AbstractNaMMT clay incorporated and maleic acid (MA) crosslinked polyvinyl alcohol (PVA)‐chitisan (CS) interpenetrating network (IPN) type nanocomposite membranes were prepared for dehydration of acetone by pervaporation (PV). FTIR, XRD, SEM, UV spectroscopy, mechanical properties, contact angle measurement, and DTA‐TGA were used to characterize these membranes. The effect of clay, CS, and MA on the flux and separation factor for water were statistically optimized by Box–Behnken design (BBD). Accordingly, the membrane prepared with 39.3 wt.% CS, 3 wt.% each of MA and NaMMT nanoclay showed a flux/separation factor of 0.176–0.733 kg/m2h/ 277–168 for the pervaporative dehydration of 99 wt.% acetone.Highlights IPN nanocomposite membranes were prepared from PVA, CS, and nano clay. Structure and properties of the IPNs were characterized. Synthesis parameters were optimized by BBD. Membranes showed high flux and water selectivity for acetone dehydration by PV.