Jhz. Dossantos et al., SILICA-SUPPORTED ZIRCONOCENES AND AL-BASED COCATALYSTS - SURFACE METAL LOADING AND CATALYTIC ACTIVITY, Macromolecular chemistry and physics, 198(11), 1997, pp. 3529-3537
The Zr surface loading from Cp2ZrCl2 toluene solutions on different ki
nds of commercial silicas (Grace 948, 952 and 956) was determined by R
utherford backscattering spectrometry. In all silicas, a saturation tr
end was observed with increasing amount of metal in the initial soluti
on, the largest Zr loading value (1 wt.-%) being observed for silica G
race 948. Solid surface areas were determined by the BET method before
and after metallocene immobilization, revealing that the values do no
t change after zirconocene impregnation. Two different kinds of cocata
lyst were used, methylaluminoxane and trimethylaluminium. The aluminiu
m loading on silica Grace 948 was determined using the Al-27(p,gamma)S
i-28 nuclear reaction and titrometry, both showing that methylaluminox
ane leads to an 'Al grafting' four times more efficient than does trim
ethylaluminium. Finally, the catalytic activity of these systems was t
ested in the polymerization of ethylene. The supported catalysts were
shown to be active, specially using the low cost trimethylaluminium as
a cocatalyst. The polymers obtained with the supported systems exhibi
ted a higher molecular weight than those obtained with the homogeneous
system.