Person: Cabañas Poveda, Albertina
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First Name
Albertina
Last Name
Cabañas Poveda
Affiliation
Universidad Complutense de Madrid
Faculty / Institute
Ciencias Químicas
Department
Química Física
Area
Química Física
Identifiers
12 results
Search Results
Now showing 1 - 10 of 12
Item Solubility of the metal precursor Ni(NO3)2⋅6H2O in high-pressure CO2 + ethanol mixtures(Journal of Chemical & Engineering Data, 2017) Tenorio, María José; Ginés, Sonia; Pando García-Pumarino, Concepción; Rodríguez Renuncio, José Antonio; Cabañas Poveda, AlbertinaThe solubility of Ni(NO3)2⋅6H2O in high-pressure CO2 + ethanol mixtures was measured using a high-pressure variable-volume view cell from (308.2 to 353.2 K) and up to 25.0 MPa. This compound has been used previously as a Ni precursor in metal deposition experiments using supercritical CO2. Ni(NO3)2•6H2O was not soluble in pure CO2 but the addition of ethanol into the system allowed the solubilisation of the hydrated salt in the mixture. Mole fraction of Ni(NO3)2•6H2O varied from 1.67 10-4 to 1.97 10-3. At these salt concentrations, the phase diagram of the CO2 + EtOH + Ni(NO3)2⋅6H2O system resembled that of the CO2 + EtOH binary system and, at the studied conditions, a vapourliquid equilibrium was observed. For the higher ethanol concentrations, the bubble points closely matched those of the CO2 + EtOH system. For the lower EtOH concentrations, however, much higher solubilisation pressures were required, due to the release of water molecules from the salt into the solution. Ni(NO3)2⋅6H2O solutions were stable in highpressure CO2 + EtOH mixtures at the studied conditions.Item One-step Sustainable Preparation of Superparamagnetic Iron Oxide Nanoparticles Supported on Mesoporous SiO2(Journal of Supercritical Fluids, 2020) Chamorro, Elena; Granados García Tenorio, María José; Calvo Garrido, María Lourdes; Torralvo Fernández, María Josefa; Sáez Puche, Regino; Cabañas Poveda, AlbertinaSuperparamagnetic iron oxide nanoparticles (SPIONs) supported on high surface area mesoporous SiO2 are advanced materials of great interest in catalysis, adsorption and biomedicine. Here we present a new process to prepare SPION/SiO2 materials by the impregnation and insitu decomposition of Fe(NO3)3.9H2O on mesoporous SiO2 supports in a 25-50% mol ethanol + CO2 mixture at 523 K and 25.0 MPa. -Fe2O3 nanoparticles (NPs) of average size between 6-9 nm were distributed homogeneously on the supports. NPs deposited into the SBA-15 mesopores but mostly on the external surface of MCM-41. Materials prepared with the highest ethanol content were very homogeneous. Magnetic measurements confirmed the superparamagnetic nature of the materials at room temperature. The process proposed is sustainable and scalable, avoids tedious preparations and the additional high temperature treatment under a controlled atmosphere, as the metal decomposition is performed insitu in the CO2-expanded liquid mixture.Item Designing nanocomposites using supercritical CO2 to insert Ni nanoparticles into the pores of nanopatterned BaTiO3 thin films(Journal of Materials Chemistry C, 2016) Castro, Alichandra; Morère, Jacobo; Cabañas Poveda, Albertina; Ferreira, Liliana; Godinho, Margarita; Ferreira, Paula; Vilarinho, PaulaA new concept to prepare nanocomposite thin films is explored. Two chemical-based bottom-up steps are used to design functional films including: i) block copolymerassisted self-assembly of a porous matrix; and ii) impregnation of nanoparticles from a ferroic phase within the pores by supercritical CO2 deposition. Porous nanopatterned BaTiO3 thin films with ca. 17 nm of thickness are prepared using a cost-effective solgel solution containing a block copolymer and evaporation-induced self-assembly methodology. Hexagonal-arranged pores with diameter of ca. 95 nm, running perpendicularly to the substrate are filled with Ni nanoparticles using the supercritical fluid deposition technique from reduction of hydrated nickel nitrate in a supercritical CO2-ethanol mixture at 250 ºC. Small Ni nanoparticles with 21 ± 5 nm nm are selectively deposited inside the pores of the porous matrix. Structural and magnetic properties prove the coexistence of both phases.Item Polymorphism in the co-crystallization of the anticonvulsant drug carbamazepine and saccharin using supercritical CO2 as an anti-solvent(The Journal of Supercritical Fluids, 2018) Cuadra Mendoza, Isaac Alfonso; Cabañas Poveda, Albertina; Rodríguez Cheda, José Antonio; Pando García-Pumarino, Concepción1:1 Co-crystals of carbamazepine (CBZ) and saccharin (SAC) were obtained for the first time through the supercritical anti-solvent (SAS) technique based on using supercritical CO2 as anti-solvent. The capability of SAS to produce the desired polymorphic form (two polymorphs are known) was assessed. Operational conditions investigated were temperature (40.0 and 60.0 °C), pressure (10.0 and 15.0 MPa), solvent choice and coformer concentration in the organic solution (CBZ: 30 and 15 mg/mL; SAC: stoichiometric ratio). Co-crystals were characterized in terms of crystallinity and coformers interactions. No homocrystals were present. Using methanol, at 40.0 °C polymorph I was obtained with yields up to 65%; whilst at 60.0 °C a mixture of polymorphs was obtained. Mixtures of polymorphs were also obtained in the ethanol and dichloromethane experiments at the studied conditions while the dimethylsulfoxide experiments failed to produce any co-crystal polymorph. For comparison purposes, pure CBZ and SAC were also processed by SAS.Item Deposition of Ni nanoparticles onto porous supports using supercritical CO2: effect of the precursor and reduction methodology(Philosophical Transactions A, 2015) Morère, Jacobo; Royuela, Sergio; Asensio, Guillermo; Enciso Rodríguez, Eduardo; Pando García-Pumarino, Concepción; Cabañas Poveda, AlbertinaThe deposition of Ni nanoparticles into porous supports is very important in catalysis. In this paper, we explore the use of supercritical CO2 (scCO2) as a green solvent to deposit Ni nanoparticles on mesoporous SiO2 SBA-15 and a carbon xerogel. The good transport properties of scCO2 allowed the efficient penetration of metal precursors dissolved in scCO2 within the pores of the support without damaging its structure. Nickel hexafluoroacetylacetonate hydrate, nickel acetylacetonate, bis(cyclopentadienyl)nickel, Ni(NO3)2⋅6H2O and NiCl2⋅6H2O were tried as precursors. Different methodologies were used: impregnation in scCO2 and reduction in H2/N2 at 400°C and low pressure, reactive deposition using H2 at 200–250°C in scCO2 and reactive deposition using ethanol at 150–200°C in scCO2. The effect of precursor and methodology on the nickel particle size and the material homogeneity (on the different substrates) was analysed. This technology offers many opportunities in the preparation of metal-nanostructured materials.Item Production and Characterization of a new Copper(II) Propanoate-Isonicotinamide Adduct obtained via Slow Evaporation and using Supercritical CO2 as an Antisolvent(Crystal Growth and Design, 2019) Cuadra Mendoza, Isaac Alfonso; Martínez Casado, Francisco Javier; Rodriguez Cheda, Jose A.; Redondo, M.I.; Pando García-Pumarino, Concepción; Cabañas Poveda, AlbertinaA new adduct of isonicotinamide (INA) with copper(II) propanoate [Cu(C3)2] was prepared [Cu2(C3)4(INA)4] using two different methods. This type of compound shows high fungicidal activity. Solvent evaporation from ethanol rendered crystals suitable for single-crystal X-ray diffraction. Furthermore, a new semicontinuous method capable of simultaneous crystallization and micronization of the adduct using supercritical CO2, the supercritical antisolvent technique (SAS), was also assessed. Crystals were characterized using powder X-ray diffraction, infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis coupled with mass spectrometry, scanning electron microscopy, and microelemental analysis. In the adduct, two copper(II) ions are coordinated through two bridging and two chelating carboxylates to the propanoate anions forming approximately a plane. Each metal ion is then coordinated with the pyridine nitrogen of two different INA molecules that behave as monodentate ligands. The amide groups of the INA form H-bonds with other amide and carboxylate groups forming a molecular crystal with a three-dimensional H-bond arrangement of the binuclear units. With the SAS technique, crystals 100-fold smaller than those obtained by slow evaporation were obtained, proving SAS as a suitable method for mixed-ligand complexes preparation with reduced particle size and therefore expected bioavailability enhancement.Item Phase equilibria for the mixtures of the deep eutectic solvent L-menthol + thymol plus CO2 at high pressure(Journal of Industrial and Engineering Chemistry, 2023) Pérez Velilla, Eduardo; Rato, Sergio; Loaisa, Gema; Cabañas Poveda, AlbertinaThe Vapour-Liquid Equilibrium (VLE) of different mixtures of CO2 + L-menthol, CO2 + thymol and CO2 + L-menthol + thymol has been determined at 35, 40, 50 and 60 °C and pressures up to 220 bar using a variable volume view cell. Menthol + Thymol form a deep eutectic solvent (DES) mixture at a 1:1 molar ratio. For selected conditions, the composition of the vapour phase was determined by 1H NMR. By interpolation of the experimental values, ternary diagrams were built. The mutual solubility between CO2 and DES decreased as the proportion menthol:thymol approached the eutectic composition (1:1). Mutual miscibility also decreased with temperature and increased with pressure. The composition of the mixture of menthol + thymol (1:1) does not remain stable at 60 °C but it does at lower temperatures. The intermolecular interactions between menthol and thymol are responsible for this behaviour. The Peng-Robinson equation of state was used to correlate the results with promising results.Item Supercritical fluid impregnation of naproxen into mesoporous SiO2 SBA-15(Journal of CO2 utilization, 2023) González, Juan; Pérez Velilla, Eduardo; Pepczynska, Marzena; Calvo Garrido, María Lourdes; Cabañas Poveda, AlbertinaNaproxen was impregnated into mesoporous SiO2 SBA-15 using the Supercritical Solution Impregnation (SSI) technique. Experiments were performed at 50–70ºC and 15–25 MPa in pure CO2 and CO2 modified with ethanol, ethyl acetate and menthol. Materials were also impregnated from liquid solutions in ethanol and chloroform. In the SSI experiments, naproxen was deposited on the internal surface of the mesopores as shown by N2-adsorption experiments. The percentage of naproxen impregnated decreased from 11.1% to 7.4% mass as the CO2 density increased. Likewise, adding ethanol, ethyl acetate or menthol to CO2 decreased the percentage of naproxen adsorbed on the support. Thermal analysis showed that naproxen impregnated on SiO2 by SSI became amorphous. FTIR and XRD confirmed the loss of crystallinity of naproxen and its interaction with the SiO2 support. Samples impregnated in liquid medium however kept partially their crystallinity. Release tests of naproxen on SiO2 SBA-15 prepared by SSI followed an almost zero-order release profile; the drug is released at a constant rate into a PBS pH= 7.4 medium. The release rate slowed down in comparison to that of pure naproxen, due to the interaction of the drug with the support and the diffusion of the drug outside the support mesopores. Thus, a sustained release system was achieved, which may help to attain a longer therapeutic effect with a lower naproxen dose.Item Green Preparation of PtRu and PtCu/SBA-15 Catalysts using Supercritical CO2(Journal of CO2 utilization, 2017) Sánchez Miguel, E.; Tenorio, María José; Morère, Jacobo; Cabañas Poveda, AlbertinaSustainability is emerging as design criteria in catalysts production. Hence, the preparation of Pt bimetallic catalysts using supercritical CO2 (scCO2) as a green solvent is proposed. PtRu and PtCu nanoparticles (NPs) were deposited on mesoporous SiO2 SBA-15 by the reduction of Pt, Ru and Cu metalorganic precursor in scCO2. The simultaneous and sequential deposition of both metals was attempted using different reduction methodologies. The materials were characterized by X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and Energy-Dispersive X-ray analysis (EDX). XRD patterns matched closely that of cubic Pt. TEM images showed small NPs homogeneously distributed throughout the SBA-15 mesopores. Smaller particles were obtained when the reduction was performed in H2/N2 at low pressure. Sequential deposition of Cu or Ru in the first place followed by Pt yielded equimolar metal ratios. Samples prepared by sequential deposition were studied by Scanning Transmission Electron Microscopy (STEM). Composition profiles of the PtRu samples suggested an alloy structure. These catalysts were used in the hydrogenation of the renewable furfural in scCO2 at 80ºC. PtRu materials presented a high activity and selectivity to furfuryl alcohol.Item Thiol group functionalization of mesoporous SiO2 SBA-15 using supercritical CO2(Microporous and Mesoporous Materials, 2018) Tenorio, M.J.; Carnerero, C.; Torralvo Fernández, María Josefa; Pando García-Pumarino, Concepción; Cabañas Poveda, AlbertinaChemical modification of mesoporous SiO2 SBA-15 with thiol groups was performed using mercaptopropyltrimethoxysilane (MPTMS) dissolved in supercritical CO2 (scCO2). Thiol groups serve as adsorbents for the selective removal of contaminant metal cations and in catalysis. Functionalization was carried out in scCO2 at temperatures ranging from 40 to 150 °C and pressures from 15.0 to 29.0 MPa. For comparison purposes, the reaction was also performed in toluene at 80 and 110 °C. As opposed to toluene, scCO2 is considered a green solvent. Grafting of the thiol groups was confirmed by FTIR spectroscopy, thermogravimetric analysis (TGA) and elemental analysis. Grafting density and surface coverage of the materials modified using scCO2increased with temperature, CO2 density, time and stirring and varied from 1.3 to 4.4 mmol g−1 and from 1.3 to 4.0 molecules nm−2, respectively. On the other hand, surface area and pore size decreased as grafting density increased. At temperatures of 80 °C or higher, the pore size remained constant, suggesting the formation of a compact monolayer. Modification at higher temperatures led to larger grafting densities but very low surface areas. Assuming total hydrolysis and condensation of the precursor, the optimum grafting density and surface coverage of 2.3 mmol g−1 and 2.4 molecules nm−2, respectively, were obtained in scCO2 at 80 °C and 25.0 MPa for 4 h. Grafting densities of the samples prepared in toluene were by far much lower than those obtained using scCO2 at lower temperatures and shorter times, which demonstrates the advantages of CO2 as a green functionalization medium.