PbO2 nanoparticles were prepared using a simple hydrothermal method with β-PbO as precursor and ammonium peroxydisulfate as oxidant. During the hydrothermal condition with ammonium peroxydisulfate, the formed hydroxyl radical has played a key role in the oxidation of β-PbO to PbO2. The size of as-prepared PbO2 nanoparticles was in the range of 25–50 nm. Reduced graphene oxide (RGO) was successfully prepared by the simple reduction reaction of graphene oxide by sodium borohydride and the obtained RGO was then incorporated into the PbO2 nanoparticles. The surface of ITO electrode was modified with the as-prepared PbO2/RGO nanocomposite. The constructed PbO2/RGO/ITO electrode was subsequently applied for the catalytic degradation of cationic red X-GRL which was an azo dye in wastewater. The effects of reaction time, applied current density, and initial concentration of dye on the color removal and COD removal were thoroughly investigated. All results demonstrated that the degradation performance of the electrode modified with PbO2/RGO nanocomposite was extremely excellent.
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