Development of a novel modified electrode for electrocatalytic oxidation of methanol in order to decrease overvoltage is importance. In this paper, carbon paste electrode (CPE) was modified by ZSM-5 nanozeolite. The average diameter of used nanozeolite was 97 nm. Ni2+ ions were incorporated to the nanozeolite by immersion of the modified electrode in a 0.1 M nickel chloride solution. Then, electrochemical studies of this electrode were performed by using cyclic voltammetry(CV) in alkaline medium. This modified electrode was used as an anode for the electrocatalytic oxidation of methanol in 0.1 M of NaOH solution. The obtained data demonstrated that ZSM-5 nanozeolite at the surface of CPE improves catalytic efficiency of the dispersed nickel ions toward methanol oxidation. The values of electron transfer coefficient, charge-transfer rate constant, and the electrode surface coverage are obtained 0.61, 0.2342 s−1, and 4.33 × 10−8 mol cm−2, respectively. Also, the mean value of catalytic rate constant between the methanol and redox sites of electrode and diffusion coefficient were found to be 2.54 × 104 cm3 mol−1 s−1 and 1.85 × 10−8 cm2 s−1, respectively. Obtained results from both CV and chronoamperometric techniques indicated that the electrode reaction is a diffusion-controlled process.