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Preparation method of graphene@ cobalt prussian blue nanocrystalline composite material, method for preparing working electrode by using graphene@ cobalt prussian blue nanocrystalline composite material and application of graphene@ cobalt prussian blue nanocrystalline composite material

A technology of ene-coated cobalt and Prussian blue, which is applied in the preparation of graphene-coated cobalt-based Prussian blue nanocrystalline composite materials, and in the field of electrocatalytic reduction of nitrate nitrogen in sewage, which can solve complex preparation methods and serious secondary pollution , Nitrogen selectivity is poor and other problems, to achieve the effect of high nitrogen selectivity, fast speed, cheap and easy-to-obtain raw materials

Active Publication Date: 2021-06-08
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of complex preparation methods, high material cost, serious secondary pollution, slow reaction speed and poor nitrogen selectivity of existing nitrate nitrogen reduction electrocatalysts, the present invention provides a graphene-coated cobalt-like Prussian blue nanocrystalline composite material preparation method

Method used

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  • Preparation method of graphene@ cobalt prussian blue nanocrystalline composite material, method for preparing working electrode by using graphene@ cobalt prussian blue nanocrystalline composite material and application of graphene@ cobalt prussian blue nanocrystalline composite material
  • Preparation method of graphene@ cobalt prussian blue nanocrystalline composite material, method for preparing working electrode by using graphene@ cobalt prussian blue nanocrystalline composite material and application of graphene@ cobalt prussian blue nanocrystalline composite material
  • Preparation method of graphene@ cobalt prussian blue nanocrystalline composite material, method for preparing working electrode by using graphene@ cobalt prussian blue nanocrystalline composite material and application of graphene@ cobalt prussian blue nanocrystalline composite material

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Embodiment 1

[0035]This embodiment provides a method for preparing graphene-coated cobalt-based Prussian blue nanocrystalline composite material Co PBA-rGO, comprising the following steps:

[0036] Add 0.5 mL of 0.2 mol / L potassium cobalt cyanide solution to 100 mL of 1 g / L graphene oxide dispersion, stir for 10 min and sonicate for 5 min respectively. Next, add 5 mL of 0.5 mol / L cobalt chloride solution to the above mixture, stir for 12 hours, centrifuge at 10,000 rpm for 10 minutes, freeze-dry the obtained solid for 24 hours, and then calcinate at 350°C for 2 hours in argon to obtain graphene-coated cobalt Prussian blue-like nanocrystalline composite CoPBA-rGO. The SEM and TEM images of the composite material CoPBA-rGO synthesized in this example are as follows: figure 1 and figure 2 shown. It can be seen that cobalt-like Prussian blue nanocrystals are uniformly coated in graphene. Co PBA-rGO, carbon black and 10g / L polyvinylidene fluoride in N-methylpyrrolidone solution (prepared ...

Embodiment 2

[0038] The preparation method and application of the graphene-coated cobalt-based Prussian blue nanocrystalline composite material provided in this example are basically the same as in Example 1, except that the volume of potassium cobaltcyanide solution is 0.25mL, cobalt chloride The volume of the solution was 2.5 mL. The removal rate of nitrate nitrogen by electrocatalytic reduction was 91.82%, the nitrogen selectivity was 63.43%, and no nitrate nitrogen was detected (<0.02mg / L).

Embodiment 3

[0040] The preparation method and application of the graphene-coated cobalt-based Prussian blue nanocrystalline composite material provided in this example are basically the same as in Example 1, except that the volume of potassium cobalt cyanide solution is 0.75mL, cobalt chloride The volume of the solution was 7.5 mL. The removal rate of nitrate nitrogen by electrocatalytic reduction was 90.60%, the nitrogen selectivity was 96.84%, and no nitrate nitrogen was detected (<0.02mg / L).

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Abstract

The invention provides a preparation method of a graphene@ cobalt prussian blue nanocrystalline composite material, a method for preparing a working electrode by adopting the graphene@ cobalt prussian blue nanocrystalline composite material and application of the graphene@ cobalt prussian blue nanocrystalline composite material. The preparation method of the composite material comprises the following steps: fully dispersing a cobalt-containing ligand solution and a graphene oxide solution in an aqueous solution through stirring and ultrasonic treatment; and adding a cobalt metal salt solution, fully stirring, centrifuging, freeze-drying, and calcining in an inert atmosphere to obtain the composite material. The preparation method has the advantages that the preparation method is simple, the energy consumption in the preparation process is low, the raw materials are cheap and easy to obtain and the like, the cobalt prussian blue nanocrystals are uniformly and tightly coated by the graphene with excellent conductivity, and the electron transfer efficiency and the active site utilization rate of the composite material are remarkably improved. When the composite material is applied to electrocatalytic reduction of nitrate nitrogen, the reaction speed is high, 98.97% of high nitrogen selectivity can be achieved without adding chloride ions, the cycling stability is good, and the composite material has a great application prospect in the field of water treatment.

Description

technical field [0001] The invention belongs to the technical field of water treatment, and in particular relates to a preparation method of a graphene-coated cobalt-like Prussian blue nanocrystal composite material and a method for preparing a working electrode by using the graphene-coated cobalt-like Prussian blue nanocrystal composite material, and will prepare The obtained working electrode is applied to the method of electrocatalytic reduction of nitrate nitrogen in sewage. Background technique [0002] Due to the extensive use of chemical fertilizers and pesticides and the massive discharge of industrial wastewater and urban sewage, the water environment has been polluted by nitrates to varying degrees. Among them, the nitrate pollution situation of groundwater, which is the source of drinking water in most areas of my country, is serious, and the concentration of nitrate in groundwater in some areas has reached 100 mg / L (calculated as nitrogen). Excessive intake of n...

Claims

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Application Information

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IPC IPC(8): C02F1/467C02F1/461C01B32/184C01C3/08B82Y30/00B82Y40/00C02F101/16
CPCC02F1/4676C02F1/46109C01B32/184C01C3/08B82Y30/00B82Y40/00C01P2002/72C01P2004/03C02F2101/163C02F2001/46133C01B32/194C02F1/4674C02F1/4618C02F2001/46138C02F2209/36C02F2209/42C01B32/198C01C3/12C01P2004/64
Inventor 王颖李风亭
Owner TONGJI UNIV
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