水杨酸乙酯的催化合成研究

论文编号:HG066  论文字数:12435,页数:25

摘 要：本论文采用正交试验法，对常规加热和微波辐射的方法催化合成水杨酸乙酯进行了研究。按照L16(44)正交表进行实验，并综合分析实验数据后，对两种方法下合成水杨酸乙酯的条件进行了最优化设计。在常规方法下，通过考察酸醇比，搅拌速率，催化剂用量，反应时间四个因素对酯化产率的不同影响，得出其最佳反应条件为：酸醇比为1:9，搅拌速率150r/min，催化剂用量3.5mL，反应时间7小时，在该条件下酯化产率为70.82%。在微波辐射的方法下，通过考察酸醇比，微波功率，催化剂用量和反应时间四个因素对产率的不同影响，得出最佳合成条件为：酸醇比1:9，微波功率325W，催化剂用量3.0ml，反应时间50分钟，在该条件下进行实验得到的产率为73.75%。相比于常规方法，微波辐射合成法具有反应时间短，产率高，副产物少，后处理简单的优点，是一种合成水杨酸乙酯的理想方法。

关键词: 水杨酸乙酯；微波辐射；催化酯化；正交设计

     
Study on the Catalysis Synthesis of Ethyl Salicylate

Abstract : This paper has carried on the orthogonal testing method to the conventional method as well as the microwave radiation synthesis of ethyl salicylate. This experiment used L16 (44) orthogonal table to complete the study of the catalysis synthesis of ethyl salicylate, and analysis of the experimental data for the optimized design . It investigated the yield of ester by using different proportion of salicylic acid and ethyl, different mix blend velocity, different quantity of sulfuric acid volume and different reaction time. The result enunciation that the most suitable and proper reaction conditions of the conventional method is that: the proportion of salicylic acid and ethyl is 1:9(the amount of salicylic acid is 0.05mol),mix blend the velocity is 150r/min, the sulfuric acid volume is 3.5 mL, and reaction time is 7 hours, and the ester produces a rate of 70.82%. The result enunciation that the most suitable and proper reaction conditions of the microwave radiation method is that:the proportion of salicylic acid and ethyl is 1:9(the amount of salicylic acid is 0.05mol),the powder is 325W,the sulfuric acid volume is 3.0 mL, and reaction time is 50 min, and the ester produces a rate of 73.75%. By comparison, the result shows that when microwave radiation technology was used in esterification, we can get short reaction times ,high yields,less byproducts and much more convenient in the process of after-treatment.
 
 
 Keywords: Ethyl  salicylate; Microwave  radiation; Catalytic  esterification;  Orthogonal design

                目　　录
 中文摘要…………………………………………………………………………Ⅰ
 英文摘要…………………………………………………………………………Ⅱ
 目录………………………………………………………………………………Ⅲ
1.绪论……………………………………………………………………………1
 1.1 引言………………………………………………………………………1
 1.2 研究现状…………………………………………………………………2
 1.3 前景展望…………………………………………………………………4
2.实验部分………………………………………………………………………5
 2.1 实验原理…………………………………………………………………5
 2.2 实验原料与仪器…………………………………………………………7
 2.3 实验方案  ………………………………………………………………8
3.结果与讨论    ………………………………………………………………9
 3.1 常规加热催化合成水杨酸乙酯的最优化设……………………………9
 3.2 微波辐射合成水杨酸乙酯的最优化设计 ……………………………13
4.总结与展望 …………………………………………………………………18
 致谢  ……………………………………………………………………………19
参考文献  ………………………………………………………………………20
 附录  ……………………………………………………………………………22