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 N 2 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.