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相转移催化合成二环已基二硫醚
引用本文:陈献,乔旭,崔咪芬,张进平,汤吉海.相转移催化合成二环已基二硫醚[J].精细化工,2005,22(11):874-877.
作者姓名:陈献  乔旭  崔咪芬  张进平  汤吉海
作者单位:南京工业大学,化学化工学院,江苏,南京,210009;南京工业大学,化学化工学院,江苏,南京,210009;南京工业大学,化学化工学院,江苏,南京,210009;南京工业大学,化学化工学院,江苏,南京,210009;南京工业大学,化学化工学院,江苏,南京,210009
摘    要:采用相转移催化剂,氯代环已烷与二硫化钠溶液反应合成了二环已基二硫醚。考察了相转移催化剂的种类、原料摩尔比、反应温度等对反应的影响,比较了相转移催化与溶剂法合成的反应结果。得到的最佳反应条件为:以PTC3为相转移催化剂,反应温度96℃,n(Na2S)∶n(S)∶n(C6H11C l)=1∶0.8∶0.8,氯代环己烷的转化率为98.8%,二环已基二硫醚的选择性为81.4%。与溶剂法相比,反应时间由12~15 h缩短到10 h,收率提高了10%,避免了因使用溶剂带来的后处理问题。

关 键 词:二环已基二硫醚  氯代环已烷  二硫化钠  相转移催化
文章编号:1003-5224(2005)11-0874-04
收稿时间:2005-02-04
修稿时间:2005-02-042005-06-23

Synthesis of Dicyclohexyl Disulfide with Phase Transfer Catalyst
CHEN Xian,QIAO Xu,CUI Mi-fen,ZHANG Jin-ping,TANG Ji-hai.Synthesis of Dicyclohexyl Disulfide with Phase Transfer Catalyst[J].Fine Chemicals,2005,22(11):874-877.
Authors:CHEN Xian  QIAO Xu  CUI Mi-fen  ZHANG Jin-ping  TANG Ji-hai
Affiliation:College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009, Jiangsu, China
Abstract:Dicyclohexyl disulfide was prepared by reaction of chlorocyclohexane and sodium disulfide using phase transfer catalyst(PTC).Effects of PTC species,material mole ratio and reaction temperature on the reaction was studied.The best conversion of chlorocyclohexane(98.8%) and selectivity for dicyclohexyl disulfide(81.4%) were obtained when PTC3 was used as catalyst with n(Na_2S)∶n(S)∶n(C_6H_(11)Cl)=1∶0.8∶0.8 reacting at 96 ℃.Compared with the solvent method,the reaction time was reduced from 12~15 h to 10 h,the yield was raised by about 10%,and the problem of aftertreatment associated with the use of solvent was avoided.
Keywords:dicyclohexyl disulfide  chlorocyclohexane  sodium disulfide  phase transfer catalysis
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