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Dual solvent step-by-step phase conversion preparation method of polymethyl methacrylate gel electrolyte microporous membrane

A polymethyl methacrylate, gel electrolyte technology, applied in the direction of electrolyte immobilization/gelation, circuits, electrical components, etc., can solve the problems of harsh synthesis conditions, low vapor pressure, wide membrane pore size distribution, etc. The effect of uniform pore size and distribution, improved mechanical strength, and high electrical conductivity

Active Publication Date: 2017-11-24
中科(淮安)新能源技术开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ionic liquid electrolytes have the advantages of wide operating temperature range, high conductivity, low vapor pressure, non-volatile, low toxicity, non-explosive, low melting point, etc., but there are also many problems: high cost, high viscosity, harsh synthesis conditions, the basis of ionic liquids lack of data, etc.
However, the gel electrolyte membrane prepared by this method still has the following problems: First, the porous membrane skeleton is prepared by immersion precipitation, although this method can obtain a variety of different pore structures, such as honeycomb, finger and sponge Pores, etc., but this method is not easy to achieve structural controllability and structural repeatability of the porous membrane; second, the mechanical strength of the porous membrane prepared by this method is still not ideal; third, the membrane pore size distribution is wide and difficult to adjust

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: Prepare gel electrolyte membrane according to the following steps

[0027] (1) Add 12g of tetrahydrofuran to 3g of ethylene glycol to obtain a mixed organic solvent with a mass ratio of ethylene glycol and tetrahydrofuran of 1:4;

[0028] (2) Add 3g of PMMA polymer to the above solution, stir magnetically, fully dissolve until there are no flocs in the solution, and obtain a uniform PMMA polymer organic solution with a mass ratio of polymer to mixed solvent of 1:5;

[0029] (3) Use a film applicator with a scale of 300 μm to evenly coat the above-mentioned PMMA polymer organic solution on a glass plate, immerse in deionized water after 10 minutes, and soak in water for 5 hours; put the film with water in 40 ℃ oven for 4 h, then moved into a vacuum oven at 60 ℃ for 48 h to obtain a PMMA polymer microporous membrane;

[0030] (4) Cut the above-mentioned fully dried microporous membrane into thin slices with a diameter of 18mm with a cutting machine, and imm...

Embodiment 2

[0031] Embodiment 2: Prepare gel electrolyte membrane according to the following steps

[0032] (1) Add 1g of glycerin to 15g of acetone to obtain a mixed organic solvent with a mass ratio of glycerin and acetone of 1:15;

[0033] (2) Add 2.667g of PMMA polymer to the above mixed organic solution, stir magnetically, fully dissolve until there is no floc in the solution, and obtain a uniform PMMA polymer organic solution with a mass ratio of polymer to mixed solvent of about 1:5 ;

[0034] (3) Use a film applicator with a scale of 400 μm to evenly coat the above PMMA polymer organic solution on a glass plate, immerse in deionized water after 40 minutes, and soak in water for 5 hours; put the film with water first into the Dry in an oven at 50°C for 3 hours, then move into a vacuum oven at 80°C, and dry for 24 hours to obtain a PMMA polymer membrane;

[0035] (4) Cut the above-mentioned fully dried film into a pick with a diameter of 18mm with a cutting machine, and immerse it...

Embodiment 3

[0036] Embodiment 3: Prepare gel electrolyte membrane according to the following steps

[0037] (1) Add 1 g of N,N-dimethylacetamide to 15 g of acetone to obtain a mixed organic solvent with a mass ratio of N,N-dimethylacetamide and acetone of 1:15;

[0038] (2) Add PMMA polymer with a mass fraction of 1.231g to the above mixed organic solution, stir magnetically, and fully dissolve until there is no floc in the solution, and a uniform polymer with a mass ratio of about 1:12 is obtained. PMMA polymer organic solution;

[0039] (3) Use a film applicator with a scale of 400 μm to evenly coat the above-mentioned PMMA polymer organic solution on a glass plate, immerse in deionized water after 80 minutes, and soak in water for not less than 5 hours; Dry in a 50°C oven for 5 hours, then move into a 60°C vacuum oven and dry for 36 hours to obtain a PMMA polymer membrane;

[0040] (4) Cut the above fully dried film into pieces with a diameter of 18 mm with a cutting machine, and imm...

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Abstract

The invention discloses a dual solvent step-by-step phase conversion preparation method of a polymethyl methacrylate gel electrolyte microporous membrane. The preparation method comprises the following steps: mixing a pore forming agent and a volatile solvent, dissolving polymethyl methacrylate polymer, after complete dissolution, uniformly painting the solution on a flat plate by using a scraper; allowing the flat plate to stand still for a while, after the volatile solvent is completely volatized, soaking the flat plate in deionized water, after the pore forming agent in the polymer membrane is dissolved in water, taking out the flat plate, drying the flat plate through baking, and after drying, soaking the polymer membrane into lithium salt electrolyte to obtain the PMMA gel electrolyte microporous membrane. A solvent, which can be easily dissolved in water and has a boiling point greater than 100 DEG C, is taken as the pore forming agent, the uniformity of the gel electrolyte microporous membrane is improved; compared with a conventional diaphragm, the electrochemical stability window and charge / discharge efficiency are higher; a better liquid absorbing effect is achieved, no leakage happens, the mechanical strength of the membrane is enhanced; the safety problem of liquid lithium ion batteries is solved, the problem that the conductivity of solid batteries is low is solved; and the method can be applied to industrial production easily.

Description

technical field [0001] The invention relates to a preparation method of a gel electrolyte microporous membrane, in particular to a method for preparing a polymethyl methacrylate gel electrolyte microporous membrane by step-by-step phase inversion with two solvents. Background technique [0002] Lithium-ion batteries have become widely used power products due to their high operating voltage, high energy density, small self-discharge, no memory effect, wide operating temperature range, light weight, long cycle life, and environmental friendliness. Ionic liquid electrolytes have the advantages of wide operating temperature range, high conductivity, low vapor pressure, non-volatile, low toxicity, non-explosive, low melting point, etc., but there are also many problems: high cost, high viscosity, harsh synthesis conditions, the basis of ionic liquids lack of data, etc. The all-solid polymer electrolyte is a system composed of lithium salt and polymer, and its conductivity is low...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0565H01M10/42H01M10/0525
CPCH01M10/0525H01M10/0565H01M10/4235H01M2300/0085Y02E60/10
Inventor 陈新德田兰兰熊莲张海荣唐伟超
Owner 中科(淮安)新能源技术开发有限公司
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