CaO催化制备碳酸甘油酯  

Synthesis of Glycerol Carbonate Catalyzed by CaO

作　　者：杜美美[1] 李秋小[1] 董万田 耿涛[1] 姜亚洁[1] 

机构地区：[1]中国日用化学工业研究院,山西太原030001 [2]上海发凯化工有限公司,上海201505

出　　处：《精细化工》2012年第2期200-204,共5页Fine Chemicals

基　　金：山西省自然科学基金(青年科技研究)项目(2010021013-1);太原市发明专利转化项目(1008)~~

摘　　要：以甘油和碳酸二甲酯为原料,CaO为催化剂合成了碳酸甘油酯。通过正交实验及单因素实验,考察了反应温度、回流温度、碳酸二甲酯用量、催化剂用量、反应时间对反应的影响,确定了优化工艺条件:反应温度75℃,回流温度60℃,碳酸二甲酯与甘油摩尔比2.5∶1,催化剂质量分数0.8%(以原料总质量计,下同),反应时间2h,在该条件下,甘油转化率及碳酸甘油酯收率分别可达97.89%和96.78%。CaO的存储稳定性及重复利用性实验结果表明,CaO虽具有较佳的存储稳定性,但其重复利用性较差,使用1次后活性即显著降低。Glycerol carbonate was synthesized from glycerol and dimethyl carbonate with CaO as catalyst. The effects of reaction temperature, reflux temperature, reactant molar ratio, catalyst dosage, and time on the reaction were studied by orthogonal experiment and single-factor test. The optimal reaction conditions were ascertained as follows：reaction temperature 75℃, reflux temperature 60℃, n （ dimethyl carbonate）：n（glycerol） =2.5：1 ,catalyst dosage 0. 8% （ based on the total raw materials）, reaction time 2 h ;the conversion of glycerol and the yield of glycerol carbonate reached 97.89% and 96.78%, respectively. An experiment was also conducted to evaluate the storage stability and reusability of CaO, which indicates that, although CaO was of relatively good storage stability, its reusability was so poor that it lost its activity after the first cycle of use.

关 键 词：碳酸甘油酯 碳酸二甲酯 CAO 酯交换 精细化工中间体 

分 类 号：TQ225.52[化学工程—有机化工]