柱层析法提取油酸的过程研究

Process of industrial oleic acid extracted by column chromatography

针对油酸提纯,设计薄层色谱展开剂比例的正交试验,优化了正己烷-乙酸乙酯-乙酸的体积比,采用相对标准偏差检验了薄层色谱法分离工业油酸的精密度。将展开剂的比例用作柱层析洗脱液,考察了硅胶装填高度、上样量对柱层析法分离油酸质量分数和收率的影响,确定柱层析分离过程条件。测试了层析柱循环使用的效果,为油酸提纯的工业化研究提供依据。结果表明:洗脱液正己烷-乙酸乙酯-乙酸的最佳体积比为85∶15∶8,方法稳定可靠;在硅胶的装填高度为40 cm,工业油酸的上样量为1.1 m L时,油酸的分离效果最好。在此条件下,油酸的质量分数达到88.74%,收率达到82.53%。

In order to purify oleie acid, the orthogonal experiment of the developing solvent on the thin-layer chromatography was designed. The volume ratio of n-hexane-ethyl acetate-acetic acid was optimized, and the precision of method was expressed as the relative standard deviation. The volume ratio of the optimum developing solvent was used as that of the eluent of column chromatography. In order to get the separation conditions, the effects of silica gel loading height and the sampling amount on the mass fraction and yield of oleic acid were investigated. The recycling use of column chromatography was also tested. The results show that the best volume ratio of n-hexane-ethylacetate-acetic is 85： 15： 8, and the method is stable and reliable. When the silica gel loading height is 40 em, and the sampling amount is 1.1 mL, the separation is best. Under this condition, the mass fraction of oleic acid reaches 88.74% and the yield reaches 82. 53%. The experiment provides a basis for further amplification of oleic acid.