• 专利标题:   Preparation of polyacrylonitrile/graphene composite based carbon fibers, involves reacting graphene, monomer, and initiator in solvent, defoaming, spinning formed polyacrylonitrile dope into monofilaments, pre-oxidizing, and carbonizing.
  • 专利号:   CN102560746-A, CN102560746-B
  • 发明人:   CHEN Y, HUANG X, MA H, MO G, OUYANG Q, YANG J
  • 专利权人:   CHINESE ACAD SCI NINGBO INST MATERIAL TE
  • 国际专利分类:   C08F220/44, D01F001/09, D01F011/06, D01F009/22
  • 专利详细信息:   CN102560746-A 11 Jul 2012 D01F-009/22 201325 Pages: 8 Chinese
  • 申请详细信息:   CN102560746-A CN10450984 29 Dec 2011
  • 优先权号:   CN10450984

▎ 摘  要

NOVELTY - Graphene, a monomer, and an initiator are uniformly dispersed in a solvent to obtain a mixed solution, which is reacted to obtain an intermediate solution. The intermediate solution is vacuum-treated and defoamed to obtain a polyacrylonitrile dope containing dispersed graphene. The dope is used as spinning solution for preparing composite monofilaments by wet spinning or dry-jet wet spinning. The monofilaments are pre-oxidized, low-temperature carbonized, and high-temperature carbonized to obtain polyacrylonitrile/graphene composite based carbon fibers. USE - Preparation of polyacrylonitrile/graphene composite based carbon fibers. ADVANTAGE - The method enables efficient and reliable preparation of polyacrylonitrile/graphene composite based carbon fibers having excellent mechanical properties, with high carbonization yield. DETAILED DESCRIPTION - (In %mass) graphene (0.01-10), a monomer, and an initiator (0.2-2) are uniformly dispersed in a solvent to obtain a mixed solution, which is reacted at 30-68 degrees C under nitrogen protection for 5-24 hours, to obtain an intermediate solution. The monomer comprises an acrylonitrile monomer (85-100) and an additional monomer (0-15). The solvent is dimethyl sulfoxide, N,N-dimethylformamide, N,N-dimethylacetamide, zinc chloride aqueous solution, or sodium thiocyanate aqueous solution. The additive monomer comprises itaconic acid, monoethyl itaconate, monoamide itaconate, methyl acrylate, methyl methacrylate, isobutyl methacrylate, n-butyl methacrylate, acrylamide, methacrylamide, and/or 2-acrylamido-2-methylpropanesulfonic acid. The initiator comprises azobisisobutyronitrile, azobisisoheptonitrile and/or azobisisovaleronitrile. The obtained intermediate solution is vacuum-treated at 55-80 degrees C and 30-3000 Pa to remove unreacted residual monomers, and then defoamed for 10-100 hours at 50-65 degrees C to obtain a polyacrylonitrile dope containing dispersed graphene. The dope is used as spinning solution for preparing polyacrylonitrile/graphene composite monofilaments by wet spinning or dry-jet wet spinning. The monofilaments are pre-oxidized at 165-300 degrees C, low-temperature carbonized at 300-900 degrees C, and high-temperature carbonized at 900-1800 degrees C to obtain polyacrylonitrile/graphene composite based carbon fibers.