A series of Rh/SiO2 catalysts were prepared by the sol-gel method. The
precursors used were tetraethoxysilane (TEOS) dissolved in ethanol an
d rhodium(III) acetylacetonate dissolved in acetone. Preparative varia
bles include the amount of water added to the sol and the gelation tem
perature. Typical BET surface areas were 550-700 m(2) g(-1) with very
narrow pore size distributions centered at approximately 4 nm. Sample
characterization studies were performed using TGA-DTA-MS to determine
the effect of O-2 pretreatment and Si-29 solid-state NMR to determine
the extent to which silica was condensed. Sintering studies of Rh/SiO2
catalysts for which there was a reasonable match between metal partic
le size and pore diameter were performed. Catalysts prepared by ion-ex
change having comparable dispersions to those prepared by the sol-gel
method also showed considerable resistance to sintering in O-2. Follow
ing heat treatment in O-2 at 650 degrees C, the particle size distribu
tion of catalysts prepared by ion-exchange appear to broaden to a grea
ter extent than catalysts prepared by the sol-gel method. This suggest
s that the sol-gel preparation is more effective in retaining the meta
l particles within the narrow pores of the support. (C) 1997 Elsevier
Science B.V.