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A preparation method of flame-retardant organic/inorganic composite diaphragm

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

Active Publication Date: 2017-01-04
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One is to start with the material itself and select high-temperature resistant resins, such as patent CN 103441228A, select polyarylsulfone amide, dissolve it in an organic solvent, and then use a wet papermaking process to prepare lithium-ion battery separators. Patent CN 103205123A proposes the use of polyphenylene sulfide and organic solvents After mixing, co-extrusion, stretching and extraction to obtain a porous membrane to prepare a diaphragm, since the material itself is a flame-retardant material, its flame retardancy must be improved, but at the same time, it is expensive and has the defects of organic pollution during the molding process.
[0007] The second is to mix the flame retardant filler with the matrix resin to prepare the diaphragm. For example, the patent CN 103700800A mentions that a composite papermaking method is used to form a flame retardant layer mixed with cotton fibers and flame retardants on the surface of polypropylene fibers. The combustion effect is limited; for example, patents CN 103242591A and CN 102376928B all mention that the flame retardant powder is mixed with polypropylene and then extruded and stretched to form a porous film. Although this method can improve the flame retardancy of the diaphragm, the uniformity of the pores Poor, prone to membrane rupture

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  • A preparation method of flame-retardant organic/inorganic composite diaphragm
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  • A preparation method of flame-retardant organic/inorganic composite diaphragm

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preparation example Construction

[0044] 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:

[0045] S01. Hexagonal zirconium phosphate

[0046] In a hydrothermal reactor, zirconium phosphate with a stable hexagonal structure was prepared by a time-temperature-concentration control method.

[0047] S02. Organic zirconium phosphate:

[0048] Use an organic stripping agent to peel off the hexagonal sheet-shaped zirconium phosphate, and add an organic segment to the surface of the zirconium phosphate to form an active zirconium phosphate with an organophilic phase;

[0049] S03. Configuration of Coating Slurry

[0050] The organic zirconium phosphate solution and the binder solution are directly mixed and stirred at a high speed to prepare a coating slurry; wherein, the mass ratio of the organic zirconium phosphate to the binder is 10-200:1;

[0...

Embodiment 1

[0064] S11 Mix zirconium oxychloride and phosphoric acid with a mass ratio of 1:5 and pour them into an autoclave, react in an oven at 150°C for 20 hours, cool to room temperature, wash with water until neutral, and dry in an oven to obtain initial six Polygonal zirconium phosphate powder;

[0065] S12 Disperse zirconium phosphate in ethylamine solution and pre-disperse for 1 hour, then add organic stripping agent cetyl trimethyl ammonium hydrogen sulfate, the mass ratio of zirconium phosphate to organic stripping agent is 0.5:1, and the stripping time is 15 hours , diluted to pH 8 after the reaction was completed.

[0066] S13 Mix the polyvinyl alcohol aqueous solution with a mass fraction of 10% and the organic zirconium phosphate aqueous solution at room temperature, and stir for 12 hours, wherein the mass ratio of the organic zirconium phosphate to polyvinyl alcohol is 17:1.

[0067] S14: Soak the dry-process PP microporous membrane in the slurry for 30 minutes, take it o...

Embodiment 2

[0070] S21 Mix zirconium oxychloride and phosphoric acid with a mass ratio of 1:13 and pour them into an autoclave, react in an oven at 190°C for 30 hours, cool to room temperature, wash with water until neutral, and dry in an oven to obtain the initial six Polygonal zirconium phosphate powder;

[0071] S22 Disperse zirconium phosphate in aniline solution and pre-disperse 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, and the stripping time is 20 hours. After the reaction is completed, dilute to pH 8.

[0072] S23 Mix an aqueous solution of methyl cellulose with a mass fraction of 20% and an aqueous solution of organic zirconium phosphate at room temperature, and stir for 12 hours, wherein the mass ratio of organic zirconium phosphate to methyl cellulose is 23:1.

[0073] S24: Soak the dry PE microporous membrane in the slurry for 30 minutes, take it out and dry it in a vacuum o...

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Abstract

The invention discloses a method for preparing a flame-retardant organic / inorganic composite diaphragm. The method adopts a time-temperature-concentration control method to prepare zirconium phosphate powder with a hexagonal structure; The layer structure becomes as thin as possible sheet filler; the organic zirconium phosphate solution is directly mixed with the water-soluble binder solution to prepare the coating slurry; the coating slurry is coated on the polyolefin microporous membrane Surface, drying, to obtain the organic / inorganic composite diaphragm; prepare a diaphragm suitable for high-power batteries; its preparation method is simple in process, low in equipment requirements, easy to control conditions, low in cost, and suitable for industrial production; simple coating can Effectively improve the flame retardancy of the separator, the oxygen index is significantly improved, and the flame retardancy level reaches VTM‑2, while meeting the needs of battery separators and realizing the high performance of ordinary separators.

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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Patent Type & Authority Patents(China)
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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