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A series of NiMoW/P-Al2O3 catalysts with different Mo/W ratios (sample containing Mo only, Mo/W = 2: 1, Mo/W = 1: 1, Mo/W = 1: 2, and sample containing W only; P2O5 content of the support 2.0 wt %) were synthesized. The precursors of the active phase were the heteropoly acids H3PMo12O40∙nH2O and H3PW12O40∙nH2O, and also nickel citrate. The sulfide phase in the samples was studied by high-resolution transmission electron microscopy and X-ray photoelectron spectroscopy; the catalytic activity of the samples in dibenzothiophene hydrodesulfurization and naphthalene hydrogenation was determined. For the dibenzothiophene hydrogenolysis in the presence of quinoline and naphthalene (content in the model mixture, wt %: dibenzothiophene 0.3, naphthalene 1.5, and quinoline 0.5), kHDS for different samples is in the range 17.6-42.5 h-1 at 275°C and 24.6-45.9 h-1 at 300°C. For the naphthalene hydrogenation, kHYD varies from 0.79 to 1.89 h-1 at 275°C and from 0.91 to 3.78 h-1 at 300°C. The sample based on molybdenum showed the highest activity in hydrogenation and hydrodesulfurization. [ABSTRACT FROM AUTHOR]