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A kind of ferrous disulfide and its preparation method using mof as precursor

A ferrous disulfide, precursor technology, used in the preparation/purification of iron sulfide, carbon, secondary batteries, etc., can solve problems such as poor conductivity restricting the development of electrode materials, and achieve good electrochemical performance, pore structure and conductivity. The effect of adjustable resistance and improved cycle life

Active Publication Date: 2022-03-18
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Ferrous disulfide has an ultra-high theoretical specific capacity, but the poor conductivity of the material itself limits its development as an electrode material

Method used

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  • A kind of ferrous disulfide and its preparation method using mof as precursor
  • A kind of ferrous disulfide and its preparation method using mof as precursor
  • A kind of ferrous disulfide and its preparation method using mof as precursor

Examples

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preparation example Construction

[0033] A kind of preparation method of ferrous disulfide taking MOF as template, concrete steps are as follows:

[0034] Step 1: Dissolve the iron salt, carbon source and precipitant in deionized water according to the molar ratio of Fe, carbon source and precipitant as 1:1.5~2:1.6~2, stir evenly, and then disperse a certain molar amount Put the agent into the uniformly stirred solution, stir and mix evenly, transfer the solution to the reaction kettle, and keep it warm at 160-180°C for 12h. Then the obtained black suspension was centrifuged and washed with deionized water and ethanol to obtain a black powder, which was dried in a vacuum oven at 60° C. for 8-12 hours to obtain an iron-based precursor.

[0035] Step 2: According to the molar ratio of iron and carboxylic acid as 2:1, dissolve the iron-based precursor and carboxylic acid obtained in step 1 in DMF, transfer the prepared solution to the reaction kettle, and keep it warm at 110-120°C After 16-20 hours, fully wash w...

Embodiment 1

[0041] Step 1: Dissolve 0.0082mol ferric chloride hexahydrate, 0.0131mol urea, and 0.0123mol sodium citrate in 100mL deionized water, place on a magnetic stirrer and stir for 30 minutes until fully dissolved, then add 0.6g PVP and stir for 1 hour, after completely dissolving The solution was transferred to a reaction kettle and kept in an oven at 180°C for 12h. Then the obtained black suspension was centrifuged and washed with deionized water and ethanol to obtain a black powder, which was dried in a vacuum oven at 60° C. for 12 hours to obtain an iron-based precursor.

[0042] Step 2: Dissolve 0.004mol of iron-based precursor and 0.002mol of terephthalic acid in 120mL of N,N-dimethylformamide (DMF), stir until dissolved and transfer to the reaction kettle, the oven condition is 110°C , 20h, after the material was taken out, it was fully washed with deionized water and absolute ethanol, and then dried in a vacuum oven at 150°C for 8h to obtain orange MIL-101-Fe.

[0043] Step...

Embodiment 2

[0046] Similar to Example 1, the difference is that the vulcanization temperature in step 3 is changed to 500°C, and the scanning electron microscope characterization is as follows image 3 As shown, the diameter of the particles is about 5 μm.

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Abstract

The invention belongs to the field of material preparation, and in particular relates to ferrous disulfide with MOF as a precursor and a preparation method thereof. The structure of ferrous sulfide is MOF type, and there is a carbon coating on the surface of the material; the specific steps of the preparation method are as follows: step (1): dissolving iron salt, carbon source, precipitant and dispersant etc. in In a solvent, heat it in an oven for a certain period of time to obtain an Fe-based precursor; step (2): dissolve the Fe-based precursor and carboxylic acid obtained in step (1) in proportion to the solvent, and heat it in an oven to obtain Fe -MOF precursor; step (3): the Fe-MOF precursor and sulfur powder obtained in step (2) are calcined in proportion under an inert atmosphere to obtain MOF-type iron disulfide coated with carbon on the surface. The method of the invention can regulate the particle size and pore structure of the precursor. The FeS2 prepared by the invention is applied to the negative electrode material of the sodium ion battery, effectively improves the cycle life of the battery, and has good electrochemical performance.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to ferrous disulfide with MOF as a precursor and a preparation method thereof. Background technique [0002] Metal-organic frameworks (MOFs) usually refer to organic groups that form a framework, inorganic metal nodes or metal cluster secondary building units as connection points, and are formed by coordination and self-assembly under hydrothermal or solvothermal conditions. Highly regular crystalline material. Other types of interactions, such as hydrogen bonding and van der Waals forces, may also play a role in forming the three-dimensional structure of MOFs. At present, scientists have discovered more than 20,000 kinds of MOFs materials. Because its structure is similar to that of zeolite and its skeleton is relatively soft, it is also called "soft zeolite". [0003] MOF materials have a large specific surface area, rich in pores and exposed active sites inside,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/12C01B32/05H01M4/58H01M4/62H01M10/054
CPCC01G49/12C01B32/05H01M4/5815H01M4/625H01M10/054C01P2004/03C01P2002/72C01P2006/40C01P2004/80C01P2004/61Y02E60/10
Inventor 邱红岳继礼路遥蒋鑫施正旖
Owner NANJING UNIV OF SCI & TECH
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