G. Fetter et al., SYNTHESIS AND CHARACTERIZATION OF PILLARED CLAYS CONTAINING BOTH SI AND A1 PILLARS, Applied catalysis. A, General, 126(1), 1995, pp. 165-176
A Wyoming montmorillonite clay has been intercalated using the competi
tive ion exchange of aluminum hydroxy polycations and oligosilsesquiox
anes. Whereas the intercalation of montmorillonite by the products of
hydrolysis of trichlorosilylethylpyridine yields an heterogeneous soli
d; with a large fraction non-intercalated, the X-ray diffraction shows
that competitive intercalation permits a nearly complete intercalatio
n of the material. The lattice spacing of 21.4 Angstrom after ion exch
ange, is determined by the size of the largest oligosilsesquioxane cat
ions. It is reduced to 17.4 Angstrom after calcination at 873 K where
Si-29 and Al-27 MAS-NMR Show the existence of the two types of pillars
with respectively the siloxane and Al-13 structure, After calcination
at 973 K, a clear 001 XRD line is observed, and the microporous volum
e is 0.13 ml g(-1), thus showing a good thermal stability. The number
and strength of acid sites determined by adsorption of ammonia is comp
arable to that of HY zeolites. This strong acidity is related in part
to the stability of the structure, and to the retention of the individ
uality of the Al-13 pillars. The tetrahedral aluminum atom of the pill
ars is assumed to be responsible for this strong acidity.