This work reports the preparation and catalytic use of Co-Cu-B nanoparticles, as catalyst for hydrogen generation from the methanolysis of sodium borohydride (NaBH4). An inexpensive and useful catalyst was characterized using a combination of advanced analytical methods including by X-ray diffraction, energy dispersive X-ray spectroscopy, F-TIR analysis, scanning electron microscopy and Brunauer-Emmett-Teller to produce hydrogen from NaBH4 in the reaction with methanol. Basically, after the synthesis of the catalysts, catalytic activity enhancement experiments were carried out by plasma and microwave irradiation. It was determined that the catalyst that is irritiated with plasma is more active on the hydrogen production rate.". The maximum hydrogen production rate in the presence of 2.5 wt% NaBH4 was 270 mL g(-1) min(-1) for catalyst irradiated in the plasma. Our report also includes the comparison of kinetic study of the catalytic methanolysis of NaBH4 depending on irritated and non-irritable Co-Cu-B catalyst in plasma medium. It was observed that the activation energy of the catalyst irradiated in the plasma (Ea = 10.835 kJ mol(-1)) was significantly lower than the non-irritable catalyst (Ea = 68.18 kJ mol(-1)).