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Preparation method and application of carbon-nitrogen-based iron cobalt oxide nanocluster MOF catalyst

A technology of carbon-nitrogen-based iron-cobalt and nano-clusters, which is applied in the field of nano-materials and catalysis, can solve the problems of reduced reaction pressure and difficulty in activation, and achieves the effects of high preparation efficiency, increased activity and high yield

Inactive Publication Date: 2019-04-26
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 a single set of equipment has increased from 30 tons to 2,500 tons, the reaction pressure of the equipment has also been greatly reduced, and the source of raw gas has also been diversified. However, N, which is the main component of air 2 , because the N≡N bond energy is too high (940.95 kJ / mol), it is difficult to activate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 A kind of preparation method of carbon-nitrogen-based iron-cobalt oxide nano-cluster MOF catalyst

[0031] Dissolve 1 mmol of ferric nitrate and 1 mmol of cobalt nitrate in 4 mL of water, and add 0.8 g of polyvinylpyrrolidone at the same time to obtain a purple-red clear mixture of ferric nitrate and cobalt nitrate; dissolve 1 mmol of 2,6-pyridinedicarboxylic acid Dissolve 2.0 mmol of sodium hydroxide in 4 mL of water to obtain a clear 2,6-pyridinedicarboxylic acid-base solution; add 2,6-pyridinedicarboxylate-base solution to the ferric nitrate-cobalt nitrate mixture, and let it stand at room temperature After standing for 2 hours, filter with suction, wash with water three times, and dry at 85°C to obtain a nanocluster composite material of Co-MOF nanosheets loaded with Fe(Ⅲ) ions, that is, FeCo-MOF nanoclusters;

[0032] The FeCo-MOF nanoclusters were placed in a tube furnace and heated in an air atmosphere at a heating rate of 3-5 °C / min, heated to 200 °...

Embodiment 2

[0034] Embodiment 2 A kind of preparation method of carbon-nitrogen-based iron-cobalt oxide nano-cluster MOF catalyst

[0035] 0.75 mmol of ferric nitrate and 1.25 mmol of cobalt nitrate were dissolved in 6 mL of water, and 0.85 g of polyvinylpyrrolidone was added to obtain a purple-red clear mixture of ferric nitrate and cobalt nitrate; 1 mmol of 2,6-pyridinedicarboxylate Acid and 2.2 mmol sodium hydroxide were dissolved in 6.0 mL of water to obtain a clear 2,6-pyridinedicarboxylic acid-base solution; 2,6-pyridinedicarboxylate-base solution was added to the ferric nitrate-cobalt nitrate mixture, at room temperature After standing for 2 hours, filter with suction, wash with water 3 times, and dry at 85°C to obtain a nanocluster composite material of Co-MOF nanosheets loaded with Fe(Ⅲ) ions, that is, FeCo-MOF nanoclusters;

[0036] The FeCo-MOF nanoclusters were placed in a tube furnace and heated in an air atmosphere at a heating rate of 4 °C / min, heated to 250 °C, kept for 2 ...

Embodiment 3

[0038] Embodiment 3 A kind of preparation method of carbon-nitrogen-based iron-cobalt oxide nano-cluster MOF catalyst

[0039] Dissolve 0.2 mmol of ferric nitrate and 1.8 mmol of cobalt nitrate in 8 mL of water, and add 0.9 g of polyvinylpyrrolidone at the same time to obtain a purple-red clear mixture of ferric nitrate and cobalt nitrate; 1 mmol of 2,6-pyridinedicarboxylic acid Dissolve 2.5 mmol sodium hydroxide in 8 mL water to obtain a clear 2,6-pyridinedicarboxylic acid-base solution; add 2,6-pyridinedicarboxylate-base solution to the ferric nitrate-cobalt nitrate mixture, and let it stand at room temperature After standing for 2 hours, filter with suction, wash with water for 3 times, and dry at 85°C to obtain a nanocluster composite material of Co-MOF nanosheets loaded with Fe(Ⅲ) ions, that is, FeCo-MOF nanoclusters;

[0040] The FeCo-MOF nanoclusters were placed in a tube furnace and heated in an air atmosphere at a heating rate of 3-5 °C / min, heated to 300 °C, kept for...

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Abstract

The invention discloses a preparation method of a carbon-nitrogen-based iron cobalt oxide nanocluster MOF catalyst and application of the catalyst in electrocatalytic nitrogen fixation, and belongs tothe fields of nanomaterials, catalytic technologies and the like. The preparation method comprises the following main steps: taking 2,6-dipicolinic acid, iron nitrate and cobalt nitrate as raw materials, and blending at room temperature to prepare FeCo-MOF nanoclusters; heating the FeCo-MOF nanoclusters in air atmosphere to obtain the carbon-nitrogen-based iron cobalt oxide nanocluster MOF catalyst. The raw materials for preparing the catalyst are low in cost; the preparation method has the advantages of simple preparation process, low reaction energy consumption and industrial application prospect. The catalyst is used for high-efficiency electrocatalytic nitrogen fixation and has good electrochemical nitrogen fixation activity.

Description

technical field [0001] The invention relates to a preparation method of a carbon-nitrogen-based iron-cobalt oxide nano-cluster MOF catalyst and the application of electrocatalytic nitrogen fixation based on the catalyst, belonging to the fields of nanomaterials, catalytic technology and the like. 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 (150-350 at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J35/10C25B1/00C25B11/06
CPCC25B1/00B01J31/28C25B11/095B01J35/33B01J35/61Y02P20/10
Inventor 刘昭轩匡轩
Owner UNIV OF JINAN
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