Volatile organic compounds (VOCs) are one of the main sources of atmospheric haze and pose a threat to human health. Electrocatalysis is a technique that catalyzes chemical reactions by applying an electrical potential, which offers mild reaction conditions and environmental friendliness, making it highly promising for the treatment of VOCs. In this research, a series of deep eutectic solvent (DES) modified Ni/SnOx nanosheets doped with different Sb doping amounts (Ni/SnOx-Sb-DES) have been prepared and applied to the electrooxidation of toluene. In the process of electrochemical gas–solid interface catalysis, the content of reactive oxygen species released on Ni/SnOx-Sb-DES electrodes are affected by the specific surface area and the number of oxygen vacancies. Electrochemical characterization discovered that there are significant differences in overpotential among catalysts of different ratios, thus affecting catalytic activity of Ni/SnOx-Sb-DES. Among them, the Ni/SnOx-Sb-DES with best ratio removal rate of toluene reached 83.07 %, while the selectivity of CO2 was greater than 95 %. This study proposes a method for removing VOCs at ambient temperatures, aiming to provide a new avenue for commercial applications in environmental-related fields.