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Solvent circulation preparation method and application of a metal atom-level dispersed nitrogen-carbon material

A technology of solvent circulation and metal nitrogen, applied in the direction of structural parts, electrolytic organic production, electrolytic components, etc., can solve the problems of not meeting the requirements of green chemistry, restricting industrial production, and low utilization of atoms, and achieve simple and easy reaction operation, The effect of low price and avoiding complicated processing

Active Publication Date: 2022-06-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, expensive metal-organic raw materials are usually used in the preparation process, accompanied by the generation of a large amount of organic waste liquid and acid waste liquid, and the low utilization rate of atoms does not meet the requirements of green chemistry, which limits its industrial production.

Method used

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  • Solvent circulation preparation method and application of a metal atom-level dispersed nitrogen-carbon material
  • Solvent circulation preparation method and application of a metal atom-level dispersed nitrogen-carbon material
  • Solvent circulation preparation method and application of a metal atom-level dispersed nitrogen-carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A solvent cycle preparation method of metal atomic dispersed nitrogen-carbon material, the preparation method comprises the following steps:

[0042] Weigh 3 mmol of zinc powder and dissolve it in 30 ml of formamide. After stirring at 60 degrees Celsius for 0.5 hours, ultrasonically disperse for 0.5 hours. Alternately perform high-temperature stirring and ultrasonic dispersion until a golden yellow clear and transparent solution is obtained. Transfer this solution to In a 40 ml hydrothermal reactor, the reaction was carried out at 220 degrees Celsius for 12 hours. Then, the product solution was suction filtered to separate the solid and the formamide solution L1, the solid was washed three times with deionized water, and the obtained filter cake was freeze-dried in a vacuum freeze dryer to obtain powder materials. After the powder material is ground and calcined at 600 degrees Celsius in an argon atmosphere for 4 hours, the black powder material obtained is the metal ni...

Embodiment 2

[0050] The difference from Example 1 is:

[0051] 3 mmol of zinc powder was changed to 10 mmol of zinc acetate, and the reaction process of solvent circulation operation was: in a 40 ml hydrothermal reactor, solvothermal reaction at 160 degrees Celsius for 20 hours to obtain metal nitrogen carbon material ZnNC-2#, Others are the same as in Example 1, and the solvent circulation operation is carried out to the first, second, and third times of Example 1, which are respectively named as metal nitrogen carbon material ZnNC-2#cycling 1st, metal nitrogen carbon material ZnNC-2# Cycling 2nd, metal nitrogen carbon material ZnNC-2#cycling 3rd.

[0052] figure 2 This is the SEM image of the metal nitrogen carbon material ZnNC-2#cycling 2nd prepared in Example 2 of the present invention. , the metal nitrogen carbon material is spherical nanoparticles with a size distribution of about 10 nm.

[0053] Figure 7 This is the XRD image of the metal nitrogen carbon material ZnNC-2#cyclin...

Embodiment 3

[0056] Except that 3 mmol of zinc powder was changed to 0.03 mmol of cobalt acetate and 3 mmol of zinc acetate, and the carbonization temperature was 700 degrees Celsius, the others were the same as in Example 1, and the metal nitrogen carbon material ZnCoNC was prepared, and the solvent circulation operation was carried out to implement In the first, second and third times of Example 1, the metal nitrogen carbon material ZnCoNC cycling 1st, the metal nitrogen carbon material ZnCoNC cycling 2nd, and the metal nitrogen carbon material ZnCoNC cycling 3rd were obtained, respectively.

[0057] image 3 This is the SEM image of the metal nitrogen carbon material ZnCoNC prepared in Example 3 of the present invention. The metal nitrogen carbon material is spherical nanoparticles with a size distribution of about 10 nm.

[0058] Figure 8 This is the XRD image of the metal nitrogen carbon material ZnCoNC prepared in Example 3 of the present invention. It can be seen from the figure ...

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Abstract

The invention belongs to the field of novel material preparation, and in particular relates to a solvent circulation preparation method and application of a metal atom-level dispersed nitrogen-carbon material. The preparation method comprises the following steps: A. dissolving metal powder or metal salt in formamide to prepare a solution, reacting at 80-240 degrees Celsius for 2-24 hours, and separating solid and liquid to obtain the first solid product and formamide Solution L1; B. Perform the first solvent circulation operation: dissolve the metal powder or metal salt in the formamide solution L1 and react at 80-240 degrees Celsius for 2-24 hours, then separate the solid and liquid to obtain the second solid product and formamide Solution L2; C. Calcining the first solid product and / or the second solid product in an argon atmosphere with the temperature controlled at 400-1200 degrees Celsius to obtain a metal nitrogen carbon material. The present invention recycles the solvent formamide in the reaction for the first time, and the metal nitrogen carbon material prepared from the recovered solvent has the same structure as the metal nitrogen carbon material prepared from fresh formamide, and the metal nitrogen carbon material has the same catalytic performance.

Description

technical field [0001] The invention belongs to the field of novel material preparation, and particularly relates to a solvent cycle preparation method and application of a metal atomic-level dispersed nitrogen-carbon material. Background technique [0002] Metal single-atom catalysts solve the problems that homogeneous catalysts are difficult to separate, recover and regenerate, as well as the defects of limited contact area between heterogeneous catalysts and reactants and low utilization of metal atoms. Single-atom catalysts have the most outstanding oxygen reduction reaction (ORR) performance. . Through the regulation of structure, crystal form, morphology, and doping, the performance of some single-atom catalysts even exceeds that of noble metal catalysts. In particular, metal and nitrogen-doped carbon (MNC) catalysts have high atomic utilization, space for structural composition regulation, and can also exhibit good ORR activity and stability in acidic media. Based o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/075C25B1/23C25B1/30C25B3/26H01M4/90
CPCC25B11/075C25B1/30C25B1/23C25B3/26H01M4/9041H01M4/9083Y02E60/50
Inventor 孙晓明汤加伦田书博周道金孙恺徐淑慧
Owner BEIJING UNIV OF CHEM TECH
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