High performance mordenite membranes were successfully prepared in a short synthesis time from fluoride-containing dilute solution without organic template under microwave-assisted heating. The effects of crystallization temperature, fluoride ion and aluminum source on the membrane morphology and separation performance for dehydration of acetic acid by pervaporation were systematically investigated. High performance mordenite membranes with a thickness about 5 mu m could be prepared from dilute solution with composition of SiO2: 0.06Al(2)O(3):0.24Na(2)O:0.3NaF:120H(2)O at 165 degrees C for 4 h using various aluminum sources. These mordenite membranes exhibited high fluxes of 0.87 +/- 0.06 kg m(-2) h(-1) and excellent selectivities, that is only pure water was detected in the permeate side for dehydration of 90 wt% acetic acid aqueous mixtures at 75 degrees C. The reproducibility of mordenite membranes was high, using the fluoride-containing dilute solution under microwave-assisted heating, which forebodes a promising prospect for industrial applications in preferential separation of water from acetic acid aqueous solutions. (C) 2016 Elsevier B.V. All rights reserved.