• 专利标题:   Synthesis of graphene loaded noble metal catalyst in organic phase comprises adding graphite powder to sulfuric acid with potassium peroxydisulfate and phosphorus pentoxide, and stripping off by ultrasonic treatment.
  • 专利号:   CN102198398-A, CN102198398-B
  • 发明人:   ZHANG X, GAO H, SHEN C, YANG S
  • 专利权人:   UNIV NANJING AERONAUTICS ASTRONAUTICS
  • 国际专利分类:   B01J023/44, B01J037/16, B82Y040/00
  • 专利详细信息:   CN102198398-A 28 Sep 2011 B01J-023/44 201203 Pages: 10 Chinese
  • 申请详细信息:   CN102198398-A CN10088151 08 Apr 2011
  • 优先权号:   CN10088151

▎ 摘  要

NOVELTY - Synthesis of graphene loaded noble metal catalyst in organic phase comprises slowly adding graphite powder to concentrated sulfuric acid with potassium peroxydisulfate and phosphorus pentoxide, adding to strong oxidized acid, adding potassium-containing strong oxidizing agent, heating at 35-40 degrees C in water bath, filtering bright yellow graphite diluting solution, dispersing in N-methyl pyrrolidone solution, stripping off by ultrasonic treatment, and in inert gas, adding stabilizer and noble metal precursor to N-methyl pyrrolidone solution of oxidized graphite. USE - Method of synthesizing graphene loaded noble metal catalyst in organic phase (claimed). ADVANTAGE - The graphene loaded noble metal catalyst prepared has good structure stability, higher specific surface area, good dispersity, high stability and high activity. DETAILED DESCRIPTION - Synthesis of graphene loaded noble metal catalyst in organic phase comprises: (A) slowly adding graphite powder to concentrated sulfuric acid with potassium peroxydisulfate and phosphorus pentoxide, stirring, reacting for 3-12 hours in oil bath of 80-90 degrees C, adding deionized water for washing, and drying to obtain pre-oxidized graphite powder; (B) slowly adding to strong oxidized acid, stirring at 0-5 degrees C, adding potassium-containing strong oxidizing agent to strong oxidizing acid, stirring, heating at 35-40 degrees C in water bath, reacting for 2-8 hours, adding deionized water, obtaining brown graphite suspension liquid, adding hydrogen peroxide and deionized water, and obtaining bright yellow graphite diluting liquid, with strong oxidizing acid comprising concentrated sulfuric acid or perchloric acid, and potassium-containing strong oxidizing agent comprising potassium permanganate or potassium perchlorate; (C) filtering bright yellow graphite diluting solution to obtain yellow brown filter cake, washing by acid, dispersing in water, centrifuging to obtain oxidized graphite gel, drying to obtain black brown oxidized graphite solid, dispersing in N-methyl pyrrolidone solution, and stripping off for 0.5-3 hours by ultrasonic treatment to obtain oxidized graphite of dispersed N-methyl pyrrolidone solution;and (D) in inert gas, adding stabilizer and noble metal precursor to N-methyl pyrrolidone solution of oxidized graphite, reacting for 1-12 hours at 180-200 degrees C to obtain graphene loaded monodisperse noble metal nano particle compound, with noble metal precursor one or alloy of more of platinum, palladium, silver, ruthenium and gold; and stabilizer comprising fatty amine or phosphine compound, fatty amine comprising oleylamine; phosphine compound comprising trioctylphosphine, trioctylphosphineoxide, triphenylphosphine, tricresyl phosphate, tri(2-furan) phosphine, 1,3-diphenyl phosphorus propane, 1,2-diphenyl phosphorus ethane, 1,4-bi(diphenylphosphine) butane, 2,2'-bis(diphenylphosphino)-1,1'-dinaphthalene, m-(sulfonated triphenylphosphine disodium salt), 1,1'-di(diphenyl phosphorus) ferrocene and 2,2'-di(diphenyl phosphorus) biphenyl. DESCRIPTION OF DRAWING(S) - The drawing shows a schematic diagram of the synthesis of graphene loaded noble metal catalyst in organic phase.