Double-chain polyethylene oxide modified covalent organic framework, preparation method and application

A technology of covalent organic framework and polyethylene oxide, applied in the field of ion conduction, preparation, covalent organic framework modified by double-chain polyethylene oxide, can solve the problem that the conductivity is not particularly ideal and there is no ion Conduction performance application research and other issues to achieve the effect of improving lithium ion conductivity, excellent ion conductivity, and high ion conductivity

Active Publication Date: 2022-06-24
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, preparation method and application
  • Double-chain polyethylene oxide modified covalent organic framework, preparation method and application
  • Double-chain polyethylene oxide modified covalent organic framework, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0049]

[0050] PEG-1,1-NHNH 2 The structure 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 mix the suspension It was frozen in liquid nitrogen, evacuated, and degassed for three times. In the state of vacuum, the tube was sealed with a flame gun, and then placed in a 120 ℃ oven for 72 hours; after taking out and cooling, the crude product was obtained. Dichlorome...

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 0.05mmol 1,3,5-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 mix the suspension It was frozen in liquid nitrogen, evacuated, and degassed for three times. In the state of vacuum, the tube was sealed with a flame gun, and then placed in a 120 ℃ oven for 72 hours; after taking out and cooling, the crude product was obtained. Dichloromethane, ethyl acetate, methanol, and acetone were washed and filtered three times with suction, then extracted with tetrahydrofuran and chloroform for three days, and then placed in a vacuum drying oven for drying at 50°C for 12 hours to obtain a white solid powder with a yield of is 85...

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 mix the suspension It was frozen in liquid nitrogen, evacuated, and degassed for three times. In the state of vacuum, the tube was sealed with a flame gun, and then placed in a 120 ℃ oven for 72 hours; after taking out and cooling, the crude product was obtained. Dichloromethane, ethyl acetate, methanol, and acetone were washed and filtered three times with suction, and then extracted with tetrahydrofuran and chloroform for three days, and then placed in a vacuum drying oven for drying at 50°C for 12 hours to obtain a white solid powder. The rate is 83%....

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PUM

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Abstract

The invention discloses a double-chain polyethylene oxide modified covalent organic framework, a preparation method and an application thereof. The covalent organic framework is obtained by PEG‑n, n‑NHNH 2 (n=1,2,3,6) and 1,3,5-tris(4-formylphenyl)benzene as raw materials, mesitylene and 1,4-dioxane as solvent, acetic acid as catalyst , prepared by solvothermal method. The covalent organic framework of the present invention has good crystallinity and thermal stability, and exhibits good lithium ion conductivity and solid state lithium battery cycle performance at high temperatures.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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