Covalent organic framework material catalyst based on loaded Ru nanoparticles as well as preparation method and application of the catalyst

A covalent organic framework and nanoparticle technology, which is applied in the field of electrocatalysis, can solve the problems of the catalytic activity of the catalyst to be improved, and achieve the effects of good recycling stability, optimized electronic structure, and small particles

Active Publication Date: 2019-11-22
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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  • Covalent organic framework material catalyst based on loaded Ru nanoparticles as well as preparation method and application of the catalyst
  • Covalent organic framework material catalyst based on loaded Ru nanoparticles as well as preparation method and application of the catalyst
  • Covalent organic framework material catalyst based on loaded Ru nanoparticles as well as preparation method and application of the catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Thoroughly grind and mix 0.64g of terephthalonitrile, 0.64g of 2,6-pyridinedicarbonitrile and 3.2g of conductive carbon black powder in a mortar to obtain mixture A. Place 6.4g of anhydrous zinc chloride, the above-mentioned mixture A and 6.4g of anhydrous zinc chloride in the crucible from bottom to top (that is, 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 the protection of nitrogen. The calcination temperature is 400°C, the calcination time is 40 hours, and the nitrogen flow rate into 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 (Step 2 of Example 1) The prepared covalent organic framework carrier pow...

Embodiment 2

[0042] 1) Thoroughly grind and mix 0.64g of terephthalonitrile, 0.64g of 2,6-pyridinedicarbonitrile and 3.2g of conductive carbon black powder in a mortar to obtain mixture A. Place 6.4g of anhydrous zinc chloride, the above-mentioned mixture A and 6.4g of anhydrous zinc chloride in the crucible from bottom to top (that is, 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 the protection of nitrogen. The calcination temperature is 400°C, the calcination time is 40 hours, and the nitrogen flow rate into 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;

[0044] 3) Put 50 mg of the covalent organic framework carrier powder o...

Embodiment 3

[0049] Take 50 mg of conductive carbon black powder and 20.8 mg of ruthenium acetylacetonate and place them in a mortar and grind them thoroughly until they are evenly mixed, then perform high-temperature calcination in a tube furnace under nitrogen protection, and heat up from room temperature at 3 °C / min to 300 °C, and Calcined at 300° C. for 3 hours, and 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 that embodiment 3 obtains 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 until the catalyst is completely dispersed to obtain a uniform catalyst slurry. Pipette 0.2 mL of the catalyst slurry prepared above and spread it evenly on a 1 cm × 1 cm carbon paper, dry it, and use it as a working ele...

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Abstract

The invention discloses a covalent organic framework material catalyst based on loaded Ru nanoparticles as well as a preparation method and application of the catalyst. The preparation method of the catalyst comprises the following steps: fully mixing a benzene derivative, a pyridine derivative and a conductive carbon material to obtain a mixture A, putting the mixture A and a non-noble metal saltinto a tubular furnace, performing calcination at a high temperature in a nitrogen atmosphere, cleaning the calcined product with a hydrochloric acid solution and deionized water in sequence, and drying to obtain covalent organic framework carrier powder; and fully grinding the covalent organic framework carrier powder and ruthenium metal salt until the covalent organic framework carrier powder and the ruthenium metal salt are uniformly mixed, putting the mixture into a tubular furnace, carrying out high-temperature calcination in a nitrogen atmosphere, washing the calcined product with ultrapure water, and drying to obtain the covalent organic framework material catalyst based on the loaded Ru nanoparticles. The catalyst has the advantages of high specific surface area, large aperture, small ruthenium metal particles loaded on the covalent organic framework carrier powder, high dispersity, and very good catalytic activity when applied to electrochemical reduction of nitrogen for ammonia synthesis.

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 loaded Ru nanoparticles and its preparation method and application. 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 making nitrogen fertilizers and compound fertilizers. In order to improve the nitrogen conversion rate and improve the economics 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 catalysts with more stable chemical and thermodynamic properties and good economic benefits. Ammonia synthesis catalyst. Many catalysts have been discovered continuously in the research. Rod et al. were the first to use density functional theory to study low-temperature elec...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J37/08B01J37/06B01J35/10C25B1/00C25B11/06
CPCB01J31/1815B01J31/2234B01J37/086B01J37/06C25B1/00B01J2531/26C25B11/095B01J35/33B01J35/615B01J35/647
Inventor 庄桂林高旭王建国
Owner ZHEJIANG UNIV OF TECH
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