本文選題：氣相色譜 + 毛細(xì)管色譜柱��； 參考：《西北大學(xué)》2016年碩士論文

【摘要】：碳酸二苯酯(DPC)是一種綠色、環(huán)保的化工產(chǎn)品,具有無污染、無毒、無腐蝕性,易于水解及氨解等特性。同時,DPC也是合成農(nóng)藥、制藥、工程塑料及有機酸酯的重要中間體。由DPC聚合反應(yīng)生成的聚碳酸酯(PC),具有透明性好、耐沖擊力高、電絕緣性強等優(yōu)良特性,是一種重要的工程塑料,廣泛的用于光學(xué)介質(zhì)、汽車工業(yè)、玻璃板材、醫(yī)療器械等領(lǐng)域。本課題是基于我院承擔(dān)的酯交換法合成DPC的中試反應(yīng)研究,課題中所使用的合成DPC反應(yīng)過程中的反應(yīng)液為項目組提供。實驗方法為碳酸二甲酯(DMC)與苯酚酯交換合成DPC,而該DPC合成過程又被分為兩步進行：第一步：DMC與苯酚(PH)合成甲醇(MeOH)與甲基苯基碳酸酯(MPC),第二步：兩個MPC合成DMC與DPC。合成DPC中試單元中采用雙塔聯(lián)合的反應(yīng)工藝設(shè)計,反應(yīng)塔身涉及眾多取樣點。我們研究各個取樣點反應(yīng)液的組成,采取先定性、后定量的分析方法,建立了一系列毛細(xì)管氣相色譜分析方法,使之盡可能的涵蓋10個取樣點及DPC成品的定性定量,從而達到快速準(zhǔn)確分析,以利于指導(dǎo)酯交換法合成DPC反應(yīng)的進行。在對酯交換法合成DPC過程中的反應(yīng)物,采用氣相色譜分析儀、利用毛細(xì)管色譜柱對酯交換法合成DPC過程中的反應(yīng)物和目標(biāo)產(chǎn)物DPC進行面積歸一化法的定量分析。通過考察實驗結(jié)果的準(zhǔn)確度和精密度,進一步論證了所建立方法的可靠性。結(jié)果表明,所建立的毛細(xì)管氣相色譜分析方法是一種快速的定量方法,具有很好的準(zhǔn)確性和穩(wěn)定性。該方法的建立對實時監(jiān)測酯交換法合成DPC具有重要的指導(dǎo)意義。
[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.
【學(xué)位授予單位】：西北大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：O657.71;TQ245.2

【參考文獻】

相關(guān)期刊論文 前10條

1 周博;;碳酸二苯酯合成工藝的比較[J];廣州化工;2014年12期

2 余海;梅支舵;姚日生;;三光氣法碳酸二苯酯的合成工藝[J];安徽化工;2010年04期

3 曹平;石衛(wèi)兵;楊先貴;康濤;雷永誠;王公應(yīng);;酯交換法合成碳酸二苯酯的技術(shù)分析[J];石油化工;2010年03期

4 曹環(huán)禮;;氣相色譜技術(shù)的研究進展及其應(yīng)用[J];廣東化工;2009年08期

5 尹振晏;李艷云;熊勝明;;碳酸二苯酯的合成工藝新進展[J];化工中間體;2006年12期

6 傅若農(nóng);近兩年國內(nèi)氣相色譜的應(yīng)用進展(Ⅲ)[J];分析試驗室;2005年06期

7 傅若農(nóng);近兩年國內(nèi)氣相色譜的應(yīng)用進展(Ⅱ)[J];分析試驗室;2005年05期

8 傅若農(nóng);近兩年國內(nèi)氣相色譜的應(yīng)用進展(Ⅰ)[J];分析試驗室;2005年04期

9 王公應(yīng),王越,曾毅;非光氣法碳酸二苯酯生產(chǎn)技術(shù)進展[J];化工中間體;2004年04期

10 石聯(lián);;聚合反應(yīng)中間體——碳酸二苯酯的工藝開發(fā)與應(yīng)用開拓[J];化工中間體;2003年12期

，

本文編號：2014051