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Iron carbide particle, and fabrication method and application thereof

A technology of iron carbide and particles, which is applied in the field of materials, can solve the problems of high energy consumption in synthesis methods, impossibility of industrial production, and complicated preparation methods, and achieve good selectivity, mass production, and high catalytic activity.

Active Publication Date: 2013-04-10
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In summary, the iron carbide prepared by the disclosed method is a variety of iron carbides (such as Fe 5 C 2 , Fe 7 C 3 , Fe 2.2 C.Fe 3 C) mixture, large size, uncontrollable shape, and the synthesis method has high energy consumption, cumbersome preparation method, and cannot be industrialized, which greatly limits its application in Fischer-Tropsch synthesis

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  • Iron carbide particle, and fabrication method and application thereof
  • Iron carbide particle, and fabrication method and application thereof
  • Iron carbide particle, and fabrication method and application thereof

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preparation example Construction

[0044] In the preparation method of the present invention, halide ammonium salt is selected as the carbonization inducer, and the halide ammonium salt is selected from ammonium halide or organic quaternary ammonium salt, or a mixture of two or more thereof. As non-limiting examples, ammonium halides such as ammonium fluoride, ammonium chloride, ammonium bromide, and ammonium iodide, while the organic quaternary ammonium salts may include: cetyltrimethylammonium bromide (CTAB) or Cetyltrimethylammonium chloride (CTAC), etc.

[0045] The present invention selects long-chain amine as the carbon source and solvent of the high-temperature liquid phase reaction at the same time, requiring the boiling point of the long-chain amine used to be higher than 250°C, for example, it can be selected from dodecylamine, hexadecylamine, octadecylamine, etc. One or more of amine, oleylamine, octadecyl tertiary amine and trioctylamine. The combination of the halide ammonium salt inducer and the ...

Embodiment 1

[0060] The present embodiment has prepared iron carbide particle, comprises the following steps:

[0061] (1) Mix 0.113g of cetyltrimethylammonium bromide (CTAB) and 20ml of cetylamine in a container to obtain a mixed solution, heat to 120°C and maintain a vacuum for 0.5 hours;

[0062] (2) Under a nitrogen protective atmosphere, heat the mixed solution to 180°C, add 0.5ml carbonyl iron, and maintain the temperature for 30 minutes;

[0063] (3) Heat up to 320°C at a heating rate of 5°C / min, and hold for 10 minutes;

[0064] (4) Cool the reaction system to 60°C and centrifuge at a speed of 11,500 rpm for 1 minute, collect the precipitate, wash the precipitate three times with n-hexane and absolute ethanol in sequence, and collect iron carbide particles by centrifugation.

[0065] Characterization of the above-mentioned iron carbide particles:

[0066] figure 1 For the powder diffraction pattern of the iron carbide particles prepared in embodiment 1; figure 2 Among them, a ...

Embodiment 2

[0075] The present embodiment has prepared iron carbide particle, comprises the following steps:

[0076] (1) Mix 0.113g of cetyltrimethylammonium bromide (CTAB) and 20ml of cetylamine in a container to obtain a mixed solution, heat to 120°C and maintain a vacuum for 0.5 hours.

[0077] (2) Under a helium protective atmosphere, heat the mixed solution to 180°C, add 3ml of iron pentacarbonyl in n-hexane solution (including 0.5ml of pentacarbonyl iron and 2.5ml of n-hexane) to the mixed solution, and maintain the temperature Keep warm for 30 minutes;

[0078] (3) Heat up to 320°C at a heating rate of 5°C / min, and hold for 10 minutes;

[0079] (4) After the reaction system is cooled to room temperature, solid-liquid centrifugation is carried out, and the solid obtained by solid-liquid separation is washed three times with non-polar solvent n-hexane and polar solvent anhydrous ethanol in sequence, and centrifuged to obtain iron carbide particles.

[0080] Dissolving the metal pr...

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Abstract

The invention provides an iron carbide particle, and a fabrication method and an application thereof. Iron carbide is a nanoparticle taking Fe5C2 as a main component, and a particle size is 1-100nm. The fabrication method of the iron carbide particle comprises the following steps that a carbonization inductive agent and a solvent are mixed to form a mixed solution, a mole ratio of the carbonization inductive agent to the solvent is 1:(100-600), the carbonization inductive agent is halogenated ammonium salt, and the solvent is a long-chain amine solvent with a boiling point greater than 250 DEG C; a zero-valent iron organic compound is added to the mixed solution which is heated to 180-200 DEG C in a protective atmosphere; a reaction system is controlled at 250-380 DEG C for 10-120min; solid-liquid separation is performed after the reaction system is cooled; and the iron carbide particle product is collected. The iron carbide particle takes Fe5C2 as a major phase, is in a nanoparticle shape, can show higher catalytic activity, and is particularly applicable to catalysis of fischer-tropsch synthesis.

Description

technical field [0001] The invention relates to material technology, in particular to an iron carbide particle, its preparation method and application. Background technique [0002] Iron carbide belongs to the intermetallic filling compound, which is formed by filling the interstitial gap of single iron iron lattice with carbon atoms, and tends to form a non-measured interstitial compound whose composition can be changed within a certain range. In recent years, due to the unique physical, chemical and structural properties, iron carbide materials have been widely used in the fields of optics, electronics, magnetism and biomedicine, and iron carbide materials as catalysts in many organic synthesis techniques have shown Catalytic activity and selectivity are of particular interest, typically the catalytic properties of iron carbide in Fischer-Tropsch synthesis. Iron-based catalysts are commonly used in the current implementation of Fischer-Tropsch synthesis technology. Althou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/30B82Y30/00C01B32/914
Inventor 侯仰龙杨策
Owner PEKING UNIV
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