• 专利标题:   Large-diameter graphene oxide comprises graphite flakes, sodium nitrate, concentrated sulfuric acid, potassium chlorate, hydrogen peroxide aqueous solution, separating agent, phenylenediamine, and dicyclohexylcarbodiimide.
  • 专利号:   CN112744811-A, CN112744811-B
  • 发明人:   CUI J, LI Y, XU P, ZHANG B
  • 专利权人:   LI Y, CHANGZHOU JINGRUISI NEW MATERIAL TECHNOL
  • 国际专利分类:   C01B032/198
  • 专利详细信息:   CN112744811-A 04 May 2021 C01B-032/198 202154 Pages: 10 Chinese
  • 申请详细信息:   CN112744811-A CN10177656 07 Feb 2021
  • 优先权号:   CN10177656

▎ 摘  要

NOVELTY - A large-diameter graphene oxide comprises 20-25 pts. wt. graphite flakes, 10-15 pts. wt. sodium nitrate, 150-250 pts. wt. concentrated sulfuric acid, 2-4 pts. wt. potassium chlorate, 50-70 pts. wt. of 10% hydrogen peroxide aqueous solution, 5-15 pts. wt. separating agent, 0.2-0.3 pt. wt. phenylenediamine, and 2-5 pts. wt. dicyclohexylcarbodiimide. The large-diameter graphene oxide is obtained by adding a separated graphene oxide to absolute ethanol, stirring, adding p-phenylenediamine and dicyclohexylcarbodiimide, continually stirring for 15 minutes, heating, blowing nitrogen to exhaust the air, stirring and reacting, washing the reaction product, freeze-drying to obtain an intermediate product, adding the intermediate product to a three-necked flask containing hydrochloric acid, uniformly dispersing, adding aniline, continually mixing for 15 minutes, transferring to an ice-water bath, dripping a mixed solution (D) into the flask, stirring, reacting, washing and drying. USE - Large-diameter graphene oxide. ADVANTAGE - The large-diameter graphene oxide has strong reactivity and particle-exchange performance, and large graphite oxide layer spacing, which is more conducive to separation. DETAILED DESCRIPTION - A large-diameter graphene oxide comprises 20-25 pts. wt. graphite flakes, 10-15 pts. wt. sodium nitrate, 150-250 pts. wt. concentrated sulfuric acid, 2-4 pts. wt. potassium chlorate, 50-70 pts. wt. of 10% hydrogen peroxide aqueous solution, 5-15 pts. wt. separating agent, 0.2-0.3 pt. wt. phenylenediamine, and 2-5 pts. wt. dicyclohexylcarbodiimide. The large-diameter graphene oxide is obtained by adding the graphite flakes to a beaker, adding sodium nitrate and 98 %mass concentrated sulfuric acid, stirring in an ice water bath for 15 minutes, adding potassium chlorate, continually stirring for 30 minutes, heating in a water bath at 40 degrees C, reacting for 3 hours, adding deionized water, heating to 75 degrees C, magnetically stirring for 30 minutes, adding 10 %mass hydrogen peroxide aqueous solution to continue the reaction for 10 minutes, adding a separating agent, stirring at a constant speed for 2 hours, filtering to obtain a separated graphene oxide, adding the separated graphene oxide to absolute ethanol, stirring at a constant speed for 15 minutes, adding p-phenylenediamine and dicyclohexylcarbodiimide in sequence, continually stirring for 15 minutes, heating to 60-80 degrees C, blowing nitrogen to exhaust the air, stirring and reacting at a constant speed for 10 hours, washing the reaction product for three times with absolute ethanol and deionized water, freeze-drying to obtain an intermediate product, adding the intermediate product to a three-necked flask containing 1 mol/L hydrochloric acid, uniformly dispersing, adding aniline, continually mixing for 15 minutes, transferring to an ice-water bath, dripping a mixed solution (D) into the three-necked flask for 10 minutes, stirring and reacting at a constant speed for 10 hours, washing and drying. The weight ratio of intermediate product and aniline is 1:2. The weight ratio of aniline and ammonium persulfate is 1:2-2.5. An INDEPENDENT CLAIM is included for preparation of the large-diameter graphene oxide.