• 专利标题:   Preparing fluorescent graphene oxide comprises e.g. performing graphite sheet pretreatment, adding phosphorus pentoxide and potassium persulfate, sonicating, filtering, treating filtrate to remove N,N-dimethylformamide, and vacuum drying.
  • 专利号:   CN107828411-A
  • 发明人:   ZHANG S
  • 专利权人:   SHAANXI QIYUAN TECHNOLOGY DEV CO LTD
  • 国际专利分类:   C01B032/198, C09K011/02, C09K011/65
  • 专利详细信息:   CN107828411-A 23 Mar 2018 C09K-011/02 201825 Pages: 4 Chinese
  • 申请详细信息:   CN107828411-A CN11207186 27 Nov 2017
  • 优先权号:   CN11207186

▎ 摘  要

NOVELTY - Preparing fluorescent graphene oxide comprises e.g. (i) performing graphite sheet pretreatment, adding concentrated sulfuric acid into flask, adding phosphorus pentoxide and potassium persulfate, adding graphite flakes into flask, (ii) adding concentrated sulfuric acid into flask, adding pretreated graphite flakes and potassium permanganate, and (iii) ultrasonically dispersing dry solid graphite oxide in N,N-dimethylformamide, transferring N,N-dimethylformamide into flask, adding ethanol into product, sonicating, filtering, treating filtrate to remove N,N-dimethylformamide, and vacuum drying. USE - The method is useful for preparing fluorescent graphene oxide. ADVANTAGE - The method has simple process flow and convenient operation; and is safe and reliable. DETAILED DESCRIPTION - Preparing fluorescent graphene oxide comprises (i) performing graphite sheet pretreatment, adding 25 ml concentrated sulfuric acid into flask and heating at 85 degrees under agitation, adding 1 g phosphorus pentoxide and 1 g potassium persulfate stirring until the solid is completely dissolved, adding 1.2 g graphite flakes into flask, reacting for 4.5 hours, stop stirring, cooling to room temperature, and then adding into the flask, diluting by adding 200 ml deionized water, filtering reaction product, and washing filter cake with deionized water to remove residual acid, drying filter cake and storing under dry conditions, (ii) adding concentrated sulfuric acid (25 ml) into flask under ice-cooling, and adding 1.2 g pretreated graphite flakes and 1 g potassium permanganate into flask while stirring, heating at 35 degrees C, and reacting for 2 hours under constant temperature conditions, adding 40 ml deionized water into flask equipped with constant pressure funnel, transferring into flask at 95 degrees oil bath and reacting for 0.5 hours, then adding 100 ml deionized water into the flask, adding 3 ml hydrogen peroxide into flask, removing flask and allowing the reaction solution to cool to room temperature, centrifugating reaction solution with 10% by volume hydrochloric acid three times, then washing the solid twice with deionized water, vacuum drying product at 35% and drying to obtain solid product i.e. graphite oxide, and (iii) ultrasonically dispersing 20 mg dry solid graphite oxide in N,N-dimethylformamide, transferring 5 ml N,N-dimethylformamide into flask, adding 20 ml thionyl chloride into flask, heating and refluxing at 80 degrees C with stirring for 48 hours, centrifugating acyl chloride-chlorinated graphite flakes, and washing twice with tetrahydrofuran, transferring centrifuged product into flask under vacuum nitrogen protection, adding 20 mg glycine and 2 ml N,N-dimethylformamide into flask, reacting for 72 hours at 60 degrees C with stirring, cooling product to room temperature, adding ethanol into product, sonicating, filtering, treating filtrate with a rotary evaporator to remove N,N-dimethylformamide, and vacuum drying product.