Since the two most commonly used methods for TiO₂ preparation are sol-gel (SG) and hydrothermal (HT) synthesis, this study attempts to compare both methods in order to determine which one is the most suitable to prepare photocatalysts for propene oxidation. In addition, this work studies how the concentration of the HCl used for hydrolysis of the TiO₂ precursor affects the properties of the obtained materials. Also, the effect of avoiding the post-synthesis heat-treatment in a selection of samples is investigated. The photocatalysts are characterized by XRD, N₂ adsorption-desorption isotherms and UV-vis spectroscopy, and the study tries to correlate the properties with the photocatalytic performance of the prepared TiO₂ samples in propene oxidation. TiO₂ materials with high crystallinity, between 67% and 81%, and surface area (up to 134 m²/g) have been obtained both by SG and HT methods. In general, the surface area and pore volume of the TiO₂-HT samples are larger than those of TiO₂-SG ones. The TiO₂-HT catalysts are, in general, more active than TiO₂-SG materials or P25 in the photo-oxidation of propene. The effect of HCl presence during the TiO₂ synthesis and of the post synthesis heat treatment are much more marked in the case of the SG materials.

The commercial P25 titania has been modified with transition metallic species (Cr, Co, Ni, and Cu), added by impregnation with aqueous solutions of the corresponding nitrates. The preparation procedure also includes a heat treatment (500 °C) in argon to decompose the nitrates, remove impurities and to strengthen the metal–TiO₂ interaction. The catalysts have been thoroughly characterized using N₂ adsorption, scanning electron microscopy (SEM), X-ray diffraction (XRD), UV-visible diffuse-reflectance spectroscopy (UV-vis DRS) and X-ray photoelectron spectroscopy (XPS), and have been tested in the aqueous phase decomposition of acetic acid and in the gas phase oxidation of propene, using an irradiation source of 365 nm in both cases. The photocatalytic activity of the four metal-containing catalysts varies with the nature of the metallic species and follows a similar trend in the two tested reactions. The effect of the nature of the added metallic species is mainly based on the electrochemical properties of the supported species, being Cu/P25 (the sample that contains copper) the best performing catalyst. In the photodecomposition of acetic acid, all the metal-containing samples are more active than bare P25, while in the gas phase oxidation of propene, bare P25 is more active. This has been explained considering that the rate-determining steps are different in gas and liquid media.

In the present manuscript, the preparation of spherical activated carbons (SACs) with suitable adsorption properties and high mechanical strength is reported, taking advantage of the retention of the spherical shape by the raw precursors. An easy procedure (carbonization followed by CO₂ activation) has been applied over a selection of three natural seeds, with a well-defined spherical shape and thermal stability: Rhamnus alaternus (RA), Osyris lanceolate (OL), and Canna indica (CI). After the carbonization-activation procedures, RA and CI, maintained their original spherical shapes and integrity, although a reduction in diameter around 48% and 25%, respectively, was observed. The porosity of the resulting SACs could be tuned as function of the activation temperature and time, leading to a spherical activated carbon with surface area up to 1600 m²/g and mechanical strength similar to those of commercial activated carbons.

The elimination of volatile organic compounds (VOCs) at low concentration is a subject of great interest because these compounds are very harmful for the environment and human health. In this work, we have developed a synthesis methodology of TiO₂ that allows obtaining meso-macroporous materials with hierarchical porosity and with high thermal stability for their application as photocatalysts in the removal of VOCs, specifically propene. The materials synthesized in this work were characterized by Scanning electron microscope (SEM), Transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Thermogravimetric Analysis (TG), and nitrogen adsorption. It is observed that the samples calcined at 250 °C and 500 °C present a high photoactivity for the photooxidation of propene, which is similar to the benchmark material P25 (commercial TiO₂). Moreover, the textural properties are better than those for P25, indicating that the samples are interesting for the preparation of photocatalysts with different conformations, such as in the form of coatings and fillings in different size scales.