反应精馏合成三氟乙酸乙酯

论文编号:SW104  论文字数:11861,页数:27

摘要：本文主要对以三氟乙酸、无水乙醇为原料进行反应精馏合成三氟乙酸乙酯的工艺进行了研究。讨论了间歇酯化反应合成三氟乙酸乙酯的反应动力学，在间歇搅拌釜式反应器中测定反应液中的三氟乙酸乙酯、乙醇以及内标物乙腈的峰面积随时间变化的趋势。分别考察了反应精馏塔中不同回流比、进料酸醇摩尔比以及催化剂用量对酯收率的影响，比较了不同催化剂的催化活性，确定了反应的较佳工艺条件。实验结果表明，回流比为2：1，进料酸醇摩尔为1：2，催化剂浓硫酸与三氟乙酸的摩尔比为2：1时，三氟乙酸乙酯的塔顶酯收率为58.19 %。
关键词：反应动力学；反应精馏；酯化反应；三氟乙酸乙酯

Synthesis of Ethyl trifluoroacetate by reactive distillation
 
 
 Abstract: Trifluoroacetic acid and absolute ethanol as raw materials on synthesizing ethyl trifluoroacetate by reactive distillation were mainly studied in this article. A discussion of the batch esterification synthesis of ethyl trifluoroacetate reaction kinetics was taken and has determined the change trend of peak area with time of ethyl trifluoroacetate, ethanol and acetonitrile which as a internal standard in the reaction solution in batch stirred tank reactor. The influence of the reflux ratio, the mole ratio of feed acid with alcohol and the amount of catalyst for ester yield was discussed, the different catalysts for catalytic activity was compared, and then the better processes conditions of reaction was confirmed. The result of experiment indicates that the reflux ratio is 2:1, the mole ratio of feed acid to alcohol is 1:2, the mole ratio of sulfuric acid to trifluoroacetic acid is 2:1, and the yield of ethyl trifluoroacetate is 58.19%.
 Keywords：reaction kinetics; reactive distillation; esterification reaction; ethyl trifluoroacetate
 
 
目  录
中文摘要 I
英文摘要 II
目录 III
 1. 绪论 1
 1.1 三氟乙酸乙酯和反应精馏简介 1
 1.2 催化剂研究进展 2
 1.3 三氟乙酸乙酯工艺研究进展 2
 1.4 本文的研究目的与意义 5
2. 实验部分 6
 2.1 反应体系理化性质 6
 2.2 试剂与仪器 6
 2.3 间歇酯化反应 7
 2.4 间歇酯化反应精馏  8
3. 结果与讨论 11
 3.1 不同进样量对分析结果的影响 11
 3.2 反应时间对组分含量的影响 12
 3.3 回流比的影响  16
 3.4 酸醇摩尔比的影响 17
 3.5 催化剂用量的影响 18
 3.6 催化剂催化活性的比较 19
4. 总结与展望 20
 致谢 21
 参考文献 22