酯交换法合成碳酸二苯酯过程中反应物的气相色谱分析

发布时间：2018-06-13 12:37

本文选题：气相色谱 + 毛细管色谱柱　；参考：《西北大学》2016年硕士论文

【摘要】：碳酸二苯酯(DPC)是一种绿色、环保的化工产品,具有无污染、无毒、无腐蚀性,易于水解及氨解等特性。同时,DPC也是合成农药、制药、工程塑料及有机酸酯的重要中间体。由DPC聚合反应生成的聚碳酸酯(PC),具有透明性好、耐冲击力高、电绝缘性强等优良特性,是一种重要的工程塑料,广泛的用于光学介质、汽车工业、玻璃板材、医疗器械等领域。本课题是基于我院承担的酯交换法合成DPC的中试反应研究,课题中所使用的合成DPC反应过程中的反应液为项目组提供。实验方法为碳酸二甲酯(DMC)与苯酚酯交换合成DPC,而该DPC合成过程又被分为两步进行：第一步：DMC与苯酚(PH)合成甲醇(MeOH)与甲基苯基碳酸酯(MPC),第二步：两个MPC合成DMC与DPC。合成DPC中试单元中采用双塔联合的反应工艺设计,反应塔身涉及众多取样点。我们研究各个取样点反应液的组成,采取先定性、后定量的分析方法,建立了一系列毛细管气相色谱分析方法,使之尽可能的涵盖10个取样点及DPC成品的定性定量,从而达到快速准确分析,以利于指导酯交换法合成DPC反应的进行。在对酯交换法合成DPC过程中的反应物,采用气相色谱分析仪、利用毛细管色谱柱对酯交换法合成DPC过程中的反应物和目标产物DPC进行面积归一化法的定量分析。通过考察实验结果的准确度和精密度,进一步论证了所建立方法的可靠性。结果表明,所建立的毛细管气相色谱分析方法是一种快速的定量方法,具有很好的准确性和稳定性。该方法的建立对实时监测酯交换法合成DPC具有重要的指导意义。
[Abstract]:Two benzyl carbonate (DPC) is a green, environmentally friendly chemical product. It has the characteristics of pollution-free, non-toxic, non corrosive, easy hydrolysis and ammoniation. At the same time, DPC is an important intermediate for synthetic pesticides, pharmaceuticals, engineering plastics and organic esters. The polycarbonate (PC) produced by DPC polymerization has good transparency, high impact resistance and electrical insulation. It is an important engineering plastic. It is widely used in the fields of optical medium, automobile industry, glass plate, medical equipment and so on. This subject is based on the study of the pilot reaction of the synthesis of DPC based on the transesterification method undertaken by our hospital. The reaction solution in the synthesis of synthetic DPC reaction used in the project is provided by the project group. The experimental method is carbonated. Two methyl ester (DMC) and phenol ester exchange synthesis DPC, and the DPC synthesis process is divided into two steps: the first step: DMC and phenol (PH) synthesis methanol (MeOH) and methyl phenyl carbonate (MPC), the second step: two MPC synthesis DMC and DPC. synthesis DPC in the pilot unit of the combination of Twin Towers reaction process design, reaction tower involves a number of samples We studied the composition of the reaction liquid at each sampling point, and established a series of capillary gas chromatography analysis methods by qualitative and quantitative analysis methods, which made it possible to cover the 10 sampling points and the qualitative and quantitative analysis of the DPC finished products so as to achieve rapid and accurate analysis in order to guide the synthesis of DPC reaction in the transesterification process. The reactant in the process of DPC was synthesized by transesterification. The quantitative analysis of the reactant and target product DPC in the synthesis of DPC by the capillary chromatography column was analyzed by the gas chromatography analyzer. The reliability of the established method was further demonstrated by investigating the accuracy and precision of the experimental results. It shows that the established method of capillary gas chromatography is a fast quantitative method with good accuracy and stability. The establishment of this method is of great guiding significance for the real-time monitoring of the synthesis of DPC by transesterification.
【学位授予单位】：西北大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.71;TQ245.2

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