A kind of high strength and high heat resistance polyimide microporous film and preparation method thereof

A polyimide and microporous film technology, applied in the field of polymer material preparation, can solve problems such as uneven cell structure, poor mechanical properties, and poor high-temperature performance, and achieve enhanced interaction, improved mechanical properties, and heat resistance good sex effect

Active Publication Date: 2019-05-07
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the dianhydrides and diamines used in these methods are all conventional monomers, and the glass transition temperature of the prepared microporous film is about 250°C, and the long-term use and high temperature resistance are about 200°C. Inhomogeneous cell structure and poor mechanical properties
[0006] In short, the above methods obtained are all conventional polyimide microporous film materials, which have poor resistance to high temperatures above 300°C and have defects such as poor mechanical properties.

Method used

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  • A kind of high strength and high heat resistance polyimide microporous film and preparation method thereof
  • A kind of high strength and high heat resistance polyimide microporous film and preparation method thereof
  • A kind of high strength and high heat resistance polyimide microporous film and preparation method thereof

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preparation example Construction

[0039] The preparation method of the high-strength and high-heat-resistant polyimide microporous film provided by the present invention comprises the following steps:

[0040](1) Dissolving the aromatic tetra-acid dianhydride in an organic solvent, adding diamine in an equimolar amount to the dianhydride and a certain amount of porogen, stirring and reacting for 6-8 hours, and finally obtaining a homogeneous polyamic acid solution.

[0041] (2) Uniformly coating the obtained polyamic acid resin solution on a glass plate to prepare a resin film with uniform thickness.

[0042] (3) heat-treat the obtained polyamic acid resin film in a nitrogen-filled oven at 80°C for 10 hours, then gradually raise the temperature to 280-300°C and keep it for 3-5 hours for thermal imidization, and finally obtain polyimide micropores film.

[0043] In the present invention, the dianhydride is one of pyromellitic dianhydride, 4,4'-biphenyltetracarboxylic dianhydride, and 3,3',4,4'-benzophenone eth...

Embodiment 1

[0054] At 0°C, add 26.34g of N,N-dimethylacetamide solvent into the three-necked flask, and add 3.22g (0.01mol) of 3,3',4,4'-benzophenone ether tetracarboxylic acid di anhydride and stir to dissolve, after the dissolution is complete, add 1.6g (0.008mol) 4,4'-diaminodiphenyl ether and 0.448g (0.002mol) 2-(4-aminophenyl)-5-aminobenzimidazole, and then Then, 3.512 g of dibutyl phthalate was added and stirred for 6 hours to obtain a homogeneous polyamic acid resin solution. The obtained polyamic acid resin solution was evenly coated on a glass plate to prepare a film with a uniform thickness of 400 μm. The polyamic acid resin film was heat-treated in a nitrogen-filled oven at 80°C for 10 hours, then gradually raised to 300°C and kept for 4 hours for thermal imidization, and finally a polyimide microporous film was obtained.

[0055] The performance of the obtained polyimide microporous film is measured, and the microscopic appearance of the obtained microporous film is as follow...

Embodiment 2

[0057] At 0°C, add 32.44g of N,N-dimethylacetamide solvent into the three-necked flask, and add 3.22g (0.01mol) of 3,3',4,4'-benzophenone ether tetracarboxylic acid di anhydride and stir to dissolve, after the dissolution is complete, add 1.608g (0.006mol) 2-trifluoromethyl-4,4'-diaminodiphenyl ether and 0.896g (0.004mol) 2-(4-aminophenyl)-5 -Aminobenzimidazole, then add 9.54g dibutyl phthalate and stir for 6 hours. Finally, a homogeneous polyamic acid resin solution is obtained. The obtained polyamic acid resin solution was evenly coated on a glass plate to prepare a film with a uniform thickness of 200 μm. The polyamic acid resin film was heat-treated in a nitrogen-filled oven at 80°C for 10 hours, then gradually raised to 300°C and kept for 3 hours for thermal imidization, and finally a polyimide microporous film was obtained.

[0058] The obtained polyimide microporous film performance is measured, and the microscopic appearance of the polyimide microporous film obtained...

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Abstract

The invention provides a high-strength high-heat-resistance polyimide microporous thin film and a preparation method thereof. The preparation method includes: enabling dianhydride and two kinds of diamine to be in copolymerization in an organic solvent; adding a certain amount of a hole forming agent in the reaction process to finally obtain a polyamide acid resin solution; coating the resin solution for film forming; performing thermal treatment and thermal imidization treatment to obtain the polyimide microporous thin film, wherein content of aromatic heterocycte diamine 2-(4-amino phenyl)-5-aminobenzooxazole or 2-(4-amino phenyl)-5-aminobenzoimidazole accounts for 20-60% of total molar weight of diamine. The polyimide thin obtained by the method is high in glass transition temperature, good in heat resistance and excellent in mechanical performance. Experimental results show that the polyimide microporous thin film prepared by the method is smooth in surface and uniform in pore distribution, pore size range is 5-30 um, tensile strength is 20-80 MPa, glass transition temperature is greater than 30 DEG C, and thermal weight loss temperature is 510-550 DEG C.

Description

technical field [0001] The invention relates to a high-strength and high-heat-resistant polyimide microporous film and a preparation method thereof, belonging to the field of polymer material preparation. Background technique [0002] Porous polymer materials are an important branch in the field of polymer materials. Porous polyimide materials have excellent properties such as heat resistance, heat insulation, noise reduction, impact resistance, dimensional stability, wave transparency and flame retardancy. They can be used as media Electricity, wave absorption, sound insulation and heat insulation and flame retardant materials have a wide range of applications. Especially in cutting-edge technology fields such as aerospace aircraft, surface ships, submarines, rail transit and microelectronics. In some special application fields, it is required to have more excellent mechanical properties, high temperature resistance, radiation resistance, heat and humidity resistance and c...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08J9/28C08G73/10
CPCC08G73/1007C08G73/1046C08G73/105C08J5/18C08J9/28C08J2379/08
Inventor 张广成李建伟姚瑶周立生李建通景占鑫
Owner NORTHWESTERN POLYTECHNICAL UNIV
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