Preparation method of high-purity Fe5C2 nanoparticles and application of high-purity Fe5C2 nanoparticles in Fischer-Tropsch synthesis reaction

A nano-particle, high-purity technology, applied in the field of materials, can solve the problems of difficult operation, large amount of waste, restricting industrial production and application, etc., and achieve the effect of stable performance and high catalytic activity.

Active Publication Date: 2019-12-31
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, water is used as a solvent in the preparation process, and the used aqueous solution contains some incompletely reacted raw materials and soluble reaction products. This will inevitably increase the difficulty and cost of wastewater treatment in today's China, where environmental protection requirements are increasingly stringent.
In addition, long-chain amines are used as carbon sources. The principle is based on iron nanoparticles catalyzing the amino dehydrogenation of long-chain amines to generate cyanide or unsaturated hydrocarbons, so as to realize the carbonization of iron nanoparticles, and there is a problem of low raw material utilization.
[0009] In summary, the currently published methods for preparing Fe 5 C 2 Among the nanoparticle methods, the products obtained by the high-temperature solid-phase preparation method and the gas-solid phase carbonization method usually contain Fe 5 C 2 , Fe 3 C.Fe 2 C, or a variety of mixtures including oxides; and the liquid phase synthesis method has problems such as high cost, more waste, difficult operation, and cumbersome preparation methods, which limit its industrial production and application

Method used

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  • Preparation method of high-purity Fe5C2 nanoparticles and application of high-purity Fe5C2 nanoparticles in Fischer-Tropsch synthesis reaction
  • Preparation method of high-purity Fe5C2 nanoparticles and application of high-purity Fe5C2 nanoparticles in Fischer-Tropsch synthesis reaction
  • Preparation method of high-purity Fe5C2 nanoparticles and application of high-purity Fe5C2 nanoparticles in Fischer-Tropsch synthesis reaction

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Experimental program
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Effect test

Embodiment 1

[0041] 0.1g Fe 3 o 4 Particles (grain size 13nm) are placed in a fixed bed reactor, and a mixed gas of hydrogen and carbon monoxide is introduced, the volume ratio of hydrogen and carbon monoxide is 1:0.5, the flow rate of the mixed gas is 35ml / min, and the temperature is raised at 5°C / min to 400°C; control the temperature of the reaction system and keep it warm for 240 minutes; after the reaction system is cooled, enter an inert atmosphere containing 5% oxygen for passivation treatment for 15 minutes, and collect Fe 5 C 2 Nanoparticle products.

[0042] To the Fe prepared by above-mentioned embodiment 1 5 C 2 Nanoparticles for Characterization:

[0043] figure 1 For the Fe prepared in Example 1 5 C 2 Powder X-ray diffraction spectrum of nanoparticles. like figure 1 As shown, the obtained Fe 5 C 2 Diffraction peaks of nanoparticles and Fe 5 C 2 The standard card (ICDD: 03-065-6169) is completely consistent without any miscellaneous peaks, which proves that the ob...

Embodiment 2

[0045] 0.1g Fe 2 o 3 Particles (grain size 38nm) are placed in a fixed bed reactor, and a mixed gas of hydrogen and carbon monoxide is introduced, the volume ratio of hydrogen and carbon monoxide is 1:1, the flow rate of the mixed gas is 20ml / min, and the temperature is raised at 5°C / min to 350°C; control the temperature of the reaction system and keep it warm for 300 minutes; after the reaction system is cooled, pass through an inert atmosphere containing 5% oxygen for passivation treatment for 15 minutes, and collect Fe 5 C 2 Nanoparticle products.

[0046] For this example Fe 5 C 2 Nanoparticles are subjected to powder X-ray diffraction tests such as Figure 4 , this embodiment obtains high-purity Fe 5 C 2 For nanoparticles, the grain size obtained by calculating the half-peak width is 22nm.

Embodiment 3

[0048] Put 0.2g of FeO particles (grain size 28nm) in a fixed bed reactor, pass in a mixture of hydrogen and carbon monoxide, the ratio of hydrogen to carbon is 1:0.5, the flow rate is 50ml / min, and the temperature is raised to 300°C at 2°C / min ; control the temperature of the reaction system and keep it warm for 30 minutes; after the reaction system is cooled, feed into an inert atmosphere containing 5% oxygen to carry out passivation treatment for 15 minutes, and collect Fe 5 C 2 Nanoparticle products.

[0049] For this example Fe 5 C 2 Nanoparticles are tested by powder X-ray diffraction spectroscopy, such as Figure 5 , this embodiment obtains high-purity Fe 5 C 2 Nanoparticles, the grain size obtained by calculating the half peak width is 12nm.

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Abstract

The invention provides a preparation method of high-purity Fe5C2 nanoparticles and an application of the high-purity Fe5C2 nanoparticles in a Fischer-Tropsch synthesis reaction. The preparation of thehigh-purity Fe5C2 nanoparticles comprises the steps: conventional cheap iron oxide is used as a precursor, and reactive gas containing hydrogen and carbon monoxide is used for reducing and carburizing iron oxide; and based on the synergistic regulation and control of the size of the iron oxide precursor, the hydrogen-carbon ratio of the reaction gas in the carbonization process, the heating rate,the reaction temperature and the like, the iron oxide essentially has appropriate oxygen atom removal, carbon atom infiltration and carbon deposition process rate and degree in the reaction process,and the high-purity Fe5C2 nanoparticles are obtained. The Fe5C2 nanoparticles provided by the invention are applied to the Fischer-Tropsch synthesis reaction, and have high catalytic activity, high C2-C4 light olefin yield and high stability.

Description

technical field [0001] The invention belongs to the technical field of materials, in particular to a high-purity Fe 5 C 2 Preparation method of nanoparticles and application in Fischer-Tropsch synthesis reaction. [0002] technical background [0003] Iron carbide is an iron-carbon interstitial compound in which carbon atoms occupy the spaces between closely packed iron atoms. According to the positions occupied by carbon atoms in the crystal structure, they can be divided into triangular prism carbides (ε-Fe 2 C and ε′-Fe 2.2 C) and octahedral carbides (θ-Fe 3 C, χ-Fe 5 C 2 and Fe 7 C 3 ). The study found that Fe 5 C 2 With very obvious characteristics such as high magnetic saturation characteristics, good photothermal effect, stability and low toxicity, it has broad application prospects in the fields of magnetism, photoelectric catalysis, environmental purification and biomedicine. Fe 5 C 2 At the same time, it has chemical activity and can be used as a catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/914B01J27/22B01J35/02C10G2/00
CPCC01B32/914C10G2/332B01J27/22B01J35/023C01P2002/72C01P2006/80C01P2004/04
Inventor 陆安慧唐磊
Owner DALIAN UNIV OF TECH
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