催化合成与微波辐射合成水杨酸甲酯的研究

文档编号:HG236  文档字数:12110,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甲酯以及微波辐射合成水杨酸甲酯进行了最优化设计。采用L25(54)正交表完成了浓硫酸催化合成水杨酸甲酯的研究，通过考察反应时间，酸醇比，搅拌速率，催化剂用量四个因素对酯化产率的不同影响，得出水杨酸甲酯的合成最适宜的反应条件为：反应时间为6小时，酸醇比为1：5，搅拌速率为200r/min，催化剂用量为11mL，该条件下的酯化产率为75.0%。然后采用L16(44)正交表完成了微波辐射合成水杨酸甲酯的研究，通过考察酸醇比，辐射功率，催化剂用量，反应时间四个因素对酯化产率的不同影响，得出合成水杨酸甲酯的最优条件为:酸醇比为1：7，反应时间为20min，功率为195W，催化剂用量为9mL，该条件下酯化产率为82.5%。通过比较发现，把微波辐射技术应用于酯化反应，可以使反应时间缩短，产率增大。
关键词: 水杨酸甲酯；微波辐射合成；催化酯化；正交设计

Abstract: This paper has carried out the optimized design with the orthogonal testing method on the strong sulfuric acid catalysis and the microwave radiation synthesis of methyl salicylate. This experiment used L25 (54) orthogonal table to complete the study of the strong sulfuric acid catalysis synthesis of methyl salicylate. It investigated the yield of ester by using different proportion of salicylic acid and methanol, different mix blend velocity, different quantity of sulfuric acid volume and different reaction time. The results enunciate that the most suitable reaction condition is that: the proportion of salicylic acid and methanol is 1:5, the mix blend velocity is 200r/min, the sulfuric acid volume is 11 mL, reaction time is 6 hours, and the ester yield is 75.0%. Then we used L16 (44) orthogonal table to complete the study of the microwave radiation synthesis of methyl salicylate. It investigated the yield of ester by using different proportion of salicylic acid and methanol, different radiation power, different quantity of sulfuric acid volume and different reaction time. The result enunciate that the most suitable reaction condition is that: the proportion of salicylic acid and methanol is 1:7, the powder is 195W, the sulfuric acid volume is 9 mL, and reaction time is 20 min, and the ester yield is 82.5%. By comparison, we can draw the conclusion that when microwave radiation technology was used in esterification with the advangtages of short reaction times and high yields.
 Key words: Methyl salicylate; Microwave radiation synthesis; Catalytic esterification; Orthogonal design

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