This research was aimed to evaluate the synthesis of mercaptoethyl ester of palm fatty acid distillate (PFAD) where water as a byproduct was removed by using vacuum distillation and azeotropic distillation. The reactions were done in a batch reactor using para-toluene sulfonic acid (pTSA) as a catalyst. The performances of the synthesis were evaluated by measuring the sulfhydryl content and yield of the product. Compared to dehydration by vacuum distillation, dehydration by azeotropic distillation gave lower sulfhydryl content and yield but faster reaction completion. Azeotropic distillation gave sulfhydryl content and yield in the range of 6–7% and 57–74%, respectively. Vacuum distillation gave sulfhydryl content and yield in the range of 7–9% and 75–85%, respectively.
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