Pd/C催化加氢法合成3,3’-二氯联苯胺  

The Synthesis of 3,3'-Dichlorobenzidine by Pd/C Catalytic Hydrogenation

作　　者：闫茂文[1] 陈宏博[1] 徐善利[1] 李树德[1] 

机构地区：[1]大连理工大学化工学院,大连116012

出　　处：《染料与染色》2005年第4期64-65,26,共3页Dyestuffs and Coloration

摘　　要：在碱性介质中,以Pd/C为催化剂,对邻硝基氟苯催化加氢制备2,2’-二氯氢化偶氮苯(DHB)进行研究,采用正交法对加氢还原进行了条件优化,优化条件为:反应温度65℃氢氧化钠质量浓度为:538g/l;Pd/C用量为4.0%;助催化剂NQON用量为2.67%。在该条件下催化剂可重复使用6次,所得产物DHB质量分数大于94.5%。在强酸性条件下,将DHB重排得5,3’二氯联苯胺盐酸盐,重排反应收率为90.0%,总收率85.0%。2,2＇-Dichlorohydrobenzene（DHB）was prepared by catalytic hydrogenation of 2-nitrochlorobenzene using Pd/C as a catalyst in alkaline medium. The optimum reaction conditions were determined by orthogonal experiments as follows： reaction temperature was 65℃ ; concentration of NaOH was 538gL^-1; the ratio of Pd/C catalyst to 2-nitrochlorobenzene was 4.0%; the amount of NQON was 2.67%; Pd/ C catalyst could be recycled at least six times under the optimum conditions, and the yield of DHB was 〉 94.5%.DHB was rearranged in strong acid medium to give 3,3＇-dichlorobenzidine （DCB） with a yield of 90.0%, the overall yield was 85.0%.

关 键 词：催化加氢 邻硝基氯苯 3 3’-二氯联苯胺 

分 类 号：TQ246[化学工程—有机化工]