A kind of covalent organic framework material catalyst based on loaded Ru nanoparticles and its preparation method and application

A covalent organic framework and nanoparticle technology, which is applied in the field of electrocatalysis, can solve the problem that the catalytic activity of the catalyst needs to be improved, and achieve the effects of good recycling stability, high specific surface area, and small particles

Active Publication Date: 2022-07-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, there are few researches on the application of catalysts based on covalent organic frameworks in electrocatalysis, and the catalytic activity of such catalysts needs to be improved.

Method used

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  • A kind of covalent organic framework material catalyst based on loaded Ru nanoparticles and its preparation method and application
  • A kind of covalent organic framework material catalyst based on loaded Ru nanoparticles and its preparation method and application
  • A kind of covalent organic framework material catalyst based on loaded Ru nanoparticles and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Mix 0.64 g of terephthalonitrile, 0.64 g of 2,6-pyridinedicarbonitrile and 3.2 g of conductive carbon black powder in a mortar and mix thoroughly to obtain mixture A. Place 6.4g of anhydrous zinc chloride, the above-prepared mixture A and 6.4g of anhydrous zinc chloride in order from bottom to top in the crucible (that is, the mixture A is placed between two layers of anhydrous zinc chloride powder);

[0029] 2) Place the crucible in step 1) in a tube furnace, and perform high-temperature calcination under nitrogen protection. The calcination temperature is 400 °C, the calcination time is 40 hours, and the nitrogen flow rate in the tube furnace is 50 mL / min. The calcined product was successively stirred and washed with 1 mol / L hydrochloric acid solution and deionized water for 12 hours, and the washed solid was vacuum-dried at 60 °C for 12 hours to obtain the covalent organic framework carrier powder (Example 1, Step 2). The obtained covalent organic framework carrie...

Embodiment 2

[0042] 1) Mix 0.64 g of terephthalonitrile, 0.64 g of 2,6-pyridinedicarbonitrile and 3.2 g of conductive carbon black powder in a mortar and mix thoroughly to obtain mixture A. In the crucible, place 6.4g of anhydrous zinc chloride, the above-prepared mixture A and 6.4g of anhydrous zinc chloride in order from bottom to top (that is, the mixture A is placed between two layers of anhydrous zinc chloride powder);

[0043] 2) Place the crucible in step 1) in a tube furnace, and perform high-temperature calcination under nitrogen protection. The calcination temperature is 400 °C, the calcination time is 40 hours, and the nitrogen flow rate in the tube furnace is 50 mL / min. The calcined product was successively stirred and washed with 1 mol / L hydrochloric acid solution and deionized water for 12 hours, and the washed solid was vacuum-dried at 60 °C for 12 hours to obtain covalent organic framework carrier powder;

[0044] 3) Take 50 mg of the covalent organic framework carrier powd...

Embodiment 3

[0049] Take 50 mg of conductive carbon black powder and 20.8 mg of ruthenium acetylacetonate in a mortar and fully grind until they are evenly mixed, then calcined at high temperature in a tube furnace under nitrogen protection, and heated from room temperature to 300 ° C at 3 ° C / min, and After calcination at 300° C. for 3 hours, the calcined product was washed with ultrapure water and dried to obtain the target catalyst.

[0050] The electrocatalytic ammonia synthesis performance test of the catalyst obtained in Example 3 is as follows:

[0051] Weigh 4.0 mg of the catalyst of Example 3, add 900 microliters of ethanol and 100 microliters of Nafion solution (the mass fraction of Nafion solution is 5%), and sonicate for 0.5 hours. After the catalyst is completely dispersed, a uniform catalyst slurry is obtained. Pipette 0.2 mL of the prepared catalyst slurry and spread it evenly on 1 cm × 1 cm carbon paper, dry it, and use it as the working electrode, Ag / AgCl (3 mol / L KCl) as ...

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Abstract

The invention discloses a covalent organic framework material catalyst based on supported Ru nanoparticles and a preparation method and application thereof. The preparation method of the catalyst is as follows: a mixture A is obtained by fully mixing a benzene derivative, a pyridine derivative and a conductive carbon material; and non-precious metal salts are placed in a tube furnace, calcined at high temperature in a nitrogen atmosphere, the calcined product is washed with hydrochloric acid solution and deionized water in turn, and dried to obtain covalent organic framework carrier powder; the obtained covalent organic framework carrier powder and The ruthenium metal salt is fully ground and mixed uniformly, and then placed in a tube furnace and calcined at high temperature in a nitrogen atmosphere. The calcined product is washed with ultrapure water and dried to obtain a covalent organic framework material catalyst based on supported Ru nanoparticles. . The catalyst of the invention has high specific surface area and large pore size, and the ruthenium metal supported on the covalent organic framework carrier powder has small particles and high dispersity, and has good catalytic activity when applied to electrochemical reduction of nitrogen to synthesize ammonia.

Description

technical field [0001] The invention belongs to the technical field of electrocatalysis, and in particular relates to a covalent organic framework material catalyst based on supported Ru nanoparticles and a preparation method and application thereof. Background technique [0002] Ammonia is an alkaline, colorless, lighter-than-air gas with a pungent odor. It is the most produced chemical worldwide and is the main raw material for the manufacture of nitrogen fertilizers and compound fertilizers. In order to improve the nitrogen conversion rate and improve the economy of the ammonia synthesis process, the selection and use of catalysts are very important. At present, a lot of research has been done to find electrochemical electrochemical properties with more stable chemical properties, thermodynamic properties and good economic benefits. Ammonia synthesis catalyst. A number of catalysts have been continuously discovered in research. Rod et al. were the first to use density ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J37/08B01J37/06B01J35/10C25B1/00C25B11/095
CPCB01J31/1815B01J31/2234B01J35/0033B01J37/086B01J37/06B01J35/1019B01J35/1061C25B1/00B01J2531/26C25B11/095
Inventor 庄桂林高旭王建国
Owner ZHEJIANG UNIV OF TECH
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