Methanol → Methoxy(ethoxyethoxy)acetate alumoxane

温度

1100 °C

Pseudoboehmite (20.0 g) and methoxy(ethoxyethoxy)acetic acid (102 mL) were refluxed in water (400 mL) resulting in a clear solution after 72 h. The solution was centrifuged at 6000 rpm for 1 hour and decanted. Removal of the volatiles in vacuo (10−2 Torr) at 90° C. yielded a gel which was then dissolved in ethanol (100 mL) while stirring (10 min.) then triturated with diethyl ether (200 mL). The white solid powder thus obtained was redissolved in water (100 mL) and dried at 50° C. for 24 h resulting in a clear glassy material. The MEEA-alumoxane is soluble in water, methanol, chloroform, and methylene chloride. 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 (FIG.

1. customresulting in a clear solution after 72 h
2. customdecanted
3. customRemoval of the volatiles in vacuo (10−2 Torr) at 90° C.
4. customyielded a gel which
5. customthen triturated with diethyl ether (200 mL)
6. customThe white solid powder thus obtained
7. customdried at 50° C. for 24 h
8. customresulting in a clear glassy material
9. waitsoaked for 30 mins
10. customat 225° C.
11. customfollowed by a temperature ramp up to 300° C. at the rate of 2° C./min.
12. waitsoaked for 80 mins

ORDレコード

ord-3a4eadf57d0c4efdbdabf043c2e658d6

出典データセット

uspto-grants-2005_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06936306B1