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Revealing the effects of high Al loading incorporation in the SBA-15 silica mesoporous material

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Abstract

High aluminum loading incorporation in the SBA-15 silica structure was investigated. Different Si/Al molar ratios (15, 10, and 2) were evaluated. The SBA-15 and the aluminum-containing materials (Al-SBA-15) were prepared by the “pH adjusting” method with modifications. The mesoporous structure of the materials was demonstrated by the type IV isotherms. The SBA-15 pore changed from a cylindrical to a slit-like structure in the presence of higher aluminum content. X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) pointed out that the structural order is compromised in the presence of a higher aluminum load in the Al-SBA-15 materials, although the mesoporous structure was preserved. Higher Al loading increases the total quantity of Lewis acid sites as well as generates Brönsted acid sites. CO adsorption FTIR spectroscopy suggests aluminum incorporation into the SBA-15 and generation of acid sites. The Si–O–Al linkage in the aluminum-containing materials was corroborated by UV–Vis DRS due to the presence of a peak centered at 241 nm related to the Al-O bond, which is ascribed to four-coordinated framework aluminum in the SBA-15 structure. XPS spectra of Al 2p suggested that the Al species are less oxidized than the Al2O3 phase giving some indication of Al incorporation into the SBA-15 framework. 27Al MAS NMR results revealed that the aluminum species are in a tetrahedral oxygen coordination environment for Al-SBA-15 with Si/Al molar ratios of 15 and 10. Aluminum species in both tetrahedral and octahedral environments were evidenced for Al-SBA-15 with a Si/Al molar ratio of 2.

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Acknowledgements

RJC, JCZ, and JG gratefully acknowledge the financial support from the Chilean National Fund for Science and Technology, Fondecyt No 1180243 and Fondecyt No 1220355. AFP acknowledges FCT/MCTES for financial support by national funds through the project UIDB/5006/2020. JG is grateful to the Universidad de Concepción for its cooperation with the UdeC Postgraduate Scholarship. JCZ acknowledges the support provided by ANID with the scholarship Grant No. 21201413. JL is a Serra Hunter Fellow and is grateful to ICREA Academia program and projects MICINN-FEDER PID2021-124572OB-C31 and 2021-SGR-01061. JS acknowledges the support of his work by the US Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences and Biosciences. His work was performed at the Environmental Molecular Sciences Laboratory in (EMSL), which is a DOE Office of Science User Facility located at Pacific Northwest National Laboratory (PNNL). PNNL is a multi-program national laboratory operated for DOE by Battelle.

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Author notes

  1. Jorge Gajardo and Julio Colmenares-Zerpa have contributed equally to this work.

Authors and Affiliations

  1. Laboratorio de Investigación de Procesos Catalíticos y Adsorción (LIPROCAD), Departamento de Fisicoquímica, Facultad de Ciencias Químicas, Universidad de Concepción, 160, Concepción, Casilla, Chile

    Jorge Gajardo, Julio Colmenares-Zerpa, C. Sepúlveda & R. J. Chimentão

  2. Laboratorio de Cinética y Catálisis, Facultad de Ciencias, Universidad de Los Andes, Mérida, 5101, Venezuela

    Julio Colmenares-Zerpa

  3. LAQV-REQUIMTE, Departamento de Química e Bioquímica, Faculdade de Ciências da Universidade Do Porto, Rua Do Campo Alegre, 4169-007, Porto, Portugal

    A. F. Peixoto

  4. Departamento de Engenharia Química, Universidade Federal de São Carlos, São Carlos, Brazil

    D. S. A. Silva, J. A. Silva, E. A. Urquieta-Gonzalez & J. B. O. Santos

  5. Servei de Recursos Científics, Universitat Rovira I Virgili, 43007, Tarragona, Spain

    F. Gispert-Guirado

  6. Institute of Energy Technologies, Department of Chemical Engineering and Barcelona Research Center in Multiscale Science and Engineering, Universitat Politècnica de Catalunya, EEBE, Eduard Maistany 10-14, 08019, Barcelona, Spain

    J. Llorca

  7. Research Center On Advanced Materials and Energy, Federal University of São Carlos, C. Postal 676, São Carlos, SP, CEP, 13565-905, Brazil

    E. A. Urquieta-Gonzalez

  8. Institute for Integrated Catalysis, Pacific Northwest National Laboratory, Richland, WA, 99352, USA

    J. Szanyi

  9. GIR-QUESCAT, Departamento de Química Inorgánica. Facultad de Ciencias Químicas, Universidad de Salamanca, Salamanca, 37008, Spain

    M. G. Álvarez

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  1. Jorge Gajardo
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Contributions

JG: Conceptualization, Methodology, Investigation, Writing—original draft, Writing—review & editing, Visualization. JCZ: Methodology, Investigation, Writing—review & editing. AFP: Resources, Writing—review & editing. DSAS: Methodology, Investigation, Writing—review & editing. JAS: Methodology, Investigation, Writing—review & editing. FGG: Resources, Writing—review & editing. JL: Resources, Writing—review & editing. EAUG: Resources, Writing– review & editing. JBOS: Resources, Writing—review & editing. JS: Resources, Writing—review & editing. CS: Resources, Writing—review & editing. MGÁ: Conceptualization, Resources, Writing—original draft, Writing—review & editing, Supervision, Project administration. RJC: Conceptualization, Resources, Writing—original draft, Writing—review & editing, Supervision, Project administration, Funding acquisition.

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Correspondence to M. G. Álvarez or R. J. Chimentão.

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Gajardo, J., Colmenares-Zerpa, J., Peixoto, A.F. et al. Revealing the effects of high Al loading incorporation in the SBA-15 silica mesoporous material. J Porous Mater 30, 1687–1707 (2023). https://doi.org/10.1007/s10934-023-01453-z

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