Preparation method of metal-organic framework compound and application thereof

A metal-organic framework and compound technology, which is used in the application field of metal-organic framework compounds and the preparation of cobalt selenide/graphite carbon composite materials, can solve the problems of poor stability during use, insufficient overall distribution, and inability to form homogeneous distribution. , to achieve the effect of uniform size, simple and feasible preparation process, and no deterioration of lithium storage performance

Inactive Publication Date: 2019-03-19
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, the preparation of cobalt selenide/graphite carbon composites still has low output, low crystallinity, inability to form a homogeneous distribution, large skeleton, uneven overall distri

Method used

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  • Preparation method of metal-organic framework compound and application thereof
  • Preparation method of metal-organic framework compound and application thereof
  • Preparation method of metal-organic framework compound and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Preparation of polyhedral metal organic framework compound ZIF-67

[0025] Weigh 4.9mmol Co(NO 3 ) 2 ·6H 2 O and 39.5mmol 2-methylimidazole were dissolved in 100ml methanol respectively, and the stirring speed was set to be 350r / min. After stirring and dissolving completely, the Co(NO 3 ) 2 · 6H 2 The O solution was poured into the 2-methylimidazole solution, stirred for 12 minutes, aged at room temperature for 20 hours after the stirring was stopped, and the product was centrifuged at a speed of 15000 r / min, and the centrifugation time was 5 minutes. After centrifugation, the precipitate was washed with methanol for 3 times. The amount of methanol used was 25 times the mass of the precipitate, and then placed in vacuum at 60°C for 12 hours. The resulting product was the polyhedral metal-organic framework compound ZIF-67.

Embodiment 2

[0026] Example 2: Preparation of cobalt selenide / graphite carbon composite based on MOFs template

[0027] Mix the polyhedral metal-organic framework compound ZIF-67 prepared in Example 1 with Se powder at a mass ratio of 1:1, mix evenly with a mortar, and then place it in a tube furnace under an argon atmosphere to raise the temperature The temperature was raised from room temperature to 800°C at a rate of 5°C / min, and kept at 800°C for 4 hours to obtain a cobalt selenide / graphite carbon composite material.

[0028] Experimental result shows: the cobalt selenide / graphitic carbon composite material that the present invention prepares has excellent lithium storage performance, at 100mA g -1 After 50 charge-discharge cycles at the current density, the discharge capacity is 849.12mAh g -1 , indicating that the high specific surface area and porosity provided by the cobalt selenide / graphitic carbon composite material is conducive to increasing the reaction area and promoting the ...

Embodiment 3

[0030] A preparation method for building cobalt selenide / graphite carbon composite material based on MOFs template, comprising the following steps:

[0031] 1) Preparation of polyhedral metal-organic framework compound ZIF-67: Weigh 5.5mmol Co(NO 3 ) 2 ·6H 2 O and 45mmol 2-methylimidazole were dissolved in 100ml methanol respectively, and the stirring speed was set to be 350r / min. After the stirring was completely dissolved, the Co(NO 3 ) 2 · 6H 2The O solution was poured into the 2-methylimidazole solution, stirred for 15 minutes, aged at room temperature for 22 hours after the stirring was stopped, and the product was centrifuged at a speed of 16000 r / min, and the centrifugation time was 3 minutes. After centrifugation, the precipitate was washed with methanol for 3 times. The amount of methanol used is 20 times the mass of the precipitate, and then placed at 60°C for 12 hours in a vacuum. The resulting product is a polyhedral metal-organic framework compound ZIF-67. The...

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Abstract

The invention discloses a preparation method of a polyhedral metal-organic framework compound ZIF-67. The preparation method comprises the following steps: preparing a solution from Co(NO3)2.6H2O, 2-methylimidazole and methanol, mixing and stirring, reacting at a normal temperature, performing centrifugal washing, drying and the like. The ZIF-67 presents bluish violet, is in the shape of rhombic dodecahedron, and has the particle size of 300-920nm. The prepared ZIF-67 is in the shape of rhombic dodecahedron, the particle size of the framework is small and uniform and can be controlled to be about 300nm, the specific surface area is large, and the overall distribution is uniform. The material disclosed by the invention is high in degree of crystallinity, has high specific surface area and porosity, homogeneous distribution can be formed, the prepared framework is small in particle size, and the overall distribution is uniform. Meanwhile, the compound is high in electric shock capacity and long in service life, has excellent lithium storage property, and can avoid attenuation after 200 charge-discharge cycles at most. The stability in the application is excellent, the condition thatthe current is unstable is avoided, and the product purity is high. The yield of the preparation method is high and can reach 70% or higher, and the preparation process is simple and feasible and worthy of market popularization.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a metal organic framework compound ZIF-67 and its application in preparing cobalt selenide / graphite carbon composite materials. Background technique [0002] With the depletion of fossil energy represented by oil and the increasingly serious environmental pollution caused by the combustion of fossil energy, people urgently need a sustainable, renewable and clean energy. Lithium-ion batteries stand out from many new energy sources due to their high energy density, long cycle life, and environmental friendliness, and are widely used in mobile electronic devices, new energy vehicles, and other fields. However, the negative electrode material of commercial lithium-ion batteries is graphite, and the theoretical capacity of graphite is only 372mAh / g, which cannot meet the capacity requirements of large electronic equipment such as electric vehicles, which limits the application a...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J27/057B01J35/00H01M4/36H01M4/58H01M4/62H01M10/0525
CPCB01J27/0573B01J35/0033C08G83/008H01M4/362H01M4/581H01M4/625H01M10/0525Y02E60/10
Inventor 柳红东李宗阳伏春平胡荣阮海波刘佳黄佳木
Owner CHONGQING UNIV OF ARTS & SCI
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