超声波协同反应-结晶耦合单离脱氢枞酸.pdfVIP

第59卷 第4期 化 工 学 报 VoI．59 No．4 2008年 4月 Journal of Chemical Industry and Engineering (China) April 2008 超声波协同反应一结晶耦合单离脱氢枞酸 祝远姣，陈小鹏，陈月圆，钟 华，陈祖芬，童张法 (广西大学化学化工学院，广西 南宁530004) 摘要：以歧化松香和2一乙醇胺为原料、乙醇为溶剂、超声波协同反应一结晶制备脱氢枞酸乙醇胺盐，经萃取、结 晶、重结晶、酸化制得脱氢枞酸。通过正交优化实验，考察了溶剂浓度、反应温度、反应时间、超声波功率、 搅拌转速对脱氢枞酸收率的影响，确定最佳单离条件为：反应时间50 min，反应温度35℃，超声波功率500 W， 溶剂浓度 5O ，搅拌转速400 r·min一，在该操作条件下脱氢枞酸的收率达 55．37 ，纯度达 99．53 。并探讨 了脱氢枞酸胺化反应一结晶过程相态变化对反应平衡和选择性的影响，当反应温度分别为35℃和7O℃时，胺化反 应是在非均相和均相下进行，所得脱氢枞酸产品的纯度为 99．53 和95．66 。采用 GC、GC-MS、元素分析、 uV、FT-IR、熔点仪和旋光仪对脱氢枞酸产品进行了分析鉴定，实验值与文献值吻合。 关键词：歧化松香；脱氢枞酸；超声波；反应一结晶 中图分类号：O 629．6 1 文献标识码：A 文章编号：0438—1157(2008)04—0920—07 Isolation of dehydr0abietic acid by reaction—crystallizati0n coupled with ultrasound wave ZHU Yuanjiao。CHEN Xiaopeng，CHEN Yueyuan，ZHONG Hua，CHEN Zufen，TONG Zhangfa (School of Chemistry and Chemical Engineering，Guangxi University，Nanning 530004，Guangxi，China) Abstract：The preparation of 2-aminoethanol salt of dehydroabietic acid from disproportionated rosin by reaction—crystallization coupled with ultrasound wave was studied by using disproportionated rosin and 2：aminoethanol as raw materials，ethanol as reaction solvent，and pure dehydroabietic acid could be obtained by extraction，crystallization，recrystallization and acidification．The effects of concentration of ethano1．reaction temperature，reaction time，ultrasound intensity and agitating velocity on the yield of dehydroabietic acid were investigated by orthogonal experiment，and the optimal conditions for isolation wete obtained as follows：reaction time 50 min，reaction temperature 35℃ ，ultrasound power 500 W， concentration of ethanol 50 9，6，agitating velocity 400 r·min_。．Under