Hostname: page-component-8448b6f56d-jr42d Total loading time: 0 Render date: 2024-04-19T05:46:29.387Z Has data issue: false hasContentIssue false

Kinetics of deintercalation of potassium acetate from kaolinite — a Raman spectroscopic study

Published online by Cambridge University Press:  09 July 2018

R. L. Frost
Affiliation:
Centre for instrumental and Developmental Chemistry, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane Queensland 4001, Australia
J. Kristof
Affiliation:
Department of Analytical Chemistry, University of Veszprem, H8201 Veszprem, PO Box 158, Hungary
T. H. Tran
Affiliation:
Centre for instrumental and Developmental Chemistry, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane Queensland 4001, Australia

Abstract

The kinetics of structural change of a highly ordered kaolinite intercalated with potassium acetate have been studied through both intercalation and deintercalation. Deintercalation of the intercalated kaolinite, brought about by washing for different time intervals was followed by both X-ray diffraction and Raman microscopy. X-ray diffraction shows the kaolinite to be highly ordered with a Hinekley index of 1.42 and intercalated to ~90%. X-ray diffraction also showed that the intercalated kaolinite was deintercalated by 80% in the first minute of washing. An additional Raman band, attributed to the inner surface hydroxyl groups, strongly hydrogen bound to the acetate, is observed at 3605 cm-1 for the potassium acetate intercalate with the concomitant loss of intensity in the bands at 3652, 3670, 3684 and 3693 cm-1. Upon deintercalation, the intensity of the 3605 cm-1 band decreased as the 3695 cm-1 band increased. The Raman spectral changes brought about upon deintercalation mirrored the changes observed by X-ray diffraction. Deintercalation of kaolinite caused disordering of the kaolinite.

Type
Research Article
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 1998

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Barrios, J., Plancon, A., Cruz, M.I. & Tchoubar, C. (1977) Qualitative and quantitative study of the stacking faults in hydrazine treated kaolinite. Relationship with the infrared spectra. Clays Clay Miner. 25, 422429.Google Scholar
Brindley, G.W. & Brown, G. (editors) (1984) Crystal Structures of Clay Minerals and their X-ray Identification. Mineralogical Society, London.Google Scholar
Brindley, G.W., Chih-Chun Kao, Harrison, J.L., Lipsiscas, M. & Raythatha, R. (1986) Relation between the structural disorder and other characteristics of kaolinites and dickites. Clays Clay Miner. 34, 233249.Google Scholar
Costanzo, P.M., Giese, R.F. & Lipsicas, M. (1984) Static and dynamic structure of water in hydrated kaolinite. I. The static structure. Clays Clay Miner. 32, 419428.Google Scholar
Farmer, V.C. (1974) The layer silicates. Pp 331-363 in: Infrared Spectra of Minerals. (Farmer, V.C., editor) Mineralogical Society, London.CrossRefGoogle Scholar
Frost, R.L. (1995) Fourier Transform Raman spectroscopy of kaolinite, dickite and halloysite. Clays Clay Miner. 43, 191195.Google Scholar
Frost, R.L. (1997) The structure of kaolinite–an FT Raman study. Clay Miner. 32, 7385.Google Scholar
Frost, R.L. & van der Gaast SJ. (1997) Kaolinite hydroxyls–a Raman microscopy study. Clay Miner. 32, 293306.Google Scholar
Frost, R.L., Fredericks, P.M. & Bartlett, J.R. (1993) FT Raman spectroscopy of the kandite clay minerals. Speetrochim. Acta, 20, 667674.Google Scholar
Hess, C.A. & Saunders, V.R. (1992) Periodic ab initio Hartree-Fock calculations of the low symmetry mineral kaolinite. J. Phys. Chem. 96, 43674374.Google Scholar
Johnston, C.T. & Stone, D.A. (1990) Influence of hydrazine on the vibrational modes of kaolinite. Clays Clay Miner. 38, 121128.Google Scholar
Johnston, C.T., Sposito, G. & Birge, R.R. (1985). Raman spectroscopic study of kaolinite in aqueous suspension. Clays Clay Miner. 33, 483489.Google Scholar
Johnston, C.T., Agnew, S.F. & Bish, D.L., (1990) Polarised single-crystal Fourier Transform Infrared Microscopy of Ouray dickite and Keokuk kaolinite. Clays Clay Miner. 38, 573583.Google Scholar
Lagaly, G. (1984) Clay organic reactions. Phil Trans. R. Soc. Lond. A311, 315332.Google Scholar
Ledoux, R.L. & White, J.L. (1966) Infrared studies of hydrogen bonding interaction between kaolinite surfaces and intercalated potassium acetate, hydrazinc, formamide and urea. J. Coll. Inter[: Sci. 21, 127152.Google Scholar
Ledoux, R.L. & White, J.L. (1967) Infrared study of intercalation complexes of kaolinite. Silicates Ind. 32, 26973.Google Scholar
Michaelian, K.H. (1986) The Raman spectrum of kaolinite #9 at 21°. Can. J. Chem. 64, 285289.CrossRefGoogle Scholar
Raupach, M., BarTon, P.F. & Thompson, J.G. (1987) Nuclear magnetic resonance, infrared, and x-ray powder diffraction study of dimethylsulfoxide and dimethylselenoxide intercalates with kaolinite. Clays Clay Miner. 35, 20819.Google Scholar
Thompson, J.G. & Cuff, C. (1985) Crystal structure of kaolinite: dimethyl sulfoxide intercalate. Clays Clay Miner. 33, 490500.Google Scholar
Weiss, A., Thielepape, W., Ritter, W., Schafer, H. & Goring, G. (1963) Zur Kenntnis von hydrazin-Wiewior kaolinit. Anorg. Allg. Chem. 320, 183204.Google Scholar
Weiss, A., Thielepape, W. & Orth, H. (1966) Intercalation into kaolinite minerals. Proc. Int. Clay Conf. Jerusalem I, 277-293.Google Scholar
Wiewiora, A., Wieckowski, T. & Sokolowska, A. (1979) The Raman spectra of kaolinite subgroup minerals and of pyrophyllite. Arch. MineraL, 135, 514.Google Scholar