Preparation method and application of a crown ether modified polyaniline solid electrolyte membrane

A technology of solid electrolyte membrane and polyaniline, which is applied in the direction of solid electrolyte, electrolyte battery manufacturing, non-aqueous electrolyte, etc., can solve the problems of high contact resistance and low ion conductivity, and achieve high ion conductivity and good electrochemical performance Effect

Active Publication Date: 2020-05-12
河南电池研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still a series of problems in solid electrolytes, such as low ionic conductivity, high contact resistance between electrolyte and electrodes, etc.

Method used

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  • Preparation method and application of a crown ether modified polyaniline solid electrolyte membrane
  • Preparation method and application of a crown ether modified polyaniline solid electrolyte membrane
  • Preparation method and application of a crown ether modified polyaniline solid electrolyte membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Preparation of benzo-12-crown-4sulfonyl chloride

[0022] Dissolve 2.24g of benzo-12-crown-4 (0.01mol) in 50mL of tetrahydrofuran, then add it to a 100mL three-necked round-bottomed flask equipped with a magnet, reflux condenser and thermometer, pass into nitrogen protection and react After cooling the system to 0°C, add 8 mL of freshly distilled sulfone dichloride (0.1 mol) dropwise into the round-bottomed flask with a glass syringe, and the dropping time is not less than 30 min. After the dropwise addition, the temperature was raised to 35°C for 6 hours. After the reaction, the mixture was dried and neutralized with quicklime, and the tetrahydrofuran was removed by vacuum rotary evaporation. The remaining oil was recrystallized in n-hexane and placed in a vacuum oven at 70°C for vacuum drying. After 24 hours or more, the obtained white solid powder was benzo-12-crown-4sulfonyl chloride (2.11 g, 0.00655 mol), and the yield was 65.5%. Its reaction equation is shown...

Embodiment 2

[0036] (1) Preparation of benzo-14-crown-4sulfonyl chloride

[0037] Dissolve 2.52g of benzo-14-crown-4 (0.01mol) in 70mL of ethyl acetate, then add it into a 250mL three-necked round-bottomed flask equipped with a magnet, reflux condenser and thermometer, pass into nitrogen protection and After the reaction system was cooled to 0°C, 10 mL of freshly distilled chlorosulfonic acid (0.15 mol) was added dropwise into the round bottom flask with a glass syringe, and the dropping time was not less than 30 min. After the dropwise addition, the temperature was raised to 45°C for 7 hours. After the reaction, the mixture was dried and neutralized with caustic soda, and the ethyl acetate was removed by vacuum rotary evaporation. The remaining oil was recrystallized in n-heptane and placed in a vacuum oven at 100°C. After vacuum drying in the oven for more than 48 hours, the obtained white solid powder was benzo-14-crown-4sulfonyl chloride (2.1 g, 0.006 mol), with a yield of 60%. Its re...

Embodiment 3

[0051] (1) Preparation of dibenzo-12-crown-4sulfonyl chloride

[0052] Dissolve 2.72g of benzo-12-crown-4 (0.01mol) in 50mL of tetrahydrofuran, then add it to a 100mL three-necked round-bottomed flask equipped with a magnet, reflux condenser and thermometer, pass into nitrogen protection and react After cooling the system to 0°C, add 16 mL of freshly distilled sulfone dichloride (0.2 mol) dropwise into the round-bottomed flask with a glass syringe, and the dropping time is not less than 30 min. After the dropwise addition, the temperature was raised to 55°C for 8 hours. After the reaction, the mixture was dried and neutralized with quicklime, and the tetrahydrofuran was removed by vacuum rotary evaporation. The remaining oil was recrystallized in n-hexane and placed in a vacuum oven at 70°C for vacuum drying. After 24 hours, the obtained yellow solid powder was dibenzo-12-crown-4sulfonyl chloride (2.88 g, 0.00615 mol), and the yield was 61.5%. Its reaction equation is shown i...

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Abstract

The invention discloses a preparation method of a crown ether modified polyaniline solid electrolyte membrane and its application in solid batteries, belonging to the technical field of solid batteries. The key points of the technical scheme of the present invention are: reacting the crown ether compound with a chlorosulfonating reagent to obtain a crown ether sulfonyl chloride, then reacting the crown ether sulfonyl chloride with polyaniline to obtain polyaniline with a crown ether group in the side chain, and then Polyaniline containing crown ether groups in the side chain is reacted with lithium salt to prepare crown ether sulfonyl chloride grafted polyaniline lithium ion complex, and finally the crown ether sulfonyl chloride grafted polyaniline lithium ion complex is mixed with polyaniline and coated Cover on the substrate, dry naturally and then vacuum dry to obtain the crown ether modified polyaniline solid electrolyte membrane. The crown ether modified polyaniline solid electrolyte membrane prepared by the invention has the advantages of high ion conductivity and elastic interface contact, and the assembled solid state battery exhibits good electrochemical performance and is suitable for industrial popularization and application.

Description

technical field [0001] The invention belongs to the technical field of solid batteries, and in particular relates to a preparation method of a crown ether modified polyaniline solid electrolyte membrane and its application in solid batteries. Background technique [0002] As a new type of electrolyte material that is expected to replace the electrolyte, the solid electrolyte has made great progress since its discovery. It can not only solve the safety problems of traditional liquid lithium-ion batteries such as leakage and explosion, but also make the battery thinner. , the shape is more flexible, and the packaging is more convenient, so it has a broad market in sensors, micro digital products, and human implantation equipment. However, there are still a series of problems in solid electrolytes, such as low ionic conductivity and high contact resistance between electrolyte and electrodes. [0003] In view of the existing problems, the researchers proposed the concept of ion...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562H01M10/058H01M10/0525
CPCH01M10/0525H01M10/0562H01M10/058H01M2300/0082Y02E60/10Y02P70/50
Inventor 杨书廷王秋娴李凯岳红云
Owner 河南电池研究院有限公司
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