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    • 3. 发明授权
    • Process for the continuous preparation of 3,3'-dichloro-benzidine
dihydrochloride
    • 连续制备3,3'-二氯苯胺二氯化物的方法
    • US5208376A
    • 1993-05-04
    • US856063
    • 1992-06-08
    • Kurt HabigKonrad BaesslerKlaus Warning
    • Kurt HabigKonrad BaesslerKlaus Warning
    • C07C209/42C07C209/54C07C211/52
    • C07C209/54
    • A process for the continuous preparation of 3,3'-dichlorobenzidine dihydrochloride from 2,2'-dichlorohydrazobenzene by treatment with aqueous sulfuric acid, which comprises treating the 2,2'-dichlorohydrazobenzene, dissolved in a water-immiscible aromatic solvent, continuously at temperatures of from about 20.degree. to about 50.degree. C. in the presence of an alkali metal salt of an alkyl (C.sub.8 -C.sub.23)polyglycol ether sulfate, with such an amount of from about 50 to about 80 % strength aqueous sulfuric acid that the suspension formed remains conveyable, subsequently diluting the suspension emerging from the reaction zone with water, again continuously, and subsequently heating the suspension to a temperature of from about 90.degree. to about 95.degree. C. until a solution is obtained, separating off the aromatic solvent from the hot, sulfuric acid aqueous phase, and precipitating the 3,3'-dichlorobenzidine dihydrochloride by adding hydrochloric acid to the sulfuric acid solution which remains and filtering off this product.
    • PCT No.PCT / EP90 / 01844 Sec。 371日期:1992年6月8日 102(e)日期1992年6月8日PCT 1990年11月3日PCT PCT。 第WO91 / 07377号公报 日本1991年5月30日。一种通过用硫酸水溶液连续制备3,3'-二氯联苯胺二盐酸盐的方法,该方法包括处理溶于水中的2,2'-二氯代苯, 不饱和的芳族溶剂,在约20至约50℃的温度下,在烷基(C 8 -C 23)聚乙二醇醚硫酸盐的碱金属盐存在下,其量为约50至约80% 形成的悬浮液的强度硫酸水溶液仍然是可输送的,随后再次用水稀释从反应区出来的悬浮液,随后将悬浮液加热到约90℃至约95℃的温度,直至获得溶液 ,从热硫酸水相中分离芳族溶剂,并通过向硫酸溶液中加入盐酸沉淀出3,3'-二氯联苯胺二盐酸盐,其中r 发出并过滤掉本产品。