• 专利标题:   Preparation of hydrophilic graphene involves mixing 4-cyano-benzoic acid and dithio-4,4'-azobis-(4-cyano)pentanoic acid, adding organic solvent, and adding mixture obtained by dissolving dimethylamine ethyl methacrylate in water.
  • 专利号:   CN103303909-A, CN103303909-B
  • 发明人:   XU X, YANG Z
  • 专利权人:   UNIV TONGJI
  • 国际专利分类:   B82Y040/00, C01B031/04
  • 专利详细信息:   CN103303909-A 18 Sep 2013 C01B-031/04 201406 Pages: 10 Chinese
  • 申请详细信息:   CN103303909-A CN10206793 30 May 2013
  • 优先权号:   CN10206793

▎ 摘  要

NOVELTY - Preparation of hydrophilic graphene involves mixing 35-55 mg 4-cyano-benzoic acid and 10-20 mg dithio-4,4'-azobis-(4-cyano)pentanoic acid, adding 0.1-1 mL organic solvent to dissolve completely, adding mixture obtained by dissolving 1.5-2.5 g dimethylamine ethyl methacrylate in 5-10 mL deionized water, adjusting pH to 4-5, magnetically-stirring under water bath condition, cooling mixture to room temperature for 15-90 minutes, adding 200-800 mL deionized water and freeze-drying for 12-72 hours and obtaining poly(dimethylaminoethyl methacrylate)PDMAEMA as hydrophilic polymer. USE - Preparation of hydrophilic graphene (claimed). ADVANTAGE - The method efficiently and economically provides hydrophilic graphene having high pH sensitivity, using simple process in short period of time. DETAILED DESCRIPTION - Preparation of hydrophilic graphene involves mixing 35-55 mg 4-cyano-benzoic acid and 10-20 mg dithio-4,4'-azobis-(4-cyano)pentanoic acid in 25 mL single neck flask, adding 0.1-1 mL organic solvent to dissolve completely, adding mixture obtained by dissolving 1.5-2.5 g dimethylamine ethyl methacrylate in 5-10 mL deionized water, adjusting pH to 4-5 under nitrogen atmosphere, magnetically-stirring under water bath condition at 60-80 degrees C for 3-12 hours, cooling mixture to room temperature for 15-90 minutes, adding 200-800 mL deionized water and freeze-drying for 12-72 hours and obtaining hydrophilic polymer PDMAEMA having molecular weight cutoff of 1000, mixing 80-120 mg graphene oxide and 10 mL anhydrous N,N-dimethylformamide in 50 mL round bottom flask, ultrasonically-treating for 15-45 minutes, adding 3-12 mg isophorone diisocyanate under nitrogen atmosphere, and ultrasonically-treating for 0.5-2.5 hours under argon atmosphere, reacting at 60-90 degrees C for 24-72 hours, adding 80-120 mL dichloromethane to mixture, flocculation-sedimenting, filtering, centrifuging, washing 5 times with dichloromethane, vacuum-drying at 45-65 degrees C for 6-24 hours and obtaining isocyanate graphene oxide, dispersing 20-40 mg isocyanate graphene oxide in N,N-dimethyl formamide, and then adding 200-400 mg hydrophilic polymer, mixing under argon atmosphere, reacting at 60-90 degrees C for 6-24 hours, treating using 60-100 mL tetrahydrofuran, filtering, centrifuging, washing with anhydrous ethanol, vacuum-drying at 60 degrees C for 6-24 hours.