<p>Physical and chemical activation methods were used to prepare two different activated carbons (ACs) from castor de-oiled cake. H<sub>2</sub>O/CO<sub>2</sub> mixture was used as the physical activating agent, and for chemical activation potassium carbonate (K<sub>2</sub>CO<sub>3</sub>) was used. For both materials, textural and chemical properties were characterized by N<sub>2</sub> adsorption–desorption isotherms, thermogravimetric analysis (TGA), Fourier Transform Infrared Spectroscopy (FTIR), thermal programmed reduction (TPR), X-ray fluorescence (XRF), and scanning electron microscopy (SEM). The ACs were used as supports for NiMo sulfide catalysts, which were prepared by wetness impregnation and in-situ sulfided for the hydrodeoxygenation (HDO) of guaiacol (GUA) as a model compound of bio-oil. The HDO reaction was carried out in a typical batch reactor at 5 MPa of H<sub>2</sub> and 350 °C. Under the same test conditions, commercial catalysts were also tested in the reaction. Although the commercial catalysts displayed higher GUA conversion, the prepared catalysts showed higher activity and non-oxygenated and saturated products yield. </p>