Coupling TiO₂ with various elements could enhance its photocatalytic activity. In this study, an innovative ultrasound-assisted sol–gel method was used to synthesize TiO₂/Ag(x%) by varying Ag–support mass (x = 9.3, 17.1, and 23.6%), followed by calcination at 450 °C for 30 min. The aim was to demonstrate that Ag compositing improves photoactivity under visible light (>400 nm). The synthesized photocatalysts were assessed for their effectiveness in the degradation and mineralization of Methylene Blue (MB) and Acid Orange 7 (AO7) using visible lamps emitting in the range of 400–800 nm. Characterization of the prepared photocatalysts was performed by using Raman spectroscopy, SEM/EDS, pH_pzc, and UV–visible spectroscopy. Raman spectroscopy confirmed the predominance of the anatase phase in all the photocatalysts. The photodegradation efficiencies of the selected dyes, MB and AO7, reached 99% (pH 6) and 95% (pH 3) after 180 min of irradiation, respectively. The best performance for the degradation of the two dyes was observed with TiO₂/Ag9.3%, showing optimal kinetics at this doping concentration. The improved photoactivity of the TiO₂/Ag composite is due to a decrease in the recombination rate of electron/hole (e⁻/h⁺) and a decrease in the band gap from 3.13 to 2.49 eV. The mineralization rate of both dyes under visible light is about 9.3%, indicating the presence of refractory by-products that resist complete degradation. Under UVA irradiation, complete mineralization is obtained. This study confirms the potential of TiO₂/Ag composite as a high-performance and cost-effective photocatalyst for solar environmental remediation, highlighting the role of silver in extending light absorption into the visible region and improving charge separation.

Highly efficient, separable, and stable magnetic iron-based-photocatalysts produced from ultra-stable Y (USY) zeolite were applied, for the first time, to the photo-Fenton removal of phenol under solar light. USY Zeolite with a Si/Al molar ratio of 385 was impregnated under vacuum with an aqueous solution of Fe²⁺ ions and thermally treated (500-750 °C) in a reducing atmosphere. Three catalysts, Fe-USY500°C-2h, Fe-USY600°C-2h and Fe-USY750°C-2h, containing different amounts of reduced iron species entrapped in the zeolitic matrix, were obtained. The catalysts were thoroughly characterized by absorption spectrometry, X-ray powder diffraction with synchrotron source, followed by Rietveld analysis, X-ray photoelectron spectroscopy, N₂ adsorption/desorption at -196 °C, high-resolution transmission electron microscopy and magnetic measurements at room temperature. The catalytic activity was evaluated in a recirculating batch photoreactor irradiated by solar light with online analysis of evolved CO₂. Photo-Fenton results showed that the catalyst obtained by thermal treatment at 500 °C for 2 h under a reducing atmosphere (FeUSY-500°C-2h) was able to completely mineralize phenol in 120 min of irradiation time at pH = 4 owing to the presence of a higher content of entrapped nano-sized magnetite particles. The latter promotes the generation of hydroxyl radicals in a more efficient way than the Fe-USY catalysts prepared at 600 and 750 °C because of the higher Fe₃O₄ content in ultra-stable Y zeolite treated at 500 °C. The FeUSY-500°C-2h catalyst was recovered from the treated water through magnetic separation and reused five times without any significant worsening of phenol mineralization performances. The characterization of the FeUSY-500°C-2h after the photo-Fenton process demonstrated that it was perfectly stable during the reaction. The optimized catalyst was also effective in the mineralization of phenol in tap water. Finally, a possible photo-Fenton mechanism for phenol mineralization was assessed based on experimental tests carried out in the presence of scavenger molecules, demonstrating that hydroxyl radicals play a major role.