In the present work, CuCo2O4 nanoparticles, CuCo2O4/Ti3C2, CuO/Ti3C2, and Co3O4/Ti3C2 hybrid nanostructures were synthesized. Various characterization and electrochemical methods were used to investigate the effect of annealing temperature on the catalytic properties. Based on the results, the hybrid of Ti3C2 MXene nanosheets with CuCo2O4 nanoparticles improved the active surface area and kinetics of electron transfer. The annealing temperature through affecting the crystalline structure, leads to a change in the electrocatalytic performance of nanostructures. On the other, the CuCo2O4/Ti3C2 hybrid nanostructure shows better performance than the single metal oxides (CuO and Co3O4) due to the synergistic effect of Cu and Co. Therefore, CuCo2O4/Ti3C2(200) hybrid nanostructure can be used as an efficient nanocatalyst in the electrooxidation process of alcohols in fuel cells due to its higher electrochemical surface area, higher current density (42 mA cm−2) and better stability (83.3 %) compared to other structures.