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Preparation method of self-crosslinking polyimide film

A polyimide film and self-crosslinking technology, which is applied in the field of preparation of self-crosslinking polyimide film, can solve the problem of polyimide film dimensional stability, heat resistance, mechanical properties and solvent resistance And other problems such as poor performance, to achieve good industrialization prospects, simple operation, and the effect that is conducive to mass production

Active Publication Date: 2019-08-06
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is to provide a preparation method of self-crosslinking polyimide film, to overcome the dimensional stability, heat resistance, mechanical properties and solvent resistance of polyimide film in the prior art. poor performance defect

Method used

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  • Preparation method of self-crosslinking polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Under nitrogen protection, in a three-necked flask, add 250mL of NMP and 8.87g (0.04mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA, Changzhou Sunshine Pharmaceutical Co., Ltd., Analytical pure), 4.42g (0.017mol) of 3-chloro-4,4'-diaminobenzanilide (Changzhou Sunshine Pharmaceutical, analytical pure), 25.1g (0.057mol) of hexafluorodianhydride (Zhejiang Nuo Cheng Technology, analytically pure), stirred and reacted at 5°C for 10h; then raised the temperature to 120°C, 140°C, and 160°C for 1h each, and finally raised the temperature to 190°C for 12h to obtain a high-viscosity polyimide solution.

[0028] (2) Use the polyimide solution prepared in step (1) as the coating slurry, coat the film at a coating speed of 45m / min at 30°C, and dry it under reduced pressure at 50°C to obtain a polyimide film , film thickness is 25 μm. In a nitrogen atmosphere, the obtained polyimide film was heat-treated, thermally cross-linked at 350° C. for 0.5 h, and reacted at 400° C. fo...

Embodiment 2

[0030] (1) Under nitrogen protection, in a three-necked flask, add 300mL of NMP and 12.74g (0.057mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA, Changzhou Sunshine Pharmaceutical Co., Ltd., Analytical pure), 11.17g (0.038mol) of 3,3'-dichloro-4,4'-diaminobenzanilide (Changzhou Sunshine Pharmaceutical, analytically pure), 25.1g (0.095mol) of 3,3 ',4,4'-Benzophenonetetraacid dianhydride (Beijing Malmo Technology Co., Ltd., analytically pure), stirred and reacted at 5°C for 12h; then raised the temperature to 120°C, 140°C, and 160°C for 1h respectively, and finally raised the temperature React at a constant temperature of 190° C. for 16 hours to obtain a high-viscosity polyimide solution.

[0031] (2) Use the polyimide solution prepared in step (1) as the coating slurry, coat the film at a coating speed of 50m / min at 40°C, and dry it under reduced pressure at 50°C to obtain a polyimide film , film thickness is 30 μm. In a nitrogen atmosphere, the obtained polyimide film wa...

Embodiment 3

[0033](1) Under nitrogen protection, in a three-necked flask, add 400mL of NMP and 17.4g (0.078mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA, Changzhou Sunshine Pharmaceutical Co., Ltd., Analytical pure), 13.5g (0.052mol) of 3-chloro-4,4'-diaminobenzanilide (Changzhou Sunshine Pharmaceutical, analytical pure), 41.66g (0.129mol) of 3,3',4, 4'-Benzophenonetetraacid dianhydride (Beijing Malmo Technology Co., Ltd., analytically pure), stirred and reacted at 8°C for 12h; then raised the temperature to 120°C, 140°C, and 160°C for 1h each, and finally raised the temperature to 190°C at a constant temperature After 18 hours of reaction, a high-viscosity polyimide solution was obtained.

[0034] (2) Use the polyimide solution prepared in step (1) as the coating slurry, coat the film at a coating speed of 50m / min at 40°C, and dry it under reduced pressure at 60°C to obtain a polyimide film , film thickness is 30 μm. In a nitrogen atmosphere, the obtained polyimide film was heat-...

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Abstract

The invention relates to a preparation method of a self-crosslinking polyimide film. The method comprises the following steps of: adding a benzimidazole heterocyclic diamine monomer and a halogen substituent-containing diamine monomer into a polar aprotic solvent, adding a dianhydride monomer for reaction, performing coating, drying and curing on the obtained polyimide solution to obtain a polyimide film, and performing heat treatment. The method is simple to operate, environmentally friendly in process, beneficial to large-scale preparation, and has a good industrialization prospect. And theobtained crosslinked film has excellent heat resistance, solvent resistance, radiation resistance and corrosion resistance, can be applied to extreme environments or special environments, and furtherexpands the application range of the materials.

Description

technical field [0001] The invention belongs to the field of preparation of polyimide films, in particular to a preparation method of self-crosslinking polyimide films. Background technique [0002] Polyimide (Polyimide, PI) is a class of high-performance organic polymers containing imide rings in the molecular chain. It has excellent comprehensive properties such as high mechanical strength, high temperature resistance, and ultraviolet resistance. It can be used in microelectronics, aerospace High-tech fields such as science and technology and military equipment. With the rapid progress of science and technology and the improvement of industrial level, many high-end application fields have put forward higher requirements on the performance of polyimide materials, such as dimensional stability, heat resistance and other properties still need to be further improved. Among them, as the most widely used type of polyimide products at present, polyimide films are widely used in ...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08G73/10C08L79/08
CPCC08G73/1039C08G73/1067C08G73/1085C08J5/18C08J2379/08
Inventor 张清华甘锋董杰赵昕吴婷婷方玉婷李琇廷李猛猛徐小尘
Owner DONGHUA UNIV
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