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In the present work, phenol was used as a model molecule to the photocatalytic evaluation of TiO2 impregnated with iron sulphide and chlorine on a visible-light reactor. The iron–chlorine catalyst was prepared by incipient impregnation with the metal precursors, Fe (NO3)3 and NaCl on previously calcined TiO2. The catalyst was sulphurized with H2S at 300 °C for 1 h. The catalysts were prepared at different chlorine concentrations using HYDRA chemical equilibrium diagrams to obtain different fractions of FeCl+. The oxide catalysts were characterized with diffuse reflectance (DRS UV–Vis) and temperature programmed reduction analysis (TPR). Sulphurized catalysts were characterized with Raman spectrometry and X-ray photoelectron spectrometry (XPS). The FeS–2Cl/TiO2 catalyst presented 8.35 times higher photodegradation than TiO2 and 6.4 times higher compared to the FeS–0.25Cl/TiO2 catalyst. DRS and XPS showed similar results of band gap, proving that the catalyst remain stable after sulphurisation. The TPR results of FeS–2Cl/TiO2 showed an increment of 86.29% in Fe2+/Fe3+ compared to FeS–0.25Cl/TiO2. XPS and Raman results for oxide and sulphated iron species relation suggested that FeS–2Cl/TiO2 decreased 4.45% compared to FeS–0.25Cl/TiO2 catalyst. XPS semiquantitative for S/Fe results showed that the FeS–2Cl/TiO2 catalyst increased 73.17% in comparison to FeS–0.25Cl/TiO2. These results suggested the increment of sulphurisation degree for FeS–2Cl/TiO2. In this regard, the catalyst characterization results showed that the presence of FeCl+ (0.85 fractions) in solution before impregnation promoted the active sulphide species maintaining the band gap and improved the degradation of phenol on visible light.

Currently, interest has grown in finding effective solutions for the treatment of water pollution by toxic compounds. Some of the latter that have acquired importance are phenols and chlorophenols, due to their employment in the manufacture of pesticides, insecticides, cords of wood, paper industry, among others. The problem is rooted in that these compounds are very persistent in the environment because they are partially biodegradable and cannot be photodegraded directly by sunlight. Chlorophenols are extremely toxic, especially 2,4,6-trichlorophenol, which is potentially carcinogenic. In this work, Mg/Al-mixed oxide catalysts were obtained from the thermal treatment of hydrotalcite-type materials, synthesized by sol-gel method with different Mg/Al ratios. Hydrotalcites and Mg/Al-mixed oxides were physicochemically characterized by X-ray diffraction, thermal analysis (DTA and TGA), and N2 physisorption. The results were obtained on having proven the photocatalytic degradation of 2,4,6-trichlorophenol as a pollutant model by water. The catalysts obtained present the hydrotalcite phase with thermal evolution until achieving Mg/Al-mixed oxides at 500°C. The catalysts are of mesoporous materials and exhibiting large surface areas. The catalysts demonstrated good photocatalytic activity with good efficiency, reaching degradation percentages with Mg/Al = 1, 2, 4, 5, and 7 ratios of 94.2, 92.5, 86.2, 84.2, and 63.9%, respectively, until achieving mineralization.

In recent years, the search for solutions for the treatment of water pollution by toxic compounds such as phenols and chlorophenols has been increasing. Phenols and their derivatives are widely used in the manufacture of pesticides, insecticides, paper, and wood preservers, among other things. Chlorophenols are partially biodegradable but not directly photodegradable by sunlight and are extremely toxic—especially 2,4,6-trichlorophenol, which is considered to be potentially carcinogenic. As a viable proposal to be applied in the treatment of water contaminated with 2,4,6-trichlorophenol, this paper presents an application study of the thermally activated Mg/Fe layered double hydroxides as photocatalysts for the mineralization of this contaminant. Activated Mg/Fe layered double hydroxides were characterized by X-ray diffraction, thermal analysis, N2 physisorption, and scanning electron microscopy with X-ray dispersive energy. The results of the photocatalytic degradation of 2,4,6-trichlorophenol in aqueous solution showed good photocatalytic activity, with an efficiency of degradation of up to 93% and mineralization of 82%; degradation values which are higher than that of TiO2-P25, which only reached 18% degradation. The degradation capacity is attributed to the structure of the MgO−MgFe2O4 oxides derived from double laminate hydroxide Mg/Fe. A path of degradation based on a mechanism of superoxide and hollow radicals is proposed.

Diffraction patterns of polyacrylic acid (PAA) encapsulated-(Fe)-modified ZnAl hydrotalcite (ZnAlH) showed the integration of Fe in the H lattice, resulting in a hybrid nanocomposite (Fe-PAA-ZnAlH), which was mainly verified with the characteristic shift in the 59–63° (2θ) region of the ZnAlH (110) reflection plane. The rise in the unit cell parameters (c and a) as the Fe % incremented, denoted incorporation of Fe in the ZnAlH red. Nonetheless, changes in the immobilizer molecular weight (PAA MW) from 1250 kDa to 5.1 kDa did not cause a difference in the distance between layers (c parameter) but in the cation-cation separation (a parameter), which meant that the nanoparticle was not located between layers, but in the lattice. The resulting band gap energies of the calcined hybrid nanocomposites were among 1.07–1.21 eV, which is an additional support of Fe+3 integration, suggesting insertion of Fe+3 3d orbitals between the valence and the conduction band of ZnO. Furthermore, nZVI were prepared through a pre-agglomeration reduction method, where COOH-groups were bound to metal cations. Initially, aqueous Fe+2 was bound to PAA [Fe+2-PAA], then reduced to obtain enclosed hybrid (nZVI-PAA). Less stability and more aggregation were observed with the lower molecular weight PAA. Additionally, PAA dissociation caused by pH changes affected the clustering of the nZVI particles. At higher MW, the hydrodynamic diameter and size distribution become smaller and tighter, respectively, allowing a more monodispersed population with sphere shape and organized in core–shell beads chains.