4.7 Article

Preparation of trityl cations in faujasite micropores through supercritical CO2 impregnation

Journal

MICROPOROUS AND MESOPOROUS MATERIALS
Volume 132, Issue 3, Pages 357-362

Publisher

ELSEVIER
DOI: 10.1016/j.micromeso.2010.03.014

Keywords

Supercritical CO2; Impregnation; Trityl cation; Ship-in-a-bottle; Zeolites

Funding

  1. EU [NMP2-CT-2005-013524]
  2. Spanish projects [MAT-2006-28189-E, CTQ2008-05370/PPQ]
  3. Generalitat of Catalonia [2009SGR-666]
  4. CSIC

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In this paper, we investigated on the preparation of three zeolite encapsulated-trityl cations (trityl, dimethoxytrityl and methoxytrityl) using supercritical CO2 (scCO(2)) as the processing media. Since the studied trityl cations had a size larger than the diameter of the zeolite channels, the fabrication was based on a ship-in-a-bottle procedure using benzene, benzaldehyde, anisole, diphenylcarbinol and benzophenone as building blocks. The different cations were prepared by nucleophilic substitution, using the inner super-cage of the acid zeolite as both a microreactor and a negative counterion for the trityl cation. The obtained impregnated samples were purified by cleaning with a continuous flow of scCO(2). Loaded amounts of ca. 8 wt.% were obtained following the supercritical procedure. The successful formation of the cation was confirmed by using optical spectroscopies, such as UV-vis diffuse reflectance and FTIR spectroscopies. (C) 2010 Elsevier Inc. All rights reserved.

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