对硝基苯胺中试制备工艺

Pilot test process for p-nitroaniline preparation

进行了以对硝基氯苯为原料制备对硝基苯胺的中试,考察了物料配比、氨水浓度、反应温度、反应时间以及设备材质对氨解反应的影响。氨解反应的最佳条件:对硝基氯苯与氨的摩尔比为1∶10,氨水质量分数为35%,反应温度180℃,反应时间10 h,设备采用钛材制作。在此条件下对硝基氯苯的转化率达100%,得到的对硝基苯胺质量分数达99.5%以上,产品收率达98%以上。

A pilot test was carried out to prepare p-nitroaniline from p-nitrochlorobenzene. The effects of material ratio, ammonia water concentration, reaction temperature, reaction time, and equipment material, on ammonolysis reaction were investigated. The best ammonolysis reaction conditions were as follows： the molecular ratio of p-nitrochlorobenzene to ammonia was 1： 10, the mass fraction of ammonia water was 35%, the reaction temperature was 180 ℃, the reaction lasted for 10 h, and the equipment was made of titanium. Under the above conditions, the conversion of p-nitrochlorobenzene reached 100% , the mass fraction of obtained p-nitroaniline was over 99.5% ,and the yield of product was greater than 98%.