草酸二乙酯催化加氢制乙二醇液相产物分析

Analysis of the Liquid Products from Catalytical Hydrogenation of Diethyl Oxalate to Ethylene Glycol

介绍了一种草酸二乙酯催化加氢制乙二醇液相产物的气相色谱分析法，色谱分析在ＧＣ－１０３型色谱仪上进行，用ＣＤＭＣ－１ＣＸ型色谱数据处理机计算，液相产物在内填５％ＦＦＡＰ／６０～８０目硅藻土８８０（ＡＷＤＭＣＳ）的不锈钢色谱柱上分离，用热导检测器检测，以２０ｍＬ／ｍｉｎ流速的氢气为载气，每个样品的分析时间约为１０ｍｉｎ。方法快速简便，数据较为精密准确。

This paper presents a rapid, quantitative gas chromatographic method for analyzing the liquid products from catalytical hydrogenation of diethyl oxalate to ethylene glycol. The liquid products include ethyl alcohol , ethylene glycol, ethyl glycollate, unreacted diethyl oxalate, trace 1,2 butanediol, etc. The chromatographic analysis of liquid products was performed on a Model GC 103 gas chromatograph, coupled with a Model CDMC 1CX chromatographic data processor. A column of 5% FFAP on Kieselguhr 880, DMCS, 60 80mesh, 2m×3mm i.d., was used to separate the liquid products. The hydrogen carrier gas flow rate was 20mL/min, injection port temperature was 170℃ and the detector temperature was kept at 145℃. The thermal conductivity cell detector was used and the bridge current was 20mA. The injection volume was 0.2 μL. The recoveries were≥95% and the relative standard deviation (RSD) was ≤2.5%. The time for each analysis was about 10min. The reported method is rapid, simple and accurate.