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Covalent Grafting of Organoalkoxysilanes on Silica Surfaces in Water-Rich Medium as Evidenced by 29Si NMR

Published online by Cambridge University Press:  17 March 2011

Christian Bonhomme
Affiliation:
Laboratoire chimie de la matière condensée, Universite P et M Curie, 4 place Jussieu, Paris, France
Sophie De Monredon
Affiliation:
Laboratoire chimie de la matière condensée, Universite P et M Curie, 4 place Jussieu, Paris, France
François Ribot
Affiliation:
Laboratoire chimie de la matière condensée, Universite P et M Curie, 4 place Jussieu, Paris, France
Florence Babonneau
Affiliation:
Laboratoire chimie de la matière condensée, Universite P et M Curie, 4 place Jussieu, Paris, France
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Abstract

Despite the huge amount of experimental investigations dedicated to the grafting of organoalkoxysilanes on silica, the characterization of covalent linkages remains a difficult task from a spectroscopic point of view. In most cases, the formation of a covalent link is taken for granted and not discussed. 29Si NMR, IR or UV spectroscopies are commonly used to study the modification of silica surface. Herein we report an unambiguous method to evidence the formation of covalent links. It is based on NMR spectroscopy analysis coupled with a rigorous synthetic grafting protocol.

Type
Research Article
Copyright
Copyright © Materials Research Society 2007

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References

REFERENCES

1. Isarov, A. and Lynch, T. J., Application: US Pat., US 2005/069708 A1, (2005).Google Scholar
2. Liu, X. and Bordunov, A. V., Application: WO Pat., WO 03/076040 A1, (2003).Google Scholar
3. Czuryszkiewicz, T., Ahvenlammi, J., Kortesuo, P., Ahola, M., Kleitz, F., Jokinen, M., Linden, M. and Rosenholm, J. B., J. Non-Cryst. Solids, 306, 1 (2002).Google Scholar
4. Price, P. M., Clark, J. H. and Macquarrie, D. J., J.Chem. Soc., Dalton Trans., 101 (2000).Google Scholar
5. Eaton, P., Holmes, P. and Yarwood, J., Appl. Spectrosc, 54, 508 (2000).Google Scholar
6. Collet, J., Tharaud, O., Chapoton, A. and Vuillaume, D., Applied Physics Letters, 76, 1941 (2000).Google Scholar
7. Meyer, J., Frahn, S. and Ettlinger, M., Application: DE Pat., WO 2004/020531 A1, (2004).Google Scholar
8. Greenwood, P., Application: US US Pat., US 2004/077768, (2004).Google Scholar
9. Dkhissi, A., Esteve, A., Jeloaica, L., Esteve, D. and Rouhani, M. D., J. Am. Chem. Soc., 127, 9776 (2005).Google Scholar
10. Caravajal, G. S., Leyden, D. E., Quinting, G. R. and Maciel, G. E., Anal. Chem., 60, 1776 (1988).Google Scholar
11. Sindorf, D. W. and Maciel, G. E., J. Phys. Chem., 86, 5208 (1982).Google Scholar
12. Bourgeat-Lami, E., Luna-Xavier, J.-L. and Guyot, A., Mater. Res. Soc. Symp. Proc., 628, CC3.5.1 (2000).Google Scholar
13. Tao, T. and Maciel, G. E., J. Am. Chem. Soc., 122, 3118 (2000).Google Scholar
14. Massiot, D., Fayon, F., Capron, M., King, I., LeCalvé, S., Alonso, B., Durand, J.-O., Bujoli, B., Gan, Z. and Hoatson, G., Magn. Res. Chem., 40, 70 (2002).Google Scholar
15. Derome, A. E., Modern NMR techniques for chemistry research., Pergamon Press, 1987).Google Scholar
16. Engelhardt, H., High resolution solid state NMR of silicates & zeolithes, (John Wiley & Sons edn., 1987).Google Scholar
17. Sutra, P., Fajula, F., Brunel, D., Lentz, P., Daelen, G. and Nagy, J. B., Colloids and Surfaces: A, 158, 21 (1999).Google Scholar
18. Sugahara, Y., Okada, S., Kuroda, K. and Kato, C., J. Non-Cryst. Solids, 139, 25 (1992).Google Scholar
19. Babonneau, F., Bois, L. and Livage, J., Mater. Res. Soc. Symp. Proc., 271, 237 (1992).Google Scholar
20. Rankin, S. E. and McCormick, A. V., Magn. Reson. Chem., 37, S27 (1999).Google Scholar
21. Babonneau, F., Polyhedron, 13, 1123 (1994).Google Scholar
22. Hasegawa, I., Ishida, M., Motojima, S. and Satokawa, S., Mater. Res. Soc. Symp. Proc., 346, 163 (1994).Google Scholar