• 专利标题:   Inorganic-organic composite hybrid three-layer core-shell particle comprises hard core of zirconium dioxide, inner shell layer of graphene oxide, and outer shell layer of hexachlorotrichlorophosphazene-triethylamine.
  • 专利号:   CN113185753-A, CN113185753-B
  • 发明人:   WU Q, WANG Y, BAI H, ZHAO R, ZHU J, YANG C, ZHANG J, ZHANG X, LIU B
  • 专利权人:   UNIV SHAANXI SCI TECHNOLOGY
  • 国际专利分类:   C08K003/04, C08K003/22, C08K005/5399, C08K009/10
  • 专利详细信息:   CN113185753-A 30 Jul 2021 C08K-009/10 202176 Pages: 8 Chinese
  • 申请详细信息:   CN113185753-A CN10629023 07 Jun 2021
  • 优先权号:   CN10629023

▎ 摘  要

NOVELTY - Inorganic-organic composite hybrid three-layer core-shell particle comprises a hard core of zirconium dioxide, an inner shell layer of graphene oxide, and an outer shell layer of hexachlorotrichlorophosphazene-triethylamine. USE - Inorganic-organic composite hybrid three-layer core-shell particle. ADVANTAGE - The core-shell particle has increased tensile strength of 74.3-95.1%, impact strength of 145.6-175.7%, and excellent toughening effect of the particles for thermosetting resins. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is included for a method for preparing the core-shell particles, involving (a) mixing 1-10 pts. wt. zirconium oxychloride octahydrate, 1-10 pts. wt. absolute ethanol and 5-70 pts. wt. water, stirring until clear, transferring to a hydrothermal kettle, heat-preserving at 100-150 degrees C, reacting for 12-24 hours, centrifuging, drying at 50-80 degrees C, adding the 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, centrifuging, washing with ethanol and deionized water, drying at 60-100 degrees C to obtain the zirconium dioxide hard core, (b) uniformly mixing the zirconium dioxide hard core and anhydrous ethanol in a mass ratio of 0.01:(10-20), adding to graphene oxide and anhydrous ethanol dispersion in a mass ratio of 0.01:(30-50), stirring at 0-10 degrees C for 4-8 hours, leaving still, collecting the precipitate, washing with deionized water, and freeze-drying to obtain a zirconium dioxide doped graphene oxide composed of hard core of zirconium dioxide and an inner shell layer of graphene oxide, and (c) mixing 0.1-0.5 part mass zirconium dioxide doped graphene oxide, 40-200 parts mass tetrahydrofuran, 0.5-2.5 parts mass hexachlorotriphosphazene, reacting at 40-60 degrees C for 15 minutes under nitrogen protection, adding 0.5-2.5 parts mass triethylamine, continuously reacting at 40-60 degrees C under nitrogen protection for 5-10 hours, washing with tetrahydrofuran and chloroform, drying at 40-60 degrees C, adding 0.1-0.5 part mass dried product to a mixed solution 0.2-1.5 parts mass hexachlorotriphosphazene, 1-2 parts mass diaminodiphenyl ether and 40-200 parts mass tetrahydrofuran, reacting at 40-60 degrees C for 15 minutes under the protection of nitrogen, adding 0.5-2.5 parts mass triethylamine, continuously reacting at 40-60 degrees C under the protection of nitrogen for 5-10 hours, washing the product with deionized water and dimethylformamide, and drying at 40-60 degrees C to obtain hard core of zirconium dioxide, inner shell layer of graphene oxide, and outer shell layer of hexachlorotrichlorophosphazene-triethylamine.