Various W and Mo co-doped titanium dioxide (TiO₂) materials were obtained through the EISA (Evaporation-Induced Self-Assembly) method and then tested as photocatalysts in the degradation of 4-chlorophenol. The synthesized materials were characterized by thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Raman spectroscopy (RS), N₂ physisorption, UV-vis diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The results showed that the W-Mo-TiO₂ catalysts have a high surface area of about 191 m²/g, and the presence of an anatase crystalline phase. The co-doped materials exhibited smaller crystallite sizes than those with one dopant, since the crystallinity is inhibited by the presence of both species. In addition, tungsten and molybdenum dopants are distributed and are incorporated into the anatase structure of TiO₂, due to changes in red parameters and lattice expansion. Under our experimental conditions, the co-doped TiO₂ catalyst presented 46% more 4-chlorophenol degradation than Degussa P25. The incorporation of two dopant cations in titania improved its photocatalytic performance, which was attributed to a cooperative effect by decreasing the recombination of photogenerated charges, high radiation absorption capacity, high surface areas, and low crystallinity. When TiO₂ is co-doped with the same amount of both cations (1 wt.%), the highest degradation and mineralization (97% and 74%, respectively) is achieved. Quinones were the main intermediates in the 4-chlorophenol oxidation by W-Mo-TiO₂ and 1,2,4-benzenetriol was incompletely degraded.

In the present study, glycerol was oxidized by photocatalysis to glyceraldehyde, formaldehyde, and formic acid. Copper-doped TiO₂ was synthesized by the evaporation-induced self-assembly approach and it was used as catalyst during the glycerol photo-oxidation reactions. The prepared mesoporous material exhibited high specific surface area (242 m²/g) and band gap energy reduction of 2.55 eV compared to pure titania (3.2 eV) by the synthesis method due to the presence of copper cations (Cu²⁺ identified by XPS). The catalyst showed only anatase crystalline phase with nanocrystals around 8 nm and irregular agglomerates below 100 μm. The selectivity and formation rate of the products were favored towards formaldehyde and glyceraldehyde. The variables studied were catalyst amount, reaction temperature, and initial glycerol concentration. The response surface analysis was used to evaluate the effect of the variables on the product’s concentration. The optimized conditions were 0.4 g/L catalyst, 0.1 mol/L glycerol, and temperature 313.15 K. The response values under optimal conditions were 3.23, 8.17, and 1.15 mM for glyceraldehyde, formaldehyde, and formic acid, respectively. A higher selectivity towards formaldehyde was observed when visible light was used as the radiation source. This study is useful to evaluate the best reaction conditions towards value-added products during the oxidation of glycerol by photocatalysis using Cu/TiO₂.