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

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%.