Abstract
The reaction of the cubic octameric silicate anion, Si8O 8−20 , with dimethyldichlorosilane in 2,2-dimethoxypropane yielded solid products. FT-IR and solid-state 29Si NMR spectra of the products indicate that the silicate anion becomes cross-linked via the dimethylsilyl group without degradation of the cubic core, resulting in the formation of organic/silica hybrids consisting of the Si8O 8−20 structure as a building block. The hybrids are thermally stable up to ca. 380°C in air. The specific surface area of the hybrids is 31 m2 g−1, while the value increases to 339 m2 g−1 after calcination at 350°C in air. The process of increasing the surface area of the hybrids by the heat-treatment was investigated using solid-state 13C NMR spectroscopy.
Similar content being viewed by others
References
P.C. Cagle, W.G. Klemperer, and C.A. Simmons in Better Ceramics through Chemistry IV, Mather. Res. Soc. Symp. Proc. 180, edited by B.J.J. Zelinski, C.J. Brinker, D.E. Clark, and D.R. Ulrich (Mater. Res. Soc., Pittsburgh, 1990), p. 29.
D. Hoebbel, I. Pitsch, D. Heidemann, H. Jancke, and W. Hiller, Z. Anorg. Allg. Chem. 583, 133 (1990).
D. Hoebbel, I. Pitsch, and D. Heidemann, Z. Anorg. Allg. Chem. 592, 207 (1991).
D. Schultze, P. Kölsch, M. Noack, P. Toussaint, I. Pitsch, and D. Hoebbel, Z. Anorg. Allg. Chem. 612, 137 (1992).
D. Hoebbel, T. Reinert, K. Endres, H. Schmidt, A. Kayan, and E. Arpac in Proceedings of the First European Workshop on Hybrid Organic-Inorganic Materials, edited by C. Sanchez and F. Ribot (Bierville, 1993), p. 319.
D. Hoebbel, K. Endres, T. Reinert, and H. Schmidt in Better Ceramics through Chemistry VI, Mater. Res. Soc, Symp. Proc. 346, edited by A.K. Cheetham, C.J. Brinker, M.L. Mecartney, and C. Sanchez (Mater. Res. Soc., Pittsburgh, 1994), p. 863.
P. Kölsch, I. Pitsch, D. Schultze, D. Heidemann, and D. Hoebbel, J. Therm. Anal. 41, 789 (1994).
D. Hoebbel, K. Endres, T. Reinert, and I. Pitsch, J. Non-Cryst. Solids 176, 179 (1994).
P.A. Agaskar, J. Am. Chem. Soc. 111, 6858 (1989).
P.A. Agaskar in Proceedings of the 2nd A.N.A.I.C. Conference on Materials Science of Main-Group Elements (Springer-Verlag, Berlin) in the press.
I. Hasegawa, M. Ishida, and S. Motojima in Proceedings of the First European Workshop on Hybrid Organic-Inorganic Materials, edited by C. Sanchez and F. Ribot (Bierville, 1993), p. 329.
I. Hasegawa, M. Ishida, S. Motojima, and S. Satokawa in Better Ceramics through Chemistry VI, Mater. Res. Soc. Symp. Proc. 346, edited by A.K. Cheetham, C.J. Brinker, M.L. Mecartney, and C. Sanchez (Mater. Res. Soc., Pittsburgh, 1994), p. 163.
F.J. Feher and K.J. Weller, Chem. Mater. 6, 7 (1994).
W.M. Meier in Molecular Sieves (Society for Chemical Industry, London, 1968), p. 10.
I. Hasegawa, S. Sakka, K. Kuroda, and C. Kato, J. Mol. Liq. 34, 307 (1987).
I. Hasegawa, S. Sakka, Y. Sugahara, K. Kuroda, and C. Kato, J. Chem. Soc., Chem. Commun. 1989, 208 (1989).
I. Hasegawa and S. Motojima, J. Organomet. Chem. 441, 373 (1992).
I. Hasegawa, M. Ishida, and S. Motojima, Synth. React. Inorg. Met.-Org. Chem. 24, 1099 (1994).
P.A. Agaskar, Inorg, Chem. 29, 1603 (1990).
I. Hasegawa, Zeolites 12, 720 (1992).
L.S.D. Glasser, E.E. Lachowski, R.K. Harris, and J. Jones, J. Mol. Struct. 51, 239 (1979).
I. Hasegawa, Polyhedron 10, 1097 (1991).
E.D. Lipp and A.L. Smith in The Analytical Chemistry of Silicones, edited by A.L. Smith (John Wiley & Sons, New York, 1991), pp. 319–330.
F. Babonneau, K. Thorne, and J.D. Mackenzie, Chem. Mater. 1, 554 (1989).
F. Babonneau, L. Bois, J. Maquet, and J. Livage in EUROGEL '91, edited by S. Vilminot, R. Nass, and H. Schmidt (Elsevier, Amsterdam, 1992), p. 319.
V. Belot, R.J.P. Corriu, D. Leclercq, P.H. Mutin, and A. Vioux, J. Polym. Sci., Polym. Chem. Ed. 30, 613 (1992).
R.H. Jarmain and M.T. Melchior, J. Chem. Soc., Chem. Commun. 1984, 414 (1984).
R.B. Taylor, B. Parbhoo, and D.M. Fillmore in The Analytical Chemistry of Silicones, edited by A.L. Smith (John Wiley & Sons, New York, 1991), p. 364.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Hasegawa, I. Building block approach to organic/silica hybrid materials. J Sol-Gel Sci Technol 5, 93–100 (1995). https://doi.org/10.1007/BF00487725
Received:
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF00487725