This work studied the bimetallic nanoparticles Fe-Ag (nZVI-Ag) activated persulfate (PS) in aqueous solution using response surface methodology. The Box–Behnken design (BBD) was employed to optimize three parameters (nZVI-Ag dose, reaction temperature, and PS concentration) using 4-chlorophenol (4-CP) as the target pollutant. The synthesis of nZVI-Ag particles was carried out through a reduction of FeCl2 with NaBH4 followed by reductive deposition of Ag. The catalyst was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Brunauer–Emmett–Teller (BET) surface area. The BBD was considered a satisfactory model to optimize the process. Confirmatory tests were carried out using predicted and experimental values under the optimal conditions (50 mg L−1 nZVI-Ag, 21 mM PS at 57 °C) and the complete removal of 4-CP achieved experimentally was successfully predicted by the model, whereas the mineralization degree predicted (90%) was slightly overestimated against the measured data (83%).

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