文献类型：期刊文献

中文题名：甲基三乙基碳酸氢铵的合成工艺研究

英文题名：Synthesis of Methyl Triethylammonium Hydrogen Carbonate

作者：郑甘霖[1];丁同梅[1];田恒水[1]

机构：[1]华东理工大学化工学院,上海200237

年份：2015

卷号：37

期号：12

起止页码：1131

中文期刊名：化学试剂

外文期刊名：Chemical Reagents

收录：CSTPCD;;北大核心:【北大核心2014】；

语种：中文

中文关键词：三乙胺;碳酸二甲酯;甲基三乙基碳酸氢铵;甲基三乙基氢氧化铵

外文关键词：triethylamine; dimethyl carbonate; methyl triethylammonium hydrogen carbonate; methyl triethylammonium hydroxide

摘要：甲基三乙基氢氧化铵是电子、催化等领域应用广泛的精细化工产品,可以由甲基三乙基碳酸氢铵经电解制得。以三乙胺和碳酸二甲酯为原料,采用两步法合成甲基三乙基氢氧化铵的原料甲基三乙基碳酸氢铵。从物料比、反应温度、氮气初始压力、反应时间、水解温度5个方面对合成工艺进行了优化。结果表明,在n(碳酸二甲酯)∶n(三乙胺)=1.5∶1、反应温度150℃、反应压力1.5 MPa、反应时间6 h,中间体甲基三乙基铵碳酸单甲酯的收率达90%。水解温度为70℃时,标题化合物的收率接近100%。
Methyl triethylammonium hydrogen carbonate,as a valuable intermediate for methyl triethylammonium hydroxide,could be used in catalysis and electronic industries. Methyl triethylammonium methyl carbonate was synthesized from triethylamine and dimethyl carbonate as raw materials and methanol as solvent in two steps. After that,methyl triethylammonium methyl carbonate was hydrolyzed to the desired methyl triethylammonium hydrogen carbonate. The influence of materials molar ratio,reaction temperature,initial nitrogen pressure,reaction time and hydrolysis temperature on the reaction was investigated. Accordingly,the reaction conditions were optimized as shown below： triethylamine and dimethyl carbonate molar ratio was 1∶ 1. 5; reaction temperature was 150 ℃,initial nitrogen pressure was 1. 5 MPa,reaction time was 6 h,the intermediate（ MTMC） yield was 90%. Under hydrolysis temperature was 70 ℃,the yield of（ MTHC） reached 100%.