5,5,5-三氯-2-甲基-2-戊烯的制备  

Preparation of 5,5,5-Trichloro-2-methyl-2-petene

作　　者：张今令[1] 王华[1] 刘中民[1] 

机构地区：[1]中国科学院大连化学物理研究所天然气化工与应用催化研究室,辽宁大连116023

出　　处：《精细化工》2002年第10期590-595,共6页Fine Chemicals

摘　　要：在耐高温强酸性阳离子交换树脂催化剂作用下 ,由 5 ,5 ,5 三氯 2 甲基 2 戊醇 (TCPOL)脱水生成 5 ,5 ,5 三氯 2 甲基 2 戊烯 (TCPE 2 ) ,同时伴有异构体 5 ,5 ,5 三氯 2 甲基 1 戊烯(TCPE 1 )的生成。当V(催化剂 )∶V(TCPOL)∶V(溶剂 ) =1∶2∶1 0 ,反应温度 1 0 0℃ ,反应时间 6h时 ,TCPOL转化率为 1 0 0 % ,n(TCPE 2 )∶n(TCPE 1 ) =91∶9。脱水后的物料在强酸性阳离子交换树脂催化剂作用下进行异构化反应 ,反应温度从 1 0 0℃到 0℃不断降低 ,可使TCPE 1不断向TCPE 2转化 ,在V(催化剂 )∶V(物料 )∶V(溶剂 ) =1∶1∶5 ,经 60h左右 ,n(TCPE 2 )∶n(TCPE 1 ) =97∶3。Trichloro 2 methyl 2 pentene (TCPE 2),the main intermediate for synthesis of permethrinic acid,was prepared by the dehydration reaction of 5,5,5 trichloro 2 methyl 2 pentanol (TCPOL) in the presence of DNW-I high temperature resin catalyst.TCPOL conversion of up to 100% and TCPE 2 selectivity of 91% were obtained under the conditions of V (catalyst)∶ V (TCPOL)∶ V (solvent)=1∶2∶10,reaction temperature100 ℃ and reaction time 6 h.The dehydrating product was treated with strongly acidic cation exchange resin catalyst under the conditions of V(catalyst)∶ V (TCPE)∶ V (solvent)=1∶1∶5 and the reaction temperature continually reduced from 100 ℃ to 0 ℃.5,5,5 Trichloro 2 methyl 1 pentene(TCPE 1),the isomer of TCPE 2,was converted to the desired product,and the mol ratio of TCPE 2 to TCPE 1 was 97∶3 after reacting for 60 h.

关 键 词：5 5 5-三氯-2-甲基-2-戊烯 制备 脱水 5 5 5-三氯-2-甲-2-戊醇 阳离子交换树脂 

分 类 号：TQ221.214[化学工程—有机化工]