▎ 摘　　要

NOVELTY - Aminated graphene is ultrasonically processed in phosphoric acid. Phosphorus pentoxide is added and stirred to obtain mixture (A). Terephthalic acid is added and reacted to obtain mixture (B). 4,6-Diaminoresorcinol dihydrochloride and tin dichloride are added to mixture (B) and heated to obtain mixture (C). Terephthalic acid is added to mixture (C), heat-reacted, and reacted with phosphorus pentoxide to obtain mixture (D). Mixture (D) is press-molded, immersed in phosphoric acid, and to obtain graphene/poly-p-phenylene benzobisoxazole (PBO) copolymer membrane. USE - Preparation of graphene/PBO composite copolymer film (claimed). ADVANTAGE - The method enables preparation of graphene/poly-p-phenylene benzobisoxazole composite copolymer films having excellent structural stability and no migration to film surface, without aggregation. Favorable graphene dispersion in PBO matrix is achieved. Reactivity of graphene and PBO is improved. DETAILED DESCRIPTION - 1-5 g Nano-graphite and 3-100 g potassium permanganate are added to a mixture of 200-2000 mL concentrated sulfuric acid and 20-200 mL concentrated phosphoric acid, and mixed at 0-50 degrees C for 24-72 hours. 0.5-10 L Distilled water is added, and the reaction mixture is cooled, stirred for 0.5-3 hours, and filtered using 0.22- mu m microporous filter membrane. The filter cake is rinsed with distilled water until the filtrate is of neutral pH, and filter cake is freeze-dried to obtain graphite oxide. 0.1-1 g Graphite oxide powder, 10-100 g amine compound, 5-40 mL N,N'-dimethylformamide, 0.5-10 g N,N'-dicyclohexyl carbodiimide, and 0.05-1 g 4-dimethylaminopyridine are ultrasonically dispersed for 1-6 hours, reacted at 40-100 degrees C for 18-72 hours, and filtered using 0.22- mu m microporous membrane filter. The filter caked is washed 3-8 times with dimethylformamide and freeze-dried to obtain aminated graphene. 0.5-5 g Aminated graphene is added to 30-200 g 80-90% phosphoric acid and ultrasonically processed for 5-10 hours, to obtain an amino acid solution of graphene. 3-5 Times 50-300 g phosphorus pentoxide is added to the solution and stirred at 60-100 degrees C for 1-5 hours, to obtain mixture (A). In nitrogen atmosphere, at 110-130 degrees C, 5-20 g terephthalic acid is added to mixture (A) and stir-reacted for 8-24 hours to obtain mixture (B). 20-150 g 4,6-Diaminoresorcinol dihydrochloride and 1-10 g tin dichloride are added to mixture (B) and heated at 60-100 degrees C for 12-36 hours, to obtain mixture (C). 10-75 g Terephthalic acid is added to mixture (C) and heated at 140-160 degrees C for 3-5 hours. After reaction completion, the reaction mixture is heated to 180-200 degrees C, 1-5 times 30-200 g phosphorus pentoxide is added, and the contents are reacted for 3-5 hours to obtain mixture (D). Mixture (D) is poured on a PTFE film super-flat stainless steel plate. The steel plate is placed on a hot press and press-molded at 120-240 degrees C and 5-300 MPa for 0.2-2 hours. The obtained film is immersed in 0-30 %mass phosphoric acid for 8-48 hours and dried at room temperature to obtain graphene/PBO copolymer membrane.