Abstract
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 568m2g−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, 13C, 29Si, and 31P solid-state NMR spectroscopy, and powder XRD.
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