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    • 3. 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。
    • 4. 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。
    • 7. 发明授权
    • Process for preparing quinacridone pigments
    • 制备喹吖啶酮颜料的方法
    • US5755872A
    • 1998-05-26
    • US834728
    • 1997-04-01
    • Manfred UrbanDieter SchnaitmannMartin Bohmer
    • Manfred UrbanDieter SchnaitmannMartin Bohmer
    • C09B67/20C09B48/00C09B67/52
    • C09B48/00
    • A process for preparing quinacridone pigments A process for preparing pigments, mixed crystal pigments and pigment preparations based on linear unsubstituted or substituted quinacridones of the formula (I) ##STR1## in which the substituents R.sup.1 and R.sup.2 are identical or different and are hydrogen, chlorine, bromine or fluorine atoms or are C.sub.1 -C.sub.4 -alkyl, C.sub.1 -C.sub.4 -alkoxy or carboxamido groups which may be substituted by C.sub.1 -C.sub.6 -alkyl groups; or are phenoxy or C.sub.6 -C.sub.10 -aryl rings onto which further aromatic, aliphatic or heterocyclic rings can be fused, which process comprises hydrolyzing the reaction mixture resulting from cyclization of the respective dianilinoterephthalic acid with polyphosphoric acid or polyphosphate at a temperature of or above 110.degree. C. with water or an aqueous mineral acid solution and then isolating the pigments thus obtained directly; or subjecting the resulting prepigments, if desired after addition of organic solvents, to a finishing treatment and isolating the pigments; or subjecting the resulting coarsely crystalline crude pigments to fine dispersion and then isolating the pigments; or subjecting the prepigments obtained after fine dispersion, if desired after addition of solvents, to a finishing treatment and isolating the pigments. This gives quinacridone pigments having excellent coloristic and rheological properties.
    • 制备喹吖啶酮颜料的方法基于式(I)的线性未取代或取代的喹吖啶酮制备颜料,混合晶体颜料和颜料制剂的方法其中取代基R 1和R 2相同或不同,并且为 氢,氯,溴或氟原子,或者可以被C 1 -C 6 - 烷基取代的C 1 -C 4 - 烷基,C 1 -C 4 - 烷氧基或甲酰胺基; 或者是其上可以稠合另外的芳族,脂族或杂环的苯氧基或C6-C10-芳基环,该方法包括水解由相应的二苯胺基对苯二甲酸与多磷酸或多磷酸盐在大于或等于110的温度环化而引起的反应混合物 用水或无机酸水溶液洗脱,然后直接分离得到的颜料; 或者如果需要,在加入有机溶剂之后对所得到的标号进行精加工处理并分离颜料; 或将所得粗结晶粗颜料进行细分散,然后分离颜料; 或者如果需要,在加入溶剂之后将精细分散后获得的标号进行精加工处理并分离颜料。 这使得喹吖啶酮颜料具有优异的色泽和流变性能。