H-732阳离子交换树脂催化酯化反应.pdf

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化工进展
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CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2012年第31卷第7期
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研究开发
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H732阳离子交换树脂催化酯化反应
赵志刚',邵大丽',秦国正,陈靠山2
(鲩南医学院药学系,安徽尭湖溯241002:2山东大学生命科学学院,山东济南250100)
摘要:以H-732阳离子交换树脂为催化进行了酯化反应研究,合成了丁ニ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。单因亲实验结果表明:催化剂荆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2h、反应温度90℃时,丁二酸单こ酯产率最高为68.76%;在丁二酸单乙酯的合成
体系中加入分高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2h、反应温度60℃
时,乙洗水杨酸产率最高为7757%6;催化剤连续使用5次时,催化能力オ有明显下降,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。
关键词:阳离子交换树脂;酯化;催化;产率
中图分类号:TQ203.2文献标志码:A文章编号:1000-613(2012)07-1592-05
Ability of cation exchange resin H-732 as catalyst for esterification
ZHAO Zhigang, SH4O Taili, OIN Guozheng CHEN Kashan 2
Department of Pharmacy, Sou her Anhui Medical College, Wuhu 241002, Anhui, China; School of Life Science
Shandong University, Jinan 250100, Shandong, China)
Abstract: 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 he quantity of the resin 20%of succinic anhydride n(ethanol) n(succinic anhydride
1. 8: 1, reaction time 2 h, reaction temperature 90C, 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 h, reaction emperature 60 C, the yield was 77. 57%. The catalyst lost its
activity after reuse 5 times and its activity could be restored by re-activation
Key words: cation exchange resin; esterification; catalysis; yield
酯类物质作为一类重要的精细化工产品,主要催化剂。作为一种传统的均相催化剂,浓硫酸具有
用来做溶剂、香料、添加剂、有机合成的原料和中价格低廉、催化效果较好的巨大优势,但也有一定
间体等?。酯化反应是获得酯类产品的主要途
径?,该类反应通常需要在催化剂的作用下才能较收稿日期:2012016:修政稿日期:20120?405
基金项目:国家863计划项目(2007AA10Z334)。
好发生,目前对酯化反应的研究也主要集中在催化
第一作者及联系人:赵志刚(1981ー),男,助教,硕士。E-mail
剂方面。酯化反应在工业生产中主要采用浓硫酸作 zhaozhigangl8!c163om