M. May et al., PRECURSOR ALUMINUM EFFECT IN THE SYNTHESIS OF SOL-GEL SI-AL CATALYSTS- FTIR AND NMR CHARACTERIZATION, Chemistry of materials, 9(11), 1997, pp. 2395-2399
Aluminosilicates were prepared by the sol-gel method using tetraethoxy
silane as silica and aluminum ethoxide, aluminum iso-propoxide, or alu
minum sec-butoxide as alumina sources. An important effect of the alky
laluminum substitutes is observed in the BET specific area, ethoxide >
isopropoxide > sec-butoxide. The Al-27 NMR spectra of the solids show
ed that the relative concentrations of tetrahedral, octahedral, or pen
tacoordinated aluminum strongly depend on the aluminum alkoxide source
. It is shown by Si-29 NMR spectra that the formation of pentacoordina
ted aluminum is related to the odd silicon substitution, Si(1Al, 3Si)
and Si(3Al, 1Si). The odd Si substitution was confirmed by FTIR spectr
oscopy following the Si-O-Si vibration band. The shift of the 1092 cm(
-1) band to 1029 cm(-1) agrees well with the Si-29 NMR odd substitutio
n. In general the aluminum coordination as well as the odd Si substitu
tion is largely affected when the hydrolysis water concentration is va
ried. High activity is shown by the aluminosilicates during the 2-prop
anol dehydration reaction.