In the crosslining reaction of poly(vinyl alcohoJ)(PVA) with sulfur-succinic acid which had been established in our previous work, reaction temperature, 15$0^{circ}C$, was so high to collapse the pore struc¬tures in support membrane for the preparation of composite membrane. Therefore, the efforts have been focused on lowering of the reaction temperature to 100$^{circ}$C by using a catalysis, HC!. The newly established crosslinking reaction was characterized through the analysis of the chemical and thermal properties. From these results, the optimum conditions for the membrane preparation couId be drawn as followings : (i) reac¬tion temperature, 100 $^{circ}C$,(ii) reaction time, 90 min, (iii) the concentration of the catalysis (HCD, 1.5%. Com¬posite membranes were fabricated by coating a casting solution containing PYA, sulfur-succinic acid and HCl on a support membrane followed by crosslinking it at 10$0^{circ}C$. The resulting membranes were applied to the pervaporation separation of methyl-tert-butyl ether(MTBE)/methanol (MeOH) mixtures at 30, 40, and 5O$^{circ}C$. The flux of 5.09 g/$m^2$hr at 5O$^{circ}C$ and the highest separation factor of 1622 were obtained, respectively.