Sa. Bagshaw et al., MESOPOROUS [M]-MSU-X METALLO-SILICATE CATALYSTS BY NONIONIC POLYETHYLENE OXIDE SURFACTANT TEMPLATING ACID [N-0(N-I+] AND BASE ((NM+I-)-M-0)CATALYZED PATHWAYS()X), MICROPOROUS AND MESOPOROUS MATERIALS, 22(1-3), 1998, pp. 419-433
Solutions of low and high pH have been used to form non-ionically temp
lated mesoporous metallo-silicates [M]-MSU-x materials; where [M] = Al
, Ti, V and Zr. Two new assembly routes are proposed which exploit the
acid and base catalysed hydrolysis and simultaneous condensation of m
etal ore-salts and silicon tetraethoxide. Acid catalysed hydrolysis, l
abeled (NX-I+)-X-0 or N+X-I+ (N-0 = nonyl-phenyl polyethylene oxide, X
- = Cl- or SO42-, I+ = protonated tetraethyl orthosilicate), produces
well-defined materials with uniform pores in the small mesoporous regi
on and moderate pore volumes, but reduced metal incorporation owing to
the high solubilities of metal cations in acidic solutions. Base cata
lysed hydrolysis, labeled (NM+I-)-M-0 (N-0 = nonyl-phenyl polyethylene
oxide, M+ = Na+ or NH4+, I- = hydroxylated tetraethyl orthosilicate),
also leads to materials with uniform channels in the small mesoporous
region. Pore volumes and metal substitution are higher and framework
shrinkage during calcination is reduced as a result of thicker pore wa
lls. These new pathways show distinct similarities to those described
by Attard et al. [Nature 378 (1995) 366] and Zhao et al. [Science 279
(1998) 548] for the formation of hexagonally symmetric silica from nan
-ionic surfactants under acidic conditions and also to mesoporous MCM-
41 assembly routes via (S+X-I+) anion mediated acid catalysed assembly
. The results demonstrate the feasibility of preparing templated mesop
orous metallo-silicates from non-ionic polyethylene oxide surfactants
and metal oxy-hydroxy cationic precursors, but indicate that further o
ptimisation of the reaction conditions is required to maximise the pot
ential of this synthesis approach. (C) 1998 Elsevier Science B.V. All
rights reserved.