• 专利标题:   Preparing poly(p-phenylenediamine)/graphite-alkenyl nitrogen-doped porous carbon material comprises carrying out graphene carboxylation treatment, mixing, reacting, stirring, placing in tube furnace and preheating.
  • 专利号:   CN110371973-A
  • 发明人:   ZHOU Z, MAO S, ZHU D, CHEN X, CHEN Y, YANG X, YU Y, SONG L
  • 专利权人:   CHINA PETROLEUM CHEM CORP, SINOPEC NANJING CHEM RES INST CO LTD
  • 国际专利分类:   B01J020/20, B01J020/28, B01J020/30, C01B032/318, C01B032/348, C01B032/55
  • 专利详细信息:   CN110371973-A 25 Oct 2019 C01B-032/348 201988 Pages: 11 Chinese
  • 申请详细信息:   CN110371973-A CN10724396 07 Aug 2019
  • 优先权号:   CN10724396

▎ 摘  要

NOVELTY - Preparing poly(p-phenylenediamine)/graphite-alkenyl nitrogen-doped porous carbon material comprises (i) carrying out graphene carboxylation treatment by refluxing graphene and mixed acid are at 85-100 degrees C; (ii) dissolving carboxylated treated graphene and p-phenylenediamine monomer in hydrochloric acid solution in mass ratio of 1:10 and ultrasonically mixing uniformly; (iii) dissolving ammonium persulfate in hydrochloric acid, ultrasonically mixing uniformly,; (iv) adding solution of step (iii) slowly into solution of step (ii) and reacting in ice bath environment at 0-5 degrees C for 5-7 hours and washing; (v) adding certain amount of obtained compound and potassium hydroxide into de-ionized water and uniformly mixing; and (vi) adding proper amount of poly-p-phenylenediamine/graphite-alkenyl nitrogen-doped porous carbon material into porcelain boat and stirring uniformly, placing in tube furnace and adjusting temperature for preheating under nitrogen atmosphere. USE - The method is useful for preparing poly(p-phenylenediamine)/graphite-alkenyl nitrogen-doped porous carbon material. ADVANTAGE - The material has large adsorption amount to carbon dioxide at room temperature, stable physical and chemical properties and good cycle regeneration performance. The method is simple, environmentally-friendly and overcomes complicated traditional solid adsorbent preparation process, non-environmentally-friendly and high energy consumption defects, facilitates batch preparation and has good application prospect. DETAILED DESCRIPTION - Preparing poly(p-phenylenediamine)/graphite-alkenyl nitrogen-doped porous carbon material comprises (i) carrying out graphene carboxylation treatment by refluxing graphene and mixed acid are at 85-100 degrees C, stirring for 90-110 minutes, cooling to room temperature, washing with ethanol and de-ionized water until neutral, drying and grinding; (ii) dissolveing carboxylated treated graphene and p-phenylenediamine monomer in hydrochloric acid solution in mass ratio of 1:10 and ultrasonically mixing uniformly, transferring solution to 0-5 degrees C water bath in ice bath environment and maintaining constant magnetic stirring speed; (iii) dissolving ammonium persulfate in hydrochloric acid, ultrasonically mixing uniformly, where molar ratio of ammonium persulfate and p-phenylenediamine monomer is 1:0.9-1.1; (iv) adding solution of step (iii) slowly into solution of step (ii) and reacting in ice bath environment at 0-5 degrees C for 5-7 hours and washing obtained product with ethanol and de-ionized water until solution is neutral to obtain polyparaphenylene diamine/graphene composite; (v) adding certain amount of obtained compound and potassium hydroxide into de-ionized water and uniformly mixing, where mass ratio of potassium hydroxide and compound is 0-4:1, pouring mixed solution uniformly into cell plate, placing in freeze dryer for freeze-drying and grinding dried product into powder; and (vi) adding proper amount of poly-p-phenylenediamine/graphite-alkenyl nitrogen-doped porous carbon material into porcelain boat and stirring uniformly, placing in tube furnace and adjusting temperature for preheating under nitrogen atmosphere, activating and washing activated complex with hydrochloric acid, washing with ethanol and de-ionized water until neutral and drying in oven and grinding into powder to obtain activated poly(p-phenylenediamine/graphite-alkenyl nitrogen-doped porous carbon material.