• 专利标题:   Manufacture of graphene/poly(p-phenylene benzobisoxazole) polymer involves reacting graphene-containing monomer and polyphosphoric acid, mixing phosphorus pentoxide and obtained mixed solution, and heating.
  • 专利号:   CN103013113-A
  • 发明人:   HU Z, SONG Y, LI Y, HUANG Y, LI J, SUN D, LIU L
  • 专利权人:   HARBIN INST TECHNOLOGY
  • 国际专利分类:   C08G073/22, C08K003/04, C08L079/04
  • 专利详细信息:   CN103013113-A 03 Apr 2013 C08L-079/04 201403 Pages: 11 Chinese
  • 申请详细信息:   CN103013113-A CN10535068 12 Dec 2012
  • 优先权号:   CN10535068

▎ 摘  要

NOVELTY - Graphene-containing monomer and polyphosphoric acid are added in a kneader in mass ratio of 1:1.3-2, reacted at 30-80 degrees C in vacuum under protection of nitrogen for 2-3 hours. The temperature is increased to 100-120 degrees C at 10-11 degrees C/hour and stirred for 4-5 hours to obtain mixed solution (A). Phosphorus pentoxide and mixed solution (A) are mixed in mass ratio of 1.2-1.5:1, heated at 140-160 degrees C and maintained for 2-10 hours to obtain a mixture. The mixture is added in a kneading machine, and heated at 180-200 degrees C for 4-5 hours to obtain graphene/ poly(p-phenylene benzobisoxazole) polymer. USE - Manufacture of graphene/poly(p-phenylene benzobisoxazole) polymer (claimed). ADVANTAGE - The graphene/poly(p-phenylene benzobisoxazole) polymer is manufactured with high molecular weight of 1.2x 104-3x 104. DETAILED DESCRIPTION - Graphene-containing monomer and polyphosphoric acid are added in a kneader in mass ratio of 1:1.3-2, reacted at 30-80 degrees C in vacuum protection of nitrogen for 2-3 hours. The temperature is increased to 100-120 degrees C at 10-11 degrees C/hour and stirred for 4-5 hours to obtain mixed solution (A). Terephthalic acid and 0.25-4 mol/L aqueous sodium hydroxide are added in molar ratio of 1:2-2:1 and mixed to obtain aqueous solution of sodium terephthalate. Graphene oxide is dispersed in deionized water at 40-50 kHz for 30-40 minutes to obtain 0.27-1 g/L aqueous solution of graphene oxide. The aqueous solution of sodium terephthalate and aqueous solution of graphene oxide are mixed in volume ratio of 1:0.5-1 and heated at 40-60 degrees C to obtain mixed solution (B). 0.125-2 mol/L 4,6-diamino phenol hydrochloride is dissolved in deionized water under nitrogen, and aqueous hydrochloric acid solution is obtained. Mixed solution (B) and aqueous hydrochloric acid solution are added in volume ratio of 1:0.2-0.5, the obtained mixture is heated at 70-95 degrees C under nitrogen for 10-30 minutes, cooled to room temperature, and filtered. The cake is processed at -50 degrees C to -60 degrees C under 8-10 Pa for 24-48 hours, and graphene-containing monomer is obtained. The phosphorus pentoxide content of polyphosphoric acid is 81-84 %mass. Phosphorus pentoxide and mixed solution (A) are mixed in mass ratio of 1.2-1.5:1, heated at 140-160 degrees C and maintained for 2-10 hours to obtain a mixture. The mixture is added in a kneading machine, and heated at 180-200 degrees C for 4-5 hours to obtain graphene/poly(p-phenylene benzobisoxazole) polymer.