碳基固体酸催化合成乙酰水杨酸.pdf

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化
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进展
2012年第31卷第5期
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
1121p
研究开发
碳基固体酸催化合成乙酰水杨酸
占昌朝2,曹小华2,严平1,王剑波2,余祖进,江小平
1九江学院化学与环境工程学院,江西九江332005:2浙江工业大学化学工程与材料学院,浙江杭州310014)
摘要:以淀粉和对甲苯磺酸为原料合成了碳基固体酸催化剂,并采用FTIR、TG、BET、SEM和EDS对催化
剂进行了表征。研究了催化剂对乙酰水杨酸合成反应的催化活性,并比较了常规加热和微波加热方式对反应的
影响。通过单因素试验确定了较佳工艺条件为:乙酸酐与水杨酸物质的量比为1.5:1,催化剂用量为水杨酸质
量的5.8%,反应时间25min,反应温度76~80℃。常规加热条件下收率82.1%,使用5次后,收率仍保持在78.2
碳基固体酸催化剂在常规加热条件下催化性能和重复使用性能均优于徽波加热条件反应
关键词:碳基固体酸;酰化反应;乙酰水杨酸;徽波加热
中图分类号:0621.25
文献标志码:A
文章编号:1000-66133(2012)05-1121-05
Synthesis of acetylsalicylic acid catalyzed by carbon-based solid acid
ZHAN Changchao 2, CAO Xiaohua. 2, YAN Ping WANG anbo, ru Zijin JIANG Xiaoping
(College of Chemistry and Environmental Engineering, Jiujiang University, Jiujiang 332005, Jiangxi, China
College of Chemical Engineering and Materials, Zhejiang University of Technology
Hangzhou 310014, Zhejiang, China)
Abstract: Carbon-based solid acid catalysts synthesized from starch and p-toluene sulphonic acid were
characterized by FTIR, TG, BET, SEM and EDS. Its catalytic activity and effect of conventional heat
and microwave heat on yield of acetylsalicylic acid were studied. The better condition was determined
with single factor tests, which is as follows: the molar ratio of acetic anhydride to salicylic acid was
1.5: 1, the weight ratio of carbon-based solid acid to salicylic acid was 5.8%, acylation reaction
temperature was 76-80 C, reaction time was 25 min under conventional heat. The yield of
acetylsalicylic acid was 82. 1% and kept 78.2% after used five times under conventional heat. The
carbon-based solid acid catalyst has high catalytic activity and retrievability under conventional heat
which are better than that of microwave heat
Key words: carbon-based solid acid; acylation; acetylsalicylic acid; microwave heat
乙酰水杨酸又称阿司匹林( Aspirin),是一种的绿色催化剂越来越受到重视。这种催化剂可通
常用的解热镇痛和抗风湿类药物,经典制备方法过不完全炭化磺酸基芳烃而得到多聚芳烃的结构并
是采用水杨酸和乙酸酐或乙跣氯在硫酸催化下反连有磺酸基,可将稳定、可溶性好的对甲苯磺酸变
应?,该工艺成熟,产率60%左右,但副反应多,
设备腐蚀严重,严重污染环境。近年来,利用负载收稿日期:201-12-20:修改稿日期:2012-01-14.
型固体酸催化剂或通过微波辅助合成阿司匹林的绿
基金项目:国家自然基金(21161009)、江西省自然科学基金
色工艺路线受到了广泛重视?。但这些方法的改进
20114BAB213002)、江西省教育厅科技基金(GJ11613)、浙江
省重中之重学科开放基金(2010945)及九江学院科研立项资助
与乙酰水杨酸的工业生产还有较大的差距,因而寻
(2011KJ007)项目。
找新的绿色催化剂仍是人们研究的重要课题
第一作者:占昌朝(1973-),男,博土研究生,副教授,主要从事
碳基固体酸作为一种催化活性高、廉价且环保催化材料及有机合成研究。联系人:严平。 E-mail ypijtu@l26com