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

Abstract : The "water-silicalite-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 μm(3)) 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.
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Submitted on : Wednesday, March 18, 2020 - 10:49:20 AM
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Thomas Karbowiak, Mohamed-Ali Saada, Séverinne Rigolet, Anthony Ballandras, Guy Weber, et al.. New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure. Physical Chemistry Chemical Physics, Royal Society of Chemistry, 2010, 12 (37), pp.11454. ⟨10.1039/c000931h⟩. ⟨hal-02510788⟩



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