【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%。更多还原

【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%.更多还原