• 专利标题:   Preparation of carboxylation modified graphene, involves adding iminodiacetic acid and paraformaldehyde to reaction flask, adding anhydrous ethanol, stirring, dispersing, adding graphene, reacting, heating, cooling, washing and filtering.
  • 专利号:   CN108751180-A
  • 发明人:   REN H, WANG L, FAN Z, SUN Q, LIU M
  • 专利权人:   AECC BEIJING AERONAUTICAL MATERIALS INST
  • 国际专利分类:   C01B032/194
  • 专利详细信息:   CN108751180-A 06 Nov 2018 C01B-032/194 201901 Pages: 5 Chinese
  • 申请详细信息:   CN108751180-A CN11041861 06 Sep 2018
  • 优先权号:   CN11041861

▎ 摘  要

NOVELTY - The preparation method of carboxylated modified graphene involves (a) installing a stirring device in a middle of a three-necked reaction flask, adding iminodiacetic acid and paraformaldehyde to reaction flask, adding anhydrous ethanol, stirring, dispersing, adding graphene to reaction flask, stirring, increasing the temperature of reaction flask, continuously stirring, stopping heating, and cooling flask and solid mixture to obtain powdery solid, (b) installing a stirring device in a middle of reaction bottle, and installing a reflux condensation pipe and a thermocouple on both side openings, heating the reaction system, stopping heating, and naturally cooling the reaction system to room temperature to obtain a mixed product containing carboxylated modified graphene, and (c) ultrasonically washing the obtained product in a glass container containing mixed solvent of water, acetone and ethanol, performing vacuum filtration, washing, collecting obtained solid, and drying. USE - Preparation method of carboxylated modified graphene. ADVANTAGE - The method enables preparation of carboxylated modified graphene with improved production efficiency and which expands production scale. DETAILED DESCRIPTION - The preparation method of carboxylated modified graphene by utilizing solid phase reaction involves (a) installing a stirring device in a middle of a three-necked reaction flask, adding 10 parts mass iminodiacetic acid and 11-12 parts mass paraformaldehyde to the reaction flask, adding 120-600 parts mass anhydrous ethanol, stirring, dispersing for 10-20 minutes, adding 5-10 parts mass graphene to the reaction flask, stirring for 30 minutes at room temperature, increasing the temperature of the reaction flask to 60-80 degrees C, continuously stirring until the ethanol is completely volatilized, stopping heating, and naturally cooling the flask and the solid mixture to room temperature to obtain powdery solid, (b) installing a stirring device in a middle of the three-necked reaction bottle, and installing a reflux condensation pipe and a thermocouple on both side openings, heating the reaction system at 180-220 degrees C for 4-6 hours, stopping heating, and naturally cooling the reaction system to room temperature to obtain a mixed product containing carboxylated modified graphene, and (c) ultrasonically washing the obtained product in a glass container containing mixed solvent of 200 parts mass water, acetone and ethanol in a mass ratio of 2:2:1 for 30 minutes, performing vacuum filtration, successively washing with water, acetone and ethanol, collecting the obtained solid, and drying in a vacuum oven at 40 degrees C for 24 hours to obtain carboxylated graphene powder.