• 专利标题:   Preparing iron-doped nickel phosphide composite nitrogen-doped reduced graphene oxide electrocatalytic material comprises e.g. reacting graphene oxide, nickel(II) chloride hexahydrate, ferrous sulfate heptahydrate and ammonium fluoride.
  • 专利号:   CN111068726-A
  • 发明人:   LIU Y, ZHAO R, YANG M, WANG H
  • 专利权人:   UNIV ZHEJIANG
  • 国际专利分类:   B01J027/185, B01J027/24, C25B001/04, C25B011/06
  • 专利详细信息:   CN111068726-A 28 Apr 2020 B01J-027/185 202050 Pages: 11 Chinese
  • 申请详细信息:   CN111068726-A CN11173612 26 Nov 2019
  • 优先权号:   CN11173612

▎ 摘  要

NOVELTY - Preparing iron-doped nickel phosphide composite nitrogen-doped reduced graphene oxide electrocatalytic material comprises e.g. dissolving graphene oxide in deionized water, adding melamine, stirring and evaporating to obtain light black solid, adding into a tube furnace, heating and warming, cooling to room temperature, washing and drying to obtain nitrogen-doped reduced graphene oxide, dissolving nitrogen-doped reduced graphene oxide in deionized water, ultrasonic treating, and homogeneously mixing, adding urea, ammonium fluoride, nickel(II) chloride hexahydrate and ferrous sulfate heptahydrate, then transferring into a reactor, reacting at 100-130 degrees C for 6-10 hours, and centrifuging, washing and drying to obtain precursor material, and placing the precursor material in a tube furnace, heating at 300-360 degrees C for 1-4 hours, and cooling to room temperature to obtain final product. USE - The method is useful for preparing iron-doped nickel phosphide composite nitrogen-doped reduced graphene oxide electrocatalytic material. ADVANTAGE - The method: has simple process, and low cost; and produces product having excellent catalytic performance. DETAILED DESCRIPTION - Preparing iron-doped nickel phosphide composite nitrogen-doped reduced graphene oxide electrocatalytic material comprises (i) dissolving graphene oxide in deionized water ultrasonically to obtain uniform graphene oxide solution, then adding melamine, stirring and evaporating to obtain light black solid, where the mass ratio between graphene oxide and melamine is 1:5-10, (ii) adding the light black solid prepared in step (i) into a tube furnace, heating at 700-900 degrees C in inert atmosphere and warming for 1-3 hours, cooling to room temperature, washing and drying to obtain nitrogen-doped reduced graphene oxide, (iii) dissolving nitrogen-doped reduced graphene oxide in deionized water, ultrasonic treating for 3-7 hours, and homogeneously mixing to obtain nitrogen-doped reduced graphene oxide solution having concentration of 0.75-1 mg/ml, (iv) adding urea, ammonium fluoride, nickel(II) chloride hexahydrate and ferrous sulfate heptahydrate into above nitrogen-doped reduced graphene oxide solution, and stirring until a homogeneous solution, where the amount ratio between nickel(II) chloride hexahydrate and ferrous sulfate heptahydrate is 2-8:1, the amount ratio between urea and ammonium fluoride is 1-3:1, (v) transferring the solution in step (iv) into a reactor, reacting at a temperature of 100-130 degrees C for 6-10 hours, and centrifuging to obtain dark green precipitate, washing the precipitate with absolute ethanol and drying at 50-70 degrees C to obtain precursor material (NiFe-LDH/NG), and (vi) placing the precursor material prepared in step (v) in a tube furnace, heating the sample to 300-360 degrees C at a heating rate of 1-5 degrees C/minute and incubating for 1-4 hours in inert atmosphere, and cooling to room temperature to obtain final product.