Acetic Acid → Acetate alumoxane

Temperature

1100 °C

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.

1. additionPseudoboehmite (20.0 g) was slowly added to
2. customThe resulting slurry was decanted after 10 minutes
3. customto yield a clear viscous solution
4. customRemoval of the volatiles in vacuo (10−2 Torr) at 90° C.
5. customresults in clear, white granules
6. customdried for 24 hours at 80° C.
7. customto yield a clear glassy material
8. waitsoaked for 30 mins
9. customat 225° C.
10. customfollowed by a temper ramp up to 300° C. at the rate of 2° C./min.
11. waitsoaked for 80 mins

ORD record

ord-86386e277e84444396ec76d48d8d5772

Source dataset

uspto-grants-2005_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06936306B1