• 专利标题:   Preparing graphene oxide based curing agent used for epoxy resin composite material comprises e.g. using Hummers method, adding e.g. graphite in flask, adding sulfuric acid, reacting, cooling, drying to obtain pre-oxidized graphite.
  • 专利号:   CN104262588-A, CN104262588-B
  • 发明人:   LI Z, LIU F, SONG Y, GUO R, GUO K
  • 专利权人:   UNIV HUNAN
  • 国际专利分类:   C01B031/04, C08G059/44, C08G059/50, C09J011/00, C09J011/04, C09J011/06, C09J163/00, C09J163/02, C09J009/02
  • 专利详细信息:   CN104262588-A 07 Jan 2015 C08G-059/50 201523 Pages: 7 Chinese
  • 申请详细信息:   CN104262588-A CN10464312 12 Sep 2014
  • 优先权号:   CN10464312

▎ 摘  要

NOVELTY - Preparing graphene oxide based curing agent comprises e.g. using Hummers method to synthesize graphene oxide comprising adding graphite, potassium persulfate and phosphorus pentoxide in a three-necked flask, adding concentrated sulfuric acid, magnetic stirring, reacting, cooling, washing to neutral, drying to obtain pre-oxidized graphite, adding in three-necked flask, adding concentrated sulfuric acid, cooling, stirring, adding potassium permanganate, dripping distilled water, adding hydrogen peroxide, filtering, placing in a dialysis bag for dialysis, drying to obtain oxidized graphite. USE - The graphene oxide-based curing agent is used for epoxy resin composite material, e.g. electric conduction epoxy resin adhesive (claimed). ADVANTAGE - The curing agent has good electric conduction ability, acid-alkaline resistant, heat stability, and mechanical properties. The adhesive is suitable for bonding electronic components. DETAILED DESCRIPTION - Preparing graphene oxide based curing agent comprises (i) synthesizing graphene oxide: using Hummers method to synthesize graphene oxide comprising adding 1-3 pts. wt. graphite, 0.5-1.5 pts. wt. potassium persulfate and 1-3 pts. wt. phosphorus pentoxide in a three-necked flask, slowly adding 100-150 pts. wt. concentrated sulfuric acid, after magnetic stirring uniformly, raising the temperature to 80 degrees C and reacting for 3-6 hours, after reaction is finished, cooling to room temperature after slowly dropwise adding 500 pts. wt. distilled water overnight, using distilled water repeatedly for washing to neutral, at 60 degrees C, using blast drying tank for drying to obtain pre-oxidized graphite, adding pre-oxidized graphite in three-necked flask, adding 100-150 pts. wt. concentrated sulfuric acid, cooling to 0 degrees C, stirring uniformly, after three-batch adding 5-8 pts. wt. potassium permanganate, at temperature not greater than 20 degrees C, then slowly dripping 250 pts. wt. distilled water, at temperature less than 50 degrees C, after dripping is finished, adding 700 pts. wt. distilled water and 10-30 pts. wt. 30% hydrogen peroxide, changing into bright yellow solution, after filtering, using hydrochloric acid aqueous solution at ratio of 1:10, then using distilled water without stopping washing to pH 3, after one week, placing in a dialysis bag for dialysis, using 60 degrees C blast drying tank for drying to obtain oxidized graphite, then carrying out ball-milling, obtaining graphene oxide, and (ii) preparing graphene oxide-based curing agent: adding 50-150 pts. wt. graphene oxide in 1-30 pts. wt. thionyl chloride and 0.5-1.5 pts. wt. anhydrous N, N- dimethylformamide, refluxing at 70 degrees C for 24 hours, maintaining the reaction system at anhydrous environment, pumping to constant weight the product of un-reacted thionyl chloride under reduced pressure, adding 2-500 pts. wt. dimethylformamide, ultrasonically processing for 1 minute in an ice bath condition, adding dropwise 20-50 pts. wt. amine compound in the mixed solution slowly for 10 minutes, reacting the mixed solution uniformly at 120 degrees C for 12 hours, washing the reaction product with 900 ml anhydrous ethyl alcohol for 6 times and vacuum drying at 60 degrees C to obtain curing agent. INDEPENDENT CLAIMS are also included for: (1) the graphene oxide based curing agent prepared according to above mentioned method; (2) use of graphene oxide-based curing agent in epoxy resin composite material; (3) epoxy resin composite material, comprising graphene oxide based curing agent; and (4) electric conduction epoxy resin adhesive comprising graphene oxide based curing agent.