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High-Temperature X-Ray Diffraction, Differential Thermal Analysis and Thermogravimetry of the Kaolinite-Dimethylsulfoxide Intercalation Complex

Published online by Cambridge University Press:  01 January 2024

F. Franco  and
M. D. Ruiz Cruz
F. Franco
Affiliation:
Departamento de Química Inorgánica, Cristalografía y Mineralogía, Facultad de Ciencias, Campus de Teatinos, Universidad de Málaga, Málaga, 29071 Spain
M. D. Ruiz Cruz*
Affiliation:
Departamento de Química Inorgánica, Cristalografía y Mineralogía, Facultad de Ciencias, Campus de Teatinos, Universidad de Málaga, Málaga, 29071 Spain
*
*E-mail address of corresponding author: [email protected]
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Abstract

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The intercalation complex of a kaolinite from Cornwall, UK, with dimethylsulfoxide (DMSO) was studied by high-temperature X-ray diffraction (HTXRD), differential thermal analysis (DTA) and thermogravimetry (TG). The X-ray pattern obtained at room temperature indicated that intercalation of DMSO into kaolinite caused an increase of the basal spacing of kaolinite from 7.14 to 11.19 Å. Heating between 25 and 300°C caused the removal of the DMSO, which occurred over several stages. In a first stage (25–125°C), an expansion (from 11.19 to 11.28 Å) followed by a contraction (from 11.28 to 11.19 Å) is observed, at the same time as the intensity of the basal reflection decreased and was replaced by a broad band extending from ~11 to ~7 Å. In a second stage (125–200°C), the loss of DMSO did not lead to changes in the HTXRD patterns; and finally, in a third stage, the loss of DMSO caused an important increase in intensity and sharpening of the basal reflections of the kaolinite. These stages were also shown by the DTA-TG curves for the complex. The TG curve indicated that the loss of ~15% of the intercalated DMSO occurs below 150°C, and caused the disruption of the structure. The remaining molecules, forming stronger bonds with the kaolinite surfaces, were lost between 150 and 300°C.

Keywords

DimethylsulfoxideDTA-TGHTXRDIntercalation ComplexKaolinite
Type
Research Article
Information
Clays and Clay Minerals , Volume 50 , Issue 1 , February 2002 , pp. 47 - 55
Copyright
Copyright © 2002, The Clay Minerals Society

References

Adams, J.M., (1978) Unifying aspect of the 3-D structures of some intercalates of kaolinite Clays and Clay Minerals 33 291–295 10.1346/CCMN.1978.0260406.Google Scholar
Adams, J.M. and Waltl, G., (1980) Thermal decomposition of a kaolinite:dimethyl sulfoxide intercalate Clays and Clay Minerals 28 130–134 10.1346/CCMN.1980.0280209.Google Scholar
Anton, O. and Rouxhet, P.G., (1977) Note on the intercalation of kaolinite, dickite and halloysite by dimethyl-sulfoxide Clays and Clay Minerals 25 259–263 10.1346/CCMN.1977.0250402.Google Scholar
Cullity, B.D. and Cohen, M., (1956) Diffraction I: The directions of diffracted beams Elements of X-ray Diffraction USA Addison-Wesley publishing company, Inc. 78 103.Google Scholar
Frost, R.L. Kristof, J. Paroz, G.N. and Kloprogge, J.T., (1998) Molecular structure of dimethylsulfoxide intercalated kaolinites The Journal of Physical Chemistry B 102 8519–8532 10.1021/jp982035f.Google Scholar
Frost, R.L. Kristof, J. Horvath, E. and Kloprogge, J.T., (1999) Deintercalation of dimethylsulphoxide intercalated kaolinites — a DTA/TGA and Raman spectroscopic study Themochimica Acta 327 155–166 10.1016/S0040-6031(98)00605-4.Google Scholar
Frost, R.L. Kristof, J. Horvath, E. and Kloprogge, J.T., (1999) Molecular structure of dimethyl sulfoxide in DMSO-intercalated kaolinites at 298 and 77 K The Journal of Physical Chemistry A 48 9654–9660 10.1021/jp991763f.Google Scholar
Gabor, M. Toth, M. Kristof, J. and Gabor, K.H., (1995) Thermal behavior and decomposition of intercalated kaolinite Clays and Clay Minerals 43 223–228 10.1346/CCMN.1995.0430209.Google Scholar
González García, S. and Sánchez Camazano, M., (1965) Complejos de adsorción de los minerales de la arcilla con dimetilsulfóxido Anales de Edafología y Agrobiología 24 495 520.Google Scholar
Hinckley, D.N., (1963) Variability in ‘crystallinity’ values among the kaolin deposits of the coastal plain of Georgia and South Carolina Clays and Clay Minerals 11 229–235 10.1346/CCMN.1962.0110122.Google Scholar
Jacobs, H. Sterckx, M. and Serratosa, J.M., (1970) A contribution to the study of the intercalation of dimethyl sulfoxide in the kaolinite lattice Proceedings of the Reunion Hispano-Belga de Minerales de la Arcilla, Madrid Madrid C.S.I.C. 154 160.Google Scholar
Johnston, C.T. Sposito, G. Bocian, D.F. and Birge, R.R., (1984) Vibrational spectroscopic study of the interlamellar kaolinite-dimethyl sulfoxide complex The Journal of Physical Chemistry 88 5959–5964 10.1021/j150668a043.Google Scholar
MacEwan, D.M.C. Wilson, M.J., Brindley, G.W. and Brown, G., (1980) Interlayer and intercalation complexes of clay minerals Crystal Structures of Clay Minerals and their X-ray Identification London Mineralogical Society 197 284.Google Scholar
Mackenzie, R.C. and Mackenzie, R.C., (1970) Simple phyllosilicates based on gibbsite- and brucite-like sheets Differential Thermal Analysis London Academic Press 497 537.Google Scholar
Olejnik, S. Aylmore, L.A.G. Posner, A.M. and Quirk, J.P., (1968) Infrared spectra of kaolin mineral-dimethylsulfoxide complexes The Journal of Physical Chemistry 72 241–249 10.1021/j100847a045.Google Scholar
Pinnavia, T.J., (1983) Intercalated clay catalysts Science 220 365–371 10.1126/science.220.4595.365.CrossRefGoogle Scholar
Plançon, A. and Zacharie, C., (1990) An expert system for the structural characterization of kaolinite Clay Minerals 25 249–260 10.1180/claymin.1990.025.3.01.Google Scholar
Raupach, M. Barron, P.F. and Thompson, J.G., (1987) Nuclear magnetic resonance, infrared, and X-ray powder diffraction study of dimethylsulfoxide and dimethylselenoxide intercalates with kaolinite Clays and Clay Minerals 35 208–219 10.1346/CCMN.1987.0350307.Google Scholar
Ruiz Cruz, M.D. and Franco, F., (1999) New data on the kaolinite-potassium acetate complex Clay Minerals 34 565–577 10.1180/000985599546451.Google Scholar
Ruiz Cruz, M.D. and Franco, F., (2000) Thermal behavior of the kaolinite-hydrazine intercalation complex Clays and Clay Minerals 48 63–67 10.1346/CCMN.2000.0480108.Google Scholar
Ruiz Cruz, M.D. and Franco, F., (2000) Thermal decomposition of a dickite-hydrazine intercalation complex Clays and Clay Minerals 48 586–592 10.1346/CCMN.2000.0480511.Google Scholar
Sáinchez Camazano, M. and González Garcia, S., (1966) Complejos interlaminares de caolinita y haloisita con líquidos polares Anales de Edafologia y Agrobiología 25 9 25.Google Scholar
Thomas, J.M. Adams, J.M. Graham, S.H. and Tennakoon, D.T.B., (1977) Chemical conversion using sheet silicates intercalates Solid State Chemistry of Energy Conversion and Storage Washington, D.C. American Chemical Society 298–315 10.1021/ba-1977-0163.ch017 Advances in Chemistry Series, 163 .Google Scholar
Thompson, J.G. and Cuff, C., (1985) Crystal structure of kaolinite: dimethylsulfoxide intercalate Clays and Clay Minerals 33 490–500 10.1346/CCMN.1985.0330603.Google Scholar
Weiss, A. Thielepape, W. Orth, H., Heller, L. and Weiss, A., (1966) Neue kaoliniteinlagerungsverbindungen Proceedings of the International Clay Conference, Jerusalem Jerusalem Israel Program for Scientific Translations.Google Scholar
Wiewióra, A. and Brindley, G.W., (1969) Potassium acetate intercalation in kaolinite and its removal; effect of material characteristics Proceedings of the International Clay Conference, Tokyo Jerusalem Israel University Press 723 733.Google Scholar