Methoxyacetic Acid → Methoxyacetate alumoxane

温度

1100 °C

Pseudoboehmite (10.0 g) and methoxyacetic acid (25.6 mL) were refluxed in water (150 mL) for 24 h. which resulted in a white cloudy solution with a trace of insoluble particles. The water was removed in vacuo (10−2 Torr) at 50° C. resulting in a white powder which was washed with diethyl ether (4×150 mL) then dissolved in ethanol (100 mL) while stirring (50 minutes). The alumoxane was precipitated via the addition of ether (300 mL). After drying overnight at 50° C. the solid yield was approximately 20 g. The powder was dissolved in water (100 mL), isolated by filtration, concentrated under vacuum and dried at 50° C. resulting in a white solid 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 temperature 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 400 minutes.

1. customresulted in a white cloudy solution with a trace of insoluble particles
2. customThe water was removed in vacuo (10−2 Torr) at 50° C.
3. customresulting in a white powder which
4. washwas washed with diethyl ether (4×150 mL)
5. dissolutionthen dissolved in ethanol (100 mL)
6. customThe alumoxane was precipitated via the addition of ether (300 mL)
7. dry with materialAfter drying overnight at 50° C. the solid yield was approximately 20 g
8. dissolutionThe powder was dissolved in water (100 mL)
9. customisolated by filtration
10. concentrationconcentrated under vacuum
11. customdried at 50° C.
12. customresulting in a white solid material
13. waitsoaked for 30 mins
14. customat 225° C.
15. customfollowed by a temperature ramp up to 300° C. at the rate of 2° C./min.
16. waitsoaked for 80 mins

ORDレコード

ord-a0c174856202461287b09583f9f9fb85

出典データセット

uspto-grants-2005_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06936306B1