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Double-chain polyethylene oxide modified covalent organic framework as well as preparation method and application thereof

A technology of covalent organic framework and polyethylene oxide, which is applied in the preparation, covalent organic framework modified by double-chain polyethylene oxide, and the application field of ion conduction, which can solve the problem that the conductivity is not particularly ideal and there is no ion Conductive performance application research and other issues

Active Publication Date: 2021-09-14
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in terms of covalent organic frameworks, there are few reports on the application of PEO-based ion conductivity and solid-state electrolytes, and the conductivity is not particularly ideal.
In 2018, Jiang Donglin's research group reported a new type of covalent organic framework modified with a single chain of PEO. However, due to the short chain and single chain, its ion conductivity only reached 5.37×10 at 80°C. -6 S cm -1 At the same time, there is no further application research on ion conductivity at higher temperatures (J.Am.Chem.Soc.2018, 140, 7429-7432)

Method used

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  • Double-chain polyethylene oxide modified covalent organic framework as well as preparation method and application thereof
  • Double-chain polyethylene oxide modified covalent organic framework as well as preparation method and application thereof
  • Double-chain polyethylene oxide modified covalent organic framework as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Double-chain polyethylene oxide-modified covalent organic framework (COF-PEO-1,1), which is composed of 1,3,5-tris(4-formylphenyl)benzene and PEG-1,1-NHNH 2 The organic framework formed by the Schiff base reaction has the following structure:

[0049]

[0050] PEG-1,1-NHNH 2 The structure of the is as follows:

[0051]

[0052] The preparation method of COF-PEO-1,1, the specific steps are as follows;

[0053] Take 0.05mmol 1,3,5-tris(4-formylphenyl)benzene, 0.075mmol PEG-1,1-NHNH 2 , add 1.8ml of mesitylene and 0.2ml of 1,4-dioxane, ultrasonically disperse the raw materials to form a suspension, add 0.2ml of 6mol / L acetic acid solution, continue to ultrasonically disperse into a suspension, and the suspension Freezing with liquid nitrogen, vacuuming, and degassing three times in sequence. Under the state of vacuuming, use a flame gun to seal the tube, and then put it in a 120°C oven for 72 hours of reaction; after taking it out and cooling, the crude product is...

Embodiment 2

[0063] This example is basically the same as Example 1, the only difference is that the monomer is PEG-2,2-NHNH 2 ,Specifically:

[0064] Take 0.05mmol1,3,5-tris(4-formylphenyl)benzene, 0.075mmol PEG-2,2-NHNH 2 , add 1.8ml of mesitylene and 0.2ml of 1,4-dioxane, ultrasonically disperse the raw materials to form a suspension, add 0.2ml of 6mol / L acetic acid solution, continue to ultrasonically disperse into a suspension, and the suspension Freezing with liquid nitrogen, vacuuming, and degassing three times in sequence. Under the state of vacuuming, use a flame gun to seal the tube, and then put it in a 120°C oven for 72 hours of reaction; after taking it out and cooling, the crude product is obtained, and the crude product is used in turn. Dichloromethane, ethyl acetate, methanol, acetone washed and suction filtered three times, then extracted with tetrahydrofuran and trichloromethane Soxhlet for three days, put into a vacuum drying oven at 50°C and dried for 12 hours to obtai...

Embodiment 3

[0066] This example is basically the same as Example 1, the only difference is that the monomer is PEG-3,3-NHNH 2 ,Specifically:

[0067] Take 0.05mmol 1,3,5-tris(4-formylphenyl)benzene, 0.075mmol PEG-3,3-NHNH 2 , add 1.8ml of mesitylene and 0.2ml of 1,4-dioxane, ultrasonically disperse the raw materials to form a suspension, add 0.2ml of 6mol / L acetic acid solution, continue to ultrasonically disperse into a suspension, and the suspension Freezing with liquid nitrogen, vacuuming, and degassing three times in sequence. Under the state of vacuuming, use a flame gun to seal the tube, and then put it in a 120°C oven for 72 hours of reaction; after taking it out and cooling, the crude product is obtained, and the crude product is used in turn. Dichloromethane, ethyl acetate, methanol, and acetone were washed and suction filtered three times, then extracted with tetrahydrofuran and trichloromethane for three days by Soxhlet, and dried in a vacuum oven at 50°C for 12 hours to obtai...

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PUM

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Abstract

The invention discloses a double-chain polyethylene oxide modified covalent organic framework as well as a preparation method and application thereof. The covalent organic framework is prepared by taking PEG-n, n-NHNH2 (n = 1, 2, 3, 6) and 1, 3, 5-tris (4-formylphenyl) benzene as raw materials, mesitylene and 1, 4 dioxane as solvents and acetic acid as a catalyst through a solvothermal method. The covalent organic framework provided by the invention has good crystallinity and thermal stability, and shows good lithium ion conduction performance and solid-state lithium battery cycle performance at high temperature.

Description

technical field [0001] The invention belongs to the field of covalent organic framework compounds, and relates to a covalent organic framework modified by double-chain polyethylene oxide, a preparation method and its application in ion conduction. Background technique [0002] Commercial lithium-ion batteries have a safety hazard of explosion due to the use of a large amount of flammable organic solvents. Solid-state electrolytes have high ionic conductivity and high safety, and can effectively inhibit the growth of lithium dendrites, which in turn can increase the energy density of lithium-ion batteries, which has attracted extensive research. Polyethylene oxide (PEO) is used as a solid polymer electrolyte because of the lithium-conducting mechanism of segmental motion. Traditional PEO polymer electrolytes have poor high-temperature stability, and are prone to loss, resulting in uneven composition, and even battery failure and short circuit. How to design PEO-based solid-...

Claims

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Application Information

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IPC IPC(8): C08G12/08H01M10/0525H01M10/0565
CPCC08G12/08H01M10/0565H01M10/0525H01M2300/0082Y02E60/10
Inventor 许冰清王宇翔张根
Owner NANJING UNIV OF SCI & TECH
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