• 专利标题:   Preparing graphene modified polyimide composite film comprises e.g. uniformly mixing graphite, concentrated sulfuric acid and concentrated phosphoric acid under ice bath conditions, placing it in oil bath, and turning on magnetic stirring.
  • 专利号:   CN112795036-A
  • 发明人:   CHANG S, AN H, XIAN L, YANG S, LU G, ZHANG H
  • 专利权人:   UNIV NANJING AERONAUTICS ASTRONAUTICS, LANZHOU INST PHYSICS
  • 国际专利分类:   C08J005/18, C08K003/04, C08K009/04, C08L079/08, C08L083/04
  • 专利详细信息:   CN112795036-A 14 May 2021 C08J-005/18 202152 Pages: 10 Chinese
  • 申请详细信息:   CN112795036-A CN11621684 31 Dec 2020
  • 优先权号:   CN11621684

▎ 摘  要

NOVELTY - Preparing graphene modified polyimide composite film comprises (i) uniformly mixing graphite, 98% concentrated sulfuric acid and 85% concentrated phosphoric acid under ice bath conditions, then placing it in an oil bath heated to 50 degrees C in advance, turning on magnetic stirring, slowly adding potassium permanganate to the reaction system, adding hydrogen peroxide to the reaction system after 6 hours of reaction, where the solution turned bright yellow, continuing to react at 50 degrees C for 3 hours and then cooling to room temperature, washing using deionized water, centrifuging, and drying to obtain graphene oxide powder, and (ii) uniformly dispersing prepared graphene oxide powder in a polar organic solvent, obtaining graphene oxide dispersion, adding stir bar and transferring to the oil bath, adding polyisocyanate, heating to 60 degrees C in a nitrogen atmosphere, reacting for 48 hours, and obtaining modified graphene oxide powder after washing, centrifuging and drying. USE - The composite film is useful for outer surface of spacecraft. ADVANTAGE - The method: increases the interlayer spacing; improves the dispersibility of graphene oxide in the polyimide matrix; enhances the film radiation resistance; achieves chain growth; and obtains polyimide with a large molecular weight, which improves the mechanical properties of the film. The composite film has excellent radiation resistance. DETAILED DESCRIPTION - Preparing graphene modified polyimide composite film comprises (i) uniformly mixing graphite, 98% concentrated sulfuric acid and 85% concentrated phosphoric acid under ice bath conditions, then placing it in an oil bath heated to 50 degrees C in advance, turning on magnetic stirring, slowly adding potassium permanganate to the reaction system, adding hydrogen peroxide to the reaction system after 6 hours of reaction, where the solution turned bright yellow, continuing to react at 50 degrees C for 3 hours and then cooling to room temperature, washing using deionized water, centrifuging, and drying to obtain graphene oxide powder, (ii) uniformly dispersing prepared graphene oxide powder in a polar organic solvent, obtaining graphene oxide dispersion, adding stir bar and transferring to the oil bath, adding polyisocyanate, heating to 60 degrees C in a nitrogen atmosphere, reacting for 48 hours, and obtaining modified graphene oxide powder after washing, centrifuging and drying, (iii) uniformly dispersing the obtained powder in a polar organic solvent to obtain a modified graphene oxide dispersion, adding cage polysilsesquioxane (POSS) to the obtained modified graphene oxide dispersion and stirring mechanically for 1 hour to make it evenly mixed, protecting by nitrogen, adding diamine monomer, continuing mechanical stirring under ice-water bath conditions, adding acid anhydride monomer three times at intervals of 0.5 hours after 2 hours, continuing stirring for 6 hours and adding small amount of diamine monomer as linking agent to increase the chain length of the polyimide molecule, continuing mechanical stirring for 6 hours, then transferring to 50 degrees C constant temperature water bath, heating and degrading for 30 minutes to obtain modified polyimide precursor solution, and (iv) uniformly coating the obtained modified polyimide precursor solution on a clean high temperature resistant glass plate, placing in a vacuum drying oven, vacuum defoaming at 25 MPa and pressure for 1 hour, then heating up to 80-120 degrees C at a heating rate of 2 degrees C/minutes for 8-12 hours heat curing treatment, after the heat curing is over, transferring the post sample to the muffle furnace, adopting the programmed heating treatment method, raising the temperature to 150-350 degrees C at a heating rate of 3 degrees C/minutes for 6 hours, then cooling to room temperature naturally, placing the sample in deionized water for 2-5 minutes, and treating the peeled film in a vacuum drying oven at 105 degrees C for 1 hour to obtain modified polyimide film.