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A gallery of hydrotalcite-type mesoporous materials with different Mg/Al molar ratios were synthesized by the coprecipitation method. The materials were activated by heat treatment to test their activity in the photodegradation of 2,4,6-trichlorophenol under UV light irradiation. The physicochemical properties of the different synthesized and activated materials were determined using XRD, physical adsorption/desorption of N2, FTIR, SEM, DTA, and TGA. Their banned band energy was determined by UV-Vis to identify their potential to be used as a semiconductor in catalytic photodegradation processes. The results of photodegradation tests of 2,4,6-trichlorophenol showed that hydrotalcites have a high degradation capacity, up to 100% for the catalyst of Mg/Al ratio = 2, with a high mineralization capacity of 80%. The degradation capacity of most of the catalysts tested is mainly due to the presence of holes and the formation of superoxide free radicals, which are the determining species within the degradation mechanism.

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.

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