无溶剂法加氢还原制备3,4-二氯苯胺  

Preparation of 3, 4-Dichloronitrobenzene by Solvent-free Catalytic Hydrogenation

作　　者：鄢冬茂[1] 李付刚[1] 闫士杰[1] 李文骁[1] 

机构地区：[1]沈阳化工研究院有限公司,沈阳110021

出　　处：《染料与染色》2014年第2期34-36,40,共4页Dyestuffs and Coloration

基　　金：国家十二五科技支撑计划资助项目(No:2011BAE07B07)

摘　　要：以新型Pt/C为催化剂,无溶剂法加氢还原3,4-二氯硝基苯制备3,4-二氯苯胺,反应温度100℃,氢气压力1.0 MPa。实验结果:3,4-二氯苯胺含量99.75%(GC),脱氯副反应<0.1%,收率>99%。建立了反应过程的液相色谱中控分析方法,对中间产物进行了LC-MS表征,发现了中间体3,4-二氯苯基羟胺浓度随反应温度的变化规律。3, 4-Diehloroaniline was synthesized from 3, 4-dichloronitrobenzene with a new Pt/C catalyst by Solvent-free hydrogenation. The reaction temperature was 100 ~C, and the hydrogen pressure was 1.0 MPa. The purity of the product was 99. 75% （GC）, the side reaction of deehlorination 〈0. 1%, the yield 〉 99%. The reaction process was researched by liquid chromatography; the structures of intermediate were characterized by LC - MS. The relation between 3, 4-dichlorophenylhydroxylamine concentration and the reaction temperature was disclosed.

关 键 词：催化加氢 PT C 3 4-二氯硝基苯 3 4-二氯苯胺 

分 类 号：TQ246.31[化学工程—有机化工]