水合肼催化还原法制备4-氨基二苯胺

SYNTHESIS OF 4-AMINODIPHENYLAMINE BY HYDRAZINE HYDRATE CATALYTIC REDUCTION

以80%的水合肼为还原剂,Fe(OH)3/C为催化剂,还原4-硝基二苯胺得到4-氨基二苯胺,通过质谱和红外光谱表征了目标产物结构,通过液相色谱测定了产物纯度。较佳工艺条件为:4-硝基二苯胺用量0.05mol,Fe(OH)3负载量约5%的Fe(OH)3/C复合催化剂用量0.45g,水合肼5mL,反应温度80℃,反应时间60min,4-氨基二苯胺的收率可达98.4%。研究表明,以Fe(OH)3为主催化剂,酸处理过的活性炭为助剂,4-硝基二苯胺可被水合肼高效还原为4-氨基二苯胺,产品收率和纯度较高,工艺过程清洁环保。

4-Aminodiphenylamine was prepared through the reduction of 4-nitrosodiphenylamine with hydrazine hydrate as reducer and Fe（OH）3/C as catalyst.The chemical structures of the target product were characterized by MS and IR,and the purity was determined by LC.The yield of 4-aminodiphenylamine could be up to 98.4 ％ under the following reaction conditions：dosage of 4-nitrodiphenylamine was 0.05 mol,composite catalyst （Fe（OH）3/C） with the loading of Fe（OH）3 about 5％ was 0.45 g,hydrazine hydrate was 5.0 mL and reacted at 80 ℃ for 1 h.The results show that composite catalyst of Fe（OH）3/C,with Fe（OH）3 as main catalyst and acid treated activated-carbon as assistant catalyst,is a efficient catalytic system for the reduction of 4-nitrosodiphenylamine to obtain 4-aminodiphenylamine with high yield and high purity under the conditions of clean process.