Hydrothermal synthesis method for iron-based spinel with high-density oxygen vacancies

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

Inactive Publication Date: 2016-06-22
SHANGHAI INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Hydrothermal synthesis method for iron-based spinel with high-density oxygen vacancies
  • Hydrothermal synthesis method for iron-based spinel with high-density oxygen vacancies
  • Hydrothermal synthesis method for iron-based spinel with high-density oxygen vacancies

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Embodiment 1

[0030] (1) 2mmolFeCl 2 4H 2 O and 4mmolFe(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 2.4gNaOH, 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 diffraction ...

Embodiment 2

[0034] (1) 2mmolMnCl 2 4H 2 O and 4mmolFe(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 2.4gNaOH, 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 di...

Embodiment 3

[0038] (1) 2mmolNiCl 2 6H 2 O and 4mmolFe(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 2.4gNaOH, 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 in ...

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Abstract

The invention discloses a hydrothermal synthesis method for iron-based spinel with high-density oxygen vacancies. The method comprises the steps: firstly, dissolving MCl26H2O (M= Mn, Ni or Fe) and Fe(NO3)39H2O in ethylene glycol, carrying out intense stirring, and clarifying the solution; then, adding NaOH into the solution, and continuing to carry out stirring; then, subjecting the stirred solution to a hydrothermal reaction in a hydrothermal kettle, carrying out natural cooling, and carrying out washing and drying, thereby obtaining iron-based spinel nano-powder with high-density oxygen vacancies. The method has the beneficial effects that the preparation process is simple and convenient, the required equipment is simple, the method is environment-friendly, industrial production is easy to achieve, and the problem that the oxygen vacancies are difficult to reduce is solved fundamentally; the synthesized iron-based spinel has the high-density oxygen vacancies, so that the obtained product is of a pure phase. Under uniform conditions, the CO2 conversion ratio of the iron-based spinel with the high-density oxygen vacancies is increased by 80% or more relative to that of 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 Applications(China)
IPC IPC(8): C01G49/08C01G49/00C01G53/00B01J23/745B01J23/755B01J23/889C07C9/04C07C1/02B82Y30/00
CPCB01J23/005B01J23/745B01J23/755B01J23/8892B01J35/004B82Y30/00C01G49/0072C01G49/08C01G53/00C01P2002/32C01P2002/72C07C1/02C07C9/04
Inventor 刘志福刘林炎程遥赵喆
Owner SHANGHAI INST OF TECH
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