A novel synthetic route has been developed for the preparation of clay
intercalated palladium catalysts, Liquid sorption and X-ray diffracti
on measurements on ethanol(1)-toluene(2)/hexadecylammonium montmorillo
nite dispersions indicated that a toluene-rich bulk liquid phase was e
quilibrated with a swollen, ethanol-rich interlamellar phase having a
volume of about 0.9 cm(3)/g organoclay. Introduction of palladium(II)
acetate into the organoclay suspension led to the generation and depos
ition of a metallic palladium dispersion in the interlamellar space. T
his system behaved as a versatile nanophase reactor, wherein the ethan
ol functioned as both solvent and reducing agent. The progress of the
Pd2+ --> Pd-0 reaction was monitored spectrophotometrically. The ethan
olic reduction afforded Pd particles 2 to 14 nm in diameter, depending
on the experimental conditions, deposited on clay particle defect sit
es, Organoclays loaded up to 10 mass% Pd were synthesized and characte
rized by BET surface area analysis, transmission electron microscopy,
low-shear rheology, X-ray diffraction, and small-angle Xray scattering
measurements, The Pd-organoclay samples proved to be catalytically ac
tive in olefin hydrogenation in the liquid phase. (C) 1996 Academic Pr
ess, Inc.