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Clays and Clay Minerals; February 2008; v. 56; no. 1; p. 82-89; DOI: 10.1346/CCMN.2008.0560107
© 2008 Clay Minerals Society
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IONIC LIQUIDS-KAOLINITE NANOSTRUCTURED MATERIALS. INTERCALATION OF PYRROLIDINIUM SALTS

Sadok Letaief* and Christian Detellier

1 Centre for Catalysis Research and Innovation, and Department of Chemistry, University of Ottawa, 10 Marie Curie, Ottawa, Ontario, Canada K1N 6N5

* E-mail address of corresponding author: lsado{at}science.uottawa.ca

Ionic liquids intercalated in kaolinite constitute a novel class of nanostructured material. Kaolinite-pyrrolidinium halide intercalates have been prepared successfully by reacting the pyrrolidinium salts with kaolinite which was preintercalated with dimethyl sulfoxide (DMSO) using the melt condition under N2. X-ray diffraction, 13C magic angle spinning nuclear magnetic resonance, differential thermal analysis (DTA)-thermal gravimetric analysis, and Fourier transform infrared spectroscopy confirm the displacement of DMSO during the intercalation process. Based on results from the various characterization techniques, a structural model is proposed in which one mole of the pyrrolidinium salt covers two or three structural units of kaolinite, depending on the structure and size of the salt. The thermal stability was improved remarkably after intercalation of the pyrrolidinium salts, compared to the pre-intercalate. The DTA-TGA data show that the largest number of organic units released and decomposed, occurs under N2 flow, at temperatures ranging from 260 to 340°C, depending on the nature of the intercalated organic salts.

Key Words: 13C CP/MAS NMR • FTIR • Intercalation • Ionic Liquids • Kaolinite • Nanohybrid Materials • Nanostructured Materials • Pyrrolidinium • 29Si CP/MAS NMR • TGA • XRD






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