• 专利标题:   Nanonickel-loaded graphene composite wave-absorbing material is layered composite material comprising nickel nanoparticles having particle size of preset value, grown on graphene sheet, and polyaniline coated on graphene sheet.
  • 专利号:   CN104694077-A
  • 发明人:   FENG D
  • 专利权人:   FENG D
  • 国际专利分类:   C09K003/00
  • 专利详细信息:   CN104694077-A 10 Jun 2015 C09K-003/00 201608 Pages: 8 Chinese
  • 申请详细信息:   CN104694077-A CN10016301 12 Jan 2015
  • 优先权号:   CN10016301

▎ 摘  要

NOVELTY - A nanonickel-loaded graphene composite wave-absorbing material is layered composite material comprising nickel nanoparticles having particle size of 20-100 nm, grown on a graphene sheet layer, and polyaniline coated on the surface of the graphene sheet loaded with the nickel nanoparticles. Preparation of composite wave-absorbing material, is also claimed. Mixture containing e.g. sulfonated graphite, and aniline are added to solution of sodium dodecylbenzenesulfonate, ammonium persulfate solution is dripped, filtered, washed and dried, to obtain wave-absorbing material. USE - Nanonickel-loaded graphene composite wave-absorbing material (claimed). ADVANTAGE - The nanonickel-loaded graphene composite material has excellent wave absorbing performance and is prepared by rapid process. DETAILED DESCRIPTION - A nanonickel-loaded graphene composite wave-absorbing material is layered composite material comprising nickel nanoparticles having particle size of 20-100 nm, grown on a graphene sheet layer, and polyaniline coated on the surface of the graphene sheet loaded with the nickel nanoparticles. Also claimed is, preparation of nanonickel-loaded graphene composite wave-absorbing material. Graphite powder having a size of 50-200 mesh is added to 35 %mass hydrochloric acid solution, stirred for 30 minutes, then rinsed using deionized water until pH of wash water is neutral, and dried. Dried graphite powder, potassium persulfate, phosphorus pentoxide and concentrated sulfuric acid in a molar ratio of 1-3:1-2:1-2:5-10 are mixed, pH is adjusted to 1.5, then stirred at 60 degrees C for 1-2 hours, heated at 80 degrees C for 2-4 hours at a rate of 5 degrees C/minute, stirred at 87 degrees C for 1-2 hours at a rate of 2 degrees C/minute, diluted using distilled water, pH is adjusted to 3.6, left still for 36 hours, filtered and solid is dried at room temperature. Concentrated nitric acid is added, stirred for 45-60 minutes, pH is adjusted to 2-4, potassium permanganate is added at -8 degrees C, stirred for 30 minutes, cooled to -12 degrees C, potassium permanganate is further added, stirred for 30 minutes, cooled to -15 degrees C, potassium permanganate is added and stirred for 20 minutes. Mixture is filtered, dried, heated at 1100 degrees C for 10-20 seconds, 1150 degrees C for 15-20 seconds and 1180 degrees C for 20-30 seconds, to obtain expanded graphite. Expanded graphite is heated at 40 degrees C for 3 hours in an incubator, distilled water is added, reacted at 40 degrees C for 2.5 hours, distilled water and hydrogen peroxide in a ratio of 4-20:1 are added, mixed for 10-60 minutes, centrifuged for 10 minutes at a rate of 8000-10000 rpm, washed using hydrochloric acid solution, where the volume of hydrochloric acid solution after centrifugation is 10-50 times the volume of the product, and dialyzed for 7-8 days, to obtain graphite oxide. Graphite oxide is dissolved in dimethyl sulfoxide, then N-hydroxysuccinimide and surfactant are added, stirred at 35 degrees C for 2 hours, filtered, washed and dried, to obtain surface-treated graphite oxide. 1 g Surface-treated graphite oxide is added to 500 g deionized water, stirred for 10-15 minutes, pH is adjusted to 11 using aqueous ammonia, temperature is raised to 70 degrees C, 5-10 g aqueous sodium borohydride is added, stirred for 30-60 minutes, temperature is reduced to 15 degrees C, then 25 g amino acid is added, stirred for 2-4 hours, leave still for 3 hours, filtered to remove the solvent, and washed with deionized water 2 times. Residue is dispersed in 400-1600 g deionized water, 1-4 g hydrazine hydrate is added, reacted at 80 degrees C for 12-24 hours, filtered, washed with deionized water 2 times, and dried for 24-48 hours, to obtain sulfonated graphite. 1-2 g sulfonated graphite is freeze-dried at -10 degrees C to -30 degrees C, 1-10 g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is added, mixed, mixture is dispersed in 500 ml ethylene glycol, to obtain uniform dispersion (a). 20-40 ml ethylene glycol solution of nickel chloride with concentration of 0.1 mol/ml, 6-25 g polyvinylpyrrolidone and 10-50 g ammonium acetate are dissolved in 500-1000 ml ethylene glycol, to obtain dispersion (b). Dispersion (a) and dispersion (b) are mixed, and pH is adjusted to 9-11 using ammonia. 100 Ml obtained solution is added into reactor, then sealed and heated at 130 degrees C for 2 hours at a rate of 2-4 degrees C/minute, further heated at 150 degrees C for 4 hours at a rate of 3-6 degrees C/minute, heated at 200 degrees C for 3 hours, cooled to 180 degrees C at a rate of 5-7 degrees C/minute, heated at 200 degrees C for 7 hours at a rate of 3-6 degrees C/minute, cooled to room temperature at a rate of 3-6 degrees C/minute, centrifuged for 10 minutes at a rate of 8000-10000 rpm, washed 3 times using ethanol and deionized water, and vacuum-dried at 50-70 degrees C for 24 hours, to obtain dried product (A). 5 g Product (A) and 5-10 g aniline monomer are added to a solution of sodium dodecylbenzenesulfonate and ultrasonically dispersed for 65 minutes, to obtain product (B). Solution of 3 g ammonium persulfate dissolved in 80-120 ml distilled water is dripped into product (B), stirred for 15 hours, filtered, washed using distilled water and ethanol, and vacuum-dried at 50-70 degrees C for 24-36 hours, to obtain nanonickel-loaded graphene composite wave-absorbing material. The ratio of dried substance and concentrated nitric acid is 1-4:50-100. The mass ratio of dried substance and total amount of potassium permanganate is 1-2:10-15. The mass ratio of product (A) and sodium dodecylbenzenesulfonate is 1-1.5:8-15.