An Ni2+-Al3+-CO32--layered double hydroxides (NiAl-LDHs) precursor has been synthesized in the pores of spherical gamma-Al2O3 particles. After calcination at 500 degrees C, a NiO/gamma-Al2O3 catalyst precursor was obtained. X-ray photoelectron spectroscopy, temperature programmed reduction, and temperature programmed desorption of hydrogen showed that in the material prepared by calcination of NiAl-LDHs supported on Al2O3, the NiO was characterized by higher reduction temperature, stronger interactions with Al2O3, and higher nickel dispersion compared with the NiO in a material prepared by conventional impregnation of gamma-Al2O3 with an aqueous solution of Ni2+ ions followed by calcination at 500 degrees C. The vapor phase hydrodechlorination of chlorobenzene using molecular hydrogen was studied using Ni/gamma-Al2O3 catalysts prepared by reduction of the NiO/gamma-Al2O3 catalyst precursors synthesized by the two different methods. Under identical reaction conditions, the Ni/gamma-Al2O3 catalyst obtained from the LDHs precursor exhibited not only higher activity but also better stability. (C) 2009 Elsevier Inc. All rights reserved.