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Concentration of alcohols in fermentation is a critical step in terms of energy consumption for biofuel technologies. Two-stage cascade separation using polymer (PTMSP/PDMSM) and NaA zeolite membranes was developed to produce dry butanol from fermentation broth. Application of this approach allowed to increase the content of butanol from 1 to 97.4 wt% and to reduce the content of water to 0.2 wt.%. NaA zeolite membrane provides for efficient dehydration of biobutanol in the presence of fermentation by-products including acetic and butyric acids.