• 专利标题:   Preparation of graphene doped with two-dimensional nitrogen and phosphorus by removing impurities from inorganic material with laminated structure, cleaning, sun drying, grinding into powder, sieving and putting into modification furnace.
  • 专利号:   CN111377439-A
  • 发明人:   HE Z, CUI W, WANG Y, ZHOU Z
  • 专利权人:   UNIV YANAN
  • 国际专利分类:   C01B032/194
  • 专利详细信息:   CN111377439-A 07 Jul 2020 C01B-032/194 202066 Pages: 14 Chinese
  • 申请详细信息:   CN111377439-A CN10427661 20 May 2020
  • 优先权号:   CN10427661

▎ 摘  要

NOVELTY - Preparation of graphene doped with two-dimensional nitrogen and phosphorus includes removing impurities from the inorganic material with the laminated structure, cleaning, drying in the sun, grinding into powder, sieving with 20-40 mesh sieve, and putting into a modification furnace for dense tiling; introducing a mixture of high-temperature water vapor and an activated carbon material into the modification furnace, where the mass ratio of the activated carbon material to the layered structure inorganic material is 1:5-8, and the activated carbon material passes through the tiled layered structure inorganic material along with the high-temperature water vapor and is retained; and slowly adding water into the modification furnace until the inorganic material with the layered structure is submerged, standing for 5-10 minutes, adding surfactant into the water until no bubbles are generated, pressurizing, heating, and aging for 6-12 hours to obtain suspension. USE - The method is for preparation of graphene doped with two-dimensional nitrogen and phosphorus. ADVANTAGE - The method improves the overall porosity and mesopore fraction, can promote lamellar structure inorganic material's ion exchange effect, improves subsequent nitrogen phosphorus atom uniform distribution, and greatly improves the graphene doping capability of two-dimensional nitrogen phosphorus. DETAILED DESCRIPTION - Preparation of graphene doped with two-dimensional nitrogen and phosphorus comprises removing impurities from the inorganic material with the laminated structure, cleaning, drying in the sun, grinding into powder, sieving with 20-40 mesh sieve, and putting into a modification furnace for dense tiling; introducing a mixture of high-temperature water vapor and an activated carbon material into the modification furnace, where the mass ratio of the activated carbon material to the layered structure inorganic material is 1:5-8, and the activated carbon material passes through the tiled layered structure inorganic material along with the high-temperature water vapor and is retained; slowly adding water into the modification furnace until the inorganic material with the layered structure is submerged, standing for 5-10 minutes, adding surfactant into the water until no bubbles are generated, pressurizing, heating, and aging for 6-12 hours to obtain suspension; taking out a suspension from the modification furnace, adding 4-dimethylaminopyridine and n-butyl phosphate into the suspension according to the corresponding amount of 0.5-1.5 mmol of 4-dimethylaminopyridine and 0.5-1.5 mmol of n-butyl phosphate to each gram of the layered structure inorganic material, stirring in a constant-temperature water bath at 60-70 degrees C for 6-8 hours, filtering to obtain a precipitate, washing with water, drying, and grinding through a 20-40-mesh sieve to obtain modified powder; placing the obtained modified powder in a vacuum tube furnace, heating at 600 degrees C under vacuum condition, vacuum calcining for 3-5 hours, and cooling to room temperature to obtain powder with a two-dimensional polymerized aromatic carbon structure after the inorganic material with a layered structure is carbonized; and adding the calcined powder into 30-40 mass% hydrochloric acid solution, where each gram of powder corresponds to 8-10 ml of hydrochloric acid solution, stirring for 3-5 hours in an atmosphere of protective gas, performing precipitation separation, drying, breaking the structure of the layered structure inorganic material after acid washing, dissolving metal oxides, and naturally stripping the interlaminar carbonaceous material; heating the obtained product at 1800-2000 degrees C under vacuum condition, carrying out heat treatment for 4-6 hours, and cooling to obtain the graphene doped with two-dimensional nitrogen and phosphorus, where the original interlayer thickness is kept.