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Physicochemical characterization of silylated functionalized materials

Title
Physicochemical characterization of silylated functionalized materials
Type
Article in International Scientific Journal
Year
2010
Authors
Tiago Borrego
(Author)
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Marta Andrade
(Author)
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Moises L Pinto
(Author)
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Ana P Carvalho
(Author)
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Joao Rocha
(Author)
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Joao Pires
(Author)
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Journal
Vol. 344
Pages: 603-610
ISSN: 0021-9797
Publisher: Elsevier
Scientific classification
FOS: Natural sciences > Chemical sciences
Other information
Authenticus ID: P-003-7FV
Abstract (EN): Silylation of several materials where the surface area arises from the internal pores (MCM-41 and FSM-16) or is essentially external (silica gel, and clays) was performed using three organosilanes: (3-aminopropyl)-triethoxysilane (APTES), 4-(triethoxysilyl)aniline (TESA) and (3-mercaptopropyl)trimethoxysilane (MPTS). The materials were characterized by nitrogen adsorption-desorption at -196 degrees C, powder XRD, XPS, bulk chemical analysis, FTIR and (29)Si and (13)C MAS NMR. For MCM-41 and FSM-16 the highest amounts of organosilane are obtained for APTES, while for the remaining materials the highest amounts are for MPTS; TESA always anchored with the lowest percentage. In terms of surface chemical analysis, TESA anchored with the highest contents irrespectively of the material, and the opposite is registered for MPTS. Comparison of bulk vs surface contents indicate that TESA is mainly anchored at the material external surface. Moreover, with N or S (surface and bulk) contents expressed per unit of surface area, MCM-41 and FSM-16 (internal porosity) show the lowest amounts of silane; the highest amounts of silane per unit of surface area are obtained for the clays. Grafting of the organosilanes to the surface hydroxyl groups was corroborated by FTIR and (29)Si and (13)C MAS NMR. Furthermore, NMR data suggested that TESA and APTES grafted mostly through a bidentate approach, whereas MPTS grafted by a monodentate mechanism.
Language: English
Type (Professor's evaluation): Scientific
Contact: acfreire@fc.up.pt; jpsilva@fc.ul.pt
No. of pages: 8
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