第 37 卷第 6 期Vol. 37 No. 6
2007 年 12 月Dec 2007

所属栏目:医药及中间体

2-乙氧基丙烯绿色合成技术的研究
李小保1,钱兵荣2,叶菊娣1 (1.南京林业大学 化学工程学院,江苏 南京210037;2.南通鸿志化工有限公司,江苏 如皋 226512)
摘 要:以酸性阳离子交换树脂为催化剂在无溶剂的条件下,采用丙酮和原甲酸三乙酯缩合来制备丙酮缩二乙醇,通过正交实验和单因素实验得到适宜的反应条件为:反应温度15℃、保温时间10 h、催化剂用量1 ∶ 80(m/m)、原料配比n(丙酮) ∶ n(原甲酸三乙酸)=1.0 ∶ 1、催化剂用量m(催化剂) ∶ m(原甲酸三乙酸)=1 ∶ 100。再以氯化铵为催化剂采用反应精馏技术由丙酮缩二乙醇制备了2-乙氧基丙烯,考察了回流比对2-乙氧基丙烯收率的影响,得到适宜的回流比为8。在适宜的操作条件下,2-乙氧基丙烯单程总收率达77.2%。该技术具有所需设备投资和能耗较低、流程简单且对环境友好的优点,是一种可行的绿色合成技术。
关键词:2-乙氧基丙烯;离子交换树脂;反应精馏;绿色合成技术
中图分类号:TQ463.24  文献标识码:A  文章编号:1009-9212(2007)06- 0028-03
The Green Synthesis Technology of 2-Ethoxypropene
LI Xiao-bao1,QIAN Bin-rong2,YE Ju-di1 (1. College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,China;2. Nantong Hongzhi Chemical Company Ltd.,Rugao 226512,China)
Abstract:2,2-Diethoxypropane was synthesized from acetone and triethyl orthoformate via condensation with acidic cation-exchange resin. The affection to the yield of some factors such as reaction temperature,persistent time,catalyst quantity and reactant ratio were discussed. and the optimal  technologic conditions are determined. 2-Ethoxypropene was prepared from 2,2-diethoxypropane with reactive distillation technology. The overall yield of 2-ethoxypropene was up to 77.2%. The technology is a feasible green synthesis,friendly to the enviroment,simple operation,low equipment investment and energy consumption.
Key words:2-ethoxypropene;cation-exchange resin;reactive distillation;green synthesis technology
作者简介:李小保(1970-),男,安徽无为人,博士研究生,主要从事精细化工中间体反应技术和分离技术的研究。(E-mail:lixiaobao@njfu.com.cn)
收稿日期:2007-11-22