E, / 2 + EE为碱土金属离子,或式N + R3R4R5R6的铵离子,其中取代基R 3,R 4,R 5和R 6彼此独立地为氢原子或C 1 -C 6 - 烷基,该烷基 可以被1〜3个羟基取代,n为0〜4的数。 或由式(I)和/或(II)的至少两种硫酸单酯的混合物制备用于由喹吖啶酮和二恶嗪类制备表面处理的颜料。