• 专利标题:   Preparing graphene oxide reinforced carbon fiber material comprises e. g. adding concentrated sulfuric acid and sodium nitrate into clean and dry beaker, uniformly stirring in ice water bath, adding graphite powder and mixing.
  • 专利号:   CN111154144-A
  • 发明人:   WEI J, HE Z, WEI Z
  • 专利权人:   UNIV TAIZHOU
  • 国际专利分类:   C01B032/198, C08J005/06, C08K007/06, C08K009/02, C08K009/12
  • 专利详细信息:   CN111154144-A 15 May 2020 C08K-009/12 202055 Pages: 8 Chinese
  • 申请详细信息:   CN111154144-A CN10092023 14 Feb 2020
  • 优先权号:   CN10092023

▎ 摘  要

NOVELTY - Preparing graphene oxide reinforced carbon fiber material comprises e. g. (i) adding 200-250 ml 98% concentrated sulfuric acid and 5 g sodium nitrate into a clean and dry beaker, uniformly stirring in ice water bath 0-5oC, adding 8-10 g graphite powder, mixing, adding 28-30 g potassium permanganate and controlling the reaction temperature to 0-10oC, placing the beaker in a constant temperature water bath at 30-40 degrees C, stirring the reaction at constant speed for 3-4 hours, adding 450-500 ml deionized water, heating to 100 degrees C at rate of 10oC, stirring the reaction for 20-30 minutes for oxidation reaction, adding hydrogen peroxide to consume excess potassium permanganate, changing the solution from brownish black to bright yellow, centrifuging the solution, and repeatedly washing and centrifuging the product with deionized water until the pH of the solution is 6-7, and obtaining the graphene oxide solution; and (ii) taking Soxhlet extractor, condensing and refluxing. USE - The method is useful for preparing graphene oxide reinforced carbon fiber material. ADVANTAGE - The method significantly improves the dispersion performance of graphene oxide, disperses and adsorbs it on the carbon fiber matrix, improves the tensile properties of the material, greatly improves the tensile strength and elongation at break and makes obvious effect of strengthening and toughening the material. DETAILED DESCRIPTION - Preparing graphene oxide reinforced carbon fiber material comprises (i) adding 200-250 ml 98% concentrated sulfuric acid and 5 g sodium nitrate into a clean and dry beaker, uniformly stirring in ice water bath 0-5oC, adding 8-10 g graphite powder, mixing, adding 28-30 g potassium permanganate and controlling the reaction temperature to 0-10oC, placing the beaker in a constant temperature water bath at 30-40 degrees C, stirring the reaction at constant speed for 3-4 hours, adding 450-500 ml deionized water, heating to 100 degrees C at rate of 10oC, stirring the reaction for 20-30 minutes for oxidation reaction, adding hydrogen peroxide to consume excess potassium permanganate, changing the solution from brownish black to bright yellow, centrifuging the solution, and repeatedly washing and centrifuging the product with deionized water until the pH of the solution is 6-7, and obtaining the graphene oxide solution; (ii) taking Soxhlet extractor, condensing and refluxing, using condensed water or ethanol as condensing and refluxing agent, using acetone as solvent and cleaning agent of carbon fiber, heating the acetone solution to 80-100 degrees C, cleaning carbon fiber for 48-64 hours, completely removing the slurry on the surface of the fibril, cooling to 50 degrees C, performing suction filtration to obtain carbon fiber solids, and drying; (iii) taking carbon fiber obtained in the step (ii), adding into the mixed acid solution with concentrated sulfuric acid/concentrated nitric acid volume ratio of 3:1, carrying out the acidification reaction at 60-80 degrees C for 9-12 hours, performing suction filter, washing 6-9 times with distilled water, drying, grinding the solidified acidified carbon fiber obtained above, dispersing the acidified carbon fiber in deionized water, where the concentration of acidified carbon fiber in water is 3-4 mg/ml, super-dispersing the solution for 4-6 hours, and obtaining uniformly dispersed aqueous solution of acidified carbon fibers; (iv) taking 2-3 ml graphene oxide, adding into 80-100 ml of the solution, mixing uniformly and sonicating for 2-3 hours to obtain mixed dispersion solution; and (v) slowly pouring the mixed dispersion solution onto the base film in the rectangular glassware, placing the glassware in the water bath, heating at 60-80 degrees C until the water completely evaporates, removing the base film carrier and the graphene reinforced carbon fiber membrane from the glassware, and drying in a vacuum oven at 60-80 degrees C for 3-5 hours.