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Dehydration and rehydration of palygorskite and the influence of water on the nanopores

Published online by Cambridge University Press:  01 January 2024

Wenxing Kuang ,
Glenn A. Facey  and
Christian Detellier
Wenxing Kuang
Affiliation:
Center for Catalysis Research and Innovation and Department of Chemistry, University of Ottawa, Ottawa, Ontario, Canada K1N 6N5
Glenn A. Facey
Affiliation:
Center for Catalysis Research and Innovation and Department of Chemistry, University of Ottawa, Ottawa, Ontario, Canada K1N 6N5
Christian Detellier*
Affiliation:
Center for Catalysis Research and Innovation and Department of Chemistry, University of Ottawa, Ottawa, Ontario, Canada K1N 6N5
*
*E-mail address of corresponding author: dete@science.uottawa.ca
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Abstract

The dehydration and rehydration processes of the clay mineral palygorskite (PFl-1) were studied by textural analysis, thermogravimetric analysis connected with mass spectrometry (TGA-MS), and 29Si and 1H solid-state NMR techniques. The TGA-MS results clearly reveal weight losses at maxima of 70°C, 190°C, 430°C and 860°C. PFl-1 is characterized by a micropore area of 93 m2/g, corresponding to a micropore volume of 47 mm3/g. These values are also obtained for the sample heated up to 200°C for 20 h. Further heating at 300°C produces a collapse of the structure, as shown by the almost complete loss of microporosity.

The 29Si NMR spectra of palygorskite show two main resonances at −92.0 and −97.5 ppm, attributed to one of the two pairs of equivalent Si nuclei in the basal plane. A minor resonance at −84.3 ppm is attributed to Q2(Si-OH) Si nuclei. The resonance at −92.0 ppm is assigned to the central Si position, while the resonance at −97.5 ppm is assigned to the edge Si sites. It is confirmed bysolid-state 29Si and 1H NMR that nearly complete rehydration is achieved by exposing palygorskite samples that have been partially dehydrated at 150°C and 300°C, to D2O or water vapor at room temperature. When the rehydration is accomplished with D2O, the atoms are disordered across all the protons sites.

Keywords

Clay MineralsMicroporosityPalygorskiteSepioliteTextural AnalysisTGA-MS29Si NMR
Type
Research Article
Information
Clays and Clay Minerals , Volume 52 , Issue 5 , October 2004 , pp. 635 - 642
Copyright
Copyright © 2004, The Clay Minerals Society

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