Ni/MgF(2) (1 wt.% Ni) catalysts were prepared by introduction of nickel nitrate into hydrogel of magnesium fluoride or impregnation of calcined MgF(2) with Ni(NO(3))(2). The samples were reduced with H(2) without or after calcination in air or helium. The catalysts were characterized by BET, H(2)-TPR, H(2)-adsorption, XRD and gas phase hydrogenation of toluene. The catalysts obtained with magnesium fluoride as a support for nickel has enabled to obtain a catalyst of high activity for hydrogenation of toluene to methylcyclohexane under atmospheric pressure. Their catalytic activity was influenced by the method of the nickel phase introduction and was higher when calcined MgF(2) was used as a support. The physicochemical characterization and activity testing showed that the catalyst reduced without previous calcination exhibits the highest dispersion of metallic Ni and most excellent catalytic performance in toluene hydorgenation. (C) 2010 Elsevier B.V. All rights reserved.