In this study, polymeric hydrogels derived from 3-sulfopropyl methacrylate (SPM) were used in the preparation of composite-catalyst system in hydrogen generation from hydrolysis of NaBH4. In order to generate pores and determine their effect on hydrogen production, silica based p(SPM) hydrogels were synthesized also prepared. Additionally, the effects of metal type, temperature, the amount of the catalyst, metal reloading, and reusability were investigated. The activation energy, activation enthalpy, and activation entropy for the hydroylsis reaction of NaBH4 solution in the presence of p(SPM)-Co catalyst system were calculated as 41.67 kJ mol(-1), 38.15 kJ mol(-1), -173.139 J/mol K, respectively. (c) 2012 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.