首页|CaO/LiCl混合固体催化制备碳酸甘油酯及产物结构分析

CaO/LiCl混合固体催化制备碳酸甘油酯及产物结构分析

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以新活化的CaO/LiCl为混合催化剂,以碳酸二甲酯和甘油为反应物,制备了碳酸甘油酯.考察反应回流时间和反应物摩尔比对产物纯度和收率的影响,通过气相色谱技术确定了反应最佳时间和最佳摩尔比,采用红外光谱、质谱、核磁共振谱技术表征了产物结构.结果表明,当碳酸二甲酯和甘油的摩尔比为 4∶1、催化剂质量分数 3.0%、反应时间 4h时,产物纯度最高(97.7%)、收率最好(95.7%);反应时间更短时或摩尔比更低时,甘油转化不完全;通过ChemDraw软件中核磁共振模拟功能对产物结构进行了研究;结合量子化学提出了五元环碳酸甘油酯生成的合理机理.
Preparation of Glycerol Carbonate with CaO/LiCl Mixed Solid Catalyst and Product Structure Analysis
Glycerol carbonate was prepared by using fresh activated CaO/LiCl as mixed catalyst and dimethyl carbonate and glycerol as reactants.The effects of reflux time and molar ratio of reactants on product purity and yield were investigated.The optimal reaction time and molar ratio were determined by gas chromatography,and the product structures were characterized by infrared spectroscopy,mass spectrometry and nuclear magnetic resonance(NMR)technology.The results showed that the highest product purity(98.7%)and the best yield(95.7%)were achieved when the molar ratio of dimethyl carbonate and glycerol was 4∶1,the catalyst dosage was 3.0%,and the reaction time was 4 h.When the reaction time was shorter,the glycerol conversion in the system was incomplete.When the molar ratio was lower,the glycerol conversion was incomplete.The structure of the product was studied by the NMR simulation function in ChemDraw software.A reasonable mechanism for the generation of five-membered cyclic carbonate glycerides was proposed by quantum chemical computational studies.

glycerol carbonateCaO/LiClmixed solid catalystreaction mechanismpolyurethane

佟拉嘎、高嵩、陈秋霞、陈洋洋、郭志武、李红英

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北京石油化工学院新材料与化工学院 北京 102617

碳酸甘油酯 CaO/LiCl 混合催化剂 反应机理 聚氨酯

2024

聚氨酯工业
中国聚氨酯工业协会 江苏省化工研究所有限公司

聚氨酯工业

CSTPCD
影响因子:0.507
ISSN:1005-1902
年,卷(期):2024.39(6)