为解决国内传统方法生产四乙基氢氧化铵（TEAH）存在的产量不足、产品纯度差以及环境污染严重等问题，对TEAH的生产工艺进行了研究与优化，提出了一条新的合成路线。首先采用氮气加压法合成四乙基氯化铵（TEAC）中间体，然后通过电解制得TEAH。实验结果表明，合成TEAC最佳的工艺条件为：乙腈、氯乙烷、三乙胺摩尔比是1.9∶1.4∶1，反应物和溶剂填充量控制在58%附近，温度为140℃，反应时间为6 h，反应前通入氮气加压反应釜到0.4 MPa，最终合成TEAC的收率为98.55%。通过TEAC电解制备TEAH最佳工艺为：在电流密度为1 200 A/m²，电解液温度为80℃，阳极室中TEAC浓度控制在3 mol/L，阴极室中TEAH初始浓度为1 mol/L，电解能耗最低，即生产每吨25% TEAH的能耗为427.58 kWh，此时的电流效率为81.81%。新工艺制备过程中，合成TEAC的收率和纯度都很高，而且TEAC电解转化为TEAH不会产生过多的含季铵化合物的废水，对环境的污染很小。

In order to solve the problems of insufficient production, poor purity and serious pollution in the production of tetraethyl ammonium hydroxide (TEAH) by traditional methods in China, a new synthetic process is proposed through research and optimization on the existing production process of TEAH.In the new process, tetraethyl ammonium chloride (TEAC) intermediate is firstly synthesized via nitrogen pressured method, and then TEAH is gained via electrolysis of TEAC.The optimum conditions for synthesis of TEAC are as follows:the molar ratio between acetonitrile, ethyl chloride and triethylamine is 1.9:1.4:1, the filling amount of reactants and solvent is controlled around 58%, temperature is set at 140℃ reaction lasts for 6 h and the initial nitrogen pressure is 0.4 MPa in the reaction tank.The yield of TEAC can reach 98.55% under the optimum conditions.The electrolysis energy consumption reaches 427.58 kWh per ton of 25 TEAH, the lowest, and the current efficiency reaches 81.81% when current density is set as 1, 200 A·m^-2, temperature is at 80℃, and the concentrations of TEAC in anodic chamber and TEAH in cathode chamber is 3 mol·L^-1 and 1 mol·L^-1, respectively.By using this new process, the both purity and yield of TEAC are higher, and not much quaternary ammonium compounds-containing sewage will be generated in the process of TEAC to TEAH, bringing negative pollution to the environment.

柳俊(1992-),男,硕士,研究方向为电化学有机合成、电化学提纯,429746101@qq.com。