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铁粉催化合成1,1,1,3,3-五氯丙烷

许晓涛,龙 辉,张未星   

  1. 浙江大学化学工程与生物工程学系,浙江 杭州 310027
  • 出版日期:2013-11-05 发布日期:2013-11-05

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

XU Xiaotao,LONG Hui,ZHANG Weixing   

  1. Department of Chemical and Biological Engineering,Zhejiang University,Hangzhou 310027,Zhejiang,China
  • Online:2013-11-05 Published:2013-11-05

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%。

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

Abstract: 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%.

Key words: 1,1,1,3,3-pentachloropropane, synthesis, optimization, catalyst, ferrous chloride, ferric chloride

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