The aim of the present work is to explore optimum preparation route of NiMo catalysts for the novel mechanochemically prepared Al2O3 in order to achieve high HDS activity. Specifically, the goals are: i) to up-scale the support synthesis to provide sufficient amount ofAl2O3, ii) to deposit NiMo from solutions of highly soluble precursors by conventional impregnation techniques (I), i.e. sequential impregnation using Mo (first) and Ni (second), and by co-impregnation (Ni+Mo together), i.e. using chelating agent NTA or nickel heteropolyoxomolybdate (HPO), iii) to deposit NiMo from solutions ofslightly soluble precursors by slurry impregnation (SI).\n