• 专利标题:   Preparing organic-inorganic hybrid three-layer core-shell particle modified carbon fiber comprises e.g. obtaining zirconium dioxide hard core, performing carbon fiber surface pretreatment, condensing carbon fiber and vacuum drying.
  • 专利号:   CN113338028-A
  • 发明人:   WU Q, BAI H, ZHAO R, ZHU J
  • 专利权人:   UNIV SHAANXI SCI TECHNOLOGY
  • 国际专利分类:   D06M011/46, D06M011/74, D06M013/44, D06M013/325, D06M011/64, C08L063/00, C08K009/02, C08K009/04, C08K007/06, C08J005/06, D06M101/40
  • 专利详细信息:   CN113338028-A 03 Sep 2021 D06M-011/46 202182 Pages: 10 Chinese
  • 申请详细信息:   CN113338028-A CN10629002 07 Jun 2021
  • 优先权号:   CN10629002

▎ 摘  要

NOVELTY - Preparing organic-inorganic hybrid three-layer core-shell particle modified carbon fiber comprises (i) obtaining zirconium dioxide hard core based on mass fraction, mixing 1-10 pts. wt. zirconium oxychloride octahydrate, 1-10 pts. wt. absolute ethanol and 5-70 pts. wt. water, stirring until clear; (ii) mixing hard core of zirconium dioxide and anhydrous ethanol, adding to the graphene oxide and anhydrous with a mass ratio of 0.01:30-50; (iii) mixing zirconium dioxide-graphene oxide, tetrahydrofuran, hexachlorotripolyphosphazene uniformly and passing nitrogen protection to react; (iv)performing carbon fiber surface pretreatment using acetone as the solvent, and using the Soxhlet extraction method to condense and reflux the carbon fiber at 70-80 degrees C for 24-48 hours and drying; and (v) mixing 0.05-0.3 pts. wt. zirconium dioxide-graphene oxide-hexachlortripolyphosphazene-triethylamine, 1-3 pts. wt. triethylamine and 40-270 pts. wt. tetrahydrofuran uniformly. USE - The method is useful for preparing organic-inorganic hybrid three-layer core-shell particle modified carbon fiber. ADVANTAGE - The method achieves the purpose of improving the interfacial bonding strength of the composite material by the core-shell particle modified carbon fiber; and increases interface bond strength of the modified carbon fiber composite material by 55.7-86.5%. DETAILED DESCRIPTION - Preparing organic-inorganic hybrid three-layer core-shell particle modified carbon fiber comprises (i) obtaining zirconium dioxide hard core based on mass fraction, mixing 1-10 pts. wt. zirconium oxychloride octahydrate, 1-10 pts. wt. absolute ethanol and 5-70 pts. wt. water, stirring until clear, and transferring to the hydrothermal kettle, incubating the reaction at 100-150 degrees C for 12-24 hours, centrifuging and drying at 50-80 degrees C, adding dried product to the mixed solution of silane coupling agent, absolute ethanol and water, where the mass ratio of the dried product, silane coupling agent, absolute ethanol and water is 1:10-20:10-30:1-5, reacting at 60-80 degrees C for 1-5 hours, after centrifugation, ethanol and water, cleaning with deionized water, drying at 60-100 degrees C to obtain the zirconium dioxide hard core; (ii) mixing hard core of zirconium dioxide and anhydrous ethanol with a mass ratio of 0.01:10-20, adding to the graphene oxide and anhydrous with a mass ratio of 0.01:30-50, stirring at 0-10 degrees C for 4-8 hours, allowing to stand, collecting the precipitate, washing it with deionized water and freeze-dry to obtain the zirconia hard core and graphene oxide inner shell layer zirconium-graphene oxide; (iii) mixing 0.1-0.5 pts. wt. zirconium dioxide-graphene oxide, 40-200 pts. wt. tetrahydrofuran, 0.5-2.5 pts. wt. hexachlorotripolyphosphazene uniformly and passing nitrogen protection to react at 40-60 degrees C for 15 minutes, adding 0.5-2.5 pts. wt. triethylamine, continue to react under nitrogen protection at 40-60 degrees C for 5-10 hours, reacting, washing product with tetrahydrofuran and chloroform and drying at 40-60 degrees C, adding 0.1-0.5 pts. wt. dried product to 0.2-1.5 pts. wt. hexachlorotripolyphosphazene, 1-2 pts. wt. diaminodiphenyl ether and 40-200 pts. wt. tetrahydrofuran, reacting at 40-60 degrees C for 15 minutes under the protection of nitrogen, adding 0.5-2.5 pts. wt. triethylamine, continuing to react at 40-60 degrees C for 5-10 hours under the protection of nitrogen, washing product clean with deionized water and dimethylformamide at 40-60 degrees C to obtain a zirconium dioxide composed of three parts including a hard core of zirconium dioxide, an inner shell layer of graphene oxide and an outer shell layer of hexachlorotriphosphonitrile-triethylamine-oxidation grapheme- phosphonitrile- triethylamine; (iv)performing carbon fiber surface pretreatment using acetone as the solvent, and using the Soxhlet extraction method to condense and reflux the carbon fiber at 70-80 degrees C for 24-48 hours and drying, oxidizing dried fiber in concentrated nitric acid at 60-100 degrees C for 2-6 hours, washing product with deionized water until the pH is 7, and drying at 60-80 degrees C to obtain oxidized carbon fiber; and (v) mixing 0.05-0.3 pts. wt. zirconium dioxide-graphene oxide-hexachlortripolyphosphazene-triethylamine, 1-3 pts. wt. triethylamine and 40-270 pts. wt. tetrahydrofuran uniformly, adding 0.2-1 pts. wt. oxidized carbon fiber to it, and reacting at 40-60 degrees C under reflux for 8-16 hours, washing with tetrahydrofuran and vacuum drying at 60-80 degrees C for 4-8 hours After the reaction is completed.