Open Access
Effect of the surface properties of Me2+/Al layered double hydroxides synthesized from aluminum saline slag wastes on the adsorption removal of drugs
(Elsevier, 2020) Santamaría Arana, Leticia; Devred, F.; Gaigneaux, E. M.; Korili, Sophia A.; Gil Bravo, Antonio; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa; Gobierno de Navarra / Nafarroako Gobernua, PI017-PI039 CORRAL
This work presents the synthesis of Me2+ (Co, Mg, Ni and Zn)/Al layered double hydroxides (LDH) with a 3:1 M ratio by the co-precipitation method. Structural characterization and comparison of the series has been achieved using powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), nitrogen physisorption at 77 K, thermogravimetry measurements (TGA), temperature-programmed reduction (TPR), X-ray photoelectron spectroscopy (XPS), ammonia temperature-programmed desorption (NH3-TPD) and point of zero charge (pHpzc). Batch experiments were performed to analyze the adsorption capacity of the different LDH on diclofenac and salicylic acid, as example of emergent pollutants. The pH, mass of adsorbent, contact time and concentration of pollutant were the parameters used to compare the adsorption performance of the synthesized materials. Samples showed different behavior and the equilibrium was reached at different times, Mg6Al2 and Zn6Al2 showed lower equilibrium times but had higher adsorption capacity. Various adsorption and isotherm equation models were employed to study both the kinetic and equilibrium results and, in general, the removal of diclofenac was greater than that of salicylic acid. 1-Butanol conversion was also used as a means of acidity and basicity characterization and the results were compared with the adsorption performance of the samples in order to explain the results found. A relationship between the amount of pollutants adsorbed and the butenes formed in the dehydrogenation reaction of 1-butanol was found.
Open Access
M(II)-Al-Fe layered double hydroxides synthesized from aluminum saline slag wastes and catalytic performance on cyclooctene oxidation
(Elsevier, 2022) Santamaría Arana, Leticia; Oliveira-Garcia, L.; Faria, Emerson H. de; Ciuffi, Katia J.; Vicente, Miguel Ángel; Korili, Sophia A.; Gil Bravo, Antonio; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
Aluminum was extracted from saline slags via an alkaline method and employed in the synthesis of Layered Double Hydroxides (LDH) with various M2+ cations (Co, Mg, Ni and Zn), while Al and Fe were the M3+ cations, using the co-precipitation method and a M2+/M3+ 2:1 ratio. The structural characterization of the samples was performed with powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), nitrogen physisorption at 77 K, thermogravimetric analysis (TGA), temperature-programmed reduction (TPR) and X-ray photoelectron spectroscopy (XPS). Their catalytic performance was tested for the oxidation of olefins (cyclooctene) and their biomimetic potential was analyzed. Results show a great selectivity towards epoxides with no other products obtained. Reaction yields followed the descending order Co4AlFe, Zn4AlFe, Ni4AlFe, and Mg4AlFe, the sample with cobalt as M2+ converting up to 85% of cyclooctene.
Open Access
Evidence for the synthesis of La-hexaaluminate from aluminum-containing saline slag wastes: correction of structural defects and phase purification at low temperature
(Elsevier, 2021) Torrez Herrera, Jonathan Josué; Fuentes Ordóñez, Edwin Gustavo; Korili, Sophia A.; Gil Bravo, Antonio; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
The synthesis of a lanthanum hexaaluminate from the aluminum extracted from a saline slag waste is presented for the first time. Briefly, a refluxing 2 M solution of HCl is used to extract the aluminum, giving 8.9 gAl/dm3 along with other metals in lower concentrations. This solution is used to synthesize the hexaaluminate by mixing with a stoichiometric amount of lanthanum nitrate. The results showed the formation of pure phase hexaaluminate at 1473 K, as well as predominance of the hexaaluminate phase at temperatures of 1273 and 1373 K. These results also indicate that the pure hexaaluminate phase can be obtained at a much lower temperature than when commercial aluminum solutions are used improving the applications as catalyst and thermal barrier material. It was also found that the presence of other metals in solution allows the structural problems and purity of the La-hexaaluminate phase to be corrected when working with stoichiometric ratios.
Open Access
Zn-Ti-Al layered double hydroxides synthesized from aluminum saline slag wastes as efficient drug adsorbents
(Elsevier, 2020) Santamaría Arana, Leticia; López Aizpún, María; García Padial, Marcos; Vicente, Miguel Ángel; Korili, Sophia A.; Gil Bravo, Antonio; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias; Gobierno de Navarra / Nafarroako Gobernua, PI017-PI039 CORRAL; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa
This work reports the synthesis of Zinc-Titanium-Aluminum (ZnTiAl) layered double hydroxides (LDH) with various proportions of Al[sbnd]Ti and a Zn/(Al[sbnd]Ti) molar ratio of 3:1 by the co-precipitation method. Two series, made with commercial aluminum (Al) and aluminum extracted from saline slags (Al*), have been considered. Structural characterization and comparison of the two series has been made using powder X-ray diffraction (PXRD), Nitrogen physisorption at 77 K, Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and Thermogravimetry measurements. The adsorption capacity of diclofenac and salicylic acid, as examples of emergent pollutants, by the different LDH on batch and fixed-bed column experiments has been analyzed. The effect of various parameters, such as the pH, the initial concentration of pollutant, the mass of adsorbent and the contact time, on the sorption behavior were studied and compared. The contact time to attain equilibrium for maximum adsorption was found to be between 100 and 400 min. The kinetic and equilibrium results were correlated to several adsorption and isotherm equation models. The synthesized materials were more effective in removing diclofenac than salicylic acid, being Zn6Al*2 the hydrotalcite that showed the highest adsorption capacity. The results showed a new application of a material obtained from the valorization of an industrial waste such as aluminum saline slags.

Korili, Sophia A.

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