The study is motivated by the industrial separation problem in the fine chemical and pharmaceutical industry, that is isobutanol removal from process wastewater. There are several options for separating the isobutanol-water system. When separating on an industrial scale, it is essential that the most suitable alternative is implemented. The classical method of isobutanol-water separation is distillation. However, since the mixture forms a heteroazeotrope, only an azeotrope composition can be achieved with traditional distillation. Azeotropic distillation is a solution, the alternative is membrane separation, including pervaporation. The aim of this study is to investigate and optimize hybrid organophilic pervaporation and distillation processes for the separation of the isobutanol-water mixture. The examination is carried out in professional flowsheet simulator environment with user-added organophilic pervaporation membrane modules, phase separator and distillation column. Applying this new process, it is possible to obtain 99.9 weight% alcohol and water product from the initial 7 weight% isobutanol - 93 weight% water mixture.