甘油法合成缩水甘油  

Synthesis of glycidol from glycerol

作　　者：刘学民 褚昭宁 刘志伟 

机构地区：[1]江南大学化学与材料工程学院,江苏无锡214122

出　　处：《化工进展》2009年第8期1445-1448,共4页Chemical Industry and Engineering Progress

基　　金："十一五"国家科技支撑项目(2007BAE52B01-2)

摘　　要：以ZnSO4为催化剂,甘油和尿素反应合成碳酸甘油酯,分别以IR和MS对产物进行了结构表征。碳酸甘油酯在磷酸钠催化下脱掉一分子CO2得到缩水甘油。重点对碳酸甘油酯脱CO2得到缩水甘油的反应时间、反应温度、反应压力、催化剂种类及用量等因素进行了考察。并通过响应面分析法得到了适宜的反应条件为:反应时间4h、反应温度215℃、反应压力2kPa、催化剂用量2.5%(质量分数)。缩水甘油经旋转蒸发提纯,通过IR、HNMR进行了鉴定,GC测定产率可达到83.8%。Glycerol carbonate was synthesized through the reaction of glycerol with urea using ZnSO4 as catalyst. The product glycerol carbonate was confirmed by IR and MS. The release of carbon dioxide from glycerol carbonate provides the target product glycidol under the catalysis of sodium phosphate. Several factors for the carbon dioxide release reaction were investigated, such as reaction time, temperature, pressure, type and dosage of catalysts etc. The appropriate reaction conditions were obtained from response surface methodology as： reaction time 4 h, reaction temperature 215℃, reaction pressure 2 kPa, amount of catalyst 2.5 %（mass ratio）. After rotary evaporation, glycidol was analyzed with IR, HNMR and GC, and the yield of which was 83.8% as measured by GC.

关 键 词：缩水甘油 甘油 碳酸甘油酯 响应面分析法 

分 类 号：TQ214[化学工程—有机化工]