正交实验优选2,4-二硝基氯苯合成的最佳工艺条件

Optimization of Synthesis of 2, 4-Dinitrochlorobenzene Conditions by Orthogonal Experiment

根据正交实验L9(34)表格设计,采用传统的硝化法-间歇式硝化法中的两步法合成2,4-二硝基氯苯,分别考察不同水浴保温温度、硝酸加入量、硫酸加入量和保温时间等4个因素在3种不同水平条件下对2,4-二硝基氯苯产量的影响。实验表明:当氯苯为10mL时,各水平条件下,2,4-二硝基氯苯产量值最高分别出现在水浴温度为95℃、硝酸加入量为29.4mL、硫酸加入量为30.9mL、保温时间50min,此时2,4-二硝基氯苯产率能达到理论值的95.72%。并确定此方案为间歇式硝化法中的两步法合成2,4-二硝基氯苯的最优方案。

According to the L9 （3^4） orthogonal form, the experiment utilized the traditional nitration method （two-step method in semi-batch nitration） to synthesize the 2,4-dinitrochlorobenzene, and examined how four factors （different temperature of water-bath, nitric acid addition, sulfuric acid addition and holding time） affected the production of 2,4-dinitrochlorobenzene under three different conditions. The experiment indicates that the productivity of 2,4-dinitrochlorobenzene can achieve 95.72% of theoretical value （the highest in each level） under every level when the quantity of chlorobenzene is 10mL, water-bath 95 degree centigrade, nitric acid addition 29.4mL, sulfuric acid addition 30.9mL, holding time 50mins, and it proves that this program is the best two-step method to synthesize the 2, 4- dinitrochlorobenzene among semi-batch nitrations.