| Summary: | A supercritical CO<sub>2</sub> drying process was used to prepare an innovative nanocomposite, formed by a poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF HFP) aerogel loaded with RuO<sub>2</sub> nanoparticles. The produced nanocomposites, at 10% and 60% w/w of RuO<sub>2</sub>, were tested for the electrochemical oxidation of model tannery wastewaters. The effect of the electrochemical oxidation parameters, like pH, temperature, and current density, on tannic acid, intermediates, and chemical oxygen demand (COD) removal, was investigated. In particular, the electrolysis of a simulated real tannery wastewater, using PVDF HFP_RuO<sub>2</sub> 60, was optimized working at pH 10, 40 °C, and setting the current density at 600 A/m<sup>2</sup>. Operating in this way, surfactants, sulfides, and tannins oxidation was achieved in about 2.5 h, ammonium nitrogen oxidation in 3 h, and COD removal in 5 h. When chloride-containing solutions were tested, the purification was due to indirect electrolysis, related to surface redox reactions generating active chlorine. Moreover, sulfide ions were converted into sulfates and ammonium nitrogen in gaseous N<sub>2</sub>.
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