四丁基氢氧化铵的电解合成工艺研究

发布时间：2018-04-29 07:51

本文选题：四丁基溴化铵 + 四丁基氢氧化铵　；参考：《青岛科技大学》2015年硕士论文

【摘要】：四丁基氢氧化铵作为一种有机季铵碱,主要应用于电子化学品、相转移催化剂、分子筛模板剂等方面。随着其应用范围的不断扩展,四丁基氢氧化铵的需求量在日益增加。但目前应用广泛的几种方法合成的四丁基氢氧化铵都存在同一缺点：由于产品中杂质含量较高,导致其纯度不够,品质较差,极大的限制了四丁基氢氧化铵的应用范围。因此,研究用电渗析法合成四丁基氢氧化铵将具有很好的市场前景。本文首先对四丁基氢氧化铵的原料---四丁基溴化铵的合成工艺进行了研究：以三正丁胺和溴代正丁烷为原料探讨其方法和工艺条件。考察了物料配比,溶剂种类,反应时间,重结晶工艺等。通过实验得到较佳合成工艺条件为：以乙腈为溶剂,物料比为：n(三丁胺)：n(溴丁烷)：n(乙腈)=1：1.2：4,反应时间24h,反应转化率达到93%。重结晶母液可套用3次,平均产率达到86.6%。其次,采用单膜法对在四丁基氢氧化铵的电渗析工艺中的阳离子膜进行了考察筛选,根据实验得到数据判定TC-1膜可用于四丁基铵根阳离子透过的阳离子膜。并对单膜法进行改进,提出了三膜四室电渗析的连续生产操作实验方案。该方案较大程度提高了电渗析法的电流效率,简化了操作条件,节约了人工成本。通过对电渗析的各项实验因素考察,得到最佳的工艺条件为：电流密度200A/m2,各槽流量150L/h,原料盐质量浓度50%,碱质量浓度6%的条件下,电流效率达到最佳。
[Abstract]:As an organic quaternary ammonium hydroxide, quaternary ammonium hydroxide is mainly used in electronic chemicals, phase transfer catalysts, molecular sieve templates and so on. With the continuous expansion of its scope of application, the demand for ammonium hydroxide of Ding Ji is increasing day by day. However, the four Ding Ji ammonium hydroxide, which has been widely used in several methods, has the same shortcoming: because of the high impurity content in the product, the purity is not enough and the quality is poor, which greatly limits the application range of the four Ding Ji ammonium hydroxide. Therefore, the study on the synthesis of ammonium hydroxide from tetra by electrodialysis will have a good market prospect. In this paper, the synthetic process of tetra- ammonium hydroxide, a raw material of tetra ammonium hydroxide, was studied. The method and technological conditions were discussed with tri-butylamine and bromo-n-butane as raw materials. The material ratio, solvent type, reaction time and recrystallization process were investigated. The optimum synthetic conditions were obtained as follows: acetonitrile was used as solvent, the molar ratio of tributylamine: n (bromobutane) was 1: 1.2: 4, reaction time was 24 h, the conversion rate of the reaction reached 933%. The recrystallization mother liquor can be applied for 3 times, and the average yield is 86.6%. Secondly, the cationic membrane in the electrodialysis process of four Ding Ji ammonium hydroxide was investigated by single membrane method. According to the experimental data, the cationic membrane of TC-1 membrane can be used for the cation permeation of the ammonium hydroxide of four Ding Ji. The single membrane method was improved and the continuous operation scheme of three-film four-compartment electrodialysis was put forward. This scheme greatly improves the current efficiency of electrodialysis, simplifies the operating conditions and saves the labor cost. Through the investigation of various experimental factors of electrodialysis, the optimum process conditions were obtained as follows: current density 200A / m ~ 2, flow rate 150L / h, salt concentration 50 and alkali concentration 6%, and the current efficiency reached the best under the conditions of current density 200A / m ~ 2, flow rate 150L / h, salt mass concentration 50% and alkali concentration 6%.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ151

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