The present invention provides an isolation process of the pure sterols from the SODD by simple acid catalyzed esterification and the separation of the reagents by distillation and water washing followed by the crystallization of phytosterols and purification. Soybean oil deodorizer distillate (SODD) and distillate from other vegetable oil refining contain free sterols, in addition to steryl esters, tocopherols squalene and unknown compounds. The process is also applicable to other vegetable oil distillate containing more than 1% phytosterols in the free form. Phytosterols thus obtained is of high purity (95-99%) and high yield (80-90%) and contains .beta.-sitosterol, Stigmasterol and campesterol.