• 专利标题:   Preparing graphene/styrene-acrylic styrene-butyl methacrylate composite material for electric conduction, involves preparing graphene oxide followed by dispersing in water, and adding in styrene and methyl acrylic acid butyl ester.
  • 专利号:   CN103951778-A, CN103951778-B
  • 发明人:   JIA S, JIANG P, TIAN L, LI R, ZHANG Z, HOU X
  • 专利权人:   UNIV SHANGHAI
  • 国际专利分类:   C08F212/08, C08F220/16, C08F226/06, C08K003/04, C08K009/02, C08K009/04
  • 专利详细信息:   CN103951778-A 30 Jul 2014 C08F-212/08 201468 Pages: 9 Chinese
  • 申请详细信息:   CN103951778-A CN10173267 28 Apr 2014
  • 优先权号:   CN10173267

▎ 摘  要

NOVELTY - Preparation of super-concentrated graphene/styrene-acrylic styrene-butyl methacrylate composite material for electric conduction, involves: pre-oxidation of main graphite body using potassium persulfate and phosphorus pentoxide; adding concentrated sulfuric acid, followed by adding potassium permanganate, water and hydrogen peroxide to obtain oxidized graphene, followed by dispersing and adding graphene into dispersed phase, to obtain graphene dispersion liquid; and adding the graphene dispersion liquid in styrene and methyl acrylic acid butyl ester in oil phase. USE - In the preparation of super-concentrated graphene/styrene-acrylic styrene-butyl methacrylate composite material for electric conduction (claimed), for coating and paper making. ADVANTAGE - The super-concentrated graphene/styrene-acrylic styrene-butyl methacrylate composite material is non-toxic and non-explosive, has good weather resistance, light resistance and corrosion resistance. DETAILED DESCRIPTION - Preparation of super-concentrated graphene/styrene-acrylic styrene-butyl methacrylate composite material for electric conduction, involves: (a) pre-oxidation of main graphite body using potassium persulfate (K2S2O8) and Phosphorus pentoxide (P2O5): adding 5 g of K2S2O8 and 5 g of P2O5 into 1 L three-mouth bottle containing 24 ml of concentrated H2SO4, and then adding 6 g of graphite powder with stirring at 80 degrees C water bath for 4 hours, and then slowly adding 1000 mL of deionized water, standing overnight, washing and drying; (b) transferring the graphite into a three-opening bottle, adding 240 ml of concentrated sulfuric acid (H2SO4), stirring to dispersing, slowly adding 30 g Potassium permanganate (KMnO4), control temperature at 10 degrees C for 1 hour, raising the temperature to 35 degrees C, continuously stirring reaction for 2 hours, to obtain a viscous ink green reaction liquid; cooling to room temperature, slowly adding 2 L diluting deionized water, and cooling to obtain brown reaction liquid, adding 40 mL/30 wt.% of Hydrogen peroxide (H2O2) to obtain yellow reaction liquid, stirring overnight, collecting filter cake, using 300 mL/10 wt.% of HCl solution dispersing filter cake, and filter to obtain the yellow solid; washing the filter cake using deionized water until the solution PH value to neutral, drying the filter cake at 60 degrees C for 24 hours, to obtain oxidized graphene; (c) ultrasonically dispersing 100 mg of graphene oxide powder in 100 mL of deionized water, to obtain a brown graphite oxide (GO) water solution, adding hydrazine hydrate solution in the dispersion, the reaction bottle is set in 95 degrees C oil bath stirring for 24 hours, filtering the reaction product and washing using deionized water and then drying to obtain the graphene black flocculent solid; (d) for styrene (St) and methylbutyl acrylate resin (BMA), pre-processing the raw material styrene and methacrylic acid by washing and moisturizing with 5 wt.% sodium hydroxide (NaOH) aqueous solution, to remove impurity, repeatedly washing with NaOH for 3-5 times, still extracting process, removing the residual liquid of NaOH, then washing with deionized water until the reagent of PH value is neutral, transferring the washed liquid in a beaker, adding anhydrous calcium chloride (CaCl2), followed by drying and then standing for 24 hours and then sealed in opaque reagent bottle and storing; (e) adding a certain mass of graphene into dispersed phase of 5 wt.% calcium chloride dihydrate (CaCl2.2H2O), ultrasonically dispersing for 0.5 hours, to obtain a graphene dispersion liquid; (f) taking 2 g of styrene and 2 g methyl acrylic acid butyl ester in oil phase containing 10% of Span 80 (RTM: surfactant), 5% of azodiisobutyronitrile initiator and 10% of crosslinking agent triallyl isocyanurate, with stirring, adding dropwise the graphene dispersion liquid with stirring for 0.5 hours, then the transfer liquid in centrifugal tube, place in 60 degrees C water bath and continuing polymerization for 24 hours, followed by purifying product using Soxhlet apparatus, then drying at 70 degrees C, to obtain super-concentrated graphene/styrene-acrylic styrene-butyl methacrylate composite material.