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a co 3 o 4 Preparation methods and applications of NP/CD/Co-MOF composites

A composite material, co-mof technology, applied in the fields of nanocomposite materials and electrocatalysis, can solve the problems of easy changes in the surrounding chemical environment, poor water stability of MOFs, poor chemical stability, etc.

Inactive Publication Date: 2021-07-30
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 triethylenediamine TED in 2 mL 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), made H 2 BDC solution;

[0039] TED solution, H 2 The BDC solution was blended, and 1.0 mL of lithium hydroxide aqueous solution with a mass fraction of 3.7% was added dropwise to obtain a ligand mixed solution;

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

[0041] Blend the ligand mixture and cobalt nitrate solution containing glucose, let stand at room temperature for 1 hour, centrifuge, wash with water and ethanol three times respectively, and prepare Co-MOF / glucose flaky microcrystals;

[0042] (2) Oxidation-pyrolysis of Co-MOF / g...

Embodiment 2

[0046] Example 2 A 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 N,N-dimethylformamide (DMF), made H 2 BDC solution;

[0050] TED solution, H 2 The BDC solution was blended, and 1.1 mL of lithium hydroxide aqueous solution with a mass fraction of 3.7% was added dropwise to obtain a ligand mixed solution;

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

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

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

Embodiment 3

[0057] Example 3 A kind of 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), made H 2 BDC solution;

[0061] TED solution, H 2 The BDC solution was blended, and 1.2 mL of lithium hydroxide aqueous solution with a mass fraction of 3.7% was added dropwise to obtain a ligand mixed solution;

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

[0063] Blend the ligand mixture solution and cobalt nitrate solution containing glucose, let stand at room temperature for 2 h, centrifuge, wash with water and ethanol three times respectively, and prepare Co-MOF / glucose flaky microcrystals;

[0064] (2) Oxidation-py...

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PUM

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Abstract

The invention discloses a Co 3 o 4 The preparation method of the NP / CD / Co-MOF composite material and the application of electrocatalysis based on the composite material belong to the technical fields of nano-catalysis, nano-materials and the like. The main steps are to prepare Co-MOF / glucose flaky microcrystals by reacting cobalt nitrate, glucose, triethylenediamine and terephthalic acid at room temperature; the microcrystals are oxidized-pyrolyzed under microwave radiation to obtain semiconductors co 3 o 4 Co-MOF composites co-doped with nanoparticles and carbon dots CD, that is, Co 3 o 4 NP / CD / Co‑MOF composites. The cost of raw materials used in the preparation of the composite material is low, the preparation process is simple, the reaction energy consumption is low, and the composite material has industrial application prospects. The catalyst is used for electrocatalytic nitrogen fixation into ammonia, and has good electrochemical activity.

Description

technical field [0001] The invention relates to a semiconductor Co 3 o 4 Co-MOF composites co-doped with nanoparticles and carbon dots CD, that is, Co 3 o 4 The preparation method of the NP / CD / Co-MOF composite material and the application of the composite material to electrocatalyze nitrogen fixation into ammonia belong to the technical field of nanocomposite materials and electrocatalysis. Background technique [0002] Ammonia is a vital chemical product in 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 attracted extensive 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 It is considered to be one of "the most important chemical reactions on earth", and its inventors, F. Haber and C. Bosch, also deservedly won the Nobel Pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J35/00B01J37/08B01J37/12B01J37/34C25B1/27C25B11/095
Inventor 童磊王志玲沈静
Owner UNIV OF JINAN