铁粉催化合成1,1,1,3,3-五氯丙烷  

Synthesis of 1,1,1,3,3-pentachloropropane catalyzed by iron powder

作　　者：许晓涛[1] 龙辉[1] 张未星[1] 

机构地区：[1]浙江大学化学工程与生物工程学系,浙江杭州310027

出　　处：《化工进展》2013年第11期2723-2726,共4页Chemical Industry and Engineering Progress

摘　　要：以氯乙烯与四氯化碳为原料，在铁粉催化剂与磷酸三丁酯助催化剂作用下，通过自由基加成反应合成1,1,1,3,3-五氯丙烷。考察了催化剂、助催化剂、氯化铁、反应温度、反应时间、原料摩尔比对反应的影响，以及氯化亚铁的生成来源。研究获得反应的最佳工艺条件为：原料摩尔比n（四氯化碳）∶n（氯乙烯）=1∶（0.1～0.4），反应温度110～115 ℃，反应时间4～5 h，采用铁粉作催化剂，用量为总物料质量的0.6%～0.9%，助催化剂磷酸三丁酯与铁粉的摩尔量比为1∶1,1,1,1,3,3-五氯丙烷的收率为85.2%，产品纯度为99.8％。1,1,1,3,3-pentachloropropane was prepared by radical addition between carbon tetrachloride and vinyl chloride in the presence of iron powder and tributyl phosphate. The effects of such factors as catalyst,co-catalyst,ferric chloride,reaction temperature,material mole ratio and reaction time on the reaction were investigated. The origin of ferrous chloride was also explored. The proper reaction condition of synthetic process of 1,1,1,3,3-pentachloropropane was as follows：material mole ratio n（CCl4）∶n（VnCl）=1∶（0.1—0.4）,reaction temperature 110—115 ℃,reaction time 4—5 h,catalyst iron powder 0.6%—0.9% of the total quantity of raw materials. Tributyl phosphate was selected as co-catalyst,and its molar weight was equal to that of iron powder. The yield of 1,1,1,3,3- pentachloropropane was 85.2% and the purity of product was 99.8%.

关 键 词：1 1 1 3 3-五氯丙烷 合成 优化 催化剂 氯化亚铁 氯化铁 

分 类 号：TQ213[化学工程—有机化工] TQ222.2