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Acid properties of organosiliceous hybrid materials based on pendant (fluoro)aryl-sulfonic groups through spectroscopic study with probe molecules

Acid properties of organosiliceous hybrid materials based on pendant (fluoro)aryl-sulfonic groups through spectroscopic study with probe molecules
Acid properties of organosiliceous hybrid materials based on pendant (fluoro)aryl-sulfonic groups through spectroscopic study with probe molecules
Two different heterogeneous catalysts carrying aryl-sulfonic moieties, in which the aromatic ring was either fluorinated or not, were successfully synthetized. The multi-step synthetic approaches implemented involved the synthesis of the silyl-derivative, template-free one-pot co-condensation (at low temperature and neutral pH) and tethering reaction. A multi-technique approach was implemented to characterize the hybrid organic-inorganic catalysts involving TGA, N2 physisorption analysis, FTIR, ss MAS NMR (1H, 13C, 29Si). Specifically, the acidity of the organosiliceous hybrid materials was studied through the adsorption of probe molecules (i.e. CO at 77 K and NH3 and TMPO at room temperature) and a combination of FTIR and ss MAS NMR spectroscopies. The catalytic activity of the two hybrids was tested in the acetal formation reaction between benzaldehyde and ethylene glycol. Preliminary results indicated superior performances for the fluoro-aryl-sulfonic acid, compared to the non-fluorinated sample. The findings hereby reported opens up to the design of heterogeneous sulfonic acids with superior reactivity in acid catalyzed reactions. Moreover, through the implementation of spectroscopic studies, using probe molecules, it was possible to investigate in detail the acidic properties of hybrid organosiliceous materials.
2044-4753
Erigoni, Andrea
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Paul, Geo
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Meazza, Marta
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Hernández-Soto, María Consuelo
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Miletto, Ivana
9a3fe0ee-6afd-4e72-abff-8e83a9114ae9
Rios, Ramon
609bedf2-e886-4d62-a676-a32b6f8c1441
Segarra, Candela
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Marchese, Leonardo
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Raja, Robert
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Rey, Fernando
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Gianotti, Enrica
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Diaz, Urbano
f47efb0d-a86c-4ccf-90f2-fe72367c6e30
Erigoni, Andrea
6f1c2f2d-0c23-4fab-96c7-83398e705347
Paul, Geo
fe93c674-eedd-4eda-8c84-190bc5b1687f
Meazza, Marta
c4665645-8c77-4cfd-aa02-6bcc3341c1aa
Hernández-Soto, María Consuelo
ebd0679b-c800-4730-b155-c0584b404440
Miletto, Ivana
9a3fe0ee-6afd-4e72-abff-8e83a9114ae9
Rios, Ramon
609bedf2-e886-4d62-a676-a32b6f8c1441
Segarra, Candela
ab833293-034e-4412-acdf-47a9d1ebd862
Marchese, Leonardo
684a36ec-9847-4604-82e7-71234cd44090
Raja, Robert
74faf442-38a6-4ac1-84f9-b3c039cb392b
Rey, Fernando
7d59e576-cf4f-485f-8a0a-61a295522b8f
Gianotti, Enrica
2496d8d3-780f-4fe0-a43e-147e68331078
Diaz, Urbano
f47efb0d-a86c-4ccf-90f2-fe72367c6e30

Erigoni, Andrea, Paul, Geo, Meazza, Marta, Hernández-Soto, María Consuelo, Miletto, Ivana, Rios, Ramon, Segarra, Candela, Marchese, Leonardo, Raja, Robert, Rey, Fernando, Gianotti, Enrica and Diaz, Urbano (2019) Acid properties of organosiliceous hybrid materials based on pendant (fluoro)aryl-sulfonic groups through spectroscopic study with probe molecules. Catalysis Science & Technology. (doi:10.1039/C9CY01609K).

Record type: Article

Abstract

Two different heterogeneous catalysts carrying aryl-sulfonic moieties, in which the aromatic ring was either fluorinated or not, were successfully synthetized. The multi-step synthetic approaches implemented involved the synthesis of the silyl-derivative, template-free one-pot co-condensation (at low temperature and neutral pH) and tethering reaction. A multi-technique approach was implemented to characterize the hybrid organic-inorganic catalysts involving TGA, N2 physisorption analysis, FTIR, ss MAS NMR (1H, 13C, 29Si). Specifically, the acidity of the organosiliceous hybrid materials was studied through the adsorption of probe molecules (i.e. CO at 77 K and NH3 and TMPO at room temperature) and a combination of FTIR and ss MAS NMR spectroscopies. The catalytic activity of the two hybrids was tested in the acetal formation reaction between benzaldehyde and ethylene glycol. Preliminary results indicated superior performances for the fluoro-aryl-sulfonic acid, compared to the non-fluorinated sample. The findings hereby reported opens up to the design of heterogeneous sulfonic acids with superior reactivity in acid catalyzed reactions. Moreover, through the implementation of spectroscopic studies, using probe molecules, it was possible to investigate in detail the acidic properties of hybrid organosiliceous materials.

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07 10 2019 CatalSciTechnol_Revised - Accepted Manuscript
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Accepted/In Press date: 9 October 2019
e-pub ahead of print date: 9 October 2019

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Local EPrints ID: 434965
URI: http://eprints.soton.ac.uk/id/eprint/434965
ISSN: 2044-4753
PURE UUID: 987c5057-084a-41a3-a7a8-bc5f147aa7b8
ORCID for Marta Meazza: ORCID iD orcid.org/0000-0003-4382-0626
ORCID for Ramon Rios: ORCID iD orcid.org/0000-0002-3843-8521
ORCID for Robert Raja: ORCID iD orcid.org/0000-0002-4161-7053

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Date deposited: 17 Oct 2019 16:30
Last modified: 18 Feb 2021 17:32

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