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Solvent circulation preparation method and application of metal atomic-scale dispersed nitrogen-carbon material

A solvent circulation and metal atom technology, applied in structural parts, electrolytic organic production, electrolytic components, etc., can solve problems such as high price, low atom utilization, and non-compliance with green chemistry requirements.

Active Publication Date: 2021-09-10
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 metal atomic-scale dispersed nitrogen-carbon material
  • Solvent circulation preparation method and application of metal atomic-scale dispersed nitrogen-carbon material
  • Solvent circulation preparation method and application of metal atomic-scale dispersed nitrogen-carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A solvent circulation preparation method for metal atomically dispersed nitrogen-carbon materials, the preparation method comprising the following steps:

[0042] Weigh 3 millimoles of zinc powder and dissolve it in 30 milliliters of formamide, stir at 60 degrees Celsius for 0.5 hours, and ultrasonically disperse for 0.5 hours. High-temperature stirring and ultrasonic dispersion are carried out alternately until a golden yellow clear and transparent solution is obtained. Transfer this solution to In a 40 ml hydrothermal reactor, react 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 a powder material. After the powder material is ground, it is calcined at 600 degrees Celsius for 4 hours in an argon atmosphere to obtain a black powder material which ...

Embodiment 2

[0050] The difference with embodiment 1 is:

[0051] 3 millimoles of zinc powder is changed to 10 millimoles of zinc acetate, and the reaction process of the solvent circulation operation is as follows: in a 40 milliliter hydrothermal reaction kettle, 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, the solvent circulation operation is carried out to the 1st, 2nd, and 3rd times of Example 1, and they are respectively named 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 SEM image of metal nitrogen carbon material ZnNC-2#cycling 2nd prepared for 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 XRD image of metal nitrogen carbon material ZnNC-2#cycl...

Embodiment 3

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

[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 XRD image of metal nitrogen carbon material ZnCoNC prepared for Example 3 of the present invention. It can be seen from the figure that there...

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Abstract

The invention belongs to the field of preparation of novel materials, and particularly relates to a solvent circulation preparation method and application of a metal atomic-scale dispersed nitrogen-carbon material. The preparation method comprises the following steps: A, dissolving metal powder or metal salt in formamide to prepare a solution, conducting reacting at 80-240 DEG C for 2-24 hours, and performing solid-liquid separation to obtain a first solid product and a formamide solution L1; B, carrying out primary solvent circulation operation, namely dissolving metal powder or metal salt in the formamide solution L1, conducting reacting at 80-240 DEG C for 2-24 hours, and carrying out solid-liquid separation to obtain a second solid product and a formamide solution L2; and C, calcining the first solid product and / or the second solid product in an argon atmosphere, and controlling a temperature at 400-1200 DEG C to obtain the metal nitrogen-carbon material. According to the method, the formamide solvent in the reaction is recycled for the first time, the metal nitrogen-carbon material prepared from the recycled solvent has the same structure as the metal nitrogen-carbon material prepared from fresh formamide, and the catalytic performance of the metal nitrogen-carbon material is equal to the catalytic performance of the metal nitrogen-carbon material prepared from fresh formamide.

Description

technical field [0001] 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. Background technique [0002] Metal single-atom catalysts solve the shortcomings of homogeneous catalysts that are difficult to separate, recycle and regenerate, as well as the defects of limited contact area between heterogeneous catalysts and reactants, and low metal atom utilization. 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 structure (MNC) catalysts have high atom utilization, structural composition control space, and can also exhibit good ORR activity and stability in acidic media....

Claims

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Application Information

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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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