MCM-41 ordered mesoporous molecular sieves synthesis and characterization

• Autor(a) principal: Melo,Rogério A.A.
• Data de Publicação: 1999
• Outros Autores: Giotto,Marcus V., Rocha,João, Urquieta-González,Ernesto A.
• Tipo de documento: Artigo
• Idioma: eng
• Título da fonte: Materials research (São Carlos. Online)
• Texto Completo: http://old.scielo.br/scielo.php?script=sci_arttext&pid=S1516-14391999000300010
• topic: MCM-41; synthesis; characterization

The aim of this work was to study the hydrothermal synthesis of Si and SiAlMCM-41 performed under both autogenic pressure and refluxing conditions. XRD data showed that the MCM-41 phase may be formed by both processes and that the synthesized material in the presence of Al and/or under reflux presents the hexagonally arrangement of less ordered mesopores. However, as verified by XRD and physisorption data, the order was improved with higher synthesis times. 29Si and 1H - 29Si C/P MAS NMR spectra showed that a great part of the Si atoms exists as silanol groups which originate resonance peaks at -110, -100 and -91 ppm. The presence of Al atoms may generate Si(3Si, Al) and Si(2Si, 2Al) environments which might be contributing to resonance peaks at -100 and -91 ppm. The 27Al MAS NMR spectrum of the as synthesized AlSiMCM-41 showed a resonance peak of tetrahedral framework aluminum close to 53 ppm and two others, one close to 14 ppm attributed to Al(H2O)6+3 species and the other a weak signal close to 32 ppm attributed to pentacoordinated Al. 27Al MAS NMR spectra of the calcined sample showed a peak at 0 ppm corresponding to an hexacoordinated extra-framework aluminum formed during calcination.