A novel ploy(Enteromorpha-g-acrylic acid) p(EP-g-AA) hydrogel was synthesized and used as a template to prepare Cu and Ni nanoparticles. Then the hydrogel-metal nanoparticles (hydrogel-M (M: Cu, Ni)) were employed as catalyst in the generation of hydrogen from the hydrolysis of NaBH4. X-ray photoelectron spectroscopy (XPS), Fourier Transform infrared spectroscopy (FTIR), thermal gravimetric analysis (TGA), energy-dispersive X-ray spectrometer (EDS) and X-ray diffraction (XRD) were employed to determine the structure of p(EP-g-AA)-M (M: Cu, Ni) composite hydrogels. The effects of several parameters such as the amount of catalyst, initial concentration of NaBH4 and reaction temperature on the hydrolysis reaction were investigated. The kinetics of the hydrolysis reaction under different temperatures was also evaluated to determine the activation parameters. Experimental results showed that the catalytic efficiency of p(EP-g-AA)-Ni was much better than the catalytic efficiency of p(EP-g-AA)-Cu. And increasing the amount of catalyst and decreasing the NaBH4 concentration help to improve the reaction rate. Activation energy for the hydrolysis reaction was 42.61 kJ mol(-1) catalyzed by p(EP-g-AA)-Cu and 39.10 kJ mol(-1) by p(EP-g-AA)-Ni, respectively. At the end of five repetitive uses, p(EP-g-AA)-Cu composites possessed 64% activity and p(EP-g-AA)-Ni owned 70% activity. And after being stored for 30 days, p(EP-g-AA)-Cu and p(EP-g-AA)-Ni both remained 85% activity. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.