Nickel-cobalt bimetallic catalysts supported on high surface area graphite with different Ni:Co ratios (3:1, 2:1 and 1:1) and the monometallic Ni and Co were prepared by wetness impregnation method. The catalysts were tested in hydrodeoxygenation (HDO) of guaiacol in the liquid phase at 50 bar of H-2 and 300 degrees C. The materials were characterized by N-2 adsorption-desorption, XRD, TEM/STEM, H-2-TPR, and CO-chemisorption to assess their properties and correlate them with the catalytic results. The activity was higher on the bimetallic catalysts and followed the trend NiCo2:1/G similar to NiCo3:1/G > NiCo1:1/G > Co/G > Ni/G. Also, selectivity results showed that Ni was more active in the hydrogenation favoring cyclohexanol production from phenol, while this was inhibited on the Co-containing catalysts. Hence, the results showed that synergy was created between Ni and Co and that their interaction, properties, and catalytic performance depend on the metals' ratio.