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In this work, a novel system composed of non-precious nickel-based metal oxide/reduced graphene oxide nanocomposite (Ni–PbO2–GN) is used for electrooxidation of ethylene glycol (EG) in 1.0 M NaOH solution and compares its activity with that of Ni, Ni–GN, and Ni–PbO2. The facile electrodeposition technique is used to prepare the catalysts on glassy carbon (GC) substrates. The outcomes of electrochemical measurements show a high performance towards EG oxidation is obtained for Ni-nanocomposite electrodes compared to that of Ni mainly due to their higher surface areas. The excellent electrocatalytic properties of the Ni-nanocomposite could be ascribed to the synergistic contributions of PbO2 and graphene (GN) nano-sheets that help the reduction of Ni grains. A smaller charge transfer resistance value of 34.5 Ω cm2 for EG oxidation reaction at + 360 mV is recorded for GC/Ni–PbO2–GN compared to the other prepared electrodes. Moreover, it exhibits higher kinetic parameters of EG such as diffusion coefficient (D = 3.9 × 10–10 cm2 s−1) and charge transfer rate constant (ks = 32.5 mol−1 cm3 s−1). The overall performance and stability of the prepared catalysts towards EG electrooxidation have been estimated to be in the order of GC/Ni–PbO2–GN > GC/Ni–GN > GC/Ni–PbO2 > GC/Ni. [ABSTRACT FROM AUTHOR]