应用薄层色谱对牛磺酸生产工艺进行流程诊断

Process Diagnosis for Taurine Production Flow by Thin Layer Chromatography(TLC)

以硅胶Ｇ为固定相，以正丁醇－冰醋酸－乙醇－水体系为流动相，研究了薄层色谱对工业合成牛磺酸及其中间产物２氨基乙基硫酸酯、反应原料乙醇胺的分离效果。实验结果表明，当流动相组成为正丁醇∶冰醋酸∶乙醇∶水＝８∶２∶１∶１（体积比）时，分离效果较佳。并应用该方法对牛磺酸生产工艺进行了流程诊断，分析了原料、酯化反应产物、还原反应产物、粗结晶产品和牛磺酸产品的组成。结果表明，酯化反应、还原反应、粗结晶和结晶精制各步收率分别为８９．５７％、７６．９５％、９３．６１％和９３．１２％，中间产物２氨基乙基硫酸酯在还原步骤发生可逆反应是导致牛磺酸收率较低的根本原因。

With mobile phase of n butanol-acetic acid-ethyl alcohol-water system,thin layer chromatography(TLC) was applied to separate and analyze of taurine,its intermediate products 2aminoethyl sulfate and feed stock 1aminoethyl alcohol on stationary phase of silica gel G.The best separation effect could be achieved when mobile phase is composed as n butanolacetic acidethyl alcoholwater=8211 (V/V) .TLC was used in process diagnosis of taurine production flow to analyze compositions of feed stock,esterification product,reduction product,primary crystallization product and final synthetic taurine.It is shown that the yield of each step is 89.57%,76.95%,93.61%,93.12% respectively for esterification,reduction,primary crystallization and purification.Diagnosis results indicate that low yield of taurine is mainly caused by reverse reaction of intermediate product 2aminoethyl sulfate in reduction process.