化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2013年
11期
2723-2726
,共4页
1,1,1,3,3-五氯丙烷%合成%优化%催化剂%氯化亚铁%氯化铁
1,1,1,3,3-五氯丙烷%閤成%優化%催化劑%氯化亞鐵%氯化鐵
1,1,1,3,3-오록병완%합성%우화%최화제%록화아철%록화철
1,1,1,3,3-pentachloropropane%synthesis%optimization%catalyst%ferrous chloride%ferric chloride
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％。
以氯乙烯與四氯化碳為原料，在鐵粉催化劑與燐痠三丁酯助催化劑作用下，通過自由基加成反應閤成1,1,1,3,3-五氯丙烷。攷察瞭催化劑、助催化劑、氯化鐵、反應溫度、反應時間、原料摩爾比對反應的影響，以及氯化亞鐵的生成來源。研究穫得反應的最佳工藝條件為：原料摩爾比 n(四氯化碳)∶n(氯乙烯)=1∶(0.1～0.4)，反應溫度110～115℃，反應時間4～5 h，採用鐵粉作催化劑，用量為總物料質量的0.6%～0.9%，助催化劑燐痠三丁酯與鐵粉的摩爾量比為1∶1。1,1,1,3,3-五氯丙烷的收率為85.2%，產品純度為99.8％。
이록을희여사록화탄위원료，재철분최화제여린산삼정지조최화제작용하，통과자유기가성반응합성1,1,1,3,3-오록병완。고찰료최화제、조최화제、록화철、반응온도、반응시간、원료마이비대반응적영향，이급록화아철적생성래원。연구획득반응적최가공예조건위：원료마이비 n(사록화탄)∶n(록을희)=1∶(0.1～0.4)，반응온도110～115℃，반응시간4～5 h，채용철분작최화제，용량위총물료질량적0.6%～0.9%，조최화제린산삼정지여철분적마이량비위1∶1。1,1,1,3,3-오록병완적수솔위85.2%，산품순도위99.8％。
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%.
