Metal-fluorine doped carbon composite material as well as preparation method and application thereof in electrocatalytic nitrogen fixation

A technology of carbon composite materials and composite materials, which is applied in the fields of electrochemistry, catalysis and material synthesis, can solve the problems of low activity and selectivity of nitrogen reduction electrocatalysts, improve reaction activity and selectivity, reduce costs, and have high catalytic activity Effect

Active Publication Date: 2020-09-22
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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Problems solved by technology

[0004] The purpose of the present invention is to overcome the problems of low activity and selectivity of nitrogen reduction electrocatalysts, and provide a metal-fluorine-doped carbon composite material and its preparation method and application in electrocatalytic nitrogen fixation

Method used

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  • Metal-fluorine doped carbon composite material as well as preparation method and application thereof in electrocatalytic nitrogen fixation
  • Metal-fluorine doped carbon composite material as well as preparation method and application thereof in electrocatalytic nitrogen fixation
  • Metal-fluorine doped carbon composite material as well as preparation method and application thereof in electrocatalytic nitrogen fixation

Examples

Experimental program
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Effect test

Embodiment 1

[0058] Embodiment 1 uses graphite oxide and chloroauric acid as raw materials to prepare Au-F / G composite material

[0059] (1) Preparation of graphene oxide: graphene oxide was prepared by the improved hummer method, and the process was as follows: 1.5 g of phosphorus flake graphite was mixed with 35 ml of concentrated sulfuric acid and 0.75 g of sodium nitrate, and stirred for 16 hours. Then add 4.5g of potassium permanganate at 0°C and stir for 2h. The system was warmed up to room temperature, continued to stir for 3h, added 200ml of water, and heated to 98°C for 15 minutes. Finally, add excess hydrogen peroxide, stir overnight, filter, pickle with 500ml of 5mol / L hydrochloric acid, and then wash with excess water, and dry the obtained sample under freeze-drying conditions for 24 hours.

[0060] (2) Preparation of F-doped graphene: Take 600 mg of graphene oxide, add 300 ml of water and ultrasonically disperse for 1 h. Then add 20ml of hydrofluoric acid solution (40wt.%) a...

Embodiment 2

[0066] Example 2 Preparation of Au-F / CNT composite material using carbon nanotubes and chloroauric acid as raw materials

[0067] (1) Preparation of oxidized carbon nanotubes: Multi-walled carbon nanotubes purchased from Aladdin Reagent Company were used as precursors to prepare oxidized carbon nanotubes. The process was as follows: 5 g of carbon nanotubes were mixed with 60 ml of concentrated nitric acid, and ultrasonicated for 1 h. Afterwards, the mixture was added into the flask, and stirred under reflux at 120° C. for 12 h. After cooling, add a certain amount of KOH to adjust the pH to between 2-7. After cooling and filtering, the material was washed 5 times with deionized water, and then dried overnight in a drying oven at 80° C. to obtain oxidized carbon nanotubes.

[0068] (2) Preparation of F-doped carbon nanotubes: Take 600 mg of oxidized carbon nanotubes, add 300 ml of water and ultrasonically disperse for 1 h. Then add 20ml of hydrofluoric acid solution (40wt.%) a...

Embodiment 3

[0071] Example 3 Preparation of Ru-F / C composite material using activated carbon and ruthenium chloride as raw materials

[0072] (1) Preparation of oxidized activated carbon: The purchased BP2000 activated carbon material was used as the precursor to prepare oxidized activated carbon. The process was as follows: 5g activated carbon was mixed with 60ml concentrated nitric acid, and ultrasonicated for 1h. Afterwards, the mixture was added into the flask, and stirred under reflux at 100° C. for 12 h. After cooling, add a certain amount of KOH to adjust the pH to between 2-7. After cooling and filtering, the material was washed 5 times with deionized water, and then dried overnight in an oven at 80°C to obtain oxidized activated carbon.

[0073] (2) Preparation of F-doped activated carbon: Take 300 mg of oxidized activated carbon, add 150 ml of water and ultrasonically disperse for 1 h. Then add 10ml of hydrofluoric acid solution (40wt.%) and stir evenly. Put the mixture into ...

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Abstract

The invention provides a metal-fluorine doped carbon composite material as well as a preparation method and application thereof in nitrogen fixation reduction, the metal-fluorine doped carbon composite material comprises metal, fluorine and a carbon carrier, and the fluorine and the metal are distributed on the surface of the carbon carrier; metal (such as Au, Ru, Fe or Mo) loaded on the surface of the carbon carrier can provide effective active sites for catalytic nitrogen reduction of the composite material, and an ammonia synthesis reaction is carried out. Besides, the surface of the carboncarrier is modified with a high-electronegativity fluorine element, and the fluorine element can react with a nitrogen reduction intermediate product to generate a hydrogen bond, stabilize the nitrogen reduction intermediate, reduce the activation energy of the nitrogen reduction intermediate and generate a synergistic effect with metal sites, so that reaction activity and selectivity are improved. In addition, when the three-dimensional sizes of metal and fluorine dispersed on the surface of the carbon carrier are both smaller than 10 nm, the synergistic effect of the metal and the fluorineis obviously enhanced.

Description

technical field [0001] The invention relates to a metal-fluorine-doped carbon composite material, a preparation method thereof and an application in electrocatalytic nitrogen fixation, belonging to the technical fields of electrochemistry, catalysis and material synthesis. Background technique [0002] Nitrogen-containing compounds are one of the most important components of living organisms such as animals and plants. It is an effective way to simulate nitrogen fixation in nature by using energy artificially, reducing nitrogen in the atmosphere to ammonia, and then preparing various nitrogen-containing inorganic / organic substances. At present, the relatively mature artificial nitrogen fixation method is the Haber-Bosch nitrogen fixation process invented in the Middle Ages. According to statistics, the amount of nitrogen fixation produced by this process accounts for about 50% of the current source of nitrogen for the human body. However, this nitrogen fixation process req...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/06B01J27/128B01J27/13C25B1/00C25B11/06
CPCB01J27/06B01J27/128B01J27/13B01J35/0033C25B1/00C25B11/04
Inventor 王要兵黄艺吟吴茂祥
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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