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This work aims to study the role of bentonite, Na + montmorillonite (Na + MMT), as a filler to design a new poly(vinyl alcohol) (PVA)-based membrane for the pervaporation of an azeotropic water/ethanol mixture to enhance its separation efficiency. PVA/Na + MMT nanocomposite membranes, containing different ratios of Na + MMT ( i.e. , 1, 5, 10, 15, and 20 wt%), were prepared using the solvent casting method and crosslinked with maleic acid. The interactions between the PVA polymer and MMT were determined using Fourier transform infrared spectroscopy. Structural characterization by X-ray diffraction and scanning electron microscopy (SEM) analysis showed that the nanoclay structure was well-exfoliated and distributed in the crosslinked PVA matrix. To determine the thermal stability of different membranes, thermogravimetric analysis and differential scanning calorimetry were used. The mechanical properties of pure PVA and the intercalated polymer material were studied. Of note, in this study, the membranes showed a simultaneous increase in the permeation flow and selectivity depending on the montmorillonite filling charge., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)