Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution

Autores
Sosa, Alexis Alberto; Gorsd, Marina Noelia; Blanco, Mirta Noemí; Pizzio, Luis René
Año de publicación
2017
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Mesoporous silica nanoparticles were prepared in aqueous/organic phase using cetyltrimethylammonium bromide and polystyrene as organic templates. The morphology and crystalline phase of the products were characterized by scanning electron microcopy, transmission electron microscopy, X-ray diffraction, small angle X-ray scattering, and N₂ adsorption/desorption isotherm analysis. The octane/water ratio influenced the pore size distribution, the morphology and size of the nanospheres obtained. Transmission electron microscopy revealed that mesoporous silica nanoparticles with “blackberry-like structure” (MSN3, MSN4, MSN5, and MSN6 samples) were obtained using octane/water ratios in the range 0.007–0.35. They present small (in the range 5–6 nm) and large (in the range 28–34 nm) mesopores. Large mesopores were mainly generated by polystyrene, and their volume contribution was clearly higher than in the MSN1 and MSN2 samples. The structure and morphology of mesoporous silica nanoparticles solids impregnated with tungstophosphoric acid were similar to those of the mesoporous silica nanospheres used as support. In addition, the characterization of all the solids impregnated with tungstophosphoric acid by Fourier transform infrared and ³¹P nuclear magnetic resonance indicated the presence of undegraded [PW₁₂O₄₀]³⁻ and [H3−XPW₁₂O₄₀](3−X)− species interacting electrostatically with the ≡Si–OH₂⁺ groups, and by potentiometric titration the solids presented very strong acid sites. In summary, they are good candidates to be used in reactions catalyzed by acids, especially to obtain quinoxaline derivatives.
Facultad de Ciencias Exactas
Centro de Investigación y Desarrollo en Ciencias Aplicadas
Materia
Ciencias Exactas
Química
Nanoparticles
Silica
Mesoporous solids
Tungstophosphoric acid
Nivel de accesibilidad
acceso abierto
Condiciones de uso
http://creativecommons.org/licenses/by-nc-sa/4.0/
Repositorio
SEDICI (UNLP)
Institución
Universidad Nacional de La Plata
OAI Identificador
oai:sedici.unlp.edu.ar:10915/130564
Acceder
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oai_identifier_str oai:sedici.unlp.edu.ar:10915/130564
network_acronym_str SEDICI
repository_id_str 1329
network_name_str SEDICI (UNLP)
spelling Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distributionSosa, Alexis AlbertoGorsd, Marina NoeliaBlanco, Mirta NoemíPizzio, Luis RenéCiencias ExactasQuímicaNanoparticlesSilicaMesoporous solidsTungstophosphoric acidMesoporous silica nanoparticles were prepared in aqueous/organic phase using cetyltrimethylammonium bromide and polystyrene as organic templates. The morphology and crystalline phase of the products were characterized by scanning electron microcopy, transmission electron microscopy, X-ray diffraction, small angle X-ray scattering, and N₂ adsorption/desorption isotherm analysis. The octane/water ratio influenced the pore size distribution, the morphology and size of the nanospheres obtained. Transmission electron microscopy revealed that mesoporous silica nanoparticles with “blackberry-like structure” (MSN3, MSN4, MSN5, and MSN6 samples) were obtained using octane/water ratios in the range 0.007–0.35. They present small (in the range 5–6 nm) and large (in the range 28–34 nm) mesopores. Large mesopores were mainly generated by polystyrene, and their volume contribution was clearly higher than in the MSN1 and MSN2 samples. The structure and morphology of mesoporous silica nanoparticles solids impregnated with tungstophosphoric acid were similar to those of the mesoporous silica nanospheres used as support. In addition, the characterization of all the solids impregnated with tungstophosphoric acid by Fourier transform infrared and ³¹P nuclear magnetic resonance indicated the presence of undegraded [PW₁₂O₄₀]³⁻ and [H<sub>3−X</sub>PW₁₂O₄₀]<sup>(3−X)−</sup> species interacting electrostatically with the ≡Si–OH₂⁺ groups, and by potentiometric titration the solids presented very strong acid sites. In summary, they are good candidates to be used in reactions catalyzed by acids, especially to obtain quinoxaline derivatives.Facultad de Ciencias ExactasCentro de Investigación y Desarrollo en Ciencias Aplicadas2017-08info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionArticulohttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdf355-364http://sedici.unlp.edu.ar/handle/10915/130564enginfo:eu-repo/semantics/altIdentifier/issn/0928-0707info:eu-repo/semantics/altIdentifier/issn/1573-4846info:eu-repo/semantics/altIdentifier/doi/10.1007/s10971-017-4428-6info:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-sa/4.0/Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International (CC BY-NC-SA 4.0)reponame:SEDICI (UNLP)instname:Universidad Nacional de La Platainstacron:UNLP2025-09-03T11:04:43Zoai:sedici.unlp.edu.ar:10915/130564Institucionalhttp://sedici.unlp.edu.ar/Universidad públicaNo correspondehttp://sedici.unlp.edu.ar/oai/snrdalira@sedici.unlp.edu.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:13292025-09-03 11:04:43.398SEDICI (UNLP) - Universidad Nacional de La Platafalse
dc.title.none.fl_str_mv Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
title Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
spellingShingle Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
Sosa, Alexis Alberto
Ciencias Exactas
Química
Nanoparticles
Silica
Mesoporous solids
Tungstophosphoric acid
title_short Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
title_full Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
title_fullStr Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
title_full_unstemmed Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
title_sort Synthesis and characterization of tungstophosphoric acid-modified mesoporous silica nanoparticles with tuneable diameter and pore size distribution
dc.creator.none.fl_str_mv Sosa, Alexis Alberto
Gorsd, Marina Noelia
Blanco, Mirta Noemí
Pizzio, Luis René
author Sosa, Alexis Alberto
author_facet Sosa, Alexis Alberto
Gorsd, Marina Noelia
Blanco, Mirta Noemí
Pizzio, Luis René
author_role author
author2 Gorsd, Marina Noelia
Blanco, Mirta Noemí
Pizzio, Luis René
author2_role author
author
author
dc.subject.none.fl_str_mv Ciencias Exactas
Química
Nanoparticles
Silica
Mesoporous solids
Tungstophosphoric acid
topic Ciencias Exactas
Química
Nanoparticles
Silica
Mesoporous solids
Tungstophosphoric acid
dc.description.none.fl_txt_mv Mesoporous silica nanoparticles were prepared in aqueous/organic phase using cetyltrimethylammonium bromide and polystyrene as organic templates. The morphology and crystalline phase of the products were characterized by scanning electron microcopy, transmission electron microscopy, X-ray diffraction, small angle X-ray scattering, and N₂ adsorption/desorption isotherm analysis. The octane/water ratio influenced the pore size distribution, the morphology and size of the nanospheres obtained. Transmission electron microscopy revealed that mesoporous silica nanoparticles with “blackberry-like structure” (MSN3, MSN4, MSN5, and MSN6 samples) were obtained using octane/water ratios in the range 0.007–0.35. They present small (in the range 5–6 nm) and large (in the range 28–34 nm) mesopores. Large mesopores were mainly generated by polystyrene, and their volume contribution was clearly higher than in the MSN1 and MSN2 samples. The structure and morphology of mesoporous silica nanoparticles solids impregnated with tungstophosphoric acid were similar to those of the mesoporous silica nanospheres used as support. In addition, the characterization of all the solids impregnated with tungstophosphoric acid by Fourier transform infrared and ³¹P nuclear magnetic resonance indicated the presence of undegraded [PW₁₂O₄₀]³⁻ and [H<sub>3−X</sub>PW₁₂O₄₀]<sup>(3−X)−</sup> species interacting electrostatically with the ≡Si–OH₂⁺ groups, and by potentiometric titration the solids presented very strong acid sites. In summary, they are good candidates to be used in reactions catalyzed by acids, especially to obtain quinoxaline derivatives.
Facultad de Ciencias Exactas
Centro de Investigación y Desarrollo en Ciencias Aplicadas
description Mesoporous silica nanoparticles were prepared in aqueous/organic phase using cetyltrimethylammonium bromide and polystyrene as organic templates. The morphology and crystalline phase of the products were characterized by scanning electron microcopy, transmission electron microscopy, X-ray diffraction, small angle X-ray scattering, and N₂ adsorption/desorption isotherm analysis. The octane/water ratio influenced the pore size distribution, the morphology and size of the nanospheres obtained. Transmission electron microscopy revealed that mesoporous silica nanoparticles with “blackberry-like structure” (MSN3, MSN4, MSN5, and MSN6 samples) were obtained using octane/water ratios in the range 0.007–0.35. They present small (in the range 5–6 nm) and large (in the range 28–34 nm) mesopores. Large mesopores were mainly generated by polystyrene, and their volume contribution was clearly higher than in the MSN1 and MSN2 samples. The structure and morphology of mesoporous silica nanoparticles solids impregnated with tungstophosphoric acid were similar to those of the mesoporous silica nanospheres used as support. In addition, the characterization of all the solids impregnated with tungstophosphoric acid by Fourier transform infrared and ³¹P nuclear magnetic resonance indicated the presence of undegraded [PW₁₂O₄₀]³⁻ and [H<sub>3−X</sub>PW₁₂O₄₀]<sup>(3−X)−</sup> species interacting electrostatically with the ≡Si–OH₂⁺ groups, and by potentiometric titration the solids presented very strong acid sites. In summary, they are good candidates to be used in reactions catalyzed by acids, especially to obtain quinoxaline derivatives.
publishDate 2017
dc.date.none.fl_str_mv 2017-08
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
Articulo
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://sedici.unlp.edu.ar/handle/10915/130564
url http://sedici.unlp.edu.ar/handle/10915/130564
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/issn/0928-0707
info:eu-repo/semantics/altIdentifier/issn/1573-4846
info:eu-repo/semantics/altIdentifier/doi/10.1007/s10971-017-4428-6
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
http://creativecommons.org/licenses/by-nc-sa/4.0/
Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International (CC BY-NC-SA 4.0)
eu_rights_str_mv openAccess
rights_invalid_str_mv http://creativecommons.org/licenses/by-nc-sa/4.0/
Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International (CC BY-NC-SA 4.0)
dc.format.none.fl_str_mv application/pdf
355-364
dc.source.none.fl_str_mv reponame:SEDICI (UNLP)
instname:Universidad Nacional de La Plata
instacron:UNLP
reponame_str SEDICI (UNLP)
collection SEDICI (UNLP)
instname_str Universidad Nacional de La Plata
instacron_str UNLP
institution UNLP
repository.name.fl_str_mv SEDICI (UNLP) - Universidad Nacional de La Plata
repository.mail.fl_str_mv alira@sedici.unlp.edu.ar
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score 13.13397

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