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Continuous synthesis process of ε-caprolactone from oxidization of cyclohexanone in micro-channel reactor

YAN Shenghu1,HAN Lingling1,SHEN Wei2,SHEN Jiefa1,LIU Jianwu1,ZHANG Yue1   

  1. 1 Design & Research Institute of Chemical Engineering,Changzhou University,Changzhou 213164,Jiangsu,China;2 Corning China (Shanghai) Regional Headquarters,Shanghai 200040,China
  • Online:2014-11-01 Published:2014-11-05

微通道中环己酮氧化合成ε-己内酯的连续流工艺

严生虎1,韩玲玲1,沈卫2,沈介发1,刘建武1,张跃1   

  1. 1常州大学化工设计研究院,江苏 常州 213164;2康宁中国(上海)管理有限公司,上海 200040

Abstract: Peracetic acid was prepared as an oxidant from acetic anhydride and H2O2 firstly,and then ε-caprolactone was synthesized by Baeyer-Villiger oxidization of cyclohexanone in a continuous flow micro-channel reactor. The effects of reactants molar ratio,reaction temperature and residence time on reactant conversion and product yield were investigated for both preparation of peracetic acid and synthesis of ε-caprolactone,and the process conditions were optimized. Under conditions of n(acetic anhydride) ∶n(H2O2) = 1.2∶1,reaction temperature at 70℃,residence time of 115s,conversion of H2O2 reached 88.9% and yield of peracetic acid reached 86.7%. Under conditions of n(peracetic acid) ∶n(cyclohexanone) = 1.1∶1,reaction temperature at 90℃,residence time of 90s,conversion of cyclohexanone reached 96.2% and yield of ε-caprolactone reached 80.9%. Comparing with the traditional batch reaction process,the selectivities and yields of target products in this continuous micro-channel reaction process were increased with shortened reaction time and lessened raw material consumption,and process continuity ensured higher operation safety.

Key words: micro-channel reactor, cyclohexanone, ε-caprolactone, Baeyer-Villiger oxidation

摘要: 在微通道反应器中,由H2O2、乙酸酐反应连续合成过氧乙酸氧化剂,再与环己酮经Baeyer-Villiger氧化连续合成ε-己内酯。先后考察了过氧乙酸氧化剂合成中乙酸酐与H2O2摩尔比、反应温度、停留时间等因素的影响,环己酮氧化反应中原料摩尔配比、反应温度、停留时间等因素对ε-己内酯合成的影响,优化了工艺条件。结果表明,当n(乙酸酐)∶n(H2O2)=1.2∶1、反应温度为70℃、停留时间为115s时,H2O2转化率达88.9%,过氧乙酸收率达86.7%;当n(过氧乙酸)∶n(环己酮)=1.1∶1、反应温度为90℃、停留时间为90s时,环己酮转化率达96.2%,ε-己内酯的收率达80.9%。与传统间歇釜式反应工艺相比,微通道反应工艺提高了ε-己内酯的收率和选择性,缩短了反应时间,减少了原料消耗,实现了连续化操作,提高了生产安全性。

关键词: 微通道反应器, 环己酮, ε-己内酯, Baeyer-Villiger氧化