• 专利标题:   Preparation of carboxylated graphene-epoxy resin composite material involves mixing epoxy resin, curing agent and carboxylated graphene powder prepared using e.g. graphene oxide and hydrazine hydrate, adding promoter, and curing.
  • 专利号:   CN104448704-A, CN104448704-B
  • 发明人:   DAI S, GENG X, YANG C, ZHANG X, YAN S
  • 专利权人:   AVIATION IND CORP CHINA BEIJING GREAT WA, AVIC BEIJING INST AERONAUTICAL MATERIALS
  • 国际专利分类:   C08K003/04, C08K009/04, C08L063/00, C09C001/46, C09C003/06, C09C003/08
  • 专利详细信息:   CN104448704-A 25 Mar 2015 C08L-063/00 201561 Pages: 9 Chinese
  • 申请详细信息:   CN104448704-A CN10647300 14 Nov 2014
  • 优先权号:   CN10647300

▎ 摘  要

NOVELTY - Preparation of carboxylated graphene-epoxy resin composite material involves ultrasonically processing graphene oxide in distilled water, adding hydrazine hydrate as reducing agent, obtaining graphene turbid liquid, cooling, adding alcohol solution of aminophenyl acid and amyl nitrite, adding strong base, condensing, obtaining carboxylated graphene precursor turbid fluid, washing with deionized water, filtering, freeze-drying, obtaining carboxylated graphene powder, mixing epoxy resin, curing agent and carboxylated graphene powder, stirring, adding promoter, heating, curing, and cooling. USE - Preparation of carboxylated graphene-epoxy resin composite material (claimed). ADVANTAGE - The method enables preparation of carboxylated graphene-epoxy resin composite material having excellent toughness, quality and stability. DETAILED DESCRIPTION - Preparation of carboxylated graphene-epoxy resin composite material involves ultrasonically processing graphene oxide in distilled water at ultra-sound power of 600-900 W for 30-60 minutes, obtaining graphene oxide suspension with concentration of 1-3 g/L, adding hydrazine hydrate as reducing agent, condensing in oil bath at 85-95 degrees C for 24-48 hours, obtaining graphene turbid liquid, cooling to 70-80 degrees C, adding alcohol solution of aminophenyl acid and amyl nitrite, adding strong base, condensing in oil bath at 70-80 degrees C for 24-48 hours, obtaining carboxylated graphene precursor turbid fluid, adjusting pH to 5-6 using strong acid, washing with deionized water, filtering, freeze-drying at -40 degrees C to 20 degrees C for 5-7 days, obtaining carboxylated graphene powder, mixing epoxy resin and curing agent at 40-60 degrees C for 0.5-1.5 hours, adding carboxylated graphene powder, stirring at room temperature for 10-20 minutes, adding promoter, stirring for 10-20 minutes, performing vacuum gas pumping at 30-50 degrees C for 40-60 minutes, heating at 110 degrees C for 2 hours, 140 degrees C for 2 hours, 170 degrees C for 3 hours, and 200 degrees C for 2 hours, curing, and cooling at room temperature. The mass ratio of graphene oxide and hydrazine hydrate is 1:1-2. Aminophenyl acid is aminophenyl formic acid or aminophenyl acetic acid. The concentration of amyl nitrite alcohol solution is 0.2 g/ml. Alcohol is methanol or ethanol. The molar ratio of aminophenyl acid and graphene oxide is 1-10:10. The molar ratio of amyl nitrite and graphene oxide is 1-2:1. The strong base is potassium hydroxide or sodium hydroxide. The molar ratio of potassium hydroxide or sodium hydroxide and aminophenyl acid is 1.2-1.5:1. Strong acid is hydrochloric acid or sulfuric acid. Epoxy resin is alicyclic epoxy resin. The curing agent is acid anhydride-type curing agent. The mass ratio of epoxy resin and curing agent is 1:1.3-1.4. The mass ratio of carboxylated graphene powder and epoxy resin is 0.5-3:100. The promoter is phenolic promoter. The mass ratio of promoter and epoxy resin is 0.1-0.5:100.