• 专利标题:   Graphene-loaded nano-nickel wave absorbing material, prepared by preparing a mixture of pre-oxidized graphite, surface processing the pre-oxidized graphite, dispersing, heating the dispersion solution, centrifuging and vacuum drying.
  • 专利号:   CN104694074-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:   CN104694074-A 10 Jun 2015 C09K-003/00 201602 Pages: 7 Chinese
  • 申请详细信息:   CN104694074-A CN10016251 12 Jan 2015
  • 优先权号:   CN10016251

▎ 摘  要

NOVELTY - Graphene-loaded nano-nickel wave absorbing material, is claimed. The absorbing material is layered nanocomposite wave-absorbing material. The nickel nanoparticles are uniformly grown in the graphene sheet layer. The size of nickel nanoparticles loaded on the graphene sheet is 20-100 nm. Preparation of the absorbing material comprises (i) preparing a mixture of pre-oxidized graphite; (ii) surface processing the pre-oxidized graphite; (iii) dispersing; and (iv) heating the dispersion solution, centrifuging and vacuum drying. USE - Used as graphene-loaded nano-nickel wave absorbing material. DETAILED DESCRIPTION - Graphene-loaded nano-nickel wave absorbing material, is claimed. The absorbing material is layered nanocomposite wave-absorbing material. The nickel nanoparticles are uniformly grown in the graphene sheet layer. The size of nickel nanoparticles loaded on the graphene sheet is 20-100 nm. The polyaniline is coated on the surface of the graphene sheet loaded with nickel nanoparticles. Preparation of the absorbing material comprises (i) adding graphite powder, potassium persulfate and phosphorus pentoxide into concentrated sulfuric acid to form a mixture, adjusting pH of the mixture to 1.5, stirring the mixture at 60 degrees C for 1-2 hours, stirring and heating to 80 degrees C for 2-4 hours at a rate of 5 degrees C/minute, stirring and heating to 87 degrees C for 1-2 hours at a rate of 2 degrees C/minute, diluting the mixture using distilled water, adjusting pH of the diluted mixture to 3.6, allowing to stand for 36 hours, filtering using distilled water, adjusting pH of the mixture to 6-7 and drying at room temperature, where the mass ratio of graphite powder, potassium persulfate, phosphorus pentoxide and concentrated sulfuric acid is 1-3:1-2:1-2:5-10, adding concentrated nitric acid into the dry mixture and stirring for 45-60 minutes, adjusting pH value to 2-4, where the mass ratio of the dry mixture and concentrated nitric acid is 1-4:50-100, stirring at -8 degrees C, adding potassium permanganate for first time, stirring for 30 minutes, cooling to -12 degrees C, adding potassium permanganate for second time, stirring for 30 minutes, finally cooling to -15 degrees C, adding potassium permanganate for third time, stirring for 20 minutes to obtain a mixture of pre-oxidized graphite, where the mass ratio of potassium permanganate added for first time, second time and third time is 1:2:3 and the ratio of the dry mixture and total potassium permanganate is 1-2:10-15; (ii) adding pre-oxidized graphite mixture into an incubator, heating to 40 degrees C, reacting for 3 hours, adding consistent volume of distilled water into pre-oxidized graphite mixture for first time, reacting for 2.5 hours, controlling the temperature of the incubator at 40 degrees C, adding distilled water for second time and hydrogen peroxide, reacting for 10-60 minutes, where the amount of water added for the second time is 1-1.5 times of distilled water added for the first time, where the volume ratio of distilled water added for the second time and hydrogen peroxide is 4-20:1, centrifuging for 10 minutes under speed of 9500 revolutions/minute after completion of the reaction, washing the centrifuged product with hydrochloric acid solution, where the volume of the hydrochloric acid solution is 10-50 times the volume of the centrifuged product, carrying out dialysis for 7-8 days to obtain graphite oxide, ultrasonic dissolving the graphite oxide in dimethylsulfoxide, adding N-hydroxysuccinimide and surface treatment agent, stirring at 35 degrees C for 2 hours, suction-filtering the product, washing and drying to obtain surface-treated graphite oxide; (iii) lyophilizing 1-2 g of surface-treated graphite oxide at -10 to 30 degrees C, adding 1-10 g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer into 500 ml of ethylene glycol, ultrasonic dispersing to form a first dispersion; dissolving 20-40 ml nickel chloride ethylene glycol solution (0.1 mol/ml), 6-25 g polyvinylpyrrolidone and 10-50 g ammonium acetate in 500-1000 ml ethylene glycol to form a second dispersion, mixing the first dispersion and second dispersion, and adjusting pH value to 9-11 using aqueous ammonia to form clear solution; and (iv) adding 100 ml clear solution into a reaction vessel, sealing, heating to 130 degrees C for 2 hours, heating at a rate of 2-4 degrees C/minute to 150 degrees C for 4 hours, heating at a rate of 3-6 degrees C/minute to 200 degrees C for 3 hours, cooling to 180 degrees C for 2 hours at a cooling rate of 5-7 degrees C/minute, heating to 200 degrees C for 7 hours at a heating rate of 3-6 degrees C/minutes, taking out the reactor after completion of the reaction, cooling to room temperature at cooling rate of 3-6 degrees C/minute, separating the resulting powder by centrifugation for 10 minutes under speed of 8000-10000 revolutions/minute, washing using ethanol and deionized water for three times, vacuum drying at 50-70 degrees C for 24 hours to obtain a first product; adding 5 g of the first product and 5-10 g aniline monomer into dodecylbenzenesulfonic acid solution, ultrasonic dispersing for 65 minutes to form a second product, where the mass ratio of the first product and dodecylbenzenesulfonic acid 1-1.5:8-15; dissolving 3 g of ammonium persulfate in 80-120 ml distilled water, dropping the second product, stirring and reacting for 15 hours, filtering, respectively washing the filtrate with distilled water and ethanol until it is colorless, and vacuum drying at 50-70 degrees C for 24-36 hours.