• 专利标题:   Nanocomposite wave absorbing material is layered nanocomposite wave absorbing material having hollow iron oxide nanoparticles grown on graphene sheet layer.
  • 专利号:   CN104592933-A, CN104592933-B
  • 发明人:   FENG D
  • 专利权人:   FENG D, FENG D
  • 国际专利分类:   C09K003/00
  • 专利详细信息:   CN104592933-A 06 May 2015 C09K-003/00 201569 Pages: 8 Chinese
  • 申请详细信息:   CN104592933-A CN10016139 12 Jan 2015
  • 优先权号:   CN10016139

▎ 摘  要

NOVELTY - A nanocomposite wave absorbing material is layered nanocomposite wave absorbing material having hollow iron oxide nanoparticles grown on graphene sheet layer. Potassium persulfate is added to graphite powder, and nitric acid is added to obtain preoxidized graphite. The preoxidized graphite is heat-treated and hydrogen peroxide is added to obtain graphite oxide. The graphite oxide is surface-treated, surface-treated graphite oxide and graft polymer are mixed, and mixture of ferric chloride and ferrous chloride is added to obtain nanocomposite wave absorbing material. USE - Nanocomposite wave absorbing material (claimed). DETAILED DESCRIPTION - A nanocomposite wave absorbing material is layered nanocomposite wave absorbing material having hollow hemispherical iron oxide nanoparticles grown on graphene sheet layer. Graphite is crushed to 50-200-mesh, 35 %mass hydrochloric acid solution is added, stirred for 30 minutes, washed with deionized water and dried to obtain graphite powder. Potassium persulfate, phosphorus pentoxide and concentrated sulfuric acid are added to graphite powder to obtain mixture. The pH of obtained mixture is adjusted to 1.5, stirred at 60 degrees C for 1-2 hours, temperature of the resulting mixture is increased to 80 degrees C for 2-4 hours at a speed of 5 degrees C/minute, heated at 87 degrees C for 1-2 hours, and the mixture is diluted with distilled water. The pH of the resulting mixture is diluted to 3.6, filtered, and dried. Concentrated nitric acid is added to dried mixture, stirred for 45-60 minutes, pH is adjusted to 2-4, potassium permanganate is added, stirred for 30 minutes, cooled to -12 degrees C, potassium permanganate is added again, and stirred for 30 minutes to obtain preoxidized graphite. The preoxidized graphite is filtered, dried, dried product is placed in muffle furnace, heat-treated at 1100 degrees C for 10-20 seconds, 1150 degrees C for 15-20 seconds, and heat-treated at 1180 degrees C for 20-30 seconds to obtain expanded graphite. The expanded graphite is heated at 40 degrees C for 3 hours, distilled water and hydrogen peroxide are added, reacted for 10-60 minutes, and centrifuged at a speed of 8000-10000 rpm. The obtained product is washed with hydrochloric acid solution, and dialyzed to obtain graphite oxide. The graphite oxide is dissolved in dimethyl sulfoxide, N-hydroxysuccinimide and artificial surface treating agent are added, ultrasonic processing is carried out at 35 degrees C for 2 hours, filtered, washed and dried to obtain surface-treated graphite oxide. The surface-treated graphite oxide and graft polymer are mixed, heated to 80-95 degrees C, nitrogen is purged to the resulting mixture, tetravalent cerium ion-containing solution is added, stirred for 2-4 hours, filtered, washed and dried to obtain polymer-grafted graphite oxide. 1-10 g Polymer-grafted graphite oxide is lyophilized at (-10)-(30) degrees C, 1-10g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer in 500 ml ethylene glycol is added and ultrasonic processing is carried out to obtain uniform dispersion (d1). 4-15 g Mixture of ferric chloride hexahydrate, ferrous chloride tetrahydrate and iron acetylacetonate is added, 6-25g polyvinylpyrrolidone and 10-50 g Ammonium acetate dissolved in 500-1000 mL ethylene glycol are added to obtain dispersion (d2). The dispersion (d1) and dispersion (d2) are mixed, pH is adjusted to 8-10 using ammonia, 100 ml obtained solution is placed in reactor, heated at 150 degrees C for 2 hours, cooled, centrifuged, washed with deionized water, and vacuum-dried to obtain product (P1). 5 g Product (P1) and 5-10 g aniline monomer are added to dodecylbenzenesulfonic acid solution, and ultrasonic processing is carried out to obtain product (P2). 3 g Ammonium persulfate is dissolved in 80-120 ml distilled water, product (P2) is dripped in the resulting mixture, stirred, filtered, the filtrate is washed with ethanol, and vacuum-dried at 50-70 degrees C for 24-36 hours to obtain nanocomposite wave absorbing material. The mass ratio of graphite powder, potassium persulfate, phosphorus pentoxide and concentrated sulfuric acid is 1-3:1-2:1-2:5-10. The mass ratio of dried mixture and concentrated nitric acid is 1-4:50-100. The volume ratio of distilled water and hydrogen peroxide is 4-20:1. The mass ratio of graphite oxide and polymer is 1-2:1-3. The polymer comprises methyl methacrylate, glycidyl methacrylate, dimethylaminoethyl methacrylate and diethylaminoethyl methacrylate in a mass ratio of 1:1:2:1. The mass ratio of ferric chloride hexahydrate, ferrous chloride tetrahydrate and iron acetyl acetonate is 1:1:0.5. The mass ratio of product (P1) and dodecylbenzenesulfonic acid is 1-1.5:8-15.