Publication details

Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate

Authors

STÝSKALÍK Aleš ŠKODA David MORAVEC Zdeněk ROUPCOVÁ Pavla BARNES Craig E. PINKAS Jiří

Year of publication 2015
Type Article in Periodical
Magazine / Source RSC Advances
MU Faculty or unit

Central European Institute of Technology

Citation
Doi http://dx.doi.org/10.1039/c5ra10982e
Field Inorganic chemistry
Keywords PHOSPHORIC-ACID CATALYST; ORGANIC-INORGANIC HYBRID; SOL-GEL SYNTHESIS; PHOSPHOSILICATE GELS; AMBIENT CONDITIONS; CRYSTAL-STRUCTURE; MOLECULAR-SIEVES; SURFACE-AREA; MAS NMR; GLASSES
Description The first synthesis of mesoporous nanocrystalline silicon orthophosphate Si5P6O25 is presented. The synthetic procedure is based on the non-hydrolytic sol-gel reaction in the presence of Pluronic P123 template and subsequent calcination in air. The condensation of silicon acetate, Si(OAc)(4), and tris(trimethylsilyl) phosphate, OP(OSiMe3)(3) (TTP), in non-aqueous solvents driven by elimination of trimethylsilyl acetate provides a homogeneous network with a high content of Si-O-P bonds and SiO6 moieties. After burning out the template, mesoporous silicon orthophosphate was obtained with surface areas up to 128 m(2) g(-1) and pore sizes around 20 nm. The nanocrystalline Si5P6O25 phase forms relatively easily (500 degrees C, 4 h) in comparison with other synthetic routes. All samples were characterized by SEM, TEM, elemental analysis, TGA, nitrogen adsorption, SAXS, H-1, C-13, Si-29, and P-31 solid-state NMR spectroscopy, and powder XRD. These xerogels showed superior catalytic activity and selectivity in methylstyrene dimerization.
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