Vanadia−silica mixed oxides were prepared via the sol−gel
method involving acid catalysis
together with prehydrolysis in order to achieve matching of the
reactivities of vanadium(V)
oxide triisopropoxide and tetraethoxysilicon(IV) precursors.
Gelation was forced by the
addition of basic solution. The as-received gels were
supercritically dried by semicontinuous
extraction with supercritical CO2 at 313 K (low-temperature
aerogels). The effects of
composition, aging, and calcination temperature on the chemical,
structural, and textural
properties of the solids were investigated. The oxides were
characterized by N2 physisorption,
XRD, vibrational spectroscopy, thermal analysis, UV−vis, and
51V NMR. The low-temperature vanadia−silica aerogels were mesoporous and highly
disperse. The increasing
V content from 5 to 20 wt % nominal V2O5
caused a gradual decline in V dispersion. For 30
wt % “V2O5” the continuous formation of
V−O−V connectivity resulted in crystallization of
V2O5. The effect of aging in basic medium
confined to the textural properties, significantly
increasing BET surface area and especially pore volume. The
prepared aerogels revealed a
marked lack of stability against both apolar solvents in the presence
of peroxides and polar
solvents. The marked thermal stability in air at ≤873 K, however,
combined with
mesoporosity and high V dispersion, render these solids promising
catalysts for gas-phase
reactions.