Silicophosphates containing SiO6 octahedra – anhydrous synthesis under ambient conditions

Sandra Jähnigen; Erica Brendler; Uwe Böhme; Gerhard Heide; Edwin Kroke

doi:10.1039/C3NJ00721A

Silicophosphates containing SiO₆ octahedra – anhydrous synthesis under ambient conditions

Sandra Jähnigen,^a Erica Brendler,^b Uwe Böhme,^a Gerhard Heide^c and Edwin Kroke*^a

* Corresponding authors

^a TU Bergakademie Freiberg, Institut für Anorganische Chemie, Leipziger Straße 29, 09596 Freiberg, Germany
E-mail: kroke@tu-freiberg.de
Fax: +49 (0)3731 394058
Tel: +49 (0)3731 393174

^b TU Bergakademie Freiberg, Institut für Analytische Chemie, Leipziger Straße 29, 09596 Freiberg, Germany

^c TU Bergakademie Freiberg, Institut für Mineralogie, Brennhausgasse 14, 09596 Freiberg, Germany

Abstract

Reactions of anhydrous H₃PO₄ with different tetraalkoxysilanes (Si(OR)₄, R = Me, Et, ⁱPr, ⁿBu) in a 1 : 1 molar ratio in diethylether at room temperature and normal pressure generate silicophosphates (SiPOs). Solid state ²⁹Si NMR investigations clearly indicate that the precipitates contain large amounts of SiO₆-species. The substructures of the products are strongly influenced by the alkyl substituents R of the tetraalkoxysilanes, as further supported by ³¹P MAS, ¹³C CP/MAS NMR and FTIR spectroscopy. All solid products are amorphous containing P : Si-ratios of 1.2–1.7, which was proved by powder XRD and elemental analysis. Since small amounts of water may be formed in the H₃PO₄–Si(OR)₄-systems upon condensation and esterification reactions (which results in reaction mixtures being not completely anhydrous), the reactivity of P₄O₁₀ towards tetraethoxysilane was investigated at room temperature confirming the formation of SiO₆-units as well.

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Publication details

The article was received on 01 Jul 2013, accepted on 23 Nov 2013 and first published on 25 Nov 2013

Article type: Paper

DOI: 10.1039/C3NJ00721A

Citation: New J. Chem., 2014,38, 744-751

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Silicophosphates containing SiO₆ octahedra – anhydrous synthesis under ambient conditions

S. Jähnigen, E. Brendler, U. Böhme, G. Heide and E. Kroke, New J. Chem., 2014, 38, 744
DOI: 10.1039/C3NJ00721A
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Silicophosphates containing SiO₆ octahedra – anhydrous synthesis under ambient conditions

Abstract

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Silicophosphates containing SiO₆ octahedra – anhydrous synthesis under ambient conditions

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