Thiol group functionalization of mesoporous SiO2 SBA-15 using supercritical CO2

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dc.contributor.authorTenorio, M.J.
dc.contributor.authorCarnerero, C.
dc.contributor.authorTorralvo Fernández, María Josefa
dc.contributor.authorPando García-Pumarino, Concepción
dc.contributor.authorCabañas Poveda, Albertina
dc.date.accessioned2023-06-17T12:26:01Z
dc.date.available2023-06-17T12:26:01Z
dc.date.issued2018-08-02
dc.description.abstractChemical 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.
dc.description.departmentDepto. de Química Física
dc.description.facultyFac. de Ciencias Químicas
dc.description.refereedTRUE
dc.description.sponsorshipMinisterio de Economía y Competitividad (MINECO)
dc.description.statuspub
dc.eprint.idhttps://eprints.ucm.es/id/eprint/44801
dc.identifier.doidoi.org/10.1016/j.micromeso.2017.07.056
dc.identifier.issn1873-3093(On line) 1387-1811 (Print)
dc.identifier.officialurlhttp://www.sciencedirect.com/science/article/pii/S1387181117305280
dc.identifier.urihttps://hdl.handle.net/20.500.14352/11945
dc.issue.number15
dc.journal.titleMicroporous and Mesoporous Materials
dc.language.isoeng
dc.page.final154
dc.page.initial147
dc.publisherElsevier
dc.relation.projectIDCTQ2013-41781-P
dc.rights.accessRightsopen access
dc.subject.cdu544
dc.subject.keywordSurface modification
dc.subject.keywordSupercritical fluids
dc.subject.keywordSustainable chemistry
dc.subject.keywordMesoporous
dc.subject.keywordSiO2 SBA-15
dc.subject.ucmQuímica física (Química)
dc.titleThiol group functionalization of mesoporous SiO2 SBA-15 using supercritical CO2
dc.typejournal article
dc.volume.number256
dspace.entity.typePublication
relation.isAuthorOfPublicationf6a2e8ec-cb28-4e8f-b54a-b503b2cb80ce
relation.isAuthorOfPublication14dc7f21-ee73-46a9-accd-f5a648b5bc0b
relation.isAuthorOfPublication08f9e67b-e7ba-420b-a651-37a03ba04f0c
relation.isAuthorOfPublication.latestForDiscovery14dc7f21-ee73-46a9-accd-f5a648b5bc0b
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