An Al/Fe-pillared clay catalyst (Al/Fe-PILC) prepared from low cost technical-grade reagents has been investigated in the photocatalytic Wet Peroxide Oxidation (photo-CWPO) of dissolved Natural Organic Matter (NOM) under circumneutral pH. The successful pillaring of the layered clay material was confirmed by X-ray diffraction (XRD), N2 adsorption at −196 °C, cation exchange capacity (CEC) and simultaneous thermal analysis (TGA/DSC). High levels of mineralization of the dissolved organic carbon and color removal of a synthetic NOM surrogate solution were achieved even under natural lab’s lighting and ambient temperature and pressure, whereas the absence of radiation (in dark) was found to strongly affect the performance of the degradation. The photo-CWPO of NOM activated by the Al/Fe-PILC clay catalyst under visible light irradiation (LED lamp, 450 and 550 nm peaks) displayed a DOC mineralization of 72% and color removal of 73% in just 210 min of irradiation at neutral pH, whereas both responses decayed under ultraviolet lightning (λ: 365 nm) to 41% and 58%, respectively. This behavior is ascribed to formation of triplet states of natural organic matter (3NOM*) by absorption of visible light, which seems to synergistically improve the rate-determining step of the heterogeneous Fenton process, namely reduction of Fe3+ into Fe2+ on the surface of the clay catalyst. Interestingly, experiments performed at neutral and pH 3.0 showed very similar efficiencies under visible light irradiation; these findings may really facilitate the application of the photo-CWPO process to assist conventional drinking water treatment plants in the removal of NOM before the typical disinfection by chlorine to produce safer drinking water.

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