对硝基苯胺水相加氢合成对苯二胺  

Synthesis of p-Phenylenediamine by Hydrogenation of p-Nitroaniline in Water

作　　者：李建昌 丁兴成 高立江 陶彬彬 路旭阳 陈宝兴 LI Jian-chang;DING Xing-cheng;GAO Li-jiang;TAO Bin-bin;LU Xu-yang;CHEN Bao-xing(Zhejiang Runtu Co.,Ltd.,Shaoxing,Zhejiang,China)

机构地区：[1]浙江闰土股份有限公司

出　　处：《精细化工》2019年第7期1488-1493,1500,共7页Fine Chemicals

摘　　要：以对硝基苯胺为原料,水为溶剂,考察了水相中负载型镍催化剂催化对硝基苯胺加氢还原的反应性能,并开展了中试实验。考察了反应温度、压力、保温时间、对硝基苯胺浓度、废水套用等因素对催化加氢反应性能的影响。实验结果表明,产品对苯二胺质量分数较高,催化剂和水可循环使用。得到较佳的工艺条件为:温度110℃,保温时间1 h,压力2.0MPa,搅拌转速800 r/min,起始催化剂用量10%(以对硝基苯胺的质量为基准,下同),催化剂损耗0.2%(以起始添加催化剂的质量为基准)。在该工艺条件下,对苯二胺产率达99.5%以上。废水套用后排放废水量很少,且对催化剂催化活性、产品质量等没有影响。The reactive behavior on hydrogenation of p-nitroaniline in water catalyzed by supported nickel catalyst was studied.The laboratory test and pilot-plant test were conducted.The effects of reaction temperature,pressure,holding time,p-nitroaniline mass concentration and wastewater recycle on the hydrogenation reaction were investigated.The results showed that the product p-phenylenediamine has high mass fraction,and catalyst and water can be recycled.The optimal reaction parameters are that temperature110℃,reaction time 1 h,pressure 2.0 MPa,stirring speed 800 r/min,dosage of initial catalyst 10%(based on the mass of p-nitroaniline,similarly hereinafter),catalyst loss 0.2%(based on the additive mass of initial catalyst).Under these optimal reaction conditions,the yield of p-phenylenediamine was over 99.5%.The amount of wastewater discharged after wastewater recycle was small and had no effect on catalytic activity and product quality.

关 键 词：对苯二胺 水 加氢还原 负载型镍催化剂 精细化工中间体 

分 类 号：TQ612[化学工程—精细化工] O625.631[理学—有机化学]