Cu based catalysts were synthesized in water and methanol solvents by chemical reduction with sodium borohydride (NaBH4). The obtained catalyst was used to catalyze the NaBH4 hydrolysis reaction with phosphoric acid (H3PO4) including different concentrations. Surface morphology and structural properties of the Cu based catalysts prepared in water and methanol solvents were studied using by X-ray diffraction (XRD), scanning electron microscopy (SEM), surface area measurements and Fourier-transform infrared spectroscopy (FTIR) analyses, respectively. The catalytic activity of the catalysts has been tested by measuring the hydrogen production rate by the acidified hydrolysis of NaBH4. The maximum hydrogen production rates in the hydrolysis reaction including 0.25 M H3PO4 using the Cu based catalyst prepared in water and methanol solvents were 825 and 660 ml g(-1)min(-1), respectively. At the same time, the hydrogen production experiments were carried out from this hydrolysis reaction with only H3PO4 and NaBH4 interactions without using Cu metal catalyst. The activation energy obtained based on the nth order reaction model was found to be 61.16 kJ mol(-1).