碳基固体酸催化合成乙酰水杨酸.pdf

学兔兔 化 工 进 展 2012年第31卷第5期 CHEMICAL INDUSTRY AND ENGINEERING PROGRESS ·l121· 碳基固体酸催化合成乙酰水杨酸 占昌朝 2，曹小华 一，严 平 ，王剑波 ，余祖进 ，江小平 ( 九江学院化学与环境工程学院，江西 九江 332005； 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25 min，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微波加热条件反应。 关键词：碳基固体酸；酰化反应；乙酰水杨酸；微波加热 中图分类号：O 621．25 文献标志码：A 文章编号：1000—6613(2012)05—1121—05 Synthesis of acetylsalicylic acid catalyzed by carbon—based solid acid ZHANChangchao ～，CA0Xiaohua 2 YANPing ，WANGJianbo ，YUZujin ，JIANGXiaoping ， ( College ofChemistry and Environmental Engineering，Jiujiang University，Jiujiang 332005，Jiangxi，China； College ofChemical Engineering and Materials，Zhejiang University ofTechnology， 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 ofconventional heat and microwave heat on yield of acetylsalicylic acid were studied．The better condition was determined with single factor tests，which iS as fclllows：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 ℃，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