化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2014年
12期
3364-3367
,共4页
曾嵘%刘冬%周宝强%高瑞昶
曾嶸%劉鼕%週寶彊%高瑞昶
증영%류동%주보강%고서창
二乙二醇%烯丙基醚%合成%优化
二乙二醇%烯丙基醚%閤成%優化
이을이순%희병기미%합성%우화
diethylene glycol%allyl ether%synthesis%optimization
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%。
以二乙二醇、氯丙烯、氫氧化鈉為原料,四丁基氯化銨為相轉移催化劑,不引入其他溶劑,經Williamson成醚法閤成瞭二乙二醇單烯丙基醚[2-(2-烯丙氧基乙氧基)-乙醇]。用紅外吸收光譜和1H覈磁共振譜對二乙二醇單烯丙基醚進行瞭錶徵。研究瞭反應時間、反應溫度、原料摩爾比、堿用量、催化劑用量對目標產物收率的影響,得到較優的操作條件為:反應時間3h、反應溫度80℃、n(二乙二醇)∶n(氫氧化鈉)∶n(氯丙烯)=6∶1.2∶1、催化劑用量為氯丙烯質量的5%。在此條件下,收率達86.7%,純度為99.2%。
이이을이순、록병희、경양화납위원료,사정기록화안위상전이최화제,불인입기타용제,경Williamson성미법합성료이을이순단희병기미[2-(2-희병양기을양기)-을순]。용홍외흡수광보화1H핵자공진보대이을이순단희병기미진행료표정。연구료반응시간、반응온도、원료마이비、감용량、최화제용량대목표산물수솔적영향,득도교우적조작조건위:반응시간3h、반응온도80℃、n(이을이순)∶n(경양화납)∶n(록병희)=6∶1.2∶1、최화제용량위록병희질량적5%。재차조건하,수솔체86.7%,순도위99.2%。
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.