Mesoporous and well-dispersed nickel-alumina composite aerogels with high surface area have been prepared by CO 2 supercritical drying of alcogels obtained by the fast sol-gel process. They were evaluated as catalysts in a batch reactor for the liquid-phase hydrogenation of benzophenone and soybean oil and showed excellent activity and accessibility of the metal particles. They were also characterized by nitrogen adsorption-desorption, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) to explain their excellent catalytic performance in comparison with other alumina-supported nickel catalysts.