五氯硝基苯催化加氢法合成3,5-二氯苯胺  

Synthesis of 3,5-Dichloroaniline by Catalytic Hydrogenation——Catalytic Hydrogenation of Pentachloronitrobenzene

作　　者：固旭[1,2] 李东[2] 张强华[2] 蒋金龙[2] 刘晓勤[1] 

机构地区：[1]南京工业大学化学化工学院,南京210009 [2]淮阴工学院生化学院,江苏淮安223003

出　　处：《农药》2010年第10期723-725,共3页Agrochemicals

基　　金：江苏省科技攻关项目(BE2004386)

摘　　要：3,5-二氯苯胺是一种重要农药中间体。采用多氯代硝基苯催化加氢脱氯合成3,5-二氯苯胺是一种清洁合成工艺。研究了合成路线中五氯硝基苯催化加氢制备五氯苯胺工艺,主要考察了催化剂、溶剂、反应温度和反应压力对加氢反应的影响。结果表明:与骨架镍相比,Pd/C催化剂具有较好的催化活性和选择性,虽然负载量为10%Pd/C比5%Pd/C催化活性高,但易发生深度脱氯;反应适宜的溶剂为环己烷;在优化的反应条件下,五氯硝基苯转化率可达99%以上,五氯苯胺选择性可达95%以上。As an important intermediate of pesticides,3,5-dichloroaniline could be synthesized by the catalytic hydrodechlorination of polychloronitrobenzene,which is a clean production process.The synthesis of 3,5-dichloroaniline from pentachloronitrobenzene via catalytic hydrogenation was explored by investigating the effects of process parameters,such as catalysts,solvents,temperature,and hydrogen pressure.Pd/C catalyst exhibited superior catalytic activity,as well as selectivity,over raney-Ni.In spite of higher catalytic activity in the comparison with 5% Pd/C,10% Pd/C coursed more deep-dechlorinated products.Cyclohexane was the best solvent in our study.Under the optimal condition,the convertion ratio of pentachloronitrobenzene and the selectivity to pentachloroaniline could reach 99 and 95%,respectively.

关 键 词：催化加氢 五氯硝基苯 五氯苯胺 3 5-二氯苯胺 

分 类 号：TQ246.34[化学工程—有机化工]