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Issue 37, 2010
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New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure

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Abstract

The “watersilicalite-1” system is known to act as a molecular spring. The successive intrusion–extrusion cycles of liquid water in small crystallites (6 × 3 × 0.5 μm3) of hydrophobic silicalite-1 were studied by volumetric and calorimetric techniques. The experiments displayed a decrease of the intrusion pressure between the first intrusion–extrusion cycle and the consecutive ones, whereas the extrusion pressures remained unchanged. However, neither XRD studies nor SEM observations revealed any structural and morphological modifications of silicalite-1 at the long-range order. Such a shift in the value of the intrusion pressure after the first water intrusion–extrusion cycle is attributed to the creation of silanol groups during the first water intrusion. Detailed FTIR and solid-state NMR spectroscopic characterizations provided a molecular evidence of chemical modification of zeolite framework with the formation of local silanol defects created by the breaking of siloxane bonds.

Graphical abstract: New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure

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Article information


Submitted
14 Jan 2010
Accepted
06 May 2010
First published
02 Aug 2010

Phys. Chem. Chem. Phys., 2010,12, 11454-11466
Article type
Paper

New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure

T. Karbowiak, M. Saada, S. Rigolet, A. Ballandras, G. Weber, I. Bezverkhyy, M. Soulard, J. Patarin and J. Bellat, Phys. Chem. Chem. Phys., 2010, 12, 11454
DOI: 10.1039/C000931H

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