• 专利标题:   Preparing array type magnetic reduction graphene oxide-carbon nanofiber comprises e.g. reacting flake graphite as raw material, concentrated sulfuric acid, sodium nitrate, hydrogen peroxide and potassium permanganate strong oxidizing agent.
  • 专利号:   CN108315834-A
  • 发明人:   HE T, YU X, WANG O, MENG X, HAN Y
  • 专利权人:   UNIV BOGHAI
  • 国际专利分类:   D01F006/56, H01G011/36, H01G011/40, H01M004/88
  • 专利详细信息:   CN108315834-A 24 Jul 2018 D01F-006/56 201864 Pages: 15 Chinese
  • 申请详细信息:   CN108315834-A CN10076423 26 Jan 2018
  • 优先权号:   CN10076423

▎ 摘  要

NOVELTY - Preparing array type magnetic reduction graphene oxide-carbon nanofiber comprises e.g. reacting flake graphite as raw material, concentrated sulfuric acid, sodium nitrate, hydrogen peroxide and potassium permanganate strong oxidizing agent by Hummer method to obtain graphene oxide, dissolving graphene oxide in solvent, and treating with ultrasonic wave to obtain graphene oxide colloid solution; transferring the graphene oxide colloid solution into stainless steel high pressure reactor, adding magnetic material precursor; controlling reaction temperature, filtering, washing with deionized water, and drying to obtain magnetic material modified graphene oxide, and mixing magnetic material modified graphene oxide with polymer and adding solvent to obtain magnetic graphene oxide-polymer mixed electrospinning precursor solution and then electromagnetic spinning of a magnetic graphene oxide-polymer mixed electrospinning precursor solution. USE - The array type magnetic reduction graphene oxide-carbon nanofiber is useful in supercapacitor and in electrospinning method for preparing magnetic graphene oxide carbon nanofiber composite material (all claimed). ADVANTAGE - The array type magnetic reduction graphene oxide-carbon nanofiber has increased charge storage density, supercapacitor specific capacitance is 240.3-254.1 CP/F.g(-1) and charging and discharging efficiency of 99.1-99.6%. DETAILED DESCRIPTION - Preparing array type magnetic reduction graphene oxide-carbon nanofiber, comprises (i) taking 10.0 g of 10000-15000 mesh flake graphite as raw material, 150-230 ml concentrated sulfuric acid, 5 g sodium nitrate, 0.5 g hydrogen peroxide and 30 g potassium permanganate strong oxidizing agent and then reacting by Hummer method to obtain graphene oxide, (ii) dissolving 1 g graphene oxide of step (i) in 200 ml solvent, and treating with 200 W ultrasonic wave for 30 minutes to obtain graphene oxide colloid solution; transferring the graphene oxide colloid solution into stainless steel high pressure reactor, adding 0.05-0.10 g magnetic material precursor; controlling reaction temperature at 220-260 degrees C for 12 hours, filtering, washing with deionized water 3 times, and drying at 80 degrees C for 12 hours to obtain magnetic material modified graphene oxide, where the magnetic material precursor is ferric chloride, ferric nitrate, ferrocene and iron acetylacetonate, and (iii) mixing magnetic material modified graphene oxide prepared by step (ii) with polymer with a mass ratio of 1:10-3:10, and adding solvent to obtain magnetic graphene oxide-polymer mixed electrospinning precursor solution having a polymer mass percentage of 17-22 wt.%, then electromagnetic spinning of a magnetic graphene oxide-polymer mixed electrospinning precursor solution, and circular magnetic field generator having a diameter of 10 cm is disposed between the electrospinning receiving plate and the electrospinning nozzle, controlling the magnetic field strength from 0.1-0.3 T, vacuum drying the electrospun fiber collected on receiving plate at 60 degrees C for 12 hours, and removing the solvent remaining in the fiber to obtain magnetic graphene oxide-polymer composite electrospun fiber, heat-treating the magnetic graphene oxide-polymer composite electrospun fiber in an air atmosphere, and heating at a heating rate of 1-3 degrees C/minute, and then heating from room temperature to 280 degrees C at a constant temperature of 280 degrees C for 2 hours in an argon atmosphere, and then heating at 280-1000 degrees C at a heating rate of 3-5 degrees C/minute and insulating at 1000 degrees C for 2 hours to obtain magnetic graphene oxide carbon nanofiber composite material, where the electrospinning voltage is 20-25 kV, the electrospinning pitch is 5-8 cm, the electrospinning flow rate is 1.5-2.5 ml/hour, the polymer is polyacrylonitrile, polymethyl methacrylate, polyvinylidene fluoride, polybenzimidazole, or polyimide, and the solvent is N,N-dimethylformamide, N-methylpyrrolidone, dimethyl sulfoxide, tetrahydrofuran, concentrated sulfuric acid, acetic acid, dichloromethane or tetrachloromethane. INDEPENDENT CLAIMS are also included for: (1) use of array magnetic reduced graphene oxide-carbon nanofiber in supercapacitor for preparing magnetic graphene oxide carbon nanofiber composite material, comprising cut the magnetic graphene oxide carbon nanofiber membrane into an electrode sheet having a diameter of 3 cm and a thickness of 300 mu m and bonding with conductive adhesive to the surface of aluminum foil collector with a thickness of 3 mu m and drying under vacuum at 120 degrees C for 12 hours, taking fluoropolymer mixed electrospinning fiber electrode separator used as an electrode separator and adding ionic liquid electrolyte in an argon atmosphere and a water content of less than 100 parts per million glove box, where the supercapacitor specific capacitance is 240.3-254.1 CP/F.g(-1), the charging and discharging efficiency is 99.1-99.6 wt.%, and the ionic liquid electrolyte is 1-methyl-3-propylimidazolium bromide, 1-butyl-3-methylimidazolium trifluoromethanesulfonate or 1-ethyl-3-methylimidazolium tetrafluoroborate; and (2) use of array magnetic reduced graphene oxide-carbon nanofiber in electrospinning for preparing magnetic graphene oxide carbon nanofiber composite material, comprising preparing N,N-dimethylformamide electrospinning solution having a polymer concentration of 15-20 wt.%, where the polymer is a mixture of polyacrylonitrile and polyvinylidene fluoride, where the mass ratio between polyacrylonitrile and polyvinylidene fluoride is 1:1, or a mixture of polyacrylonitrile and ethylene-tetrafluoroethylene copolymer with a mass ratio of 1:2, or mixture of polyvinylidene fluoride and ethylene-tetrafluoroethylene copolymer with a mass ratio of 2:1, the electrospinning parameter is an electrospinning voltage of 15-17 kV, the spinning pitch is 10-15 cm, the electrospinning solution flow rate of 0.5-1.5 ml/hour and drying the obtained fluoropolymer electrospun fiber membrane at 80 degrees C for 12 hours to obtain fluoropolymer mixed electrospinning fiber electrode separator.