苄基三乙基氯化铵的合成工艺探究

Study on Synthesis Process of Benzyltriethylammonium Chloride

以乙酸乙酯和乙腈为溶剂,氯化苄和三乙胺为反应物,在加热条件下经过季胺化反应合成相转移催化剂苄基三乙基氯化铵。考察溶剂乙酸乙酯和乙腈的质量比、反应物料摩尔比、反应温度、反应时间、洗涤剂(乙酸乙酯)用量、溶剂回收利用对产品的影响,并对纯化后的产品进行傅里叶变换红外光谱(FTIR)分析。优化结果显示:溶剂体系中乙酸乙酯与乙腈的质量比为7:10,氯化苄和三乙胺摩尔比为1.1:1.0,反应温度为70℃,反应时间为2 h为最优条件,收率达84%,纯度为98%。采用乙酸乙酯可将粗产品洗涤纯化至纯度99%以上,溶剂回收利用可提高产品的收率。FTIR分析结果表明,合成样品具有苄基三乙基氯化铵主要特征吸收峰,说明合成样品为目标物。

Ethyl acetate and acetonitrile were used as solvents,and benzyl chloride and triethylamine were used as reactants to synthesize benzyl triethylammonium chloride,a phase transfer catalyst,by quaternary amination under heating conditions.In this paper,the effects of different mass ratios,molar ratios of reaction materials,reaction temperature,reaction time,detergent dosage(ethyl acetate),and solvent recycling on the products were considered,and the purified products were analyzed by Fourverner conversion infrared spectroscopy(FTIR).According to the optimization results,the mass ratio of ethyl acetate to acetonitrile in the solvent system was 7:10,the molar ratio of benzyl chloride and triethylamine was 1.1:1.0,the reaction temperature was 70°C,and the reaction time was 2 h as the optimal conditions,with a yield of 84%and a purity of 98%.The use of ethyl acetate can purify crude washing to a purity of more than 99%,and solvent recovery can improve the yield of the product.The FTIR results showed that the synthetic sample had the main characteristic absorption peak of benzyltriethylammonium chloride,indicating that the synthetic sample was the target.