Synthesis and characterization of tin oxide-modified mesoporous SBA-15 molecular sieves and catalytic activity in trans-esterification reaction

Pallavi Shah, Arumugamangalam V. Ramaswamy, K. Lázár, Veda Ramaswamy

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Abstract

Mesoporous silica molecular sieve SBA-15 has been synthesized and incorporated with various amounts of tin via incipient-wetness impregnation using tin chloride in ethanol followed by calcination. Characterization was done by X-ray fluorescence spectrophotometry (XRF), powder X-ray diffraction (PXRD), nitrogen adsorption, diffuse reflectance ultraviolet (DRUV), scanning and transmission electron microscopy (SEM, TEM), FTIR, 29Si and 119Sn MAS NMR, and Sn-Mössbauer spectroscopic techniques to understand the chemical nature of incorporated tin. The silanol groups on the internal walls of SBA-15 are suggested to be the sites for tin incorporation. Bulk structural characterization techniques (X-ray diffraction and BET) are used to demonstrate that the hexagonal structure is maintained during impregnation. Tin oxide exists as a thin film anchored inside the mesopores of SBA-15. Complementarily, 119Sn NMR and Mössbauer spectroscopies are used to investigate the microstructure of the Sn centers grafted to the mesoporous walls. Sn-Mössbauer spectroscopic studies reveal that Sn 2+ may form upon reductive treatments and can probably be stabilized atomically in the pore wall, whereas Sn4+ is stabilized as large entities. While SBA-15 itself shows some activity in transesterification of diethyl malonate with various alcohols, Sn-SBA-15 samples are found to possess enhanced catalytic activity for the same.

Original languageEnglish
Pages (from-to)239-248
Number of pages10
JournalApplied Catalysis A: General
Volume273
Issue number1-2
DOIs
Publication statusPublished - Oct 8 2004

Fingerprint

Transesterification
Molecular sieves
Tin oxides
Tin
Catalyst activity
Impregnation
Nuclear magnetic resonance
Transmission electron microscopy
Scanning electron microscopy
Spectrophotometry
Calcination
X ray powder diffraction
Alcohols
Ethanol
Silicon Dioxide
Fluorescence
Silica
Spectroscopy
Nitrogen
Adsorption

Keywords

  • SBA-15
  • Sn-SBA-15
  • SnO
  • Transesterification

ASJC Scopus subject areas

  • Catalysis
  • Process Chemistry and Technology

Cite this

Synthesis and characterization of tin oxide-modified mesoporous SBA-15 molecular sieves and catalytic activity in trans-esterification reaction. / Shah, Pallavi; Ramaswamy, Arumugamangalam V.; Lázár, K.; Ramaswamy, Veda.

In: Applied Catalysis A: General, Vol. 273, No. 1-2, 08.10.2004, p. 239-248.

Research output: Contribution to journalArticle

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