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Preparation method of ferriferrous oxide@nitrogen doped carbon compound

A technology of ferroferric oxide and nitrogen-doped carbon, which is applied in the direction of ferric oxide, iron oxide/iron hydroxide, etc., can solve the problems of low degree of carbonization of activated carbon and the inability to control the thickness of the carbon coating layer, etc. Achieve high degree of carbonization and improve electrical conductivity

Inactive Publication Date: 2016-01-20
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Su et al. (J.Mater.Chem.A, 2014, 2, 7281-7287) used a one-step hydrothermal method to prepare ferric oxide nitrogen-doped carbon composites, but the degree of carbonization of activated carbon was not high
Meng et al. (NanoEnergy, 2014, 8, 133-140) obtained iron ferric oxide nitrogen-doped carbon composites by carbonizing nitrogen-containing metal organic framework compounds, but the thickness of the carbon coating layer could not be adjusted
Therefore, the preparation of composites with good binding force between ferroferric oxide and nitrogen-doped carbon, high degree of carbonization of nitrogen-doped carbon and controllable thickness remains to be explored

Method used

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  • Preparation method of ferriferrous oxide@nitrogen doped carbon compound
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  • Preparation method of ferriferrous oxide@nitrogen doped carbon compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Mix analytically pure aniline with a volume ratio of 0.5:1 and hydrochloric acid with a concentration of 0.01mol / L to prepare aniline hydrochloric acid solution.

[0020] (2) Under room temperature and mechanical stirring conditions, add ferric oxide and distilled water into a mechanical stirrer and stir, and disperse ferric oxide in distilled water to prepare a ferric oxide solution with a mass concentration of 10 mg / mL.

[0021] (3) After stirring for 40 minutes, add 1 mL of the aniline hydrochloric acid solution obtained in step (1) to 10 mL of the ferric oxide solution obtained in step (2), and stir mechanically for 40 minutes.

[0022] (4) Add 1 mL of 30% hydrogen peroxide dropwise to the solution obtained in step (3), stir and react for 12 hours, magnetically separate, wash the precipitate with water, and dry at 60°C for 24 hours to obtain trioxide Iron polyaniline nanoparticles.

[0023] (5) Using a high temperature of 900 ° C, the polyaniline nanoparticles ...

Embodiment 2

[0025] (1) Mix analytically pure aniline with a volume ratio of 2:3 and hydrochloric acid with a concentration of 0.01mol / L to prepare aniline hydrochloric acid solution.

[0026] (2) Under room temperature and mechanical stirring conditions, add ferric oxide and distilled water into a mechanical stirrer and stir, and disperse ferric oxide in distilled water to prepare a ferric oxide solution with a mass concentration of 5 mg / mL.

[0027] (3) After stirring for 30 minutes, add 1 mL of the aniline hydrochloric acid solution obtained in step (1) to 10 mL of the ferric oxide solution obtained in step (2), and stir mechanically for 40 minutes.

[0028] (4) Add 3 mL of 30% hydrogen peroxide dropwise to the solution obtained in step (3), stir and react for 12 hours, magnetically separate, wash the precipitate with water, and dry at 60°C for 24 hours to obtain trioxide Iron polyaniline nanoparticles.

[0029] (5) Using a high temperature of 800 ° C, the carbonization step (4) obtain...

Embodiment 3

[0031] (1) Mix analytically pure aniline with a volume ratio of 4:1 and phosphoric acid with a concentration of 0.01mol / L to prepare aniline phosphoric acid solution.

[0032] (2) Under room temperature and mechanical stirring conditions, add ferric oxide and distilled water into a mechanical stirrer and stir, disperse ferric oxide in distilled water, and prepare ferric oxide solution with a mass concentration of 8mg / mL.

[0033] (3) After stirring for 35 minutes, add 1 mL of the aniline phosphoric acid solution obtained in step (1) to 10 mL of the ferric oxide solution obtained in step (2), and stir mechanically for 40 minutes.

[0034] (4) Add 3 mL of 30% hydrogen peroxide dropwise to the solution obtained in step (3), stir and react for 24 hours, magnetically separate, wash the precipitate with water, and dry at 60°C for 24 hours to obtain trioxide Iron polyaniline nanoparticles.

[0035] (5) Using a high temperature of 700°C, carbonizing the ferric iron tetroxide polyanil...

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Abstract

The invention discloses a preparation method of a ferriferrous oxide@nitrogen doped carbon compound. The preparation method comprises the following steps: 1, mixing analytically pure aniline with 0.01mol / L of an inorganic acid to prepare an aniline-inorganic solution; 2, using ferriferrous oxide and distilled water to prepare a ferriferrous oxide solution with the mass concentration of 5-20mg / mL; 3, adding the aniline-inorganic solution into the ferriferrous oxide solution; 4, adding hydrogen peroxide with the mass percentage of 30% into the solution obtained in step 3 in a dropwise manner, reacting for 5-24h, carrying out magnetic separation, washing the obtained precipitate with water, and drying to prepare ferriferrous oxide@polyaniline nanoparticles; and 5, carrying out high temperature carbonization on the ferriferrous oxide@polyaniline nanoparticles obtained in step 4, and annealing in N2 atmosphere for 3-5h to prepare the ferriferrous oxide@nitrogen doped carbon compound. The ferriferrous oxide@nitrogen doped carbon compound prepared in the invention has the advantages of strong binding force, high carbonization degree, controllable thickness, and improvement of the conductivity of nitrogen doped carbon.

Description

technical field [0001] The invention relates to a preparation method of ferric iron tetroxide nitrogen-doped carbon compound. Background technique [0002] Ferroferric oxide is a kind of abundant, non-toxic and cheap magnetic transition metal oxide, which has been widely used in lithium-ion batteries, supercapacitors, catalysis, drug carriers and so on. However, the low conductivity of ferroferric oxide and its instability in acidic conditions severely limit its application. Combination with carbon materials is beneficial to improve the conductivity and stability of ferroferric oxide (J.Mater.Chem., 2009, 19, 2710-2714; Electrochim.Acta, 2013, 114, 674-680; J.Mater.Chem. A,2015,3,7036-7043; Chinese invention patent, CN103417974A). [0003] Carbon materials include graphene, carbon nanotubes, activated carbon, and the like. Due to the high price of graphene and carbon nanotubes, activated carbon with low cost and abundant sources has been widely used. Nitrogen doping of c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 罗志虹罗鲲
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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