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Preparation method and application of Co3O4 NP/CD/Co-MOF composite material

A composite material, co-mof technology, applied in the fields of electrocatalysis and nanocomposite materials, can solve the problems of easy changes in the surrounding chemical environment, poor water stability of MOFs, loss of material stability, etc., to achieve high product preparation efficiency and easy industrialization. , the effect of increasing the reduction to ammonia activity

Inactive Publication Date: 2019-05-17
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, MOFs still generally have defects such as poor water stability and poor chemical stability. The easy change of the surrounding chemical environment of the metal / metal coordination center in the MOFs framework structure is the direct cause of the loss of stability of the material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 A kind of Co 3 O 4 Preparation method of NP / CD / Co-MOF composite material

[0036] (1) Preparation of Co-MOF / glucose microcrystals

[0037] Dissolve 0.9 mmol of triethylenediamine TED in 2 mL of absolute ethanol to prepare a TED solution;

[0038] Take 1.8 mmol terephthalic acid H 2 BDC, dissolved in 6 mL N, N-dimethylformamide (DMF), to obtain H 2 BDC solution;

[0039] Put the TED solution, H 2 Blend the BDC solution and add 1.0 mL of a 3.7% lithium hydroxide aqueous solution dropwise to prepare a ligand mixture;

[0040] Dissolve 2.0 mmol of cobalt nitrate and 1.5 mmol of glucose in 8 mL of DMF solution to prepare a glucose-containing cobalt nitrate solution;

[0041] Blend the ligand mixture with the glucose-containing cobalt nitrate solution, stand at room temperature for 1 hour, centrifuge, and wash with water and ethanol 3 times to prepare Co-MOF / glucose flake crystallites;

[0042] (2) Oxidation-pyrolysis of Co-MOF / glucose flake crystallites

[0043] The Co-MOF / glu...

Embodiment 2

[0046] Example 2 A kind of Co 3 O 4 Preparation method of NP / CD / Co-MOF composite material

[0047] (1) Preparation of Co-MOF / glucose microcrystals

[0048] Dissolve 1.0 mmol of triethylenediamine TED in 2.5 mL of absolute ethanol to prepare a TED solution;

[0049] Take 2.0 mmol terephthalic acid H 2 BDC, dissolved in 7 mL of N,N-dimethylformamide (DMF) to obtain H 2 BDC solution;

[0050] Put the TED solution, H 2 The BDC solution is blended, and 1.1 mL of lithium hydroxide aqueous solution with a mass fraction of 3.7% is added dropwise to prepare a ligand mixture;

[0051] Dissolve 2.1 mmol of cobalt nitrate and 1.6 mmol of glucose in 9 mL of DMF solution to prepare a glucose-containing cobalt nitrate solution;

[0052] Blend the ligand mixture with the glucose-containing cobalt nitrate solution, stand at room temperature for 1.5 h, centrifuge, and wash with water and ethanol 3 times to prepare Co-MOF / glucose flake crystallites;

[0053] (2) Oxidation-pyrolysis of Co-MOF / glucose flake ...

Embodiment 3

[0057] Example 3 One Co 3 O 4 Preparation method of NP / CD / Co-MOF composite material

[0058] (1) Preparation of Co-MOF / glucose microcrystals

[0059] Dissolve 1.1 mmol of triethylenediamine TED in 3 mL of absolute ethanol to prepare a TED solution;

[0060] Take 2.2 mmol terephthalic acid H 2 BDC, dissolved in 8 mL N, N-dimethylformamide (DMF), to obtain H 2 BDC solution;

[0061] Put the TED solution, H 2 The BDC solution is blended, and 1.2 mL of lithium hydroxide aqueous solution with a mass fraction of 3.7% is added dropwise to prepare a ligand mixture;

[0062] Dissolve 2.3 mmol of cobalt nitrate and 1.7 mmol of glucose in 10 mL of DMF solution to prepare a glucose-containing cobalt nitrate solution;

[0063] Blend the ligand mixture with the glucose-containing cobalt nitrate solution, stand for 2 h at room temperature, centrifuge, and wash with water and ethanol 3 times to prepare Co-MOF / glucose flake crystallites;

[0064] (2) Oxidation-pyrolysis of Co-MOF / glucose flake crystallit...

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Abstract

The invention discloses a preparation method of aCo3O4NP / CD / Co-MOF composite material and application of electrocatalysis based on the composite material, and belongs to the technical fields of nanocatalysis, nanomaterials and the like. The preparation method mainly comprises the following steps: reacting cobalt nitrate, glucose, triethylene diamine and terephthalic acid at room temperature to obtain Co-MOF / glucose flaky microcrystals; performing oxidation and pyrolysis on the microcrystals under microwave irradiation to obtain a Co-MOF composite material with semiconductor Co3O4 nanoparticlesand carbon dot CD which are co-doped, namely, the Co3O4 NP / CD / Co-MOF composite material. The composite material has the advantages of low raw material cost for preparation, simple preparation process, low reaction energy consumption and industrial application prospect. The catalyst has high electrochemical activity for the electrocatalytic nitrogen fixation to form ammonia.

Description

Technical field [0001] The present invention relates to a semiconductor Co 3 O 4 Nanoparticles and carbon dots CD co-doped Co-MOF composite material, namely Co 3 O 4 The preparation method of the NP / CD / Co-MOF composite material and the application of the composite material for electrocatalytic nitrogen fixation into ammonia belong to the technical field of nanocomposite materials and electrocatalysis. Background technique [0002] Ammonia is a very important chemical product for human society and is widely used in the production of fertilizers, pharmaceuticals, dyes, etc. At the same time, because of its strong hydrogen content and high energy density, it has also received widespread attention as an alternative energy carrier in order to promote the development of a low-carbon society. Therefore, N 2 And H 2 Catalytic synthesis of NH 3 Considered to be one of the "most important chemical reactions on earth", its inventors F. Haber and C. Bosch also deservedly won the Nobel Prize...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J35/00B01J37/08B01J37/12B01J37/34C25B1/00C25B11/06
Inventor 童磊王志玲沈静
Owner UNIV OF JINAN
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