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Acid-Treated Montmorillonites—A Study by 29Si and 27Al MAS NMR

Published online by Cambridge University Press:  09 July 2018

I. Tkáč
Affiliation:
Institute of Inorganic Chemistry, Slovak Academy of Sciences, 842 36 Bratislava, Slovakia
P. Komadel
Affiliation:
Institute of Inorganic Chemistry, Slovak Academy of Sciences, 842 36 Bratislava, Slovakia
D. Müller*
Affiliation:
Wissenschaftler-Integrations-Programm, KAI e.V., 0-1199 Berlin-Adlershof, Germany

Abstract

The JP (Jelšový Potok, Slovakia) and SWy-1 (Wyoming, USA) montmorillonites were treated in 6 m HCl at 95°C. The rates of dissolution of tetrahedral and octahedral Al (Altet and Aloct) are comparable. Aluminium in the tetrahedral sheets was also identified in both untreated samples by 29Si MAS NMR spectroscopy. About 12% of total Si in SWy-1 was found to be bound in quartz. Traces of undecomposed montmorillonite and a small amount of Altet in the three-dimensional SiO4 framework were found in the reaction product of montmorillonite decomposition. Three different types of structural units were identified in acid-treated samples: Q4(OAl) units of amorphous silica with three-dimensional crosslinked framework; (SiO)3SiOH units, remaining as a result of poor-ordering of the framework without the possibility of cross-linking; and Q4(1A1) units.

Type
Research Article
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 1994

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References

Adams, J.M. (1987) Synthetic organic chemistry using pillared, cation-exchanged and acid treated montmorillo- nite catalysts—A review. Appl. Clay Sd.. 2, 309342.CrossRefGoogle Scholar
Adams, S. J., Hawkes, G.E. & Curzon, E.H. (1991) A solid state 29Si nuclear magnetic resonance study of opal and other hydrous silicas. Am. Miner.. 76, 18631871.Google Scholar
Breen, C. (1988) the acidity of trivalent cation-exchanged montmorillonite. II. Desorption of mono- and di-substi- tuted pyridines. Clay Miner.. 23, 323328.Google Scholar
Breen, C. (1991a) Thermogravimetric study of the desorption of cyclohexylamine and pyridine from an acid- treated Wyoming bentonite. Clay Miner. 26, 473–186.CrossRefGoogle Scholar
Breen, C. (1991b) Thermogravimetric and infrared study of the desorption of butylamine, cyclohexylamine and pyridine from Ni- and Co-exchanged montmorillonite. Clay Miner. 26, 487—496.Google Scholar
Breen, C., Deane, A.T. & Flynn, J.J. (1987) The acidity of trivalent cation-exchanged montmorillonite. Temperature-programmed desorption and infrared studies of pyridine and n-butylamine. Clay Miner.. 22, 169178.Google Scholar
Cetisli, H. & Gedikbey, T. (1990) Dissolution kinetics of sepiolite from Eskisehir (Turkey) in hydrochloric and nitric acids. Clay Miner. 25, 207215.CrossRefGoogle Scholar
Čičel, B. & Novak, I. (1977) Dissolution of smectites in HCl: I. Half-time of dissolution as a measure of reaction rate. Proc. 7th Conf. Clay. Miner. Petrol. Karlovy Vary. 163-171.Google Scholar
Číčel, B., Novak, I. & Pivovarníček, F. (1965) Dissolution of montmorillonites in HCl and its possible application in the study of their activation. Silikat. 9, 130139.(in Slovak).Google Scholar
Cíčel, B., Komadel, P., Bednáriková E. & Madejová J. (1992) Mineralogical composition and distribution of Si, Al, Fe, Mg and C. in the fine fraccións of some Czech and Slovak bentonites. Geol. Carpath., Ser. Clay.. 43, 37.Google Scholar
Corma, A., Mifsud, A. & Sanz, E. (1990) Kinetics of the acid leaching of palygorskite: Influence of the octahedral sheet composition. Clay Miner. 25, 197205.CrossRefGoogle Scholar
Engelhardt, G. & Michel, D. (1987) High-Resolution Solid-State NMR of Silicates and Zeolites, p. 154. J. Wiley, Chichester.Google Scholar
Fahn, R. (1973) Influence of the structure and morphology of bleaching earths on their bleaching action on oils and fats. Fette, Seifen, Anstrichmit. 75, 7782.Google Scholar
Fahn, R. & Fenderl, K. (1983) Reaction products of organic dye molecules with acid treated montmorillonite. Clay Miner. 18, 447–158.Google Scholar
Gracia, M., Gancedo, J.R., Marco, J.F., Franco, M.J., Mendioroz, S. & Pajares, J.A. (1989) Mössbauer study of iron removal in a montmorillonite. Hyperfine Interaction. 46, 629634.Google Scholar
Gregor, M. & Číčel, B. (1969) Bleaching earth. Pp. 218-254 in: Bentonite and its Application. Publishing House SAS, Bratislava (in Slovak).Google Scholar
Güler, C. & Sarier, N. (1990) Kinetics of the thermal dehydration of acid-activated montmorillonite by the rising temperature technique. Thermochim. Act.. 159, 2933.Google Scholar
Heidemann, D., Grimmer, A.R., Hüber, C., Starke, P. & Magi, M. (1985) Hochauflosende 29Si-festkorper-NMR- untersuchungen and polykristallinen Phyllokieselsauren (H2Si2O5)x bei tiefem und hohem Magnetfeld. Z. Anorg. Allg. Chem.. 528, 2236.Google Scholar
Jovanovič, N. & Janačkovič J. (1991) Pore structure and adsorption properties of an acid activated bentonite. Appl. Clay Sci.. 6, 5968.CrossRefGoogle Scholar
Kirkpatrick, R.J. (1988) MAS NMR spectroscopy of minerals and glasses. Pp. 341403.in: Spectroscopic Methods in Mineralogy and Geology (F. C. Hawthorne, editor), Mineralogical Society of America, Washington DC.CrossRefGoogle Scholar
Komadel, P., Madejová, J., Putyera, K. & Číčel, B. (1991) Structural formulas of SWy-1 montmorillonite. Proc. 7th Euroclay Conf. Dresden, 605610.Google Scholar
Komadel, P., Schmidt, D., Madejová, J. & Číčel, B. (1990) Alteration of smectites by treatments with hydrochloric acid and sodium carbonate solutions. Appl. Clay Sci.. 5, 113122.Google Scholar
Komarneni, S., Fyfe, C. A., Kennedy, G.I. & Strobl, H. (1986) Characterization of synthetic and naturally occur- ing clays by 27Al and 29Si magic-angle spinning NMR spectroscopy. J. Am. Ceram. Soc., 69, C45C47.Google Scholar
Lippmaa, E. T., Samoson, A. W., Brei, W.W. & Gorlov, Yu. J. (1981) High-resolution solid-state 2,Si and 'H NMR study of the surface structure of highly disperse silicates. Doki. Akad. Nuuk. SSSR.. 259, 403408.(in Russian).Google Scholar
Luca, V. & MacLachlan, D.J. (1992) Site occupancy in nontronite studied by acid dissolution and Mössbauer spectroscopy. Clays Clay Miner. 40, 17.Google Scholar
Maciel, G.E. & Sindorf, D.W. (1980) Silicon-29 nuclear magnetic resonance study of the surface of silica gel by cross-polarization and magic-angle spinning. J. Am. Chem. Soc... 102, 76067607.CrossRefGoogle Scholar
Madejová, J., Komadel, P. & Číčel, B. (1992) Infrared spectra of some Czech and Slovak smectites and their correlation with structural formulas. Geol. Carpath., Ser. Clay.. 43, 912.Google Scholar
Morgan, D.A., Shaw, D.B., Sidebottom, M. J., Soon, T.C. & Taylor, R.S. (1985) The function of bleaching earths in the processing of palm, palm kernel and coconut oil. J. Am. Oil Chem. Soc.. 62, 292299.Google Scholar
Morris, H.D., Bank, S. & Ellis, P.D. (1990) 27Al NMR spectroscopy of iron bearing montmorillonite clays. J. Phys. Chem.. 94, 31213129.CrossRefGoogle Scholar
Novak, I. & Číčel, B. (1978) Dissolution of smectites in HCl: II. Dissolution rate as a function of crystallochemical composition. Clays Clay Miner.. 26, 341344.Google Scholar
Osthaus, B.B. (1956) Kinetic studies on montmorillonite and nontronite by the acid dissolution technique. Clays Clay Miner. 4, 301321.Google Scholar
Rhodes, C.N., Franks, M., Parkes, G.M. B. & Brown, D. R. (1991) The effect of acid treatment on the activity of clay supports for ZnCl2 alkylation catalysts. J. Chem. Soc., Chem. Commun. 805-807.CrossRefGoogle Scholar
Sherriff, B. L., Grundy, H.D. & Hartman, J.S. (1991) The relationship between 29Si MAS NMR chemical shift and silicate mineral structure. Eur. J. Mineral.. 3, 751768.Google Scholar
Siddiqui, M. K. H. (1968) Bleaching Earths. 86 pp. Pergamon Press, Oxford.Google Scholar
Thompson, J. G. (1984) 29Si and 27Al nuclear magnetic resonance spectroscopy of 2:1 clay minerals. Clay Miner. 19, 229236.Google Scholar
Woessner, D. E. (1989) Characterization of clay minerals by 27A1 nuclear magnetic resonance spectroscopy. Am. Mineral.. 74, 203215.Google Scholar