水杨酸乙酯的催化合成与微波辐射合成研究

文档编号:HG243  文档字数:12012,页数:21

摘 要:本文档用正交试验法对浓硫酸催化合成水杨酸乙酯以及微波辐射合成水杨酸乙酯进行了最优化设计。采用L25(54)正交试验完成了对浓硫酸催化合成水杨酸乙酯的研究，通过考察反应时间，酸醇比，搅拌速率，催化剂用量等各个因素对酯化产率的不同影响，选择了四因素五水平的正交试验方案，得出合成水杨酸乙酯的最优实验方案是：醇酸比为1:5，搅拌速率为160r/min，催化剂用量为9mL，反应时间为11小时。在此最优方案的实验条件下进行合成实验，所得的产率约为64%。然后采用L16(44)正交试验完成了对微波辐射合成水杨酸乙酯的研究，通过考察酸醇比，反应功率，催化剂用量，反应时间等各个因素对酯化产率的不同影响，选择了四因素四水平的正交试验方案，得出合成水杨酸乙酯的最优实验方案是：醇酸比为1:7，反应功率为65W，催化剂用量为11mL，反应时间为10min，在此最优方案的实验条件下进行合成实验，所得的产率约为65.26%。把微波辐射技术应用于酯化反应，结果表明反应时间更快，反应产率更高。
关键词:水杨酸乙酯；微波合成；催化酯化；正交设计

Abstract: This paper used orthogonal test to carry out optimization design of concentrated sulfuric acid catalytic synthesis and microwave radiation synthesis ethyl salicylate. This experiment used L25(54) orthogonal table to complete the strong sulfuric acid catalysis synthesis of ethyl salicylate. After through compare different influence factors of the esterification, such as different proportion of salicylic acid and ethanol, stirring rate, the amount of catalyst, and selection the orthogonal experiment scheme of four factors and five levels, we obtained the optimal conditions for synthesis of ethyl salicylate: molar ratio of 1:5, stirring rate of 160r/min, catalyst amount of 9mL, reaction time of 11 hours, and the yield of approximately 64%. And used L16(44) orthogonal table to complete microwave radiation synthesis ethyl salicalate. Then we compared the influences of the different proportion of salicylic acid and ethanol, the reaction power, the amount of catalyst, and the reaction time on the esterification yield. We selected the orthogonal experiment scheme of four factors and four levels, and obtained the optimal conditions for synthesis of ethyl salicylate: molar ratio of 1:7, radiation power of 65W, catalyst amount of 11mL, reaction time of 10min, the yield of approximately 65.26%. The results showed microwave radiation technology applied to esterification with the advantages of shorter reaction time, higher reaction yields than catalyzed synthesis.
Key words：Ethyl salicylate; Microwave reaction; Catalytic esterification; Orthogonal design

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