中华医学超声杂志

应用化学 ›› 2010, Vol. 27 ›› Issue (12): 1392-1395.DOI: 10.3724/SP.J.1095.2010.00122

• 研究论文 • 上一篇    下一篇

环氧环戊烷的无溶剂合成工艺

朱丹丹,章亚东*,王振兴   

  1. (郑州大学化工与能源学院 郑州 450001)
  • 收稿日期:2010-03-03 修回日期:2010-05-18 出版日期:2010-12-10 发布日期:2010-12-10
  • 通讯作者: 章亚东，男，教授，博士生导师; E-mail:zhangyadong@zzu.edu.cn; 研究方向：精细化工
  • 基金资助:
    河南省高校科技创新人才计划(2010HASTIT037)资助项目

A Solvent-free Method for Preparation of 1,2-Epoxycyclopentane

ZHU Dan-Dan, ZHANG Ya-Dong*, WANG Zhen-Xing   

  1. (School of Chemical Engineering and Energy,Zhengzhou University,Zhengzhou 450001)
  • Received:2010-03-03 Revised:2010-05-18 Published:2010-12-10 Online:2010-12-10

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摘要：

以聚苯乙烯-二乙烯苯接枝磷钨酸季铵盐为三相相转移催化剂，以H2O2为氧化剂，KCl为助催化剂，研究了环戊烯(CPE)合成环氧环戊烷(CPEO)的无溶剂工艺。 讨论了催化剂和助催化剂用量、反应温度、反应时间、环戊烯与H2O2摩尔比对反应的影响。 确定了无溶剂环氧环戊烷合成反应的条件为(以0.056 mol H2O2计)：催化剂1.0 g、助催化剂0.025 g、反应温度40 ℃、反应时间5 h、n(CPE)∶n(H2O2)=2.1∶1.0。 CPEO的平均收率约为96%。 催化剂回收重复使用6次活性无明显降低。

关键词: 环戊烯, 环氧环戊烷, 双氧水, 无溶剂, 三相相转移催化

Abstract:

A solvent-free process was developed to synthesize 1,2-epoxycyclopentane(CPEO) from cyclopentene(CPE) using hydrogen peroxide as green oxidant, KCl as cocatalyst and polystyrene-divinylbenzene(PS-DVB) grafted quaternary ammonium phosphor tungsten heterpoly acid salts as tri-phase phase transfer catalysts. Effects of the amount of catalyst and cocatalyst, reaction temperature, reaction time and the molar ratio of CPE to hydrogen peroxide on the product yield were investigated. The suitable reaction conditions with solvent-free were obtained as follows(based on 0.056 mol H2O2):catalyst 1.0 g, cocatalyst 0.025 g, reaction temperature 40 ℃, reaction time 5 h, n(CPE)∶n(H2O2)=2.1∶1.0. Under these conditions, the average yield of CPEO was about 96%. The catalysts can be recovered and even reused for six times without significant decrease of catalytic activity.

Key words: cyclopentene, epoxycyclopentane, hydrogen peroxide, solvent-free, tri-phase phase transfer catalysis

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