• 专利标题:   Preparing platinum/graphene sheet composite material comprises cooling the concentrated sulfuric acid in ice bath, adding e.g. graphite powder, stirring, heating, adding hydrogen peroxide, heating, cooling, filtering and drying.
  • 专利号:   CN106115664-A
  • 发明人:   PAN Z, SI R, LIU C
  • 专利权人:   TIANJIN BAOXINGWEI TECHNOLOGY CO LTD
  • 国际专利分类:   B22F009/22, C01B031/04
  • 专利详细信息:   CN106115664-A 16 Nov 2016 C01B-031/04 201709 Pages: 6 Chinese
  • 申请详细信息:   CN106115664-A CN10413872 13 Jun 2016
  • 优先权号:   CN10413872

▎ 摘  要

NOVELTY - Preparing platinum/graphene sheet composite material comprises (a) cooling the concentrated sulfuric acid in ice bath, adding e.g. graphite powder, stirring to obtain brown product, adding e.g. dilute sulfuric acid, heating, cooling, adding hydrogen peroxide, filtering, drying, sealing, (b) ultrasonically dispersing the oxidized graphite in the sealed quartz tube, heating, and (c) mixing e.g. grinded graphene sheet, magnetic stirring, heating, reacting, mixing, taking e.g. precursor into a high pressure stainless steel reactor, heating, cooling, filtering and drying. USE - The method is useful preparing platinum/graphene sheet composite material (claimed). ADVANTAGE - The platinum/graphene sheet composite material is environmentally friendly, has high values for methanol point oxidation, electrocatalytic activity and is stable. DETAILED DESCRIPTION - Preparing platinum/graphene sheet composite material comprises (a) high temperature reaction by cooling the concentrated sulfuric acid in ice bath under the stirring condition, slowly adding graphite powder and anhydrous sodium nitrate, mixed uniformly, slowly adding potassium permanganate, concentrated sulfuric acid, graphite powder, where the mass ratio of anhydrous sodium nitrate and potassium permanganate is 16:1:115:45, controlling the feeding time for more than 1 hour, after finishing feeding reaction for 1.5 hours, maintaining temperature and reacting at low temperature after the reaction is completed, removing from the ice water bath, controlling temperature at 30 degrees C, stirring for 6 days to obtain brown product, slowly adding 5% sulfuric acid dilute solution at high temperature reaction, rapidly increase temperature of mixed liquid, adding dilute sulfuric acid, heating at 90 degrees C for 2.5 hours, naturally cooling, cooling to 60 degrees C, adding 30% hydrogen peroxide and un-reacted potassium permanganate, reacting for 2 hours, vacuuming and filtering the reaction mixed solution, washing with de-ionized water, filtering by filter membrane, until the pH value is neutral, drying at 50 degrees C for 1 days, vacuum drying at 60 degrees C for 2 days, sealing and storing the product, (b) ultrasonically dispersing the oxidized graphite in the sealed quartz tube under nitrogen atmosphere, heating at 1100 degrees C, after high temperature treatment product of brown oxide graphene sheet becomes black grapheme to obtain graphene sheet, (c) mixing and grinded graphene sheet and dimethyl (1,5-cyclooctadiene) platinum in a mass ratio of 1:1.5-1.9, taking the mixed sample into a high pressure stainless steel reactor, sealing the reactor, filling carbon dioxide, removing the air in the reactor, magnetic stirring, heating at 80 degrees C, pressurizing at 25 MPa after reacting for 5.5 hours, completely mixing, taking precursor and graphene sheet into a high pressure stainless steel reactor, using the nitrogen gas air in the reactor, slowly introducing nitrogen gas, heating at 200 degrees C, reacting for 5 hours, cooling to room temperature, slowly discharging the gas, collecting the sample, washing with ethanol, filtering, removing impurity, drying in the vacuum drying box at 60 degrees C for 7 hours.