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Sulfonyl conjugated microporous polymer, preparation method and application

A technology of conjugated micropores and sulfonic acid groups, applied in electrochemical generators, electrical components, secondary batteries, etc., can solve problems such as explosions, achieve high chemical stability, high lithium ion conductivity, and good electrochemical The effect of cycle stability

Active Publication Date: 2021-08-31
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Traditional commercial lithium-ion batteries have potential safety hazards such as explosion due to the use of a large amount of flammable organic solvents
So far, there have been no reports of sulfonic acid-based conjugated microporous polymers as solid electrolyte materials

Method used

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  • Sulfonyl conjugated microporous polymer, preparation method and application
  • Sulfonyl conjugated microporous polymer, preparation method and application
  • Sulfonyl conjugated microporous polymer, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The preparation method of sulfonic acid group conjugated microporous polymer, the steps are as follows:

[0052] 1,4-dibromo-2,5-bis(3-sulfopropoxy)benzene (834.2mg, 1.5mmol), tetrakis(triphenylphosphine)palladium (138.5mg, 0.12mmol) and iodide Copper (22.9 mg, 0.12 mmol), and 1,3,5-triethynylbenzene (150.2 mg, 1.0 mmol) were dissolved in 25 mL of toluene and 25 mL of triethylamine under an argon atmosphere. The reaction was heated to 80°C and stirred at 80°C for 36 hours. After cooling to room temperature, the solid was filtered with suction, washed with chloroform, water, methanol and acetone successively, and then Soxhlet extracted with dichloromethane and methanol for 48 hours to remove unreacted monomer or catalyst residue. The sample was dried under vacuum at 80° C. for 24 hours to obtain 563 mg of sulfonic acid-conjugated microporous polymer, with a yield of 76%.

Embodiment 2

[0054] The preparation method of sulfonic acid group conjugated microporous polymer, the steps are as follows:

[0055] 1,4-dibromo-2,5-bis(3-sulfopropoxy)benzene (834.2mg, 1.5mmol), tetrakis(triphenylphosphine)palladium (138.5mg, 0.12mmol) and iodide Copper (22.9 mg, 0.12 mmol), and 1,3,5-tris(4-ethynylphenyl)benzene (378.5 mg, 1.0 mmol) were dissolved in 25 mL of toluene and 25 mL of triethylamine under an argon atmosphere. The reaction was heated to 80°C and stirred at 80°C for 36 hours. After cooling to room temperature, the solid was suction filtered, washed sequentially with chloroform, water, methanol and acetone, and then Soxhlet extracted with dichloromethane and methanol for 48 hours to remove any unreacted monomer or catalyst residue. The sample was dried under vacuum at 80° C. for 24 hours to obtain 815 mg of sulfonic acid group-conjugated microporous polymer, with a yield of 84%.

[0056] figure 1 The synthesis route and structural diagram of the sulfonic acid ...

Embodiment 3

[0061] Example 3: Preparation of sulfonic acid conjugated microporous polymer solid electrolyte and AC impedance test

[0062] 1) Preparation of sulfonic acid-conjugated microporous polymer solid electrolyte: Take 100 mg of sulfonic acid-conjugated microporous polymer powder, add it to 20 mL of 1 mol / L lithium bistrifluoromethanesulfonylimide solution, and ultrasonicate for 5 minutes. Stir for a day. The solid was collected by centrifugation at 10000 rpm. Repeat the operation three times until the alkali metal ion exchange is complete, and dry at 80°C overnight; take 6 mg of ion-exchanged sulfonic acid conjugated microporous polymer powder, 3 mg of 1-butyl-3-methylimidazole bis(trifluoromethylsulfonyl ) imide, ground for 10 min, and the mixed powder was kept under pressure at 5 Mpa for 0.5 h, and pressed into a solid electrolyte sheet with a diameter of 5 mm and a thickness of 0.253 mm.

[0063] In the present invention, the alkali metal ion salt is an alkali metal ion salt ...

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Abstract

The invention discloses a sulfonyl conjugated microporous polymer, a preparation method and application. The conjugated microporous polymer is formed by coupling aryl dibromide containing sulfonyl and ethynyl compounds through Sonogashira, the material structure contains rich sulfonyl group sites, and alkali metal ions can be effectively replaced and combined through ion exchange. The sulfonyl sites can promote cation migration, and high migration number and stable high conductivity are obtained. The sulfonyl conjugated microporous polymer solid electrolyte has good lithium ion conductivity, the lithium ion conductivity is 1.71*10<-4> S*cm<-1> at 40 DEG C and reaches 2.34*10<-3> S*cm<-1 > at the high temperature of 120 DEG C, and an assembled solid lithium ion battery can stably run at the high temperature.

Description

technical field [0001] The invention belongs to the field of conjugated microporous polymers, and relates to a sulfonic acid group conjugated microporous polymer, a preparation method and its application as a solid electrolyte material in the field of electrochemistry. Background technique [0002] Traditional commercial lithium-ion batteries have potential safety hazards such as explosion due to the use of a large amount of flammable organic solvents. Solid electrolytes have attracted extensive attention due to their low flammability, high thermal stability, no leakage, and low risk of explosion. Replacing the liquid electrolyte with a nonflammable solid electrolyte can effectively improve the safety of the battery. Designing and developing solid electrolytes with high-efficiency ionic conductivity is of great significance for improving the performance of lithium-ion batteries. [0003] Conjugated Microporous Polymers (CMPs) are rigid porous polymers with large conjugated...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02H01M10/0565H01M10/0525H01M10/054
CPCC08G61/02H01M10/0565H01M10/0525H01M10/054C08G2261/124C08G2261/1452C08G2261/3422C08G2261/516Y02E60/10
Inventor 许冰清武苗苗张根
Owner NANJING UNIV OF SCI & TECH
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