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The present work is the first investigation of the electrocatalytic performances of ZrP2O7 as a cathode in a single-chamber Microbial Fuel Cell (MFC) for the conversion of chemical energy from wastewater to bioelectricity. This catalyst was prepared by a coprecipitation method, then characterized by X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), ultraviolet–visible–near-infrared spectrophotometry (UV–Vis–NIR), and cyclic voltammetry analyses. The acid–basic characteristics of the surface were probed by using 2-butanol decomposition. The conversion of 2-butanol occurs essentially through the dehydrating reaction, indicating the predominantly acidic character of the solid. The electrochemical test shows that the studied cathode material is electroactive. In addition, the ZrP2O7 in the MFC configuration exhibited high performance in terms of bioelectricity generation, giving a maximum output power density of around 449 mW m−2; moreover, it was active for wastewater treatment, reducing the chemical oxygen demand (COD) charge to 50% after three days of reaction.