NiCo2O4 is synthesized by the hydrothermal route in the presence of urea. Material is characterized by a complementary combination of X-ray diffraction, nitrogen sorption, and Scanning electron microscopy. The electrochemical oxidation of methanol is investigated at NiCo2O4 modified electrode in the alkaline medium using cyclic voltammetry and chronoamperometry methods. Electrocatalytic activity of NiCo2O4 is compared with the NiO and Co3O4 modified electrodes. A detailed investigation is made for the electrocatalytic oxidation of methanol by varying several reaction parameters such as potential scan rate, methanol concentration, etc. Mechanism of methanol oxidation is proposed based on the cyclic voltammetry study. Double steps chronoamperometry study shows that the methanol electro-oxidation is an irreversible reaction. Electrocatalytic activity of the methanol oxidation at NiCo2O4 modified electrode is found to be significantly higher than that of NiO and Co3O4 modified electrodes.