Sol-gel and Pechini niobium modified: synthesis, characterization and application in the 2,4-D herbicide degradation.

In this work, a comparison was made between the synthesis of niobium-based materials (Nb2O5), both in terms of material characterization and catalytic performance. The methods used were chemical mixtures: modified sol-gel and Pechini. The materials were calcined at different temperatures (753, 873 and 993K) and characterized by the following techniques: photoacousticspectroscopy (PAS), zero charge point (pHPZC), scanning electron microscopy (SEM/EDS), thermogravimetric analysis (TGA/DTG) and X-ray diffraction (XRD). The photocatalytic process was carried out to evaluate the degradation of 2,4-dichlorophenoxyacetic acid (2,4-D) under UV radiation (250 W mercury vapor lamp) and different experimental conditions. In addition, to better understand the influence of parameters such as pH, catalyst concentration (0.2, 0.5 and 0.8 g L-1) and calcination temperature, a Design of Experiments (DoE) was used. The results indicated that despite having similar structures and phases in the XRD analysis, the morphology presents two distinct surfaces, due to the preparation method. Differences in the synthesis method affected the catalytic activity in the parameters studied. Although the zero charge point values are close (6.18-6.36), we observed differences in the band gap depending on the calcination temperature. In the optimal condition studied, the catalyst prepared by the sol-gel method obtained the best results.

Cu/Nb2O5, Fe/Nb2O5 and Cu-Fe/Nb2O5 applied in salicylic acid degradation: Parameters studies and photocatalytic activity.

This study describes the synthesis of Cu/Nb2O5, Fe/Nb2O5, and Cu-Fe/Nb2O5 catalysts obtained by incorporating copper and/or iron metals into niobium pentoxide (Nb2O5). The new materials were characterized by the following techniques: Thermogravimetric Analysis (TA), surface and pore analysis, X-ray diffractometry (XRD), and Fourier Transform Infrared Spectroscopy (FT-IR). The catalyst was applied in the photocatalytic degradation of salicylic acid (SA). The influence of different parameters (calcined temperature, pH, and metal addition) on the photocatalytic reaction was evaluated. The results indicated that catalysts containing copper were more active and pH influenced the SA degradation process. SA removal results indicated that Cu/Nb2O5 photocatalyst presented a 1.5 fold higher degradation after 120 min in comparison to Cu-Fe/Nb2O5 and 4.6 fold higher than Fe/Nb2O5 catalyst, all them calcined at 400 °C. In tests carried out in the presence of formic acid, increasing the pH from about 3 to 7 allowed an almost 3.4-fold increase in SA degradation for the Cu-Fe/Nb2O5 catalyst calcined at 400 °C.