• 专利标题:   Preparation of modified graphene by reacting bis-aryl derivatives of diazomethane with dichloromethane, adding graphite oxide, washing, dispersing solids in acetone, filtering, and vacuum drying solids.
  • 专利号:   CN105271192-A, CN105271192-B
  • 发明人:   HU Z, HUANG Y, SONG C
  • 专利权人:   HARBIN INST TECHNOLOGY, HARBIN INST TECHNOLOGY
  • 国际专利分类:   C01B031/04, C01B032/184
  • 专利详细信息:   CN105271192-A 27 Jan 2016 C01B-031/04 201642 Pages: 7 English
  • 申请详细信息:   CN105271192-A CN10677400 16 Oct 2015
  • 优先权号:   CN10677400

▎ 摘  要

NOVELTY - Preparation of modified graphene involves preparing graphite oxide using sulfuric acid and graphite powders with nitric acid; preparing benzophenone hydrazone derivative using benzophenone derivative, ethanol and hydrazine hydrate solution; preparing bis-aryl derivatives of diazomethane using benzophenone hydrazone derivative, tetrahydrofuran, anhydrous sodium sulfate, manganese oxide, potassium hydroxide and ethanol; and reacting bis-aryl derivatives of diazomethane with dichloromethane, adding graphite oxide, washing, dispersing solids in acetone, filtering, and vacuum drying solids. USE - Method for preparing modified graphene (claimed). ADVANTAGE - The method utilizes highly active graphite oxide with carbene reactive functional group, improves degree of modification and simplifies preparation process which fits for large-scale industrial production. DETAILED DESCRIPTION - Preparation of modified graphene comprises adding 0.3-3 L 98% concentrated sulfuric acid in dried reactor, adding 10-100 g graphite powders, stirring, adding 0.1-1 L 65% concentrated nitric acid, sonicating for 10-60 minutes, insulating at 20-60 degrees C for 10-100 minutes, filtering, washing solid with distilled water, vacuum drying at 20-60 degrees C for 12-36 hours to obtain graphite oxide; adding 2-20 g benzophenone derivative in round flask, adding 50-1000 ml ethanol and 1-50 g 85% hydrazine hydrate solution, stirring at 80 degrees C for 24-72 hours, vacuum distilling to distill off ethanol, cooling remaining reaction solution with ice crystal for 10-60 minutes, filtering, washing solid with distilled water for 3-5 times, and vacuum drying at 20-60 degrees C for 12-36 hours to get benzophenone hydrazone derivative; adding 0.1-5 g benzophenone hydrazone derivative with 5-200 mL tetrahydrofuran in round bottomed flask, adding 0.1-10 g anhydrous sodium sulfate, 0.1-10 g manganese oxide and 0.1-10 ml potassium hydroxide and ethanol saturated solution, stirring at room temperature for 1-12 hours under dark conditions, frit funnel filtering, washed repeatedly with 5 times dichloromethane, drying filtrate at 20-60 degrees C for 12-36 hours to get bis-aryl derivatives of diazomethane; and adding 0.1-5 g bis-aryl derivatives of diazomethane in round bottom flask with 10-100 ml dichloromethane, adding 0.1-50 g graphite oxide, distilling off solvent under vacuum, reacting at 100-200 degrees C for 10-20 minutes, washing with 3-5 times methylene chloride and 3-5 times distilled water, dispersing solids in acetone, sonicating for 1-6 hours, filtering, and vacuum drying solids for 12-36 hours at 20-60 degrees C.