• 专利标题:   Preparation doped graphite, involves using supercritical fluid and is specifically carried out by micro-jet processing, low temperature processing, and preparation doped with graphite under action of intercalation agent.
  • 专利号:   CN114590804-A
  • 发明人:   ZHOU P, ZHAO D, BAI Y, SONG H, TENG K
  • 专利权人:   FUJIAN XIANGFENGHUA NEW ENERGY MATERIAL, SHENZHEN XFH TECHNOLOGY CO LTD
  • 国际专利分类:   C01B032/192
  • 专利详细信息:   CN114590804-A 07 Jun 2022 C01B-032/192 202295 Chinese
  • 申请详细信息:   CN114590804-A CN10091430 26 Jan 2022
  • 优先权号:   CN10091430

▎ 摘  要

NOVELTY - Preparing doped graphite involves using supercritical fluid and is specifically carried out by adding the expansion graphite the thermal reduction of preparation graphite and the intercalation agent in the mixture of strong acid and nitrate after, it is mixed uniformly, potassium- containing strong oxidant is added, the temperature of the system is raised to 45-60 ℃, and continuously stirred for 4-12 hour, then a certain amount of water is slowly added, the temperature of the reaction system is raised to 85-95 ℃ and kept for 30-60 minutes, then water and a certain amount of hydrogen peroxide is added, the concentration of the hydrogen peroxide water solution is 3 %, until the foam is disappeared uniformly, it is stirred and reacted repeatedly, washed with diluted acid solution and deionized water various ions in the remove system, then solid is collected by vacuum drying, collected in the quartz tube, USE - Method for high-efficient preparation of graphite. ADVANTAGE - The method enables high-efficient preparation of graphite by supercritical fluid with high efficiency, the size distribution of the graphene sheet and the layer number of the graphite can be adjusted by adjusting the pressure of the micro-jet treatment and pressure of super-critical fluid in the process of preparation, the interlayer distance can be effectively expanded by the intercalation effect of the super critical fluid, the micelle conversion mechanism can effectively realize the high efficiency of surface layer graphite peeling graphene preparation, and by adjusting pressure of micro jet treatment, effectively adjusting the size distribution and the size of the obtained graphene sheet, the micro-explosion can be generated by the particle graphite to provide a beneficial burst for subsequent molecular inter-calibration, the graphite is prepared in a simple and cost-effective manner. DETAILED DESCRIPTION - Preparing doped graphite involves using supercritical fluid and is specifically carried out by adding the expansion graphite the thermal reduction of preparation graphite and the intercalation agent in the mixture of strong acid and nitrate after, it is mixed uniformly, potassium- containing strong oxidant is added, the temperature of the system is raised to 45-60 ℃, and continuously stirred for 4-12 hour, then a certain amount of water is slowly added, the temperature of the reaction system is raised to 85-95 ℃ and kept for 30-60 minutes, then water and a certain amount of hydrogen peroxide is added, the concentration of the hydrogen peroxide water solution is 3 %, until the foam is disappeared uniformly, it is stirred and reacted repeatedly, washed with diluted acid solution and deionized water various ions in the remove system, then solid is collected by vacuum drying, collected in the quartz tube, micro-jet processing is performed by mixing the thermal reduction expansion of graphite with the surface-active agent, water and ethanol to obtain the raw material mixed solution and the raw material mixed solution is used for micro-jet treatment, the pressure of the micro-jet treatment is 100-200MPa, performed 20-100 times to obtain the material, low temperature processing is performed by mixing the material with the active doped element compound, transferring to the low temperature container and cooling to -30-(-0) ℃, obtaining low temperature of graphite slurry, injecting supercritical fluid into the sealed high pressure kettle of the preparation graphite, adjusting the temperature to 100-260 ℃ and pressure to 15-45MPa, when the supercritical fluid reaches the supercritical state, then quickly spraying the low temperature graphite into the high pressure kettle, and reacting for 1-10 hours under the magnetic stirring, discharging by the air release valve, taking out the reaction product, preparing the element doped with graphene.