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二乙二醇甲乙醚的合成及其合成条件优化
Synthesis of Diethylene Glycol Ethyl Methyl Ether and Optimization of Its Synthetic Conditions
【摘要】 以二乙二醇单乙醚(DEGME)和氯甲烷为基本原料,氢氧化钠为催化剂、苯为带水剂,通过Williamson反应合成了二乙二醇甲乙醇(DEGMEE);用正效实验法对DEGMEE的合成条件进行了优化,气相色谱法分析了产品中DEGMEE的含量、FT IR和1H NMR法表征了产物结构。实验结果表明适宜的反应条件为:反应温度为60.0°C、醚化时间为4.0 h、n(CHCl)/n(DEGME)=1.15、n(NaOH)∶(DEGME)=1.30;在此条件下二乙二醇甲乙醚的收率可达93%以上。
【Abstract】 Diethylene glycol ethylmethyl ether(DEGMEE) was synthesized through Williamson Reaction with diethylene glycol mono-ether(DEGME) and chloromethane(CH3Cl)as raw materials,hydrate of sodium as catalysis,and benzene as water carrier.According to the yield of DEGMEE,its synthetic condition was optimized by orthogonal experiment.The purity of DEGMEE was analyzed by gas chromatography,its structure was characterized by FT IR and()1H NMR.The result of experiment indicated the suitable conditions of synthesis were as following:reaction temperature was 60.0°C,reaction time was 4.0 h,n(CH3Cl)/n(DEGME)=1.15 and n(NaOH)∶n(DEGME)=1.30.Under these condition,the yield of DEGMEE was up to 93%.
- 【文献出处】 化学世界 ,Chemical World , 编辑部邮箱 ,2006年05期
- 【分类号】TQ223.24
- 【被引频次】2
- 【下载频次】270