Microwave And Ultrasonic Assisted Reactive-Crystallization Of Hydrogenated Abietic Acid Purification

Hydrogenated rosin is an important modified rosin and its main component is hydrogenated abietic acid. This article is about the purification of hydr-ogenated abietic acid by using organic amine salt method combined with ultrasonic wave and microwave by using hydrogenated rosin as raw material, the purification process conditions were optimized by single factors and orthogonal test, the isolated hydrogenated abietic acid products were analyzed and ident-ificated, the results showed that microwave purification method was better than the ultrasonic method by comparing the ultrasonic puritied method and microwave puritied method. The main research contents are as follows:In the purificated test of hydrogenated abietic acid combined with ultra-sonic wave, the preparation of ethanolamine salt of hydrogenated abietic acid by using hydrogenated rosin as raw material, then the hydrogenated abietic acid could be obtained by extraction,crystallization,recrystallization and acidifyca-tion. In the experiments of single factors, different organic amines, different am-inating solvent,reaction temperature,reaction time,ultrasound power,agitating speed,extracted ethanol concentration,extracted times,recrystallizated ethanol concentrateion and recrystallizated times were investigated,and the conditions of isolation were obtained as follow:ethanol amine as organic amine, ethyl acetate as reacted solvent,ultrasonic power of400W,reaction temperature of40℃, agitating speed of400r/min,reaction time of40min,extracted ethanol concentration of50%,extracted times of three times,recrystallizated ethanol concentration of50%,recrystallizated times of three times,acetic acid as reducted acid. In order to further optimize the purification process conditions, the effects of reaction temperature, reaction time, ultrasound power, and agitating speed on the purity of hydrogenated abietic acid were investigated by the orthogonal experiment, the experimental results show that the significant degree sequences of the factors affecting the purification of hydrogenated abietic acid were as follows:reaction temperature>reaction time>ultrasonic power>agitating velocity. The optimal purificated process conditions of hydrogenated abietic acid were obtained as follows:reaction temperature of40℃, reaction time of40min, ultrasonic power of400W, agitating speed of400r/min. Under above optimized reaction conditions,the purity and yield of hydrogenated abietic acid were94.50%and10.48%respectively, the isolated hydrogenated abietic acid products were analyzed and identified with the GC,GC-MS, FT-IR,UV, melting point meter and polarimeter,and the melting point and specific rotation of hydrogenated abietic acid were165～167℃and[α]D/20+27.33°respectively.In the experiments of single factors of purificated hydrogenated abietic acid combined with microwave, dropping ways of amine, stirring ways, reaction temperature, reaction time and material proportion on the purification of hydrogenated abietic acid were investigated. The experimental results show that the significant degree sequences of the factors affecting the purification of hydrogenated abietic acid were as follows:reaction temperature>material proportion>reaction time, the optimal purificated reaction conditions of hydrogenated abietic acid were obtained as follows:reaction temperature of50℃, reaction time of25min, material proportion of1.1:1, Under above optimized reaction conditions,the purity and yield of hydrogenated abietic acid were96.80%and15.21%respectively, and the melting point and specific rotation of hydrogenated abietic acid were166.4-171℃and [α]D/20+29.98°respectively.The microwave purification method was best than the ultrasonic purific ation method and traditional amine purification method, and he ultrasonic purif-ication method was better than traditional amine purification method by comparing this three puritied methods.