| Summary: | The present work is the first investigation of the electrocatalytic performances of ZrP<sub>2</sub>O<sub>7</sub> 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 ZrP<sub>2</sub>O<sub>7</sub> in the MFC configuration exhibited high performance in terms of bioelectricity generation, giving a maximum output power density of around 449 mW m<sup>−2</sup>; moreover, it was active for wastewater treatment, reducing the chemical oxygen demand (COD) charge to 50% after three days of reaction.
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