The application of niobium oxides as photocatalytic materials for the removal of contaminants is scarcely reported in the literature. This work reports the methodology to synthesize four different mesoporous niobium oxide materials and the correlation between the physicochemical properties and the photocatalytic activity. X‐ray diffraction, UV–vis diffuse reflectance spectra (DRS), transmission electron microscopy, and nitrogen adsorption techniques are used to characterize the structure and composition of the obtained materials. The photocatalytic oxidation of methanol is used as reaction test to assess the photocatalytic activities and photonic efficiencies of the materials as a function of the catalyst concentration. Nb
2
O
5
materials display lower reaction rates, which can be attributed to the relatively high average particle size. By contrast, NaNbO
3
materials show higher activity, especially for high catalyst loading. No significant differences in absorption and scattering of light are observed among the materials, indicating that the higher photonic efficiency of NaNbO
3
should be the result of a lower charge recombination derived from its microstructure, sodium composition, low particle size, and high specific surface area of these materials.
The TiO<sub>2</sub>/MCM-41 nanomaterials were synthesized by impregnation with an excess solvent with different percentages of titanium dioxide. They were used for catalytic degradation of Benzene Toluene Ethylbenzene and Xylenes (BTEX) in the presence of hydrogen peroxide in aqueous media. The obtained materials were characterized by X-ray Diffraction, nitrogen adsorption-desorption using the BET method and Fourier Transform Infrared Spectroscopy. The nanostructured phase of the hexagonal ordered materials was obtained even after modification with titanium oxide and calcination. The characterizations have proven the effectiveness of the synthesis method used to incorporate titanium with anatase structure impregnated in the nanoporous of the MCM-41 material. Anatase is the main active phase of TiO<sub>2</sub> to oxidize organic compounds. The catalytic evaluation wascarried out in a semi-bath reactor with 20 mL of a mixture containing BTEX (100 mg/L), hydrogen peroxide (2.0 mol/L) and TiO<sub>2</sub>/MCM-41 (2.0 g/L) in aqueous media. The reactions were carried out at a temperature of 60°C for 5 hours, and the analyses were performed by gas chromatography with a photoionization detector and headspace sampler. The catalytic tests showed satisfactory results with more than 95% of conversion, where the catalyst 48%TiO<sub>2</sub>/MCM-41 presented higher performance.
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