Open Access
Hydrocalumite-TiO2 hybrid systems synthesized from aluminum salt cake for photodegradation of ibuprofen
(Elsevier, 2024) Rebollo, Beatriz; Jiménez, Alejandro; Trujillano, Raquel; Rives, Vicente; Gil Bravo, Antonio; Vicente, Miguel Ángel; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
Synthesis of hydrocalumite–TiO2 hybrid systems and their use in photodegradation of ibuprofen is reported for the first time. Hydrocalumite was prepared with Al3+ recovered from an aluminum slag (circular economy), TiO2 was deposited on hydrocalumite by hydrolysis of titanium(IV) isopropoxide, and the solids thus obtained were calcined at 400 and 750 ºC. The solid calcined at 400 ºC was essentially amorphous, showing the presence of calcite due to the fixation of atmospheric CO2, while the solid calcined at 750 ºC was composed of mayenite, perovskite and rutile. The calcined solids were used for catalytic degradation of ibuprofen (50 ppm in aqueous solutions) under UV irradiation, obtaining better results than when using commercial TiO2–P25 from Degussa. Under the specific conditions used, the degradation took place in the initial steps of the process, mainly giving rise to species with higher molecular mass than initial ibuprofen.
Open Access
Optimization of hydrocalumite preparation under microwave irradiation for recovering aluminium from a saline slag
(Elsevier, 2021) Jiménez, Alejandro; Misol, Alexander; Morato, Álvaro; Rives, Vicente; Vicente, Miguel Ángel; Gil Bravo, Antonio; Institute for Advanced Materials and Mathematics - INAMAT2
Aluminium was successfully extracted by treating an aluminium slag with aqueous NaOH under reflux conditions. This solution was purified by precipitation of silicon species by addition of HCl up to pH = 1, and used for preparing hydrocalumite (Ca2Al(OH)6Cl·2H2O) by the coprecipitation method. The effect of temperature on the properties of hydrocalumite prepared under microwave (MW) irradiation was studied. Characterization of the obtained solid was carried out by powder X-ray diffraction (PXRD), thermal analysis, FT–IR spectroscopy, chemical analysis, electron microscopy and N2 adsorption–desorption at −196 °C. The results showed that the use of the extracted aluminium solution allowed to obtain hydrocalumite by the coprecipitation method and that the temperature of the MW ageing treatment had a large effect on the formation of side phases, in addition to hydrocalumite. The results here reported demonstrate that formation of hydrocalumite is an effective method for the recovering of aluminium from its waste.
Embargo
Hydrocalumite and hydrocalumite-type compounds: a special type of layered double hydroxides
(Elsevier, 2025-04-01) Jiménez, Alejandro; Trujillano, Raquel; Gil Bravo, Antonio; Rives, Vicente; Vicente, Miguel Ángel; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
An exhaustive bibliographical review of one of the most peculiar Layered Double Hydroxides, LDH, namely hydrocalumite and hydrocalumite-type compounds, has been carried out. The main differences that make hydrocalumite a special and interesting LDH are described, as well as the main methods of synthesis. A comprehensive comparison is also made with respect to MgAl/carbonate hydrotalcite with a Mg/Al molar ratio of 2. Thermal behavior of hydrocalumite is also different than that of other LDH, leading to the formation of attractive Mixed Metallic Oxides, MMO. Thus, the applications of hydrocalumite, hydrocalumite-type compounds and the derived MMO in environmental remediation and heterogeneous catalysis and photocatalysis are presented. Hydrocalumite, contrary to hydrotalcite, is not currently commercialized on an industrial scale, probably because its preparation is more complicated. Considering the excellent properties of hydrocalumite and the price, abundance and biocompatibility of its components, the scaling of its production should be a key challenge to take advantage in its industrial application.
Embargo
Photodegradation of paracetamol on CaAlGa and ZnAlTi mixed metal oxides (MMO) synthesized via LDH from Al-saline slags
(Elsevier, 2025-04-01) Jiménez, Alejandro; Guerra, Miguel; Pascual, Dana; Trujillano, Raquel; Rives, Vicente; Vicente, Miguel Ángel; Gil Bravo, Antonio; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
Preparation of CaAlGa and ZnAlTi mixed metal oxides (MMO) synthesized via CaAlGa–hydrocalumites and ZnAl–hydrotalcite impregnated with TiO2 using saline slags as aluminum source, is reported for the first time. The solids obtained by calcination at 750 ºC are highly crystalline and the photocatalytically active crystalline phases Ca12Al14-xGaxO33, ZnO, ZnAl2O4 and Zn2TiO4 have been identified. The MMO were used for the catalytic degradation of paracetamol under UV irradiation, obtaining good results for the removal of this emerging pollutant, reaching a removal above 90 % for the sample containing 25 % Ga3 +, under the optimum photodegradation conditions ([Paracetamol]0 = 40 mg/L and catalyst dose = 1 g/L), showing better results than the commercial photocatalyst TiO2–P25 from Degussa and other more complex catalysts based on MMO. In addition, this photocatalyst was submitted to a cyclic process study, finding that it maintained its performance after at least two cycles.
Open Access
Preparation of Ca2Al1–mFem(OH)6Cl 2H2O-doped hydrocalumites and application of their derived mixed oxides in the photodegradation of ibuprofen
(MDPI, 2022) Jiménez, Alejandro; Valverde, Marta; Misol, Alexander; Trujillano, Raquel; Gil Bravo, Antonio; Vicente, Miguel Ángel; Institute for Advanced Materials and Mathematics - INAMAT2
Aluminum from saline slags generated during the recycling of this metal, extracted under reflux conditions with aqueous NaOH, was used in the synthesis of hydrocalumite-type solids with the formula Ca2Al1–mFem(OH)6Cl 2H2O. The characterization of the obtained solids was carried out by powder X-ray diffraction, infrared spectroscopy, thermal analysis, element chemical analysis, N2 adsorption-desorption at -196ºC and electron microscopy. The results showed the formation of Layered Double Hydroxide-type compounds whose characteristics varied as the amount of incorporated Fe3+ increased. These solids were calcined at 400ºC and evaluated for the catalytic photodegradation of ibuprofen, showing promising results in the elimination of this drug by advanced oxidation processes. The CaAl photocatalyst (without Fe) showed the best performance under UV light for the photodegradation of ibuprofen.