• 专利标题:   Preparing three-dimensional graphene hollow sphere modified polyimide material, comprises e.g. adding graphene oxide solution into spherical silicon dioxide sol, ultrasonically dispersing, freezing and drying.
  • 专利号:   CN111793208-A
  • 发明人:   LIU Y, HU M, LV X, GU W, QIU Y
  • 专利权人:   CHONGQING YUNTIANHUA HANEN NEW MATERIAL
  • 国际专利分类:   C01B032/19, C08G073/10, C08K007/24, C09J179/08, C09J009/02
  • 专利详细信息:   CN111793208-A 20 Oct 2020 C08G-073/10 202091 Pages: 10 Chinese
  • 申请详细信息:   CN111793208-A CN10690352 17 Jul 2020
  • 优先权号:   CN10690352

▎ 摘  要

NOVELTY - Preparing three-dimensional graphene hollow sphere modified polyimide material, comprises e.g. (i) adding graphene oxide solution into spherical silicon dioxide sol, then ultrasonically dispersing, freezing and drying to obtain spherical silicon dioxide coated with graphene oxide, (ii) dispersing the spherical silicon dioxide coated with graphene oxide in sodium hydroxide solution, heating and reacting to obtain hollow spherical graphene oxide, (iii) subjecting the hollow spherical graphene oxide to high temperature reduction at 800-1000 degrees C for 2-4 hours under the protective gas atmosphere and further transferring to a graphitization furnace to carrying out reduction to obtain graphene hollow sphere, and (iv) mixing the graphene hollow sphere with solvent to obtain graphene hollow sphere dispersion, then mixing graphene hollow sphere dispersion with aromatic diamine and aromatic dianhydride for polymerization reaction and performing thermal imidization of reaction product. USE - The three-dimensional graphene hollow sphere modified polyimide material is useful for preparing modified polyimide adhesive (claimed). ADVANTAGE - The three-dimensional graphene hollow sphere modified polyimide material: produces modified polyimide adhesive which has better conductivity than the simple two-dimensional graphene modification, viscosity of 10,000-20,000 Pa.s, excellent dispersibility, and measured surface resistance of less than 0.05 ohm after coating. DETAILED DESCRIPTION - Preparing three-dimensional graphene hollow sphere modified polyimide material, comprises (i) adding graphene oxide solution into spherical silicon dioxide sol, then ultrasonically dispersing, freezing and drying to obtain spherical silicon dioxide coated with graphene oxide, (ii) dispersing the spherical silicon dioxide coated with graphene oxide in sodium hydroxide solution, heating and reacting to obtain hollow spherical graphene oxide, (iii) subjecting the hollow spherical graphene oxide to high temperature reduction at 800-1000 degrees C for 2-4 hours under the protective gas atmosphere and further transferring to a graphitization furnace at 2000-2800 degrees C to carrying out further reduction for 1-5 hours to obtain graphene hollow sphere, and (iv) mixing the graphene hollow sphere with solvent to obtain graphene hollow sphere dispersion, then mixing graphene hollow sphere dispersion with aromatic diamine and aromatic dianhydride for polymerization reaction, when the viscosity of the system reaches the requirement, stopping the reaction and then performing thermal imidization of reaction product to obtain final product. INDEPENDENT CLAIMS are also included for: (1) three-dimensional graphene hollow sphere modified polyimide material obtained by above method; and (2) use of three-dimensional graphene hollow sphere modified polyimide material for preparing modified polyimide adhesive, where the aromatic diamine is p-phenylenediamine and diaminodiphenyl ether, the aromatic dianhydride is benzophenone-3,3',4,4'-tetracarboxylic dianhydride and 3,3',4,4'-biphenyltetracarboxylic dianhydride.