Co-Ni-Mo-P catalysts were synthesized on the gamma-Al2O3 by electroless deposition. The as prepared Co-Ni-Mo-P/gamma-Al2O3 catalysts were characterized by inductively coupled plasma atomic emission spectrometer (ICP-AES), field emission scanning electron microscope (SEM), energy dispersive X-ray spectrometer (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and nitrogen adsorption-desorption isotherm. The hydrogen generation activity of Co-Ni-Mo-P/gamma-Al2O3 catalysts was tested through hydrolysis of sodium borohydride alkaline solution. The concentrations of Na2MoO4, NaOH and NaBH4, electroless deposition time as well as solution temperature were found to have considerable influences on the hydrogen generation rate of hydrolysis of alkaline NaBH4 solution. The results show that the obtained Co-Ni-Mo-P/gamma-Al2O3 catalysts exhibit excellent catalytic activity. The hydrogen generation rate increases apparently from 10.125 L min(-1) g(catalyst)(-1) to 13.842 L min(-1) g(catalyst)(-1) with the concentration of Na2MoO4 increasing from 0.5 g L-1 to 0.8 g L-1 at 45 degrees C. The catalysts also exhibit favorable cycling performance and lower activation energy (52.43 kJ mol(-1)) in comparison with that of other reported catalysts. Copyright (c) 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.