催化加氢制备4-氨基二苯胺的工艺研究

A Study on the Preparation of 4-Aminodiphenylamine by Catalytic Hydrogenation

本文探索了4-氨基二苯胺合成方法中的最新工艺硝基苯法加氢工艺的研究。经实验确定的优化条件为:Raney镍为催化剂,催化剂用量为对硝基二苯胺质量的10%,甲醇为溶剂,用量为与对硝基二苯胺缩合液体积比为1∶1,于80℃以下,反应起始压力0.5MPa,反应压力1.5MPa,反应时间90分钟,加氢转化率达100%,4-氨基二苯胺收率95%,并用气相色谱和高效液相色谱对产物进行了定性和定量分析。

4-Aminodiphenylamine was prepared from 4-nitrodiphenyamine by means of liquid catalytic hydrogenation. The optimized condition was confirmed by experiment, the catalyst was Raney Ni, the useage of catalyst is 10% of 4-nitrodiphenyamine in weight, use methanol as the solvent,the volume of which was equal to the volume of 4-nitrodiphenyamine. And then under 80℃/1.5 MPa for 90 min, the conversion of hydrogenation was 100%, the yield of 4-aminodiphenyamine was 95%, the compound was identified and characterized by melting point, chromatography and mass spectrometry.