• 专利标题:   Forming large-scale graphene via industrial large-scale reaction kettle involves oxidizing graphite powder into graphene oxide slurry in the kettle, washing, drying and reducing the slurry into graphene in high temperature sintering furnace.
  • 专利号:   CN102745673-A
  • 发明人:   DING R, GUO X, NI Z
  • 专利权人:   TAIZHOU JUNA NEW ENERGY CO LTD
  • 国际专利分类:   B82Y040/00, C01B031/04
  • 专利详细信息:   CN102745673-A 24 Oct 2012 C01B-031/04 201327 Pages: 13 Chinese
  • 申请详细信息:   CN102745673-A CN10207295 21 Jun 2012
  • 优先权号:   CN10207295

▎ 摘  要

NOVELTY - Preparing large-scale graphene via industrial large-scale reaction kettle involves oxidizing graphite powder into graphene oxide slurry in the industrial large-scale reaction kettle, washing and drying, reducing the slurry into the graphene in the high temperature sintering furnace. USE - For preparing large-scale graphene via industrial large-scale reaction kettle (claimed). ADVANTAGE - The graphene prepared by the method is featured with high yield, low cost, short preparation period, and low impurity ion content. DETAILED DESCRIPTION - Preparing large-scale graphene via industrial large-scale reaction kettle involves mixing graphite with concentrated sulfuric acid, adding commerce graphite powder or waste recovered graphite powder (50-500 g) and concentrated sulfuric acid (98%) in the industrial reaction kettle and mixing evenly, using the cycle cooling device for keeping the temperature in the kettle less than 20 degrees C; adding the potassium permanganate and mixing evenly, slowly adding the potassium permanganate in the kettle, stirring the solution via a machine stirrer at high speed, contacting potassium permanganate with the solution totally, using the cycle cooling device for keeping the temperature in the kettle less than 20 degrees C; dropping the distilled water, slowly adding certain amount of distilled water in the reaction kettle, using the external cycle heating device for raising the temperature in reaction kettle to 70-95 degrees C; the solution changes into daffodil yellow and there is pink smog, keeping the temperature for 10-40 minutes; adding the hydrogen peroxide, slowly adding hydrogen peroxide (250-2500 ml) in the reaction kettle, the solution changes into luminous yellow, finishing oxidizing to obtain the graphene oxide slurry; washing, drying the graphene oxide slurry, using the hydrochloric acid for washing the graphene oxide slurry until that the solution has no sulfate radical, adding the potassium hydroxide solution with certain concentration in the graphene oxide slurry until that the pH is 9-10, stirring and contacting the potassium hydroxide and the graphene oxide slurry totally, using the clean water for washing the excess ion and baking and drying at 40-90 degrees C; reducing and obtaining the graphene, locating the graphene oxide sample in the high temperature furnace, heating to 300-900 degrees C in the argon or hydrogen environment and keeping for 1-4 hours, fast swelling the sample and changing into black, the graphene sample of thickness of 1-5 atom layers is prepared in large-scale mode.