Preparation method and application of composite material based on bi-metal MOF nanometer crystals

A technology of composite materials and nanocrystals, applied in the field of nanocomposites and electrocatalysis, can solve the problems of reduced reaction pressure and difficulty in activation, and achieve the effects of high preparation efficiency, increased activity and high yield

Inactive Publication Date: 2019-04-19
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, industrially synthesized NH 3 It is realized by the Haber-Bosch method, which requires the use of iron-based catalysts, high temperature (350-550 ° C) and high pressure (150-350 atm) conditions, although the synthesis of NH 3 Great progress has been made in technology, for example, the daily production capacity of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 A kind of preparation method based on bimetallic MOF nanocrystalline composite material

[0034] (1) Preparation of CoCu-MOF nanocrystals

[0035] Co-dissolve 0.75 mmol of copper nitrate and 0.75 mmol of cobalt nitrate in 4 mL of water, and continue to add 0.8 g of polyvinylpyrrolidone to obtain a blue-purple clear copper nitrate-cobalt nitrate mixture;

[0036] Dissolve 1 mmol of 2,6-pyridinedicarboxylic acid and 2.0 mmol of sodium hydroxide in 4 mL of water to obtain a clear 2,6-pyridinedicarboxylate solution;

[0037] Add the 2,6-pyridinedicarboxylate solution to the copper nitrate-cobalt nitrate mixture, let it stand at room temperature for 2 hours, then filter it with suction and wash it with water for 3 times to prepare bimetallic MOF nanocrystals, that is, CoCu-MOF nanocrystals. crystal;

[0038] (2) Oxidation-pyrolysis of CoCu-MOF nanocrystals

[0039] The CoCu-MOF nanocrystals were placed in a tube furnace for oxidation-pyrolysis in an air atmos...

Embodiment 2

[0042] Embodiment 2 A kind of preparation method based on bimetallic MOF nanocrystalline composite material

[0043] (1) Preparation of CoCu-MOF nanocrystals

[0044] Co-dissolve 0.825 mmol of copper nitrate and 1.375 mmol of cobalt nitrate in 6 mL of water, and continue to add 0.85 g of polyvinylpyrrolidone to obtain a blue-purple clear copper nitrate-cobalt nitrate mixture;

[0045] Dissolve 1 mmol of 2,6-pyridinedicarboxylic acid and 2.3 mmol of sodium hydroxide in 6 mL of water to obtain a clear 2,6-pyridinedicarboxylate solution;

[0046] Add the 2,6-pyridinedicarboxylate solution to the copper nitrate-cobalt nitrate mixture, let it stand at room temperature for 2 hours, then filter it with suction and wash it with water for 3 times to prepare bimetallic MOF nanocrystals, that is, CoCu-MOF nanocrystals. crystal;

[0047] (2) Oxidation-pyrolysis of CoCu-MOF nanocrystals

[0048] The CoCu-MOF nanocrystals were placed in a tube furnace for oxidation-pyrolysis in an air at...

Embodiment 3

[0050] Embodiment 3 A kind of preparation method based on bimetallic MOF nanocrystalline composite material

[0051] (1) Preparation of CoCu-MOF nanocrystals

[0052] Co-dissolve 0.3 mmol of copper nitrate and 2.7 mmol of cobalt nitrate in 8 mL of water, and continue to add 0.9 g of polyvinylpyrrolidone to obtain a blue-purple clear copper nitrate-cobalt nitrate mixture;

[0053] Dissolve 1 mmol of 2,6-pyridinedicarboxylic acid and 2.5 mmol of sodium hydroxide in 8 mL of water to obtain a clear 2,6-pyridinedicarboxylate solution;

[0054] Add the 2,6-pyridinedicarboxylate solution to the copper nitrate-cobalt nitrate mixture, let it stand at room temperature for 2 hours, then filter it with suction and wash it with water for 3 times to prepare bimetallic MOF nanocrystals, that is, CoCu-MOF nanocrystals. crystal;

[0055] (2) Oxidation-pyrolysis of CoCu-MOF nanocrystals

[0056] The CoCu-MOF nanocrystals were placed in a tube furnace for oxidation-pyrolysis in an air atmosph...

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PUM

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Abstract

The invention discloses a preparation method of a semiconductor oxide nanometer particle doped carbon nitrogen/MOF nanometer composite material and application thereof to electrocatalysis nitrogen fixation, and belongs to the technical field of nanometer composite materials and electrocatalysis. The preparation method includes the steps that with 2,6-dipicolinic acid, copper nitrate and cobalt nitrate being raw materials, CuCo-MOF nanometer crystals are synthesized at room temperature and heated under the atmosphere of air to prepare the composite material. The raw materials used for preparinga catalyst are low in cost, the preparation technology is simple, reaction energy consumption is low, and industrialized application prospects are realized. The catalyst is used for efficient electrocatalysis nitrogen fixation, and has good electrochemical nitrogen fixation activity and electrochemical stability.

Description

technical field [0001] The invention relates to a preparation method based on a bimetallic MOF nanocrystalline composite material and an application of electrocatalytic nitrogen fixation based on the composite material, belonging to the technical fields of nanocomposite materials and electrocatalysis. Background technique [0002] NH 3 It is one of the most important chemicals at present, and its annual output ranks first among all kinds of chemicals, and our country is the first to synthesize NH 3 As a large industrial country, as a high-energy-consuming industry, the synthesis of NH 3 Industry consumes 1-2% of the global energy, NH 3 Its downstream products are mainly chemical fertilizers, and other important chemical products such as synthetic fibers, explosives, and industrial fuels. Currently, industrially synthesized NH 3 It is realized by the Haber-Bosch method, which requires the use of iron-based catalysts, high temperature (350-550 ° C) and high pressure (150-3...

Claims

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Application Information

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IPC IPC(8): B01J23/75C01C1/04
CPCB01J23/75B01J35/0033C01C1/0411Y02P20/52
Inventor 刘昭轩匡轩
Owner UNIV OF JINAN
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