微波强化胺盐法单离枞酸  

Isolation of abietic acid by amine salt combined with microwave

作　　者：韦珍苑 黎跃[1] 韦小杰[1] 江文夺 吴嘉超 陈小鹏[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004 [2]广西梧州日成林产化工股份有限公司,广西梧州543100

出　　处：《广西大学学报（自然科学版）》2014年第3期532-537,共6页Journal of Guangxi University（Natural Science Edition）

基　　金：国家自然科学基金资助项目(20976031;31060102);广西自然科学基金重点项目(2011GXNSFD018011);广西自然科学基金资助项目(2010GXNSFA013042;2013GXNSFAA019050;2013GXNSFBA019037);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(11-B-04;2012Z02)

摘　　要：为提高枞酸的纯度和收率,以松香为原料,乙醇为溶剂,利用微波强化松香异构和胺化反应-结晶耦合的方法单离枞酸,通过单因素和正交试验考察酸种类、微波功率、温度、时间和原料配比对枞酸提纯的影响。结果表明,微波强化松香异构反应的最优条件是:异构反应催化剂为盐酸、微波功率为500 W、反应温度为40℃、反应时间为30 min;胺化反应的温度为35℃、反应时间为25 min、原料配比(n松香∶n乙醇胺)为1∶1,此条件下单离得到枞酸的纯度和收率分别为98.60%及57.47%。微波强化胺盐法降低了反应温度,实现反应与结晶分离的耦合,提高了枞酸纯度和收率。In order to obtain abietic acid with high purity and high yield,abietic acid isolation was studied using rosin isomerization coupling amination reaction and crystallization with rosin as raw material and ethanol as solvent under mircrowave irradiation. The effects of acids,power of microwave,reaction temperature and time,and material proportion on the purification of abietic acid were investigated by single factor and orthogonal experiments. The result showed that the optimal reaction conditions of rosin isomerization under mircrowave irradiation were as follows： hydrochloric acid as catalyst,microwave power 500 W,reaction temperature 40 ℃,and reaction time 30min. The optimal reaction conditions of amination were obtained as follows： reaction temperature 35 ℃,reaction time25min and material proportion 1∶ 1. Under above reaction conditions,the purity of abietic acid obtained could reach 98. 60% with a yield of 57. 47%. The isolation of abietic acid by microwave-assisted amine salt method is benefited by reducing the reaction temperature,achieving the coupling of reaction and crystallization separation,and increasing the purity and yield of abietic acid.

关 键 词：枞酸 微波 单离 胺盐法 

分 类 号：TQ351.471[化学工程]