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作 者:韦小杰[1] 陈远萍[1] 陈小鹏[1] 陈建云[1] 郑文峰[1] 刘蓓珊[1]
机构地区:[1]广西大学化学化工学院,广西石化资源加工及过程强化技术重点实验室,广西南宁530004
出 处:《化学研究与应用》2013年第8期1189-1194,共6页Chemical Research and Application
基 金:国家自然科学基金项目(20976031)资助;广西自然科学基金重点项目(2011GXNSFD018011)资助;广西石化资源加工及过程强化技术重点实验室主任课题基金项目(11-B-04)资助
摘 要:以氢化松香为原料、乙醇胺为有机胺、乙酸乙酯为溶剂,在超声波辅助下进行胺化反应制备氢化枞酸乙醇胺盐,再经萃取、重结晶和酸化得到氢化枞酸,采用正交试验考察了超声功率、搅拌转速、反应温度、反应时间对氢化枞酸纯度的影响,结果表明,影响氢化枞酸纯度因素按显著程度依次为反应温度>反应时间>超声波功率>搅拌转速,确定了最佳的胺化反应条件为:反应温度40℃、反应时间40min、超声波功率400W、搅拌转速400r/min,所得氢化枞酸的纯度为94.5%。采用GC、GC-MS、FT-IR、熔点仪和旋光仪对氢化枞酸产品进行了分析鉴定。The preparation of ethanolamine salt of hydrogenated abietic acid by aminting reaction coupled with ultrasound wave was studied by using hydrogenated rosin as raw material,ethanol amine as organic amine and ethyl acetate as reaction solvent.Then the hydrogenated abietic acid could be obtained by extraction,crystallization,recrystallization and acidification.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 showed that the significant degree sequences of the factors affecting the purity of hydrogenated abietic acid were as follows:reaction temperature>reaction time>ultrasonic power>agitating velocity.The optimized aminating conditions were obtained as follows:reaction temperature of 40 ℃,reaction time of 40 min,ultrasonic power of 400W,agitating speed of 400 r·min-1.Under above optimized reaction conditions,the purity of hydrogenated abietic acid were 94.5%.The isolated hydrogenated abietic acid products were analyzed and identified with the GC,GC-MS,FT-IR,melting point meter and polarimeter.
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