Distillation is one of the industrial operations responsible for the high overall energy consumption in industrial plants. The dehydration of aqueous solutions of glycerine by heteroazeotropic batch distillation was investigated. For each entrainer, the effects of variables on the rate water withdrawal were studied. The process was only possible after removing the salts of the raw glycerine. Xylene removed more water than toluene according to the paired comparison design. The best situation for dehydration of glycerine was for higher heat flow and lower initial concentration due to the interaction. The combined method for deodorization, bubbling with air followed by extraction with hexane, was more effective for removing the entrainer. This is an abstract of a paper presented at the 7th European Congress of Chemical Engineering-7 and 19th International Congress of Chemical and Process Engineering CHISA (Prague, Czech Republic 8/28/2010-9/1/2010).