三氯乙酰氯合成研究

Study on the Synthesis of Trichloroacetyl Chloride

研究了以氯乙酸为起始原料经三次氯化合成三氯乙酰氯的新方法。氯气与熔融状态的氯乙酸接触反应制备一氯化料,一氯化料与一氯化硫、氯气加热反应制备二氯化料,在催化剂条件下二氯化料与氯气进行加热反应,精馏后制得三氯乙酰氯。该工艺的最佳条件为:一次氯化温度和时间分别为:105～135℃,15～20 h;二次氯化温度和时间分别为:90～115℃,20～25 h;三次氯化温度100～125℃。最终产品的总收率达到94.5%以上,含量达到99.0%。

The new synthetic method of trichloroacetyl chloride through three chlorination by chloroacetic acid was studyed. Primary chlorine material was preparated by chlorination and liquid chloroacetic acid, then heating with chlorination and sulfur monochloride to preparate second chlorine material, the second chlorine material heate again with chlorination in the presence of Catalyzer, trichloroacetyl chloride was got after rectification at the most. The best process condition was reported that the temperature and time of primary chlorine were 105 -135℃ and 15 -20 h, the temperature and time of second chlorine were 90 -115℃ and 20 -25 h, the temperature of third chlorine was 100 - 125℃. It was concluded that the total yield and purity of the product trichloroacetyl chloride were promoted by more than 94.5% and 99.0%.