2003
DOI: 10.1021/jp0351472
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Study of the Acidic Sites and Their Modifications in Mesoporous Silica Synthesized in Acidic Medium under Quiescent Conditions

Abstract: The number and nature of silanol groups could be estimated in mesoporous silica prepared with cetyltrimethylammonium bromide (CTMBr) in acidic medium to obtain a material appropriate as a stationary chromatographic phase, using thermogravimetric analysis (TGA) and diffuse reflectance infrared spectroscopy (DRIFT). The temperature-programmed desorption of pyridine in the DRIFT cell was quantitatively correlated to the change in intensity of the two IR bands, 1595 and 1446 cm -1 , assigned to pyridine interactin… Show more

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Cited by 59 publications
(63 citation statements)
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“…[24,25] Secondly, silica species are less-condensed, linear oligomers in acidic conditions (M1 synthesis), while in alkaline solution (M2 synthesis), they contain more crosslinked clusters. [26] The 29 Si MAS-NMR (MAS: magic-angle-spinning) spectra of the samples synthesized in acidic conditions have a Q 3 /Q 4 ratio above unity accompanied with clear Q 2 peaks, [27] implying incomplete polymerization and condensation of the silanol groups. However, the Q 2 peaks disappeared in the spectra of the analogue sample synthesized under basic conditions and the Q 3 and Q 4 peak areas seemed very similar, which indicates the relative complete condensation between the silanol groups.…”
Section: Full Papermentioning
confidence: 99%
“…[24,25] Secondly, silica species are less-condensed, linear oligomers in acidic conditions (M1 synthesis), while in alkaline solution (M2 synthesis), they contain more crosslinked clusters. [26] The 29 Si MAS-NMR (MAS: magic-angle-spinning) spectra of the samples synthesized in acidic conditions have a Q 3 /Q 4 ratio above unity accompanied with clear Q 2 peaks, [27] implying incomplete polymerization and condensation of the silanol groups. However, the Q 2 peaks disappeared in the spectra of the analogue sample synthesized under basic conditions and the Q 3 and Q 4 peak areas seemed very similar, which indicates the relative complete condensation between the silanol groups.…”
Section: Full Papermentioning
confidence: 99%
“…These bands are due to pyridine interacting with hydrogen-bonded and free weakly acidic silanol groups, respectively (Bronsted groups). 33,34 The signal around 1633 cm -1 for S-Al samples is assigned to pyridine interacting with tetrahedral or octahedral Al in Bronsted and Lewis sites, respectively. 34 The 27 Al NMR was used to differentiate the coordination of the aluminium atom in the structure (Figure 2).…”
Section: Resultsmentioning
confidence: 99%
“…33,34 The signal around 1633 cm -1 for S-Al samples is assigned to pyridine interacting with tetrahedral or octahedral Al in Bronsted and Lewis sites, respectively. 34 The 27 Al NMR was used to differentiate the coordination of the aluminium atom in the structure (Figure 2). The 27 Al NMR spectrum shows just a signal at 53 ppm typically assigned to tetrahedral aluminium atoms suggesting the formation of Bronsted groups, because of the formation of Al-O-Si bonds in the structure.…”
Section: Resultsmentioning
confidence: 99%
“…The high temperature treatment of silica induces the following condensation reaction between associated silanol (SiOH) groups to form siloxane (SiOSi) moieties: [20,25,26,[39][40][41][42][43][44] …”
Section: Ftir Analysismentioning
confidence: 99%