T. Skapin, PREPARATION AND PROPERTIES OF HIGHLY FLUORINATED ALUMINA PREPARED FROM BOEHMITE AEROGELS OR COMMERCIAL GAMMA-AI(2)O(3), Journal of materials chemistry, 5(8), 1995, pp. 1215-1222
Pellets of alumina-based aerogels, doped with chromium or chromium and
titanium, have been prepared according to a proposed preparation proc
edure from preformed and partly dried aqueous gels precipitated from m
etal chloride solutions. After supercritical drying, low density and h
igh surface area (> 300 m(2) g(-1)) aerogel pellets were obtained, con
sisting of ca. 5 nm boehmite crystals. Fluorination of such aerogels w
ith CHF3 resulted in high conversion to fluoride with the formation of
mainly alpha-AIF(3) and some beta/gamma-AIF(3). Substantial crystal g
rowth was observed with uniform pellet shrinkage and a large decrease
in surface area. in contrast to fluorinated materials prepared from co
mmercial gamma-Al2O3 by fluorination with HF1 fluorinated aerogels hav
e a much more expanded and heterogeneous structure with a broad distri
bution of size/shape of particles and pores. Fluorinated aerogels show
catalytic activity in trichloroethene hydrofluorination to CF3CH2Cl.
By the fluorination of alumina-based aerogels, very porous, high surfa
ce area and catalytically active fluorides can be prepared. Such highl
y dispersed materials are believed to be very useful in studying heter
ogeneous catalytic reactions of technically important fluoro-derivativ
es of lower halogenated hydrocarbons.