• 专利标题:   Preparing graphene filler comprises preparing graphite oxide and then adding thionyl chloride to obtain a mixed solution, refluxing, adding micro dimethyl formamide, treating with anhydrous calcium chloride and distilling.
  • 专利号:   CN103865298-A, CN103865298-B
  • 发明人:   CAO G, MA Y, TANG B, ZANG L, HE C, SHANG T, YANG X, ZHOU Y, ZHU M
  • 专利权人:   GANSU KANGBOSITE NEW MATERIAL CO LTD
  • 国际专利分类:   C08K003/04, C08L063/00, C09C001/46, C09C003/06, C09C003/08
  • 专利详细信息:   CN103865298-A 18 Jun 2014 C09C-001/46 201456 Pages: 6 Chinese
  • 申请详细信息:   CN103865298-A CN10049583 13 Feb 2014
  • 优先权号:   CN10049583

▎ 摘  要

NOVELTY - Preparing graphene filler comprises (1) preparing graphite oxide using Hummer's method, (2) adding the prepared graphite oxide with thionyl chloride to obtain a mixed solution, refluxing the mixed solution, adding dimethyl formamide (DMF) with the obtained product and treating with anhydrous calcium chloride, and (3) distilling the reflux material to remove excess of thionyl chloride and then adding anhydrous DMF in the remaining solid material, carrying out ultrasonic dispersion to obtain a mixed solution and adding m-xylylenediamine into the mixed solution. USE - The method is useful for preparing graphene filler (claimed). ADVANTAGE - The method is capable of preparing the graphene filler with improved disperibility and mechanical property. DETAILED DESCRIPTION - Preparing graphene filler comprises (1) preparing graphite oxide using Hummers method, (2) adding the prepared graphite oxide with thionyl chloride to obtain a mixed solution, refluxing the mixed solution in a reflux device, adding dimethyl formamide (DMF) with the obtained product at 70 degrees C to reflux for 24-36 hours and treating with anhydrous calcium chloride as protecting material, (3) distilling the reflux material to remove excess of thionyl chloride and then adding anhydrous DMF in the remaining solid material, carrying out ultrasonic dispersion for 10 minutes to obtain a mixed solution, adding m-xylylenediamine (m-XDA) into the mixed solution by dropwise in an ice bath, continuously carrying out ultrasonic treatment for 10 minutes, raising the temperature to 120 degrees C for 6-12 hours, (4) flushing the obtained product in step (3) using large amount of ethanol to obtain graphene oxide derivatives with amino end groups and functionalized graphene oxide diamine, (5) dispersing the obtained product in step (4) in acetone to obtain dispersion of functionalized graphene oxide diamine and then adding epoxy resin, carrying out ultrasonic treatment in vacuum at 60 degrees C to remove air bubbles and excess acetone from the mixture solution, and (6) cooling the obtained product in step (5) to room temperature, transferring the suspension to a template and adding then curing agent at 60 degrees C and 150 degrees C, respectively and naturally cooling to room temperature.