Hydrogen production through hydrolysis of sodium borohydride (NaBH4) by using metal catalysts is promising for fuel cell applications. Nickel (Ni) and its alloys are favorable due to their high catalytic activity, relatively low cost and availability. In present study, the effects of temperature, pH, reduction rate and reducing agent concentration, which significantly affect the catalyst performance, were investigated using the response surface methodology (RSM). A mathematical model was derived according to results which were obtained from four-level orthogonal Taguchi L16 (44) experimental design used for the optimization of multiple parameters in the process. From the RSM analyses, that compatible with the predicted experimental results, maximum hydrogen generation rate (HGR) 49.81 L min−1 gcat−1 was obtained temperature of 278.12 K, pH of 5.52, reducing agent concentration of 85.96 NaBH4.water−1 and reduction rate of 6.82 mL min−1. Analysis of variance reveals that both pH and rate of reduction have significant effect than the temperature on the HGR.