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NMR Study of Dynamics and Evolution of Guest Molecules in Kaolinite/Dimethyl Sulfoxide Intercalation Compound

Published online by Cambridge University Press:  28 February 2024

Shigenobu Hayashi
Shigenobu Hayashi*
Affiliation:
National Institute of Materials and Chemical Research, 1-1 Higashi, Tsukuba, Ibaraki 305, Japan
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Abstract

Motion of the guest molecules in kaolinite/dimethyl sulfoxide (DMSO) intercalation compounds Al2Si2O5(OH)4∙(CH3)2SO has been studied by means of solid-state nuclear magnetic resonance (NMR) in the temperature range between 300 and 380 K, which is just below the evolution temperature. The 13C magic angle spinning (MAS) NMR spectra show 2 inequivalent methyl carbons: 1 methyl carbon is keyed in the ditrigonal hole of the silicate sheet, while the other is located parallel to the sheet. Above 320 K, the 2 peaks have different intensities, suggesting that the keyed methyl groups from some of the DMSO molecules are released from the hole. The 2H NMR spectra have been measured for kaolinite/DMSO-d6 intercalate. The methyl group of the interlayer DMSO molecule undergoes free rotation around its C3 axis over the temperature range studied. The axis of rotation is fixed at the low temperature (about 160 K), and the methyl group initiates a wobbling motion whose amplitude increases with temperature. The wobbling angles have an anisotropy, estimated from theoretical analysis of the 2H spectral line shapes. The DMSO molecules released from the silicate layer undergo anisotropic rotation of the whole molecule.

Keywords

2H NMR13C NMRDimethyl SulfoxideIntercalation CompoundKaoliniteLayered Silicate
Type
Research Article
Information
Clays and Clay Minerals , Volume 45 , Issue 5 , October 1997 , pp. 724 - 732
Copyright
Copyright © 1997, The Clay Minerals Society

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