• 专利标题:   Synthesizing graphene polymer material by radical polymerization involves forming graphene oxide with active functional groups, adding to e.g. concentrated sulfuric acid, ultrasonically dispersing, filtering, drying and determining.
  • 专利号:   CN110483668-A
  • 发明人:   CUI L, LV Y, LI G, LI C, ZHOU S
  • 专利权人:   UNIV SHANDONG SCI TECHNOLOGY
  • 国际专利分类:   C08F120/14, C08F002/44, C08F004/04, C08K003/04, C08K009/04
  • 专利详细信息:   CN110483668-A 22 Nov 2019 C08F-120/14 201999 Pages: 7 Chinese
  • 申请详细信息:   CN110483668-A CN10734106 09 Aug 2019
  • 优先权号:   CN10734106

▎ 摘  要

NOVELTY - Synthesizing graphene polymer material by radical polymerization involves oxidizing graphene to form graphene oxide with active functional groups and large number of carboxyl, hydroxyl, and cycloalkyl groups formed on its surface, adding oxidized graphene to concentrated sulfuric acid and potassium permanganate solution, ultrasonically dispersing, filtering, washing, drying, determining the content of hydroxyl groups in graphene oxide by thermogravimetric analysis, infrared analysis and other elemental analysis, mixing graphene oxide with dimethylformamide in three-necked flask, ultrasonically oscillating, mixing 4,4'-azobis and dimethylformamide in another three-necked flask, magnetically stirring, adding N,N-dicyclohexylcarbimide as catalyst, reacting, adding 4-dimethylaminopyridine as catalyst, reacting, mixing two bottles of test solution together, magnetically stirring, adding distilled water, washing, suction filtering, rinsing and drying the reaction product. USE - Synthesizing graphene polymer material by radical polymerization. ADVANTAGE - The method produces graphene polymer material having improved heat resistance and mechanical properties. DETAILED DESCRIPTION - Synthesizing graphene polymer material by radical polymerization involves oxidizing graphene to form graphene oxide with active functional groups and large number of carboxyl, hydroxyl, and cycloalkyl groups formed on its surface, adding oxidized graphene to 98 wt.% concentrated sulfuric acid and 5 wt.% potassium permanganate solution at normal temperature, ultrasonically dispersing for 0.5-1 hour or magnetic stirring for 4-6 hours, filtering, washing, drying, determining the content of hydroxyl groups in graphene oxide by thermogravimetric analysis, infrared analysis and other elemental analysis, mixing 0.30 g graphene oxide with 30 mL dimethylformamide in three-necked flask, ultrasonically oscillating for 1 hour, mixing 4,4'-azobis and 20 mL dimethylformamide in another three-necked flask, magnetically stirring for 10 minutes, adding 0.15 g N,N-dicyclohexylcarbimide as catalyst at 0 degrees C, reacting for 15 minutes, adding 0.15 g 4-dimethylaminopyridine as catalyst, reacting for 15 minutes, mixing two bottles of test solution together, magnetically stirring at room temperature for 24 hours, adding 30 mL distilled water, washing for 30 minutes, suction filtering, rinsing with distilled water to adjust the pH of the filtrate to neutral, placing the reaction product into a low temperature oven, drying, esterifying azo initiator having carboxyl group with hydroxyl group on graphene oxide to form a modified graphene covalently bonded to radical initiator, using modified graphene as a free radical initiator and in situ polymerization to perform homopolymerization or copolymerization of free radical polymerization monomers to obtain polymer/graphene composite materials with good dispersibility and compatibility, mixing 5 ml pure methyl methacrylate and 0.0821 g modified graphene, adding 20 mL tetrahydrofuran at 80 degrees C for 3 hours, ultrasonically processing the mixture at room temperature, immersing the reaction flask and the reaction mixture in a silicone oil bath through dry nitrogen, polymerizing at 80 degrees C under the protection of nitrogen, suction filtering, washing with absolute ethanol solution and vacuum drying at 60 degrees C for 24 hours in vacuum drying box.