Publication details

Synthesis of homogeneous silicophosphate xerogels by non-hydrolytic condensation reactions

Authors

STÝSKALÍK Aleš ŠKODA David MORAVEC Zdeněk ABBOTT JG BARNES CE PINKAS Jiří

Year of publication 2014
Type Article in Periodical
Magazine / Source MICROPOROUS AND MESOPOROUS MATERIALS
MU Faculty or unit

Central European Institute of Technology

Citation
Web http://www.sciencedirect.com/science/article/pii/S1387181114003370#
Doi http://dx.doi.org/10.1016/j.micromeso.2014.06.019
Field Inorganic chemistry
Keywords Sol-Gel; Non-hydrolytic; Silicophosphate; Phosphosilicate; Xerogel
Description A novel non-hydrolytic synthesis of silicophosphate xerogels and optimization of reaction conditions to obtain products with a high degree of condensation and a large specific surface area are presented. Homogeneous products with a high content of Si-O-P bonds and SiO6 moieties were synthesized by an ester elimination route at low temperature from silicon acetate, Si(OAc)(4), and tris(trimethylsilyl) phosphate, OP(OSiMe3)(3) (TTP). Depending on the reaction conditions (temperature, solvent, time) it was possible to control the degree of condensation (up to 85.7%) and porosity of amorphous xerogels (apparent surface areas from 230 to 568 m(2) g(-1)). The composition and morphology of the xerogels, volatile reaction byproducts, thermal transformations and surface modification with methanol were followed by elemental analysis, IR spectroscopy, thermal analysis TG-DSC, nitrogen adsorption, C-13, Si-29, and P-31 solid-state NMR spectroscopy, and powder XRD. (C) 2014 Elsevier Inc. All rights reserved.
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