Acetic Acid → Acetate alumoxane

HRID 586107

反応式

HRID 586107 の反応式
[C:1]([OH:4])(=[O:3])[CH3:2].[AlH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][O:6]1>O>[C:1]([O-:4])(=[O:3])[CH3:2].[AlH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][O:6]1

参加物

4

反応条件

温度
1100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-86386e277e84444396ec76d48d8d5772
出典データセット
uspto-grants-2005_08
特許番号
US06936306B1

関連ノート

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