A cationic hydrogel synthesized from (3-acrylamidopropyl) trimethyl ammonium chloride as poly[(3-acrylamidopropyl) trimethyl ammonium chloride] [p(APTMACl)] was put into contact with the chloride salts of metals such as CoCl2, NiCl2, and CuCl2 in ethanol. The metal-loaded p(APTMACl) hydrogels were used as catalyst systems in hydrogen generation from the hydrolysis of sodium borohydride (NaBH4) and ammonia borane. The activation energy values for the hydrolysis reaction were calculated for all of the catalyst systems and were found to be 53.43 and 26.74 kJ/mol for p(APTMACl)–[CoCl4]2− and p(APTMACl)–[NiCl4]2−, respectively. These activation parameters were better than values reported in the literature for the ionic liquid metal complexes of smaller molecules used for the same purpose. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40183.