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摘要
通过两步反应合成了磺酸型功能化离子液体1-(3-磺酸)丙基-3-乙基咪唑硫酸氢盐BAIL,利用1HNMR对其结构进行表征。将该离子液体用于催化巯基丙酸和甲醇酯化反应合成3-巯基丙酸甲酯,探讨了反应温度、巯基丙酸(MPA)与甲醇摩尔比、催化剂BAIL质量分数对酯化反应的影响。结果表明,BAIL对3-巯基丙酸甲酯合成反应有较好的催化活性,在n(CH3OH):n(MPA)为2:1、反应时间为1.5 h、反应温度为70℃、催化剂质量分数为10%(相较于巯基丙酸的质量)最佳工艺条件下,巯基丙酸转化率高达93.2%。催化剂稳定性良好,重复使用5次后仍保持较高活性。
Abstract
1-(3-Sulfonic acid)propyl-3-ethylimidazole hydrogen sulfate BAIL, a sulfonic acid-based functionalized ionic liquid, is synthesized through a two-step reaction method, and its structure is characterized by 1H-NMR.The ionic liquid is used to catalyze the esterification reaction between mercaptopropionic acid and methanol to synthesize methyl 3-mercaptopropionate.The effects of reaction temperature, the molar ratio of mercaptopropionic acid to methanol, and the addition amount of catalyst BAIL on the esterification reaction are discussed.It is shown that BAIL exhibits a good catalytic activity for the synthesis of methyl 3-mercaptopropionate.The conversion rate of mercaptopropionic acid can reach as high as 93.2% under the optimal conditions that n(CH3OH):n(MPA)=2:1, the reaction time is 1.5 h, and the reaction temperature is at 70℃, and the amount of catalyst is 10% that of mercaptopropionic acid.The catalyst has a good stability and maintains high activity after 5 times of repeated use.
关键词
1-(3-磺酸)丙基-3-乙基咪唑硫酸氢盐
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巯基丙酸甲酯
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离子液体
Key words
1-(3-sulfonic acid) propyl-3-ethylimidazole bisulfate
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methyl mercaptopropionate
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ionic liquid
Author summay
杨红军(1997-),男,硕士研究生,研究方向为硫化物有机合成,yhj274599@126.com
磺酸基离子液体催化合成3-巯基丙酸甲酯的研究[J].
现代化工, 2022, 42(5): 202-205 DOI:10.16606/j.cnki.issn0253-4320.2022.05.039