Currently, wastewater containing high urea levels poses a significant risk to human health. Else, electrocatalytic methodologies have the potential to transform urea present in urea-rich wastewater into hydrogen, thereby contributing towards environmental conservation and facilitating the production of sustainable energy. The characterization of the NiCo2O4@chitosan catalyst was performed by various analytical techniques, including scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Furthermore, the activity of electrodes toward urea removal was investigated by several electrochemical techniques. As a function of current density, the performance of the modified NiCo2O4@chitosan surface was employed to remove urea using electrochemical oxidation. Consequently, the current density measurement was 43 mA cm−2 in a solution of 1.0 M urea and 1.0 M KOH. Different kinetic characteristics were investigated, including charge transfer coefficient (α), Tafel slope (29 mV dec−1), diffusion coefficient (1.87 × 10−5 cm2 s−1), and surface coverage 4.29 × 10−9 mol cm−2. The electrode showed high stability whereas it lost 10.4% of its initial current after 5 h of urea oxidation.