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Silylation of mechanically ground kaolinite

Published online by Cambridge University Press:  27 February 2018

Q. Tao ,
L. Su ,
R.L. Frost ,
D. Zhang ,
M. Chen ,
W. Shen  and
H. He
Q. Tao
Affiliation:
Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, P.R. China
L. Su
Affiliation:
Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, P.R. China Shenzhen Polytechnic, Shenzhen 518055, P.R. China
R.L. Frost
Affiliation:
School of Chemistry, Physics and Mechanical Engineering, Science and Engineering Faculty, Queensland University of Technology, GPO Box 2434, Brisbane Queensland 4001, Australia
D. Zhang
Affiliation:
Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, P.R. China Shenzhen Polytechnic, Shenzhen 518055, P.R. China
M. Chen
Affiliation:
Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, P.R. China Shenzhen Polytechnic, Shenzhen 518055, P.R. China
W. Shen
Affiliation:
Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, P.R. China
H. He*
Affiliation:
Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, P.R. China
*
*E-mail: [email protected]
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Abstract

Silylated kaolinites were synthesized at 80°C without the use of inert gas protection. The method presented started with mechanical grinding of kaolinite, followed by grafting with 3- aminopropyltriethoxysilane (APTES). The mechanical grinding treatment destroyed the ordered sheets of kaolinite, formed fine fragments and generated broken bonds (undercoordinated metal ions). These broken bonds served as new sites for the condensation with APTES. Fourier transform infrared spectroscopy (FTIR) confirmed the existence of −CH2 from APTES. 29Si cross-polarization magic-angle spinning nuclear magnetic resonance spectroscopy (29Si CP/MAS NMR) showed that the principal bonding mechanism between APTES and kaolinite fitted a tridentate silylation model (T3) with a chemical shift at −66.7 ppm. The silane loadings of the silylated samples were estimated from the mass loss obtained by TG-DTG curves. The results showed that the 6-hour ground kaolinite could be grafted with the most APTES (7.0%) using cyclohexane as solvent. The loaded amount of APTES in the silylated samples obtained in different solvents decreased in the order as: nonpolar solvent > polar solvent with low dielectric constant (toluene) > polar solvent with high dielectric constant (ethanol).

Keywords

silylationmechanical grindingkaolinitebroken bondssolvents
Type
Research Article
Information
Clay Minerals , Volume 49 , Issue 4 , September 2014 , pp. 559 - 568
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2014

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