• 专利标题:   Preparation of sulfonated graphene used for semiconductor, involves mixing concentrated sulfuric acid and nitric acid solution, adding graphite powder, adding sodium nitrate and sodium bisulfate, and cooling.
  • 专利号:   CN108545730-A
  • 发明人:   CHENG G
  • 专利权人:   CHENG G
  • 国际专利分类:   C01B032/194
  • 专利详细信息:   CN108545730-A 18 Sep 2018 C01B-032/194 201872 Pages: 11 Chinese
  • 申请详细信息:   CN108545730-A CN10368710 23 Apr 2018
  • 优先权号:   CN10368710

▎ 摘  要

NOVELTY - The preparation of sulfonated graphene involves mixing concentrated sulfuric acid and nitric acid solution, adding graphite powder, adding sodium nitrate and sodium bisulfate, cooling, adding potassium permanganate and potassium nitrate, reacting, adding water and hydrogen peroxide, filtering, washing, drying, diluting in deionized water and treating to obtain graphene oxide dispersion, placing in dialysis bag for dialysis, centrifuging, collecting upper layer solution, adding with sodium carbonate solution to adjust the pH, dissolving sodium borohydride in deionized water, mixing with prepared solution, centrifuging, washing to obtain reaction mixture, adding p-aminobenzenesulfonic acid and sodium carbonate to hydrochloric acid solution, treating, adding sodium nitrite and sodium chloride to form diazonium salt of p-aminobenzenesulfonic acid, mixing with reaction mixture, reacting, centrifuging, washing, adding hydrazine hydrate to system, refluxing, centrifuging and washing. USE - Preparation of sulfonated graphene used for semiconductor (claimed). DETAILED DESCRIPTION - The preparation of sulfonated graphene involves mixing 70 ml 98 wt.% concentrated sulfuric acid and 5 ml 25 wt.% nitric acid solution at room temperature, slowly adding 3.0 g graphite powder while stirring, adding 1.5 g sodium nitrate and 1.1 g sodium bisulfate, transferring the mixture to ice bath and cooling under vigorous stirring, slowly adding 9.0 g potassium permanganate and 1 g potassium nitrate, transferring reaction system to 40 degrees C water bath after the end of the feeding, stirring at constant temperature, reacting for 30 minutes, slowly adding 150 ml deionized water, increasing the temperature of the water bath to 90 degrees C, reacting for 15 minutes, adding 500 ml water, and 15 ml 30 wt.% hydrogen peroxide, suction filtering of resulting mixture, washing with 250 ml 3.5 wt.% diluted hydrochloric acid to remove metal ions, washing with 200 ml deionized water to remove residual acid, drying the solid filter cake in air, diluting in deionized water and ultrasonically treating to obtain graphene oxide dispersion, placing dispersion in dialysis bag for dialysis to remove residual acid and metal ions, changing water once a day for dialysis for seven days, taking out the dialyzed graphene oxide dispersion and centrifuging at 4000 rpm, discarding the underlying unoxidized or incompletely oxidized graphite powder, and collecting the upper layer solution, taking 75 ml upper layer solution, adding 5% sodium carbonate solution to adjust the pH to 9.5, dissolving 600 mg sodium borohydride in 15 ml deionized water and mixing with the prepared solution, placing in a water bath at 80 degrees C for 1 hour, centrifuging, washing three times with deionized water to redisperse the product in 75 ml water to obtain reaction mixture, adding 92 mg p-aminobenzenesulfonic acid and 2 mg sodium carbonate to 20 ml hydrochloric acid solution, ultrasonically treating for 5 minutes, placing reaction vessel in an ice water bath, adding 36 mg sodium nitrite and 2 mg sodium chloride, stirring for 15 minutes to form diazonium salt of p-aminobenzenesulfonic acid, mixing 5 g reaction mixture and 5 ml diazonium salt of p-aminobenzenesulfonic acid, reacting in an ice water bath for 2 hours, centrifuging the product, washing several times with water, and redispersing in 75 ml water, adding 25 mu l hydrazine hydrate to system and refluxing at 100 degrees C for 24 hours, centrifuging the product and washing with water until neutral. An INDEPENDENT CLAIM is included for usage of sulfonated graphene for semiconductor.