This study reports the green synthesis of activated carbon (ANC) from Cocoa Pod Husk (CPH), a lignocellulosic agrowaste, using sulphuric acid and sodium hydroxide treatments for Methylene Blue (MB) removal. Among the synthesised samples, ANCSH5 (NaOH, 5 M) exhibited superior performance due to extensive delignification, enhanced graphitization, and an abundance of oxygenated functionalities, as confirmed by Fourier Transform Infrared (FTIR), Scanning Electron Microscopy – Energy Dispersive X-ray (SEM–EDX), the Brunauer–Emmett–Teller Method (BET), X-ray Diffraction (XRD), Point of Zero Charge (pH_PZC), and Raman analyses. ANCSH5 achieved 92% MB removal (1.16 mg g⁻¹), surpassing CPH (24%, 0.30 mg g⁻¹) and ANCSA10 (44%, 0.50 mg g⁻¹). Adsorption followed pseudo-second-order kinetics, while equilibrium data fitted best to the Freundlich, Sips, Toth, and Redlich–Peterson models (R² > 0.999). Process optimisation via a central composite design (CCD) and Response Surface Methodology (RSM) determined optimal conditions (49.6 °C, pH 6.0), achieving a 99.05% removal rate. Importantly, isotherm modelling predicted a competitive q_max of 100 mg g⁻¹ for ANCSH5 under practical conditions. Unlike conventional biomass carbons, the hemicellulose-rich CPH precursor promoted extensive delignification, partially graphitised domains, and tailored surface chemistry, providing a distinctive adsorption mechanism. These features underscore CPH valorisation as a sustainable route to high-performance, low-cost adsorbents for dye remediation in cocoa-producing regions.

The Cocoa Pod Husk (CPH) accounts for 67–76% of the total cocoa fruit weight, making it its main agro-industrial waste of cocoa production. A valorization of this waste is possible through the extraction of pectin. In this study, pectin was extracted from CPH powder by acid hydrolysis using citric acid and sulfuric acid. Fourier transform infrared spectroscopy (FT-IR) was employed as a qualitative and quantitative characterization technique. The FT-IR of the pectin samples showed the bands visible at 1732 and 1626 cm⁻¹ corresponding to the esterified and free carboxylic groups, respectively. These bands can be differentiated according to their degree of methyl esterification (DE) by analyzing the area under the curve. The extracted pectin showed no significant difference in yields (p ≤ 0.05) between the two acids; however, significant differences (p ≤ 0.05) were observed in DE and methoxylation percentage (MeO). According to the FT-IR results, pectin extracted with citric acid presented a lower DE (7.43%) and MeO (1.12%) compared to pectin extracted with sulfuric acid, which showed a DE of 18.15% and a 2.96% MeO. Pectin with a DE below 50% is classified as low-methylated, making it unsuitable for the food industry. However, these create a raw material that has a potential use in the pharmaceutical and bioenergy industries.

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).

This paper studies Cu/Al₂O₃ catalysts, synthesized in two ways: copper deposit in the synthesis of alumina (sol gel) and incipient impregnation stabilized at 400 °C. The materials were characterized by X‐ray diffraction studies, nitrogen physisorption, temperature programmed reduction of H₂, dehydration of isopropanol, scanning electronic microscopy, transmission electronic microscopy, which were evaluated in the liquid phase oxidation reaction of ethyl tert‐butyl ether and tert‐amyl methyl ether. The formation of CuAl₂O₄ and CuAlO₂ in the samples synthesized by sol gel, led to a modification of the texture, thus resulting in an expansion of the specific area of the materials. CuAl₂O₄ and CuAlO₂ have been identified by DRX from a content of 10 % Copper, the first showed the highest intensity with this technique. In the same way, these species favor the presence of Lewis acid sites; this is reflected in the materials with (Di‐isopropyl Ether) DIPE of 96.7 % and 91.1 % for the samples SAlCu5 and SAlCu15 respectively. The catalytic activity of the materials prepared by sol gel is in the function of the number of surface acid sites, the smaller particle size of the Cu and the surface of the contact, in the case of the ETBE meanwhile for TAME the activity was based mainly on the strength of the present acid sites. With impregnated materials, the activity is attributed to the smaller particle size of the Cu and the greater strength of the surface acid sites in the solid. The formation of spinel species inhibits the leaching phenomenon in the reaction milieu.

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.