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.