• 专利标题:   Preparation of composite meta-material involves adding dried high-molecular polymer to three-dimensional porous graphene solution, stirring, dropping mixed solution into glass culture dish, drying, melting dried block, and hot-pressing.
  • 专利号:   CN108794942-A
  • 发明人:   LIU X, ZHU B, CHAO D, YAN K, YUE D, LI Y
  • 专利权人:   UNIV HEILONGJIANG SCI TECHNOLOGY
  • 国际专利分类:   C08L027/16, C08L023/06, C08L023/12, C08K007/24, C01B032/184
  • 专利详细信息:   CN108794942-A 13 Nov 2018 C08L-027/16 201906 Pages: 17 Chinese
  • 申请详细信息:   CN108794942-A CN10749235 09 Jul 2018
  • 优先权号:   CN10749235

▎ 摘  要

NOVELTY - Preparation of polymer-three-dimensional porous graphene composite meta-material involves drying polymer in an oven at 70-90 degrees C for 6-9 hours, obtaining dried high-molecular polymer, adding the dried high-molecular polymer to 5-10 mg/mL three-dimensional porous graphene solution, stirring at 45-55 degrees C and 100 rpm for 7-9 hours, ultrasonically processing obtained viscous mixed solution at power of 100-500 W for 3-5 hours, obtaining a mixed liquid comprising polymer and three-dimensional porous graphene solution, spin-coating or dropping the mixed solution into a clean glass culture dish, drying at 70-80 degrees C for 8-12 hours, melting the dried block at 120-170 degrees C for 2-10 hours, and hot-pressing at 120-150 degrees C and 10-30 MPa for 1-2 hours. The composite meta-material has thickness of 50-100 mu m. The high-molecular polymer is polyvinylidene fluoride, polyethylene or polypropylene. USE - Preparation of polymer-three-dimensional porous graphene composite meta-material. ADVANTAGE - The method enables economical preparation of polymer-three-dimensional porous graphene composite meta-material with excellent mechanical property. DETAILED DESCRIPTION - Preparation of polymer-three-dimensional porous graphene composite meta-material involves drying polymer in an oven at 70-90 degrees C for 6-9 hours, obtaining dried high-molecular polymer, adding the dried high-molecular polymer to 5-10 mg/mL three-dimensional porous graphene solution, stirring at 45-55 degrees C and 100 rpm for 7-9 hours, ultrasonically processing obtained viscous mixed solution at power of 100-500 W for 3-5 hours, obtaining a mixed liquid comprising polymer and three-dimensional porous graphene solution, spin-coating or dropping the mixed solution into a clean glass culture dish, drying at 70-80 degrees C for 8-12 hours, melting the dried block at 120-170 degrees C for 2-10 hours, and hot-pressing at 120-150 degrees C and 10-30 MPa for 1-2 hours. The composite meta-material has thickness of 50-100 mu m. The high-molecular polymer is polyvinylidene fluoride, polyethylene or polypropylene. The volume ratio of dried high-molecular polymer and 5-10 mg/mL three-dimensional porous graphene solution is 0.4-0.95 g:10 mL. The three-dimensional porous graphene solution is prepared by dissolving graphene oxide in water, obtaining graphene oxide solution, adding a polymer or a metal chloride to the graphene oxide solution, stirring at 500-1000 rpm for 1-2 hours, ultrasonically dispersing for 1-2 hour, obtaining a dark mixed solution, spray-drying the dark mixed solution at 130-180 degrees C or freeze-drying at -50 degrees C to 55 degrees C, obtaining a pale yellow fluffy powder, placing the pale yellow fluffy powder in a tube furnace, heating the tube furnace at rate of 3-5 degrees C/minute from room temperature to 180-240 degrees C for 50-80 minutes under the protection of inert gas, and at rate of 3-5 degrees C/minute to 750-800 degrees C for 120-150 minutes, respectively, cooling at rate of 5-8 degrees C/minute to 180-240 degrees C, naturally cooling to room temperature, obtaining a black powder, washing the black powder once or twice with 0.1 mol/L hydrochloric acid, further washing the black powder 2 or 3 times with deionized water, filtering, drying at 75-85 degrees C for 5-10 hours, and dissolving obtained three-dimensional porous graphene powder in an organic solvent. The concentration of three-dimensional porous graphene solution is 5-10 mg/mL. The mass ratio of polymer or metal chloride and graphene oxide in the dark mixed solution is 8-10:1-10. The polymer is a water-soluble polymer or a water-insoluble polymer. The concentration of graphene oxide solution is 5-15 g/L. The graphene oxide is prepared by adding natural graphite and potassium permanganate to 98 %mass sulfuric acid, stirring at 300-400 rpm for 1-2 hours in an ice bath, obtaining mixture (A), heating the mixture (A) to 35 degrees C, maintaining at 35 degrees C for 1 hour, adding deionized water to the mixture (A), heating to 90-95 degrees C, incubating at 90-95 degrees C for 30-35 minutes, obtaining mixture (B), naturally cooling the mixture (B) to room temperature, adding 35 %mass hydrogen peroxide solution, reacting at room temperature for 10 minutes under stirring at speed of 100-300 rpm, centrifuging obtained aqueous graphene oxide solution at 3000-3500 rpm, removing supernatant, centrifuging the supernatant at 8000-8500 rpm, and drying the precipitated material at 60-80 degrees C for 1-3 hours. The mass ratio of natural graphite and potassium permanganate is 1:5. The mass ratio of natural graphite and 98 %mass sulfuric acid is 1 g:60-100 mL. The volume ratio of mixture (A) and deionized water is 1:1. The volume ratio of natural graphite and 35 %mass hydrogen peroxide solution is 1 g:5-6 mL.