• 专利标题:   Preparing three-dimensional graphene oxide comprises adding concentrated sulfuric acid into conical flask, heating, adding e.g. potassium persulfate, stirring, cooling, adding natural graphite powder, cooling, washing, filtering and drying.
  • 专利号:   CN107673344-A
  • 发明人:   ZHANG S
  • 专利权人:   SHAANXI QIYUAN TECHNOLOGY DEV CO LTD
  • 国际专利分类:   C01B032/198
  • 专利详细信息:   CN107673344-A 09 Feb 2018 C01B-032/198 201818 Pages: 4 Chinese
  • 申请详细信息:   CN107673344-A CN11211244 28 Nov 2017
  • 优先权号:   CN11211244

▎ 摘  要

NOVELTY - Preparing three-dimensional graphene oxide comprises adding concentrated sulfuric acid into conical flask, heating, adding potassium persulfate and phosphorus pentoxide, stirring, cooling the obtained mixture to 80 degrees C, adding natural graphite powder, foaming, heating the mixture in water bath, cooling, washing, filtering the obtained product, drying, placing the product into three-necked bottle, taking the solution into three mouth flask, adding deionized water, stirring, washing, dissolving anhydrous sodium carbonate in water, using a preservative film to seal the water bath port, and drying. USE - The method is useful for preparing three-dimensional graphene oxide. ADVANTAGE - The method is simple, convenient for operation, is safe, improves product quality and is economical. DETAILED DESCRIPTION - Preparing three-dimensional graphene oxide comprises (a) adding 25 ml concentrated sulfuric acid into 100 ml conical flask, heating at 90 degrees C, adding 5 g potassium persulfate and 5 g phosphorus pentoxide, continuously stirring, until the mixture is completely dissolved, (b) cooling the obtained mixture to 80 degrees C, adding 6 g natural graphite powder, foaming, foam gradually fades in the 30 minutes, (c) heating the mixture in water bath at 80 degrees C for 4.5 hours under stirring condition, cooling the mixture to room temperature, washing by 1 l de-ionized water, taking the product obtained allowing to stand overnight at room temperature, (d) filtering the obtained product, using de-ionized water to wash the solution until the last filtering is neutral, drying the solid microporous filter membrane for one day at normal temperature, (e) placing the product into 500 ml three-necked bottle, and then slowly adding 230 ml concentrated sulfuric acid and 30 g potassium permanganate, continuously stirring, maintaining the temperature not more than 10 degrees C, until completely dissolved, (f) placing the mixture in water bath and reacting at 35 degrees C for 2 hours, adding 460 ml de-ionized water, controlling the three-mouth flask solution temperature at lower than 50 degrees C, continuously adding water, where the activity of the reactant is continuously reduced, adding deionized water no longer cause temperature changes, (g) taking the solution into three mouth flask and placing into 2 l beaker, adding 1.4 l deionized water, stirring and dropping 25 ml hydrogen peroxide 30% into the mixture, reacting for 2 hours, simultaneously the mixture solution changed to bright yellow, allowing to stand overnight, (h) removing the supernatant, washing with plenty 5% hydrochloric acid solution, washing using large amount of de-ionized water, until the solution is neutral, taking the obtained mixture solution for centrifuging to obtain graphite oxide with high concentration, (i) adding water to dilute the graphite oxide, ultrasonically treating to obtain uniform dispersion of brown graphite oxide solution, (j) taking resorcinol, formaldehyde, anhydrous sodium carbonate, where the mol ratio of resorcinol to formaldehyde is 1:2, (k) dissolving 0.025 g anhydrous sodium carbonate in 40 g water, (l) weighing graphene oxide, formaldehyde with anhydrous sodium carbonate solution, using ultrasonic instrument for 0.5 hour or more, (m) setting up a three-necked flask on a constant temperature water bath, weighing 150 ml cyclohexane, 5 ml Span-80 (RTM: Sorbitan monooleate 80) into three-necked bottle, starting stirring and heating to 60 degrees C, using a preservative film to seal the water bath port, preventing from water loss, (n) adding the ultrasonic mixture obtained into three-mouth flask, preheating at 60 degrees C, stirring, reacting for 2 hours, pre-calculating the molecular weight of resorcinol, preparing into 3 ml solution, adding into a three-opening bottle, continuously stirring, reacting for two days after taking out, and (o) allowing the liquid to stand, after settling completely, filtering, washing with alcohol and drying at normal pressure.