A process of Ni/Al2O3 eggshell type catalyst preparation has been developed in laboratory scale. Active catalysts with high Ni content, in which the active metal is concentrated in a very thin layer below the particle surface, were prepared by this process. Wet impregnation of carrier particles with a solution of inorganic Ni salt in organic solvent, in particular ethanol and acetone, was the basic principle of the preparation method. Catalysts with a maximum Ni content of 20.9 mass % , concentrated into a layer of thickness of 770 µm were prepared when ethanol was used as the solvent, while 15.4 % Ni maximum concentration and 622 µm layer thickness were achieved when acetone was used as the solvent. The catalysts prepared were characterized by following analytical methods: XRD, BET, Raman spectroscopy and EDS. The catalysts activities were tested in the gas phase C5 olefins hydrogenation. Despite the lower Ni content, the catalyst impregnated by Ni nitrate, dissolved in acetone was characterized by higher activity in comparison with the catalyst impregnated by ethanol solution.