Pyridinium based dicationic ionic salts [C-6(mpy)(2)] containing transition metal halide anions [NiCl4](2-) and [CoCl4](2-) were synthesized and characterized by H-1 NMR, C-13 NMR, LRMS-MS & TGA. The catalytic activities of dicationic ionic liquids were studied for the first time in the hydrolysis reaction of sodium borohydride. The reported work includes the full experimental details for the collection of a wealth of kinetic data to determine the activation energy (Ea = 56.36 kJ/mol) and effects of the amount of catalyst, amount of substrate and temperature on the rate for the catalytic hydrolysis of NaBH4. The activation energy of the catalyst dicationic tetrachloronickelate (II) anion for hydrogen production is comparable to that of other metal halide catalysts. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.