• 专利标题:   Catalyst used for catalytic cyclohexanone oxime caprolactam Beckmann rearrangement comprises acidic ionic liquid 1-(4-sulfonic group) butyl-3-methylimidazolium hydrogen sulfate supported on graphene oxide.
  • 专利号:   CN105597819-A
  • 发明人:   ZHU M, ZHOU Y, GU W, CHEN H
  • 专利权人:   UNIV ZHEJIANG
  • 国际专利分类:   B01J031/02, C07D201/04, C07D223/10
  • 专利详细信息:   CN105597819-A 25 May 2016 B01J-031/02 201667 Pages: 9 Chinese
  • 申请详细信息:   CN105597819-A CN11007187 30 Dec 2015
  • 优先权号:   CN11007187

▎ 摘  要

NOVELTY - Catalyst comprises acidic ionic liquid 1-(4-sulfonic group) butyl-3-methylimidazolium hydrogen sulfate (HSO3Bmim) (HSO4) supported on graphene oxide. USE - Catalyst used for catalytic cyclohexanone oxime caprolactam Beckmann rearrangement (claimed). ADVANTAGE - The catalyst has good activity and selectivity. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is included for preparation of catalyst comprising preparing graphite oxide by adding 50 mL 98% concentrated sulfuric acid in dry flask, cooling to 5 degrees C, electromagnetic stirring, adding 2 g graphite powder, 1 g sodium nitrate, and 6 g potassium permanganate, reacting at 10-15 degrees C, keeping reaction for 0.5 hour for low-temperature reaction, placing at 35 degrees C water bath, stirring for 2 hours, adding 90 mL deionized water while stirring, reacting at 65 degrees C for 0.5 hour, adding hydrogen peroxide, hot filtering, washing with 5% hydrochloric acid and water, placing resulting cake in oven and drying at 40 degrees C; preparing acidic ionic liquid by weighing N-1-methylimidazole and 1,4-butane sultone at molar ratio of 1.1:1, placing in reflux condenser, reacting at 40 degrees C for 24 hours, filtering and vacuum drying to yield zwitterionic intermediates, adding intermediate and concentrated sulfuric acid to flask, stirring under reflux at 80 degrees C for 4 hours, washing repeatedly with toluene and ethyl acetate for 3 times and vacuum drying; and taking 0.06-0.15 g acidic ionic liquid, adding 50 mL anhydrous ethanol, dissolving, adding 0.5 g graphite oxide, stirring at room temperature for 24 hours, completing reaction, filtering, washing with ether, and vacuum drying.