以低纯度2-氯丙烯合成1,1,1,3,3-五氯丁烷的间歇、连续工艺研究及优化  

Study and Optimization of Batch and Continuous Synthesis of 1,1,1,3,3-Pentachlorobutane From low Purity 2-chloropropene

作　　者：熊显云 Xiong Xianyun(Zhejiang Quhua Fluor-Chemistry Co.,Ltd.,Zhejiang,324000)

机构地区：[1]浙江衢化氟化学有限公司,浙江324000

出　　处：《当代化工研究》2024年第18期150-152,共3页Modern Chemical Research

摘　　要：以纯度75%的2-氯丙烯(2-CPe)和四氯化碳(CTC)为原料,铁粉为催化剂,磷酸三丁酯(TBP)为助剂,分别采用间歇工艺和连续工艺合成了目标产物R360jfa。研究结果表明,R360jfa最优间歇合成工艺条件为:反应温度80℃,反应时间90 min,助剂浓度1.0%,CTC与2-CPe投料摩尔比3:1;最优连续合成工艺条件为:催化剂质量分数1.2%,CTC与2-CPe投料摩尔比为4:1,助剂质量分数1.0%。在上述最佳工艺参数下,75%纯度的2-CPe合成R360jfa的最高收率可达92%。本研究为采用低纯度2-CPe为原料制备R360jfa的工业化生产提供了思路,为此类反应实施节能降耗提供了基础数据。1,1,1,3,3-pentafluorobutane(R360jfa)is an important intermediate for the synthesis of 1,1,1,3,3-pentafluorobutane(R365mfc).The target product R360jfa was synthesized by batch and continuous processes using 75% purity 2-chloropropene(2-CPe)and carbon tetrachloride(CTC)as raw materials,iron powder as catalyst,and tributyl phosphate(TBP)as additive in this paper.The results showed that the optimal batch synthesis conditions of R360jfa were as followings:reaction temperature of 80℃,reaction time of 90 min,additive concentration of 1.0%,CTC and 2-CPe feeding molar ratio of 3:1;the optimal continuous synthesis conditions were:catalyst concentration 1.2%,CTC and 2-CPe feeding molar ratio 4:1,additive concentration 1.0%.Under the above optimal parameters,the maximum yield of R360jfa synthesized from 75% purity 2-CPe could reach 92%.The study in this paper provides a new idea for the industrial production of R360jfa by using low purity 2-CPe as raw materials,and provides basic data for the implementation of energy saving and consumption reduction in this kind of reaction.

关 键 词：1 1 1 3 3-五氯丁烷 HCC-360jfa 2-氯丙烯 四氯化碳 氟化工 

分 类 号：TQ21[化学工程—有机化工]