低温化学甘油解法制备1,3-甘油二酯工艺优化

Optimization of low-temperature chemical glycerolysis process for preparation of 1,3-diacylglycerol

为制备富含1,3-甘油二酯(1,3-DAG)的甘油二酯油,以大豆油和甘油为原料,采用低温化学甘油解法制备1,3-DAG。利用单因素实验考察溶剂种类、溶剂用量、催化剂种类、催化剂用量、反应时间、反应温度对产品组成的影响,以优化工艺条件,并在最优条件下进行放大实验。结果表明:低温化学甘油解法制备1,3-DAG的最优条件为以丙酮为溶剂、溶剂与反应物质量比2∶1、以甲醇钠为催化剂、催化剂用量0.6%(以反应物质量计)、反应温度50℃、反应时间3 h;在最优条件下经验证实验,产物中甘油三酯(TAG)含量为44.03%,DAG含量达43.97%,其中1,2-DAG含量为13.53%,1,3-DAG含量为30.44%;将反应物用量放大10倍,产物中TAG含量为46.35%,1,3-DAG含量为29.13%。综上,以大豆油为原料,采用低温化学甘油解法得到了富含1,3-DAG的甘油二酯油,且该方法具有可以应用于大规模生产1,3-DAG的潜力。

In order to prepare oil rich in 1,3-diacylglycerols(1,3-DAG),using soybean oil and glycerol as raw materials,1,3-DAG was prepared by low-temperature chemical glycerolysis.The effects of solvent type,solvent dosage,catalyst type,catalyst dosage,reaction time and reaction temperature on product composition were investigated by single factor experiment to optimize the process conditions.The scale-up experiment was conducted under the optimal conditions.The results showed that the optimal conditions of preparing 1,3-DAG by low-temperature chemical glycerolysis were obtained as fllows:with acetone as solvent,mass ratio of solvent to reactant 2:1,with sodium methoxide as catalyst,catalyst dosage 0.6%(based on reactant mass),reaction temperature 50℃,and reaction time 3 h.Under these conditions,the content of TAG in the product was 44.03%,and the content of DAG was 43.97%,with the content of 1,2-DAG 13.53%,and the content of 1,3-DAG 30.44%.Increasing the dosage of reactants by 10 times,the TAG content was 46.35%and the 1,3-DAG content was 29.13%.In conclusion,with soybean oil as raw material,diglyceride oil rich in 1,3-DAG can be obtained by low-temperature chemical glycerolysis,and this method has the potential to be applied to large-scale production of 1,3-DAG.