High-loading Ni–Mo carbide catalysts were prepared by the modified gel-combustion method under various thermal treatment conditions. All samples were studied by X-ray diffraction (XRD) analysis, which showed that the catalysts could contain cubic and hexagonal molybdenum carbides, nickel, nickel oxide and Ni–Mo solid solutions, depending on the thermal treatment conditions. Study of catalyst activity and selectivity in the hydrogenation of furfural was carried out in a batch reactor at 150◦ C and hydrogen pressure 6.0 MPa. Analysis of the reaction products showed that the highest yields of 2-methylfuran (2-MF) and furfuryl alcohol (FA) were achieved using catalysts synthesized by calcination of the nickel-molybdenum-carbon precursor at 400◦ C with the following reduction in a stream of hydrogen at 600◦ C. The best results for production of FA with a yield of 80 mol % and 2-MF with a yield of 29 mol % were observed using Ni6 MoC–SiO2 (400/600) and Ni1 MoC–SiO2 (400/600) catalysts, respectively. It has been shown that the addition of nickel to the carbide molybdenum catalyst significantly increases the activity of the catalytic systems. In addition, nickel also contributes to the formation of products formed by hydrogenation of the aromatic ring tetrahydrofurfuryl alcohol (THFA) and 2-methyltetrahydrofuran (2-MTHF).