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A hydrothermal synthesis method of iron-based spinel with high density of oxygen vacancies

A technology of hydrothermal synthesis and oxygen vacancy, applied in the directions of iron compounds, chemical instruments and methods, iron oxide/iron hydroxide, etc., to achieve the effects of simple synthesis process, high selectivity and short synthesis period

Inactive Publication Date: 2017-06-27
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the deficiencies of the prior art, the object of the present invention is to provide a method for hydrothermal synthesis of iron-based spinel with high-density oxygen vacancies, which is effective and simple, and aims to solve the problem of low oxygen vacancy density and reduced oxygen Improve the catalytic efficiency of products and expand the applicable fields of nanomaterials

Method used

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  • A hydrothermal synthesis method of iron-based spinel with high density of oxygen vacancies
  • A hydrothermal synthesis method of iron-based spinel with high density of oxygen vacancies
  • A hydrothermal synthesis method of iron-based spinel with high density of oxygen vacancies

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Effect test

Embodiment 1

[0030] (1) 2mmol FeCl 2 4H 2 O and 4mmol Fe(NO 3 ) 3 9H 2 After O is mixed, dissolve in a certain volume of ethylene glycol, and stir vigorously for 30 minutes at a speed of 800 r / min to make the solution clear. Then add 2.4g NaOH, continue to stir until the solution is clear again; the FeCl 2 6H 2 O, Fe(NO 3 ) 3 9H 2 Both O and NaOH are analytically pure;

[0031] (2) Place the mixed solution obtained after mixing in step (1) in a hydrothermal kettle, and control the temperature to 200° C. to react for 10 hours to obtain a reaction product;

[0032] (3) After the reaction product is naturally cooled, it is centrifugally filtered, and the obtained product is washed 3-5 times with deionized water, and then washed 2 times with absolute ethanol, and then the product is dried in an oven at a temperature of 60° C. for 6 hours to obtain Ferrous spinel with a high density of oxygen vacancies (FeFe 2 o 4 ) Black nanopowder of nanopowder. figure 1 It is the X-ray diffracti...

Embodiment 2

[0034] (1) 2mmol MnCl 2 4H 2 O and 4mmol Fe(NO 3 ) 3 9H 2 After O is mixed, dissolve in a certain volume of ethylene glycol, and stir vigorously for 30 minutes at a speed of 800 r / min to make the solution clear. Then add 2.4g NaOH, continue to stir until the solution is clear again; the MnCl 2 6H 2 O, Fe(NO 3 ) 3 9H 2 Both O and NaOH are analytically pure;

[0035] (2) Place the mixed solution obtained after mixing in step (1) in a hydrothermal kettle, and control the temperature to 200° C. to react for 10 hours to obtain a reaction product;

[0036](3) After the reaction product is naturally cooled, it is centrifugally filtered, and the obtained product is washed 3-5 times with deionized water, and then washed 2 times with absolute ethanol, and then the product is dried in an oven at a temperature of 60° C. for 6 hours to obtain Manganese ferrite spinel with a high density of oxygen vacancies (MnFe 2 o 4 ) Black nanopowder of nanopowder. figure 2 It is the X-ray...

Embodiment 3

[0038] (1) 2mmol NiCl 2 6H 2 O and 4mmol Fe(NO 3 ) 3 9H 2 After O is mixed, dissolve in a certain volume of ethylene glycol, and stir vigorously for 30 minutes at a speed of 800 r / min to make the solution clear. Then add 2.4g NaOH, continue to stir until the solution is clear again; the NiCl 2 6H 2 O, Fe(NO 3 ) 3 9H 2 Both O and NaOH are analytically pure;

[0039] (2) Place the mixed solution obtained after mixing in step (1) in a hydrothermal kettle, and control the temperature to 200° C. to react for 10 hours to obtain a reaction product;

[0040] (3) After the reaction product is naturally cooled, it is centrifugally filtered, and the obtained product is washed 3-5 times with deionized water, and then washed 2 times with absolute ethanol, and then the product is dried in an oven at a temperature of 60° C. for 6 hours to obtain Nickel ferrite spinel (NiFe 2 o 4 ) Black nanopowder of nanopowder.

[0041] image 3 It is the XRD of the iron-based spinel prepared ...

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Abstract

The invention discloses a hydrothermal synthesis method of iron-based spinel with high-density oxygen vacancies. First, dissolve MCl26H2O (M=Mn, Ni or Fe) and Fe(NO3)39H2O in ethylene glycol and stir vigorously to clarify the solution. Add more NaOH and continue stirring. Then, the stirred solution is hydrothermally reacted in a hydrothermal kettle, cooled naturally, washed and dried to obtain iron-based spinel nanopowder with high-density oxygen vacancies. The beneficial effects of the present invention are: the preparation process is simple, the required equipment is simple, the environment is friendly, it is easy to realize industrial production, and it fundamentally solves the problem of difficult reduction of oxygen vacancies; the synthesized iron-based spinel has its own high-density oxygen vacancies, and the obtained The product is pure phase. Under the same conditions, its CO2 conversion rate is more than 80% higher than that of a single corresponding iron-based spinel.

Description

technical field [0001] The invention relates to a hydrothermal synthesis method and application of iron-based spinel with high-density oxygen vacancies, and belongs to the technical field of nanometer catalysis. Background technique [0002] With the rapid development of the world economy, energy shortage and environmental pollution have become serious problems faced by all countries in the world. Therefore, it is imperative to develop clean and pollution-free renewable energy. my country is currently a CO 2 The country with the largest emitter is under increasing pressure from the international community. Using solar energy as an energy source, the CO 2 and H 2 O is directly converted into hydrocarbon fuels, which can reduce CO in the atmosphere 2 Concentration, and can convert solar energy into high-energy fuels that are easy to store and transport. 2 resources are of great significance. Artificial solar energy conversion to CO 2 There are many ways such as photoca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08C01G49/00C01G53/00B01J23/745B01J23/755B01J23/889C07C9/04C07C1/02B82Y30/00
CPCB82Y30/00C01G49/0072C01G49/08C01G53/00C07C1/02B01J23/005B01J23/745B01J23/755B01J23/8892C01P2002/72C01P2002/32B01J35/39C07C9/04
Inventor 刘志福刘林炎程遥赵喆
Owner SHANGHAI INST OF TECH
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