Preparation method of flame-retardant organic/inorganic composite membrane

An inorganic composite and organic technology, applied in the field of high-performance diaphragm preparation, can solve the problems of poor pore formation uniformity, limited flame retardant effect, high price, etc., and achieve the effects of low equipment requirements, low cost, and easily controllable conditions.

Active Publication Date: 2014-10-15
GUANGDONG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One is to start with the material itself, select high temperature resistant resin such as patent CN 103441228A, select polyaryl sulfone amide, dissolve it with organic solvent and then prepare lithium ion by wet papermaking process Battery diaphragm, the patent CN 103205123A proposes to use polyphenylene sulfide and organic solvent to mix, co-extrude and then stretch and extract to obtain a porous film to prepare a diaphragm. Since the material itself is a flame-retardant material, its flame retardancy must be improved, but at the same time there is a price Expensive, with the drawback of organic contamination in the molding process
[0007] The second is

Method used

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  • Preparation method of flame-retardant organic/inorganic composite membrane
  • Preparation method of flame-retardant organic/inorganic composite membrane
  • Preparation method of flame-retardant organic/inorganic composite membrane

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Example Embodiment

[0047] The embodiment of the present invention provides a method for preparing a flame-retardant organic / inorganic composite diaphragm containing a hexagonal zirconium phosphate coating layer. Including the following steps:

[0048] S01. Hexagonal zirconium phosphate

[0049] In the hydrothermal reactor, a time-temperature-concentration control method is used to prepare zirconium phosphate with a stable hexagonal structure.

[0050] S02. Organic zirconium phosphate:

[0051] Use an organic peeling agent to peel off the hexagonal flake zirconium phosphate, and add organic segments to the surface of the zirconium phosphate to form an organic active zirconium phosphate;

[0052] S03. Coating slurry configuration

[0053] The organic zirconium phosphate solution and the binder solution are directly mixed and stirred at high speed to prepare the coating slurry; wherein the mass ratio of the organic zirconium phosphate to the binder is 10 to 200:1;

[0054] S04. Preparation of organic / inorgani...

Example Embodiment

[0066] Example 1

[0067] In S11, the mixture of zirconium oxychloride and phosphoric acid with a mass ratio of 1:5 is uniformly poured into an autoclave, reacted in an oven at 150°C for 20 hours, cooled to room temperature, washed with water to neutral, and dried in an oven to obtain the initial six Edge-shaped zirconium phosphate powder;

[0068] S12 Disperse zirconium phosphate in ethylamine solution for pre-dispersion for 1 hour, then add organic stripping agent cetyltrimethylammonium hydrogen sulfate, the mass ratio of zirconium phosphate to organic stripping agent is 0.5:1, and the stripping time is 15 hours After the reaction is completed, it is diluted to pH 8.

[0069] S13 The 10% mass fraction of polyvinyl alcohol aqueous solution and the organic zirconium phosphate aqueous solution are mixed uniformly at room temperature and stirred for 12 hours, wherein the mass ratio of the organic zirconium phosphate to the polyvinyl alcohol is 17:1.

[0070] S14: Soak the dry-process ...

Example Embodiment

[0072] Example 2

[0073] In S21, the mixture of zirconium oxychloride and phosphoric acid with a mass ratio of 1:13 is uniformly poured into the autoclave, reacted in an oven at 190°C for 30 hours, cooled to room temperature, washed with water to neutral, and dried in the oven to obtain the initial six Edge-shaped zirconium phosphate powder;

[0074] S22 Disperse zirconium phosphate in aniline solution for 1.5 hours, then add organic stripping agent sodium lauryl sulfate, the mass ratio of zirconium phosphate to organic stripping agent is 0.9:1, the stripping time is 20 hours, and it is diluted after the reaction is completed To pH 8.

[0075] S23 Mix the 20% mass fraction of methylcellulose aqueous solution and the organic zirconium phosphate aqueous solution uniformly at room temperature and stir for 12 hours, wherein the mass ratio of the organic zirconium phosphate to methylcellulose is 23:1.

[0076] S24: The dry method PE microporous membrane is soaked in the slurry for 30 mi...

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Abstract

The invention discloses a preparation method of a flame-retardant organic/inorganic composite membrane. The method comprises the steps of preparing zirconium phosphate powder with a hexagonal structure by a time-temperature-concentration control method, organizing the prepared zirconium phosphate powder, stripping a multilayer structure to become a laminal filler as thin as possible, directly mixing an organized zirconium phosphate solution with a water-soluble binder solution, preparing coating pulp, coating the coating pulp on the surface of a polyolefin microporous membrane, drying the coating pulp, and obtaining the organic/inorganic composite membrane. The preparation method is used for preparing a membrane suitable for a high-power battery; the preparation method of the flame-retardant organic/inorganic composite membrane is simple in technology, low in equipment requirement, easy in condition control and low in cost, and is suitable for industrial production; the flame retardance of the membrane can be improved effectively by simple coating; an oxygen index is increased obviously; the flame-retardant grade reaches VTM-2; a demand of a battery membrane is met; and high performance of a common membrane is achieved.

Description

technical field [0001] The invention belongs to the technical field of high-performance diaphragm preparation for lithium battery diaphragms, and in particular relates to a method for preparing a flame-retardant organic / inorganic composite diaphragm. Background technique [0002] As an important part of lithium-ion batteries, separators have attracted extensive attention from researchers. The high performance of lithium-ion batteries is closely related to the properties of separators. Especially in lithium batteries with high rate and fast charge and discharge, the performance requirements of separators are more obvious. In view of the fact that the separator has a crucial impact on the performance of the actual battery, it must have good chemical and electrochemical stability and maintain a high degree of wettability to the electrolyte during repeated charge and discharge. The interface phase between the separator material and the electrode Both the capacitive capacity and ...

Claims

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Application Information

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IPC IPC(8): H01M2/16H01M50/446
CPCH01M10/0525H01M50/403H01M50/446Y02E60/10
Inventor 徐睿杰黄晓蕊雷彩红蔡启陈昌滨陈贤德张丰
Owner GUANGDONG UNIV OF TECH
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