合成氢化松香乙酯的新工艺研究

STUDY ON A NEW TECHNOLOGY OF SYNTHESIZING HYDROGENATED ROSIN ETHYL ESTER

以DRC为催化剂,在无溶剂条件下,通过氢化松香与乙醇的直接酯化反应合成氢化松香乙酯。探索了反应温度、催化剂用量、反应时间、物料配比等因素对反应酯化率的影响,确定最佳反应条件为:反应温度180℃,催化剂用量为原料氢化松香质量的6%,反应时间6h,醇与酸的摩尔比为3∶1。在最佳条件下酯化率达92.2%。还探讨了用阴离子交换树脂柱层析分离纯化氢化松香乙酯粗产物的方法。此外,利用红外光谱对氢化松香乙酯精制产物进行了表征;用GC-MS分别对氢化松香乙酯粗产物及其精制产物进行了定性和定量分析,比较了柱层析前后化学组成的变化。

Hydrogenated rosin ethyl ester was prepared by the reaction of hydrogenated rosin with ethanol in the absence of solvent and in the presence of DRC as a catalyst.Various factors such as reaction temperature,catalyst dosage,reaction time,the molar ratio of ethanol to hydrogenated rosin which may influence the esterification rate were investigated.The optimum conditions were found to be as follows:reaction temperature 180 ℃,catalyst dosage 6%(based on the weight of hydrogenated rosin ),reaction time 6 h,the molar ratio of ethanol to hydrogenated rosin 3∶1.The esterification rate amounted to 92.2% under the optimum conditions.Additionally,the ion exchange chromatography was used to purify the crude hydrogenated rosin ethyl ester by the removal of the unreacted resin acid.Besides,the refined hydrogenated rosin ethyl ester was characterized by IR,and the crude and refined hydrogenated rosin ethyl esters were analyzed with GC-MS,respectively,for comparing changes of chemical components before and after the column chromatography separation.