• 专利标题:   Preparing composite mesoporous material, used as electromagnetic wave absorbing material, comprises e.g. preparing graphite powder, surface-treated graphite oxide, and graphene, ferroferric oxide or polyaniline nano-composite material.
  • 专利号:   CN104689798-A
  • 发明人:   FENG Y
  • 专利权人:   FENG Y
  • 国际专利分类:   B01J020/26, B01J020/28, B01J020/30, C01B031/04, C01G049/08, C09K003/00
  • 专利详细信息:   CN104689798-A 10 Jun 2015 B01J-020/26 201572 Pages: 8 Chinese
  • 申请详细信息:   CN104689798-A CN10016052 12 Jan 2015
  • 优先权号:   CN10016052

▎ 摘  要

NOVELTY - Preparing composite mesoporous material comprises (i) preparing graphite powder; (ii) preparing surface-treated graphite oxide; (iii) lyophilizing step (ii) product, adding polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, and adding polymethyl methacrylate and polyacrylamide mixture to ethanol, performing ultrasonic dispersion, and irradiating; (iv) preparing graphene/hollow ferroferric oxide/polyaniline nano-composite material; and (v) sintering the step (iv) product with potassium permanganate, and heating at a rate of 10 degrees C/minute. USE - The composite mesoporous material is used as electromagnetic wave absorbing materials. ADVANTAGE - The method has easy preparation procedure, and is environmental friendly. DETAILED DESCRIPTION - Preparing composite mesoporous material comprises (i) preparing graphite powder by adding pre-oxidized graphite with potassium persulfate, and adding phosphorus pentoxide in concentrated sulfuric acid, to obtain a mixture having pH of 1.5, and uniformly stirring the mixture at 60 degrees C for 1-2 hours, and then heating at a rate of 5 degrees C/min, uniformly mixing for 2-4 hours by raising temperature to 80 degrees C by, and heating at a rate of 2 degrees C/min, raising temperature to 87 degrees C while uniformly mixing for 1-2 hours, and then diluting the mixture using distilled water, until the pH of the mixture reaches 3.6, filtering for 36 hours using distilled water, allowing the mixture to attain pH of 6-7, drying at room temperature, adding graphite powder, potassium persulfate, concentrated sulfuric acid and phosphorus pentoxide in a ratio of 1-3:1-2:1-2:5-10, and drying the mixture, adding concentrated nitric acid and uniformly mixing for 45-60 minutes, to obtain mixture having pH of 2-4, where the mass ratio of dry mixture and concentrated nitric acid is 1-4:50-100, and carrying out (a) cooling to -8 degrees C, adding potassium permanganate, and uniformly mixing for 30 minutes, (b) cooling to -12 degrees C, adding potassium permanganate, and uniformly mixing for 30 minutes, and (c) cooling to -15 degrees C, adding potassium permanganate, and uniformly mixing for 20 minutes, where the mass ratio of potassium permanganate added in steps (a), (b) and (c), is 1:2:3, and the mass ratio of dry mixture and potassium permanganate, is 1-2:10-15; (ii) preparing surface-treated graphite oxide by preoxidizing the step (i) product by placing in an incubator at 40 degrees C for 3 hours, adding distilled water for first time into graphite mixture, pre-oxidizing by adding water, reacting for 2.5 hours, adding distilled water for second time into hydrogen peroxide, and reacting for 10-60 minutes, where the amount of distilled water added second time is 1-1.5 times to the volume of distilled water added second time, and the ratio of distilled water added second time and hydrogen peroxide, is 4-20:1, and then centrifuging at a speed of 9500 rotations/min for 10 minutes, washing the centrifuged product with hydrochloric acid, where the volume of hydrochloric acid used is 10-50 times the volume of the centrifuged product, and finally carrying out dialyzation process for 7-8 days to obtain graphite oxide, and preparing graphite oxide by mixing with purified liquid, purifying, performing shock dispersion, and filtering, to obtain purified graphite oxide, where the amount of hydrochloric acid used in purifying process is 1.72 g/ml, and the mass ratio of hydrochloric acid and hydrogen peroxide, is 1-2:2-5, and dissolving purified graphite oxide in dimethyl sulfoxide using ultrasound, adding N-hydroxysuccinimide and a surface processing agent, reacting by uniformly mixing at 35 degrees C for 2 hours, and filtering the product through suction, washing, and drying, to obtain surface-treated graphite oxide; (iii) dispersing 1-2 g of step (ii) product, lyophilizing at -10 degrees C to -30o?C, adding 1-10 g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, and adding 1 g polymethyl methacrylate and polyacrylamide mixture, in a mass ratio of 1:1 into 500 ml ethanol, and subjecting to ultrasonic dispersion, irradiating for 36 hours under UV irradiation, to obtain first uniform dispersion liquid, and adding mixture of 4-15 g iron(III) chloride hexahydrate, iron(II) chloride tetrahydrate, and acetylacetone, and 6-25 g polyvinylpyrrolidone and 10-50 g ammonium acetate, dissolving in 500-1000 ml ethanol, to obtain a second dispersion liquid, mixing the first dispersion liquid and second dispersion liquid, and adjusting pH to 8-10, to obtain a clear solution, where the mass ratio of iron(III) chloride hexahydrate, iron(II) chloride tetrahydrate and acetylacetone, is 1:1:0.5; (iv) adding 100 ml of step (iii) product to a reactor, sealing and heating to 150 degrees C for 2 hours, and heating at the rate of 2-4 degrees C/minute to 200 degrees C for 4 hours, heating at a rate of 3-6 degrees C/minute to 235 degrees C for 3 hours, then cooling at a rate of 5-7 degrees C/minute to 200 degrees C for 2 hours, and heating at a rate of 3-6 degrees C/minute to 235 degrees C for 7 hours, removing the reactor, and allowing to cool at a rate of 3-6 degrees C/minute to room temperature, and centrifuging the resulting black powder for 10 minutes at 8000-10000 rotations/minute, washing thrice with anhydrous ethanol and deionized water, drying under vacuum at 50-70 degrees C for 24 hours, and adding 5 g first product and 5-10 g aniline monomer to a solution of dodecylbenzenesulfonicacid, dispersing under ultrasonic conditions for 65 minutes, to obtain a first product, and adding the first product into dodecylbenzenesulfonicacid in mass ratio of 1-1.5:8-15, dissolving 3 g ammonium persulfate in 80-120 ml distilled water, and adding the mixture dropwise to second product, reacting for 15 hours, filtering with distilled water, and washing the product with ethanol until the filtrate turns colorless, drying under vaccum conditions at 50-70 degrees C for 24-36 hours, to obtain graphene/hollow ferroferric oxide/polyaniline nano-composite material; and (v) paving step (iv) product in a ceramic crucible, adding potassium permanganate into a muffle furnace for sintering, heating at a rate of 10-300 degrees C for 30 minutes, heating at a rate of 12-600 degrees C for 30 minutes, cooling at a rate of 15 degrees C/minute to 500 degrees C for 20 minutes, and heating at a rate of 15 degrees C/minute to 950 degrees C for 1-3 hours, and heating step (iv) product and potassium permanganate in a mass ratio of 1:3-5 at a rate of 10 degrees C/minute, to obtain the final product.