Three hydrocalumite-like compounds in a Ca/Al ratio of 2 containing nitrate and acetate anions in the interlaminar region were prepared by a simple, economic, and environmentally friendly method. The solids were characterized by X-ray powder diffraction (XRD), thermogravimetric (TG) analysis, nitrogen adsorption-desorption at −196°C, scanning electron microscopy (SEM), infrared spectroscopy (FTIR), and UV-Vis Diffuse Reflectance Spectroscopy (DRS). The catalytic activity of the calcined solids at 700°C was tested in the photodegradation of 2,4-dichlorophenoxyacetic acid (2,4-D) where 57% degradation of 2,4-D (40 ppm) and a mineralization percentage of 60% were accomplished within 150 minutes. The photocatalytic properties were attributed to mayenite hydration, since the oxide ions in the cages are capable of reacting with water to form hydroxide anions capable of breaking down the 2,4-D molecules.
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