用气相色谱-蒸馏测定仪联合测定1,2-二氯乙烷生产中的循环母液

Combined Determination of Circulating Mother Liquorin the Production of 1,2-Dichloroethane by Gas Chromatography and Distillation Analyzer

为了有效监控1,2-二氯乙烷生产中的母液质量,提前控制以防工艺“恶化”,保证产品纯度,本文研究了母液成分的定量分析方法。通过利用馏程测定仪和气相色谱仪联合进行测定,控制蒸馏温度90～100℃,冷凝温度-10～5℃,馏出液用色谱分析其中低沸物,蒸馏残渣的质量经称量后得到母液中高沸物和固体颗粒的总含量。本方法具有良好的线性关系（r〉0.9996）,方法回收率为99.91%～103.12%,相对标准偏差为0.14%～2.38%。其过程操作简便,是一种准确、快速检测1,2-二氯乙烷循环母液的方法。本方法特别适用于使用稀乙烯为原料、氯化反应过程中副反应较多的1,2-二氯乙烷生产过程。

In order to effectively monitor the quality of mother liquor in the production of 1, 2 - dichloroethane, and prevent the process ＂deterioration＂ by pre - control, and ensure the purity of the product, quantitative analysis method of the mother liquor compositionis studied. By using distillation range analyzer and gas chromatography combined with measurement, control the distillation temperature 90～ 100℃, condensing temperature - 10～ 5 ℃, By chromatographic analysis of the distillate which low boiling, After the distillation residue weighed by mass, the total content of the mother liquor to give high boiling and solid particles. This method has a good linear relationship （r 〉 0. 9996）, recoveries were 99.91% ～ 103.12%, the relative standard deviation was 0.14% ～ 2.38%. The process is simple, is an accurate and rapid detection of 1,2 - dichloroethane circulating liquor approach. The method is particularly applicable to the chlorination reaction of 1,2 - dichloroethane production process which has more by products with low concentration ethylene as raw material.