An interpolymer anionic composite membrane for reverse osmosis was prepared from poly(vinyl alcohol) and poly(styrene sulfonic acid). The effects of composition of a casting solution, heat-curing periods, and casting thickness on the reverse osmosis performance of resulted membranes have been examined. A mixture of water and ethyl alcohol (12/7, wt %) was found to be a proper solvent for casting an interpolymer membrane on the supporter. The composite membrane was formed by casting the polymer solution in ultrathin film on a microporous polypropylene supporter, evaporating the solvent, and heat-curing at 120°C for a proper period. the optimum composition of a casting solution was as follows: wt % of poly(vinyl alcohol)/poly(styrene sulfonic acid)/solvent was 3/2/95. The membrane heat-cured at 120°C for 2 h has a good performance for reverse osmosis, viz., water flux of 9.1–28.4 L/m2.h at salt rejection level of 88.1–93.4% under applied pressure of 80 kg/cm2 with 0.5% NaCl aqueous solution. The formation mechanism of a water-insoluble membrane was discussed.