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二乙二醇单烯丙基醚的合成新工艺

曾嵘,刘冬,周宝强,高瑞昶   

  1. 天津大学化工学院,天津 300072
  • 出版日期:2014-12-05 发布日期:2014-12-05

New process in the synthesis of diethylene glycol monoallyl ether

ZENG Rong,LIU Dong,ZHOU Baoqiang,GAO Ruichang   

  1. School of Chemical Engineering and Technology,Tianjin University,Tianjin 300072,China
  • Online:2014-12-05 Published:2014-12-05

摘要: 以二乙二醇、氯丙烯、氢氧化钠为原料,四丁基氯化铵为相转移催化剂,不引入其他溶剂,经Williamson成醚法合成了二乙二醇单烯丙基醚[2-(2-烯丙氧基乙氧基)-乙醇]。用红外吸收光谱和1H核磁共振谱对二乙二醇单烯丙基醚进行了表征。研究了反应时间、反应温度、原料摩尔比、碱用量、催化剂用量对目标产物收率的影响,得到较优的操作条件为:反应时间3h、反应温度80℃、n(二乙二醇)∶n(氢氧化钠)∶n(氯丙烯)=6∶1.2∶1、催化剂用量为氯丙烯质量的5%。在此条件下,收率达86.7%,纯度为99.2%。

关键词: 二乙二醇, 烯丙基醚, 合成, 优化, 二乙二醇, 烯丙基醚, 合成, 优化

Abstract: Without the introduction of other solvents,the synthesis of diethylene glycol monoallyl ether[2-(2-allyloxy-ethoxy)-ethanol] was prepared with diethylene glycol,allyl chloride and sodium hydroxide as the raw material and tetrabutylammonium chloride as phase transfer catalyst by the method of Williamson. The product was characterized by IR and 1H NMR spectra. The effects of reaction time,reaction temperature,molar ratio,the amount of alkali and catalyst on the yield of target product were investigated. The optimal condition was determined as follows:n(diethylene glycol)∶n(sodium hydroxide)∶n(allyl chloride) =6∶1.2∶1,m(catalyst)∶m(allyl chloride)=0.05∶1,at 80℃ for 3h. The yield of the product could reach 86.7% and the purity was 99.2% under the optimal reaction condition.

Key words: diethylene glycol, allyl ether, synthesis, optimization, diethylene glycol, allyl ether, synthesis, optimization

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