Person: Torralvo Fernández, María Josefa
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First Name
María Josefa
Last Name
Torralvo Fernández
Affiliation
Universidad Complutense de Madrid
Faculty / Institute
Ciencias Químicas
Department
Química Inorgánica
Area
Química Inorgánica
Identifiers
4 results
Search Results
Now showing 1 - 4 of 4
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 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.Item Deposition of Au nanoparticles into mesoporous SiO2 SBA-15(The Journal of Supercritical Fluids, 2022) Huerta, Andrea; Torralvo Fernández, María Josefa; Tenorio, María José; Pérez Gómez, Eduardo; Bermúdez, Jonathan; Calvo Garrido, María Lourdes; Cabañas Poveda, AlbertinaAu/SiO2 SBA-15 materials were prepared using supercritical CO2 (scCO2) and by wet impregnation. First, SiO2 SBA-15 was functionalized with thiol groups at different grafting densities using 3-(Mercaptopropyl)trimethoxysilane dissolved in scCO2. The support was then impregnated with HAuCl4·3H2O in scCO2 modified with EtOH. Wet impregnation of the supports with HAuCl4·3H2O in ethanol was also performed. Materials were calcined at 500 ºC to remove the organic matter and promote particle growth. Materials prepared on the highest thiol grafting density support showed Au NP between 2.5-5 nm homogeneously distributed within the mesopores. Slightly larger Au NPs were obtained in scCO2 modified with EtOH. Materials prepared on the low thiol grafting density support showed a bimodal particle size distribution with particles up to 7 nm located inside the mesopores and larger ones of 10-20 nm on the external surface. A possible reaction mechanism was proposed. These materials can be used in catalysis, sensing and biomedicine.Item Supercritical fluid deposition of Ru nanoparticles into SiO2 SBA-15 as a sustainable method to prepare selective hydrogenation catalysts(RSC Advances, 2015) Morère Rodríguez, Jacobo; Torralvo Fernández, María Josefa; Pando García-Pumarino, Concepción; Rodríguez Renuncio, Juan Antonio; Cabañas Poveda, AlbertinaRu nanoparticles were successfully deposited into mesoporous SiO2 SBA-15 using supercritical CO2 (scCO2). The use of scCO2 favoured the metal dispersion and Ru nanoparticles uniformly distributed throughout the support were obtained. Different precursors and methodologies were employed: impregnation with Ru(tmhd)2(COD) in scCO2 at 80 ºC and 13.5 and 19.3 MPa and further reduction in H2/N2 at 400 ºC at low pressure, reactive deposition of Ru(tmhd)2(COD) with H2 in scCO2 at 150 ºC and reactive deposition of RuCl3•xH2O with ethanol in scCO2 at 150 and 200 ºC. The size of the particles was limited in one dimension by the pore size of the support. The metal loading varied with the methodology and experimental conditions from 0.9 to 7.4% Ru mol. These materials exhibited remarkable catalytic activity. The Ru/SiO2 SBA-15 materials prepared by reactive deposition with H2 in scCO2 were selective catalysts for the hydrogenation reactions of benzene and limonene, allowing the production of partly hydrogenated hydrocarbons that may serve as building blocks for more complex chemicals. scCO2 is shown to be a green solvent that allows the preparation of efficient heterogeneous catalysts to design sustainable processes. Furthermore, in the hydrogenation of limonene, scCO2 was also used as the solvent.