Acetic Acid → Acetate alumoxane

Participants

Reaction Conditions

Reaction Steps

Pseudoboehmite (20.0 g) was slowly added to a vigorously stirring mixture of acetic acid (51.0 mL) in water (200 mL). The resulting slurry was decanted after 10 minutes and then centrifuged at 6000 rpm for 1 hour to yield a clear viscous solution. Removal of the volatiles in vacuo (10−2 Torr) at 90° C. results in clear, white granules. The granules were dissolved in water and dried for 24 hours at 80° C. to yield a clear glassy material. The alumoxane was heated from 25° C. to 225° C. at the rate of 1° C./min., soaked for 30 mins. at 225° C., followed by a temper ramp up to 300° C. at the rate of 2° C./min., and soaked for 80 mins., with a final ramp to the maximum temperature of 1100° C. (over 360 minutes) which was then maintained for 400minutes.

Provenance & Evidence