合成四氯苯酐最佳工艺条件的选择

Optimum conditions for the synthesis of tetrachlorophthalic anhydride synthesis

通过正交试验及对正交试验结果进行统计分析 ,检验了因子的显著性 ,确定了由苯酐氯化合成四氯苯酐的最佳工艺条件为 :反应时间 12h ,反应温度 80～ 16 0℃ ,原料配比为n(苯酐 )∶n(工业级溶剂 )∶n(催化剂 )∶n(氯气 ) =1∶10∶B1∶C2 ,在此条件下摩尔产率为 98%。溶剂和催化剂可回收循环使用 ,溶剂回收率 >85 %,催化剂回收率 >5 0 %。此种方法合成四氯苯酐具有产品产率高、质量好、成本低且不产生大量废硫酸的优点。用工业级溶剂代替化学纯试剂 ,并将反应器放大 5倍 。

According to statistically analysis of orthogonal experiment results and test of significance level of each factor,optimum conditions for the synthesis of tetrachlorophthalic anhydride by chlorina- ting phthalic anhydride with chlorine gas were obtained,which were as follows:reaction time 12 h,temperature from 80 ℃ to 160 ℃,1∶10∶B 1∶C 2 material molar ratio of phthalic anhydride,industrial solvent,catalyst and chlorine gas.Under these conditions,the product molar yield was 98%,and catalyst and solvent could be recovered,with recovery rate of over 85% for solvent and over 50% for catalyst.This process had some advantages,such as high yield,high product quality,low cost and no large amounts of waste sulfuric acid.The same results were obtained when solvent was industrial grade instead of chemical grade and the reactor was magnified by 5 times.