Photocatalysis is an effective advanced oxidation process to mineralize recalcitrant contaminants in aqueous media. TiO₂ is the most used photocatalyst in this type of process. To improve the deficiencies of this material, one of the most used strategies has been to dope TiO₂ with metallic ions. Chemical reagents are often used as dopant precursors. However, due to the depletion of natural resources, in this work it was proposed to substitute chemical reagents and instead use a metallic residue (door key) as a doping precursor. The materials were synthesized using the sol–gel method and calcined at 400 °C to obtain the crystal structure of anatase. The characterization of the materials was carried out using X-ray diffraction (XRD), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS), scanning electron microscopy–energy-dispersive X-ray analysis (SEM-EDX) methods X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma optical emission spectroscopy (ICP-OES). The results obtained indicate that Cu⁺/Cu²⁺ and Zn²⁺ ions coexist in the support, which modifies the physicochemical properties of TiO₂ and improves its photocatalytic efficiency. The synergistic effect of the dopants in TiO₂ allowed the mineralization of diclofenac in an aqueous medium when T-DK (1.0) was used as photocatalyst and simulated solar radiation as an activation source.

In recent past development of silver nanoparticles and their application in the treatment of wastewaters is becoming a major area of research. It is mainly applicable to the removal of three major pollutants like pesticides, heavy metals, and microorganisms. Variety of synthesis techniques have been reported for preparation and characterization of silver nanoparticles. In our research, we synthesized Ag nanoparticles supported on ZrO2 and ZrO2-CeO2 by a “deposit-precipitation method” as the first step and later sequentially synthesized Ag-Au supported on ZrO2 and ZrO2-CeO2 by Redox method. Catalysts were evaluated in catalytic wet air oxidation (CWAO) of methyl tert-butyl ether and phenol. The CWAO is a liquid phase process for the treatment of organic pollutants operating at temperatures in the range of 100–325°C at 5–200 bar pressures. The selectivity and efficient of catalysts were evaluated by total organic carbon (TOC) and high-performance liquid chromatograph (HPLC). Ideally, the total mineralization of pollutants into CO2 and H2O is preferred.

5-Hydroxymethylfurfural (5-HMF) has been described as one of the 12 key platform molecules derived from biomass by the US Department of Energy, and its hydrogenation reaction produces versatile liquid biofuels such as 2,5-dimethylfuran (2,5-DMF). Catalytic hydrogenation from 5-HMF to 2,5-DMF was thoroughly studied on the metal nickel catalysts supported on Al₂O₃-TiO₂-ZrO₂ (Ni/ATZ) mixed oxides using isopropanol and formic acid (FA) as hydrogen donors to find the best conditions of the reaction and hydrogen donor. The influence of metal content (wt%), Ni particle size (nm), Nickel Ni⁰, Ni⁰/NiO and NiO species, metal active sites and acid-based sites on the catalyst surface, and the effect of the hydrogen donor (isopropanol and formic acid) were systematically studied. The structural characteristics of the materials were studied using different physicochemical methods, including N₂ physisorption, XRD, Raman, DRS UV-Vis, FT-IR, SEM, FT-IR Py_ad, H₂-TPD, CO₂-TPD, H₂-TPR, TEM and XPS. Second-generation 2,5-DMF biofuel and 5-HMF conversion by-products were analyzed and elucidated using ¹H NMR. It was found that the Ni⁰NiO/ATZ3_WI catalyst synthesized by the impregnation method (WI) generated a good synergistic effect between the species, showing the best catalytic hydrogenation of 5-HMF to 2,5-DMF using formic acid as a hydrogen donor for 24 h of reaction and temperature of 210 °C with 20 bar pressure of Argon (Ar).

γ-Valerolactone (GVL) has been considered an alternative as biofuel in the production of carbon-based chemicals; however, the use of noble metals and corrosive solvents has been a problem. In this work, Ni supported nanocatalysts were prepared to produce γ-Valerolactone from levulinic acid using methanol as solvent at a temperature of 170 °C utilizing 4 MPa of H₂. Supports were modified at pH 3 using acetic acid (CH₃COOH) and pH 9 using ammonium hydroxide (NH₄OH) with different tungsten (W) loadings (1%, 3%, and 5%) by the Sol-gel method. Ni was deposited by the suspension impregnation method. The catalysts were characterized by various techniques including XRD, N₂ physisorption, UV-Vis, SEM, TEM, XPS, H₂-TPR, and Pyridine FTIR. Based on the study of acidity and activity relation, Ni dispersion due to the Lewis acid sites contributed by W at pH 9, producing nanoparticles smaller than 10 nm of Ni, and could be responsible for the high esterification activity of levulinic acid (LA) to Methyl levulinate being more selective to catalytic hydrogenation. Products and by-products were analyzed by ¹H NMR. Optimum catalytic activity was obtained with 5% W at pH 9, with 80% yield after 24 h of reaction. The higher catalytic activity was attributed to the particle size and the amount of Lewis acid sites generated by modifying the pH of synthesis and the amount of W in the support due to the spillover effect.

Three bimetallic catalysts of the type M–Cu with M = Ag, Au and Ni supports were successfully prepared by a two-step synthesized method using Cu/Al₂O₃-CeO₂ as the base monometallic catalyst. The nanocatalysts were characterized using X-ray diffraction (XRD), temperature-programmed reduction of H₂ (H₂-TPR), N₂ adsorption-desorption, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and ultraviolet–visible spectroscopy with diffuse reflectance (DR-UV-Vis) techniques. This synthesized methodology allowed a close interaction between two metals on the support surface; therefore, it could have synthesized an efficient transition–noble mixture bimetallic nanostructure. Alloy formation through bimetallic nanoparticles (BNPs) of AgCuAlCe and AuCuAlCe was demonstrated by DR–UV–Vis, EDS, TEM and H₂-TPR. Furthermore, in the case of AgCuAlCe and AuCuAlCe, improvements were observed in their reducibility, in contrast to NiCuAlCe. The addition of a noble metal over the monometallic copper-based catalyst drastically improved the phenol mineralization. The higher activity and selectivity to CO₂ of the bimetallic gold–copper- and silver–copper-supported catalysts can be attributed to the alloy compound formation and the synergetic effect of the M–Cu interaction. Petroleum Refinery Wastewater (PRW) had a complex composition that affected the applied single CWAO treatment, rendering it inefficient.

NiWAu trimetallic nanoparticles (NPs) on the surface of support Al₂O₃-CeO₂-TiO₂ were synthesized by a three-step synthetic method in which Au NPs were incorporated into presynthesized NiW/Al₂O₃-CeO₂-TiO₂. The recharge method, also known as the redox method, was used to add 2.5 wt% gold. The Al₂O₃-CeO₂-TiO₂ support was made by a sol–gel method with two different compositions, and then two metals were simultaneously loaded (5 wt% nickel and 2.5 wt% tungsten) by two different methods, incipient wet impregnation and ultrasound impregnation method. In this paper, we study the effect of Au addition using the recharge method on NiW nanomaterials supported on mixed oxides on the physicochemical properties of synthesized nanomaterials. The prepared nanomaterials were characterized by scanning electron microscopy, BET specific surface area, X-ray diffraction, diffuse reflectance spectroscopy in the UV–visible range and temperature-programmed desorption of hydrogen. The experimental results showed that after loading of gold, the dispersion was higher (46% and 50%) with the trimetallic nanomaterials synthesized by incipient wet impregnation plus recharge method than with impregnation plus ultrasound recharge method, indicating a greater number of active trimetallic (NiWAu) sites in these materials. Small-sized Au from NiWAu/ACTU1 trimetallic nanostructures was enlarged for NiWAu/ACT1. The strong metal NPs–support interaction shown for the formation of NiAl₂O₄, Ni-W-O and Ni-Au-O species simultaneously present in the surface of trimetallic nanomaterial probably plays an important role in the degree of dispersion of the gold active phase.