• 专利标题:   Preparation of flame retardant graphene-modified epoxy resin nanocomposite material by preparing graphene oxide, preparing cage-like octa(3-aminopropyl)silsesquioxane, and preparing functionalized graphene; and graphene-modified epoxy resin.
  • 专利号:   CN108641292-A
  • 发明人:   ZUO D, LIU H, XU X
  • 专利权人:   PANJIN VOCATIONAL TECH COLLEGE
  • 国际专利分类:   C08L063/00, C08K009/06, C08K003/04, C08G077/26
  • 专利详细信息:   CN108641292-A 12 Oct 2018 C08L-063/00 201880 Pages: 14 Chinese
  • 申请详细信息:   CN108641292-A CN10412307 03 May 2018
  • 优先权号:   CN10412307

▎ 摘  要

NOVELTY - A flame retardant graphene-modified epoxy resin nanocomposite material is prepared by (A) preparing graphene oxide; preparing cage-like octa(3-aminopropyl)silsesquioxane (ApPOSS); (C) preparing functionalized graphene; and (D) graphene-modified epoxy resin. The step (D) weighing 1-ethyl pyridinium chloride (EP) in beaker, putting on bidirectional magnetic force, stirring, heating, weighing m-phenylenediamine and 4,4'-diaminodiphenylmethane in beaker, putting into double-way magnetic force heating stirrer, heating to melt; weighing modified graphene, adding to molten EP, and continuously stirring to uniformly disperse, uniformly dispersing modified graphene, stopping heating, naturally reducing temperature to 50 degrees C to make mixture; and pouring molten curing agent in mixture, agitating, pouring into mold, putting in electric heating constant temperature, blasting drying at 150 degrees C, and curing for 2-3 hours. USE - Method for preparation of flame retardant graphene-modified epoxy resin nanocomposite material. ADVANTAGE - The prepared nanocomposite material has comprehensive effect. DETAILED DESCRIPTION - Flame retardant graphene-modified epoxy resin nanocomposite material is prepared by (A) preparing graphene oxide; preparing cage-like octa(3-aminopropyl)silsesquioxane (ApPOSS); (C) preparing functionalized graphene; and (D) graphene-modified epoxy resin. The step (A) comprises putting potassium peroxydisulfate and phosphorus pentoxide into three-mouth flask, adding concentrated sulfuric acid, uniformly stirring, slowly adding graphite powder at 80 degrees C, and reacting for 4.5 hours, transferring reactant to tapered bottle, washing and filtering to filtrate, and drying at 80 degrees C to obtain oxidized graphite; measuring concentrated sulfuric acid to conical flask, completely dispersing, slowly adding potassium permanganate, heating to 35 degrees C and reacting for 3 hours, diluting reaction liquid, standing overnight, slowly pouring supernatant, washing slurry by 3% hydrochloric acid, standing, and pouring supernatant; and adding deionized water into slurry, centrifuging, slowly dripping hydrogen peroxide, putting filtrate into diluted, centrifuging and taking centrifugal liquid, freezing and drying to obtain graphene oxide. The step (B) comprises adding deionized water, n-propanol, acetonitrile, and tetraethylammonium hydroxide in three-mouth flask, stirring, weighing KH-550, placing in funnel, gradually dripping into three-neck flask, gradually raising temperature to 50 degrees C, reacting for 24 hours, mixing solution at 50 degrees C, rotary steaming until no bubble generated, distilling colloidal product, washing by water and 3 times filtering, 2 times washing filter with acetonitrile, putting in 80 degrees C, vacuum oven drying for 24 hours; taking out and drying, grinding and crushing, and sieving by 200-mesh sieve. The step (C) comprises putting graphene oxide into beaker, taking acetonitrile into beaker, stirring mixed solution in beaker, putting in ultrasonic oscillator for oscillation, putting ApPOSS into beaker, taking acetonitrile into beaker in mixed solution, heating, dissolving solute, adding magneton, stirring at 78 degrees C, and reacting for 24 hours; and filtering mixed solution when it is hot, taking out and drying in 80 degrees C vacuum drying box, grinding and crushing, and sieving with 200-mesh sieve. The step (D) weighing 1-ethyl pyridinium chloride (EP) in beaker, putting on bidirectional magnetic force, stirring, heating, weighing m-phenylenediamine and 4,4'-diaminodiphenylmethane in beaker, putting into double-way magnetic force heating stirrer, heating to melt; weighing modified graphene, adding to molten EP, and continuously stirring to uniformly disperse, uniformly dispersing modified graphene, stopping heating, naturally reducing temperature to 50 degrees C to make mixture; and pouring molten curing agent in mixture, agitating, pouring into mold, putting in electric heating constant temperature, blasting drying at 150 degrees C, and curing for 2-3 hours.