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采用等体积浸渍法制备了一系列氧化铝负载碱金属氟化物固体碱催化剂,用于甘油(丙三醇)与碳酸二甲酯酯交换反应合成碳酸甘油酯,其中KF/γ-Al2O3催化剂能够更好地促进碳酸甘油酯的生成。进一步考察了KF/γ-Al2O3催化剂的制备条件、反应条件对甘油与碳酸二甲酯酯交换反应的影响。当KF负载在γ-Al2O3的负载量为15%(质量分数,下同),于400℃焙烧5 h后制得固体碱催化剂,在n(碳酸二甲酯)∶n(甘油)=3∶1,反应温度80℃,反应时间1.5 h的条件下,甘油的转化率达96.1%,碳酸甘油酯选择性和收率分别达98.1%和94.3%。
A series of alumina-supported alkali metal fluoride solid base catalysts were prepared by the same volume impregnation method for the synthesis of glycerol carbonate by transesterification of glycerol (glycerol) with dimethyl carbonate. Among them, KF / γ-Al2O3 catalyst can be more Good to promote the production of glycerol carbonate. The preparation conditions of KF / γ-Al2O3 catalyst and the influence of reaction conditions on transesterification of glycerol and dimethyl carbonate were further investigated. When the loading of KF on γ-Al2O3 was 15% (mass fraction), the solid base catalyst was prepared by calcination at 400 ℃ for 5 h. The reaction was carried out at n (dimethyl carbonate): n (glycerol) = 3: 1, the reaction temperature was 80 ℃, the reaction time was 1.5 h, the conversion of glycerol reached 96.1%, and the selectivity and yield of glycerol carbonate reached 98.1% and 94.3%, respectively.