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Porous polyimide film and preparation method and application thereof

A technology of polyimide film and polyamic acid, which is applied in the direction of electrical components, circuits, battery components, etc., can solve the problems of low porogen removal efficiency, long etching treatment time, and difficult process, and achieve Achieve large-scale industrial application, good wettability and good repeatability

Inactive Publication Date: 2019-09-20
杭州阳名新能源设备科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The etchant used in the above method is generally a strong acid such as hydrofluoric acid, concentrated sulfuric acid or concentrated hydrochloric acid, and the etchant is difficult to penetrate into the material, and the pore-forming agent is generally a non-porous material, so there is pollution to the environment and the etching process time Long and pore-forming agent removal efficiency is low, the technical cost is high, and the process is difficult, etc.

Method used

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  • Porous polyimide film and preparation method and application thereof
  • Porous polyimide film and preparation method and application thereof
  • Porous polyimide film and preparation method and application thereof

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preparation example Construction

[0033] A kind of porous polyimide film preparation method of the present invention, comprises the following steps:

[0034] S1. Polycondensation of dibasic anhydrides and diamines in a polar solvent at low temperature, mechanically stirring for 18-20 hours to generate a precursor polyamic acid (PAA) solution, wherein the molar ratio of monomeric dibasic anhydrides to diamines is 1 :1;

[0035] The dibasic anhydrides are diphenylsulfone tetracarboxylic dianhydride, pyromellitic dianhydride, biphenyltetracarboxylic dianhydride, benzophenone tetraacid dianhydride, diphenylhexafluoroisopropyl tetraacid dianhydride, diphenylsulfide One or more of ether tetra-acid dianhydrides;

[0036] The diamines are m-phenylenediamine, p-phenylenediamine, 4,4'-diaminodiphenyl ether, 4,3'-diaminodiphenyl ether, 3,3'-diphenylenediamine, 4,4 One or more of '-diphenylfengdiamine.

[0037] The polar solvent is one or more of N,N-dimethylacetamide, N,N-dimethylformamide, and N-methylpyrrolidone.

...

Embodiment 1

[0048] see figure 1 , Add 2.39g of 4,4'-diaminodiphenyl ether in a three-necked flask and dissolve it in 20.35g of N,N-dimethylacetamide, stir well, then add in batches a total mass of 2.61g of pyromellitic tetracarboxylic acid diphenyl ether anhydride, stirred at room temperature for 5h to obtain a PAA solution;

[0049] Weigh 3.50g of PAA solution and add 5% glycerin, stir well for 2h to obtain casting solution;

[0050] Leave the casting solution to stand or vacuum degassing, use a 100 μm scraper to obtain a film according to the conventional casting method, and then immerse it in an ethanol coagulation bath for 15 minutes, take out the film, dry it naturally, and put it in a muffle furnace for thermal imidization. According to the program of 100°C / 1h, 200°C / 1h, 300°C / 1h, stepwise heating and curing;

[0051] After the temperature dropped to room temperature, the film was peeled off from the glass plate to obtain a polyimide porous film with a thickness of 10 μm, a pore d...

Embodiment 2

[0054] see figure 2 , add 2.39g of 4,4'-diaminodiphenyl ether in a three-necked flask and dissolve it in 20.35g of N,N-dimethylacetamide, stir well, and then add in batches a total mass of 2.61g of pyromellitic tetracarboxylate Acid dianhydride, stirred at room temperature for 5h to obtain PAA solution;

[0055] Weigh 3.50g of PAA solution and add 20% dibutyl phthalate, fully stir for 2h to obtain casting solution;

[0056] Leave the casting solution to stand or vacuum degassing, use a 150 μm scraper to obtain a film according to the conventional casting method, and then immerse it in an ethanol coagulation bath for 25 minutes, take out the film, dry it naturally, and put it in a muffle furnace for thermal imidization. According to the program of 100°C / 1h, 200°C / 1h, 300°C / 1h, stepwise heating and curing;

[0057] After the temperature dropped to room temperature, the film was peeled off from the glass plate to obtain a polyimide porous film with a thickness of 25 μm, a pore...

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Abstract

The invention discloses a porous polyimide film and a preparation method and application thereof. Binary anhydride and diamine are subjected to low-temperature polycondensation reaction in a polar solvent to generate a precursor polyamic acid PAA solution; additives are added into the precursor polyamic acid PAA solution and stirred to form a casting film solution; the casting film solution is defoamed, scraped, coated on a glass plate and immersed in a coagulation bath; then the glass plate is taken out and naturally dried; and the porous polyimide film is obtained through thermal imidization or chemical imidization treatment. The preparation method does not need high temperature and high pressure, has simple requirements on film making equipment, and is favorable for realizing large-scale industrial application. In addition, the film has adjustable thickness, porosity of more than 40%, high liquid absorption rate, good lithium ion electrolyte wettability and excellent high temperature resistance, and is expected to become one of the diaphragm materials for the next generation of lithium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of polyimide film preparation, and in particular relates to a porous polyimide film and its preparation method and application. Background technique [0002] Porous polymer films have attracted considerable attention for their potential applications in catalysts, separation membranes, battery separators, biotechnology, or the synthesis of fine nanostructures. In terms of power batteries, the separator is an indispensable and important part, which requires it to have good ionic conductivity, good electrolyte wettability, high mechanical strength, and thermal and electrochemical stability. In addition, the diaphragm should be as thin as possible and the porosity should be as large as possible under the premise of ensuring sufficient mechanical strength. The substrates for preparing polymer porous membranes are currently mainly polyethylene, polypropylene and additives. However, the melting point of polyethyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08L79/08C08G73/10H01M2/14H01M2/16
CPCC08G73/1007C08G73/1071C08J9/28C08J2201/0502C08J2379/08H01M50/403H01M50/411Y02E60/10
Inventor 韩晓刚李曼妮张洲杰赵斌沈飞白宇鸽尹玉婷
Owner 杭州阳名新能源设备科技有限公司
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