缩水甘油的低温合成与表征  

Synthesis and Characterization of Glycidol

作　　者：于良民[1] 韩青龙[1] 李昌诚[1] 徐焕志[1] 

机构地区：[1]中国海洋大学海洋化学理论与工程技术教育部重点实验室,山东青岛266100

出　　处：《精细化工》2007年第5期517-520,共4页Fine Chemicals

基　　金：新世纪优秀人才支持计划(NCET-04-0644)~~

摘　　要：以一氯代丙二醇为原料,与碱性化合物在低温作用下合成了缩水甘油,并通过IR、1HNMR对其进行了结构表征。测得其折光率(nD20)为1.430 0,环氧值(Ev)为1.347 6 eq/100 g,沸点为160℃。探讨得出缩水甘油的最佳合成条件为:当一氯代丙二醇用量为2 mol时,以异丙醇为溶剂,用量为500 mL;碱性化合物为w(NaOH)=37%的水溶液;反应温度为0℃;反应时间90 min;吸水剂为无水硫酸镁,且宜在反应50 min后加入效果最佳。最佳合成条件下反应收率为82.5%。Glycidol was synthesized through the reaction of 3-chloro-1,2-propanediol with alkaline compound at low temperature. When the dosage of 3-chloro-1,2-propanediol was 2 mol, with 500 mL isopropanol as solvent,the reaction was kept running at 0 ℃ for 90 min on dropping w（NaOH） = 37% aqueous solution. Anhydrous magnesium sulfate was added as desiccant 50 min after the beginning of reaction in order to absorb the overfull water. The structure of glycidol was confirmed by IR and 20 1^HNMR. The refractive index（nD^20 ）,epoxide value（Ev） and boiling point of the product are very close to those of standard sample （ CAS No. 556 - 52 - 5 ）. The yield of the reaction is 82. 5 % under the optimal conditions.

关 键 词：缩水甘油 低温合成 表征 精细化工中间体 

分 类 号：TQ214[化学工程—有机化工]