Ni-based catalysts were synthesized in water, methanol and ethanol solvents by chemical reduction with sodium borohydride (NaBH4). The obtained catalyst for the first time was used to catalyze the NaBH4 hydrolysis reaction with phosphoric acid and acetic acid including different concentrations. The maximum hydrogen production rates obtained in the hydrolysis reaction including 0.5M phosphoric acid and 0.1M acetic acid of the Ni-based catalyst prepared in ethanol solvent were 5214 and 3650ml g(-1)min(-1), respectively.