Method for preparing micropore polymer electrolyte by using glyoxaline cation-intercalated montmorillonite

An imidazolium cationic, microporous polymer technology, applied in the polymer field, can solve problems such as low thermal stability, and achieve the effects of improving electrical conductivity, convenient operation, and improving film thermal stability and flame retardancy

Inactive Publication Date: 2009-04-22
NORTHWEST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alkylammonium-modified organomontmorillonites as inorganic fillers for polymer electrolyte membranes have the following disadvantages: For health reasons, the usable concentration of alkylammonium compounds should not be higher than 5 ppm, low thermal stability, its thermal decomposition The temperature does not exceed 220-250°C

Method used

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  • Method for preparing micropore polymer electrolyte by using glyoxaline cation-intercalated montmorillonite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 2 grams of dry Na-montmorillonite to 15ml of 1-ethyl-3-methylimidazolium tetrafluoroborate and 150ml of secondary aqueous solution, stir vigorously at 80°C for 6 hours, then centrifuge the hot solution, Wash twice with water (not more than 10 times) to remove halogen and tetrafluoroborate ions on the surface of montmorillonite (use 0.1mol / L silver nitrate solution to detect the presence of halogen). The obtained montmorillonite was put into an oven for vacuum drying at 100° C. for 24 hours, then ground and passed through a 325 mesh sieve to obtain the montmorillonite intercalated with imidazolium cations,

[0023] Get 0.06 gram of imidazolium cation-intercalated montmorillonite, disperse in 15 ml of N, N-dimethylformamide and ultrasonically disperse for 40 minutes to obtain a uniform solution, then add 1.5 ml of glycerol, 1.5 gram of poly Vinylidene fluoride, 1.5 grams of polyethylene glycol (molecular weight 10,000), vigorously stirred at 80°C for 6 hours to obtain...

Embodiment 2

[0026] Example 2: Add 2 grams of dry Na-montmorillonite to 15ml of 1-ethyl-3-methylimidazolium tetrafluoroborate and 150ml of secondary aqueous solution, stir vigorously at 80°C for 6 hours, and then Centrifuge the hot solution, wash with secondary water (no more than 10 times) to remove halogen and tetrafluoroborate ions on the surface of montmorillonite, and detect the presence of halogen with 0.1mol / L silver nitrate solution. The obtained modified montmorillonite was vacuum-dried at 100°C for 24 hours, then ground and passed through a 325-mesh sieve to obtain imidazolium cation-intercalated montmorillonite;

[0027] Disperse 0.12 g of imidazolium cation-intercalated montmorillonite in 15 ml of N,N-dimethylformamide and ultrasonically disperse for 40 minutes, then add 1.5 ml of glycerin, 1.5 g of polyvinylidene fluoride, and 1.5 g of polyethylene Diol (molecular weight 10,000), vigorously stirred at 80°C for 6 hours to obtain a homogeneous hot solution.

[0028] Pour the ho...

Embodiment 3

[0030] Example 3: Add 2 grams of dry Na-montmorillonite to 15ml of 1-ethyl-3-methylimidazolium tetrafluoroborate and 150ml of secondary aqueous solution, stir vigorously at 80°C for 6 hours, and then Centrifuge the hot solution, wash with secondary water (no more than 10 times) to remove halogen and tetrafluoroborate ions on the surface of montmorillonite, and detect the presence of halogen with 0.1mol / L silver nitrate solution. The obtained modified montmorillonite was vacuum-dried at 100° C. for 24 hours, then ground and passed through a 325-mesh sieve to obtain imidazolium cation-intercalated montmorillonite.

[0031] Take 0.18 g of imidazolium cation-intercalated montmorillonite and disperse it in 15 ml of N,N-dimethylformamide and ultrasonically disperse it for 40 minutes, then add 1.5 ml of glycerin, 1.5 g of polyvinylidene fluoride, and 1.5 g of polyethylene Diol (molecular weight 10000), vigorously stirred at 80°C for 6 hours to obtain a homogeneous hot solution;

[0...

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Abstract

The invention provides a method for preparing high thermal stability microporous polymer electrolyte from imidazole cation intercalation montmorillonite. In the method, firstly, the imidazole cation intercalation montmorillonite is used to prepare high thermal stability montmorillonite; secondly, by the phase transition method, polyvinylidene fluoride, polyethylene glycol and the imidazole cation intercalation montmorillonite are added to the mixed solution of N,N-dimethylformamide and glycerin and violently stirred at a temperature of between 70 and 85 DEG C for 6 to 10 hours, the obtained evenly mixed solution is poured on a clean and preheated glass plate and vacuum dried at a temperature of between 100 and 130 DEG C for 30 t0 40 hours to obtain a polymer membrane with the thickness of between 100 and 300 micrometers; and finally the polymer membrane is soaked in electrolyte in a simple glass box for 24 to 72 hours to obtain the microporous polymer electrolyte. Tests show that the electrical conductivity of the microporous polymer electrolyte prepared by the method reaches 1.6 to 6.15mS/cm, and the residual mass of the dry membrane at a temperature of 400 DEG C(N2) is between 60 and 70 percent.

Description

technical field [0001] The invention belongs to the technical field of polymers, and relates to the preparation of a conductive polymer material, in particular to a preparation method of a microporous polymer electrolyte with high thermal stability and high conductivity. Background technique [0002] In lithium-ion secondary batteries, polymer electrolyte materials function as both electrolyte and separator. Exothermic reactions will occur during the charging and discharging process of the battery, and this thermal effect will cause the degradation of the polymer electrolyte, and lead to low efficiency of the charging and discharging process, and more seriously, lead to unsafe use of the battery. Therefore, the polymer membrane as the electrolyte matrix must have high thermal stability. Alkylammonium-modified organomontmorillonites as inorganic fillers for polymer electrolyte membranes have the following disadvantages: For health reasons, the usable concentration of alkylam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/04C08L27/16C08L71/08H01M10/40C08K5/3445C08K3/34
CPCY02E60/122
Inventor 王云普高祥虎刘汉功张继
Owner NORTHWEST NORMAL UNIVERSITY
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