• 专利标题:   Preparing graphene airgel-loaded carbon nanotube and ZIF-67 lithium battery electrode material comprises e.g. adding graphite powder, adding nitric acid, heating, cooling, adding carbon nanotubes and carrying out hydrothermal reaction.
  • 专利号:   CN106252634-A, CN106252634-B
  • 发明人:   SUN W, WANG Y, LI H, LIANG M, CAI C, YANG Q, CHEN S, ZHANG W, YIN X
  • 专利权人:   UNIV SHANGHAI, UNIV SHANGHAI
  • 国际专利分类:   H01M010/0525, H01M004/139, H01M004/1393, H01M004/36, H01M004/583, H01M004/60
  • 专利详细信息:   CN106252634-A 21 Dec 2016 H01M-004/36 201714 Pages: 8 Chinese
  • 申请详细信息:   CN106252634-A CN10847675 24 Sep 2016
  • 优先权号:   CN10847675

▎ 摘  要

NOVELTY - Preparing graphene airgel-loaded carbon nanotube and ZIF-67 lithium battery electrode material comprises e.g. adding natural graphite powder into 1000 ml flask, adding nitric acid, adding sulfuric acid, stirring, adding potassium permanganate, heating, cooling, adding hydrogen peroxide and hydrochloric acid, drying, adding carbon nanotubes, carrying out hydrothermal reaction, adding methanol solution, adding cobalt(II) nitrate hexahydrate, then mixing with acetylene black and polyvinylidene fluoride adhesive, then adding N-methyl-2-pyrrolidone, dispersing, coating to obtain final product. USE - The method is useful for preparing graphene airgel-loaded carbon nanotube and ZIF-67 lithium battery electrode material (claimed). ADVANTAGE - The method has high relative capacity, and excellent cycle stability. DETAILED DESCRIPTION - Preparing graphene airgel-loaded carbon nanotube and ZIF-67 lithium battery electrode material comprises (i) adding 2-2.5 g natural graphite powder into 1000 ml flask, adding 100-150 ml 65% nitric acid, reacting at 0 degrees C under ice water bath, adding 100-150 ml 98% sulfuric acid, stirring for 1-2 hours, adding 8-15 g potassium permanganate, reacting at 30-40 degrees C for 2-3 hours, then heating to 70-90?OC for 1 -2 hours, cooling to room temperature, adding 300-500 ml distilled water diluted acid to obtain brown colloid material, then adding 30-50 ml 35% hydrogen peroxide and 100-150 ml 10% hydrochloric acid to obtain brown yellow solution, centrifugal washing to neutral, drying at 50-60 degrees C under air to obtain graphene oxide, (ii) adding 0.04 g graphene oxide obtained in step (i), into 20 ml distilled water, carrying out ultrasonic dispersion for 30-60 minutes, then adding 0.02 g carbon nanotubes, continuing ultrasonic dispersion for 1-1.5 hours, carrying out hydrothermal reaction at 180 degrees C for 12 hours, and then freeze-drying and drying at -30 to 40 degrees C to obtain carbon nanotubes gas, (iii) adding 0.05 g carbon nanotubes gas mixture obtained in step (ii) into 25 ml methanol solution, dispersing by ultrasonic for 20-30 minutes, adding 0.249 g cobalt(II) nitrate hexahydrate, then dropping 25 ml 2-methyl imidazole methanol solution, stirring for 10-20 minutes, allowing to stand for 24 hours, ethanol centrifugal washing for 6-8 times, drying to obtain carbon nanotubes gas and ZIF-67 complex, (iv) mixing carbon nanotubes gas and ZIF-67 complex, acetylene black and polyvinylidene fluoride adhesive in a mass ratio of 8:1:1, then adding the mixture into N-methyl-2-pyrrolidone, dispersing the slurry in a high-speed internal-rotary beater at a rate of 5-10 times per minute for 5 minutes to obtain homogeneous carbon nanotubes gas and ZIF-67 black colloidal paste, and (v) coating black colloidal paste on the pre-treated metal copper current collector, and placing in vacuum oven drying at 60-80 degrees C for 12-24 hours to obtain final product.