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作 者:赵志刚[1] 邵太丽[1] 秦国正[1] 陈靠山[1,2]
机构地区:[1]皖南医学院药学系,安徽芜湖241002 [2]山东大学生命科学学院,山东济南250100
出 处:《化工进展》2012年第7期1592-1596,共5页Chemical Industry and Engineering Progress
基 金:国家863计划项目(2007AA10Z334)
摘 要:以H-732阳离子交换树脂为催化剂进行了酯化反应研究,合成了丁二酸单乙酯和乙酰水杨酸,通过单因素实验和正交实验优化了反应工艺。单因素实验结果表明:催化剂用量为丁二酸酐质量的20%、乙醇与丁二酸酐的摩尔比1.8∶1、反应时间2 h、反应温度90℃时,丁二酸单乙酯产率最高为68.76%;在丁二酸单乙酯的合成体系中加入分离出的副产物丁二酸二乙酯可以抑制副反应的发生,大大提高单酯的产率(90.79%)。正交实验结果表明:乙酸酐与水杨酸的摩尔比为3∶1,催化剂用量为水杨酸质量的14.50%,反应时间2 h、反应温度60℃时,乙酰水杨酸产率最高为77.57%;催化剂连续使用5次时,催化能力才有明显下降,对连续使用过5次的催化剂重新活化后催化能力无明显降低。Catalytic ability of cation exchange resin H-732 for esterification reaction was investigated,and monoethyl ester of succinic acid and acetylsalicylic acid were synthesized by esterification reaction,and the optimum experimental conditions were optimized by single factor experiment and orthogonal experiment.The results of single factor experiment showed that under the following condition:the quantity of the resin :20% of succinic anhydride,n(ethanol)∶n(succinic anhydride)= 1.8∶1,reaction time 2 h,reaction temperature 90 ℃,the yield was 68.67%;.The yield of monoethyl ester of succinic acid was greatly improved by adding diethyl ester of succinate acid(side product),and the yield was 90.79%.The results of orthogonal experiment show that under the following condition:n(acetic anhydride)∶n(salicylic acid)= 3∶1,the quantity of the resin is 14.50% of salicylic acid,reaction time 2 h,reaction temperature 60℃,the yield was 77.57%.The catalyst lost its activity after reuse 5 times and its activity could be restored by re-activation.
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