The MgO supported amorphous Ni-B catalyst was synthesized by a modified electroless plating method and its deactivation behavior in the hydrogenation of sulfolene and acetophenone (AP) was studied. The fresh and used catalysts were characterized by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectra (FIF-IR), and hydrogen chemisorption. Carbon disulfide was used to test the sulfur-poison-resistive property of the supported Ni-B/MgO catalyst. No significant sintering of the active component and crystallization of the amorphous structure was found in the hydrogenation. The deactivation of catalyst was ascribed to the sulfur-poisoning by SO2 in the hydrogenation of sulfolene and the change of porous structure for Ni-B particles in the acetophenone hydrogenation. (C) 2007 Elsevier B.V. All rights reserved.