• 专利标题:   Preparing folic acid-modified fluorinated graphene comprises e.g. cooling the container, adding concentrated sulfuric acid, adding flake graphite powder and sodium nitrate, sonicating abd stirring the reaction.
  • 专利号:   CN109091676-A
  • 发明人:   WANG B, JIN X, HUANG Q, HU J, CHEN B
  • 专利权人:   UNIV ZHEJIANG SCI TECH
  • 国际专利分类:   A61K047/04, A61K047/22
  • 专利详细信息:   CN109091676-A 28 Dec 2018 A61K-047/04 201920 Pages: 11 Chinese
  • 申请详细信息:   CN109091676-A CN10969441 23 Aug 2018
  • 优先权号:   CN10969441

▎ 摘  要

NOVELTY - Preparing folic acid-modified fluorinated graphene comprises e.g. cooling the container, adding concentrated sulfuric acid, adding flake graphite powder and sodium nitrate and sonicating, stirring the reaction, maintaining the reaction temperature, adding 2-4 g potassium permanganate and adding in batches, heating, taking deionized water, adding distilled water to stop the reaction, adding H2O2 and stirring; adding hydrochloric acid solution and allowing to stand; taking out the supernatant of the solution with a dropper, centrifuging the lower layer of viscous liquid until it is thick, adding the viscous liquid in the centrifuge tube into the evaporating dish and freeze-drying to obtain a graphene oxide sheet, (viii) grinding the graphene oxide sheet into graphene oxide powder, adding 0.5-1.5 g graphene oxide powder and 20-40 ml dichloromethane or 1,2-dichloroethane in a container and stirring. USE - The method is useful for preparing folic acid-modified fluorinated graphene. DETAILED DESCRIPTION - Preparing folic acid-modified fluorinated graphene comprises (i) cooling the container to 0 degrees C in an ice water bath, adding 20-25 ml concentrated sulfuric acid, adding 0.5-2 g flake graphite powder and 0.2-1 g sodium nitrate and sonicating for 20-30 minutes, (ii) stirring the reaction, maintaining the reaction temperature for less than 10 degrees C, adding 2-4 g potassium permanganate and adding in batches within 25-30 minutes, where the reaction in this stage is 1.5-2.5 hours, (iii) heating to 35-40 degrees C and reacting for 25-30 minutes, (iv) taking 70-120 ml deionized water, adding 0 degrees C after cooling in an ice water bath, adjusting the temperature to 90-95 degrees C and stirring the reaction for 25-30 minutes, (v) adding 50-70 ml distilled water to stop the reaction, adding 20-30 ml 25-35% H2O2 and stirring for 15-20 minutes, (vi) adding 30-50 ml hydrochloric acid solution with a volume fraction of 8-12% and allowing to stand for 4-5 days, (vii) taking out the supernatant of the solution with a dropper, centrifuging the lower layer of viscous liquid until it is thick, where the liquid is neutral, adding the viscous liquid in the centrifuge tube into the evaporating dish and freeze-drying for 24-48 hours to obtain a graphene oxide sheet, (viii) grinding the graphene oxide sheet into graphene oxide powder, (ix) adding 0.5-1.5 g graphene oxide powder and 20-40 ml dichloromethane or 1,2-dichloroethane in a container and stirring for 10-14 hours, (x) dropping 0.5-1 ml fluorinating agent diethylaminosulfur trifluoride, sonicating at room temperature for 4-6 hours and stirring the reaction for 24-72 hours, (xi) adding 15-30 ml methanol to terminate the reaction, filtering the partially fluorinated graphene product, washing uniformly with ethanol and deionized water and drying at 50-70 degrees C, (xii) dispersing 25-30 mg partially fluorinated graphene in 45-60 ml deionized water and ultrasonically treating to obtain a partially fluorinated graphene solution, (xiii) taking 1-1.5 g sodium hydroxide and 1.2-1.5 g sodium hypochlorite, adding into a partially fluorinated graphene solution and sonicating for 3-4 hours, (xiv) centrifuging and removing the supernatant, adding deionized water to obtain a uniform dispersion, adding dilute hydrochloric acid until the pH is neutral and dissolving in deionized water for 48-72 hours, (xv) adding 0.1-0.12 g folic acid, sonicating for 0.5-1 minutes, adding 25-30 mg 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 25-30 mg N-hydroxysuccinimide and ultrasonicating for 2-2.5 hours, (xvi) carrying out dialysis treatment of the solution using a sodium hydrogen carbonate solution of pH=8, changing water for every 3-4 hours and transferring to deionized water for 48-36 hours after 48-60 hours and (xvii) taking out the water in the solution by rotary evaporation and drying at 35-45 degrees C.