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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 th

Method used

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  • Preparation method of self-crosslinking polyimide film
  • Preparation method of self-crosslinking polyimide film

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0026] Example 1

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

[0028] (2) Using the polyimide solution obtained in step (1) as the coating slurry, coating a film at a coating speed of 45 m / min at 30°C, and drying under reduced pressure at 50°C to obtain a polyimide film , the film thickness is 25 μm. In a nitrogen atmosphere, the obtained polyimide film is heat-treated, thermally crosslinked ...

Example Embodiment

[0029] Example 2

[0030] (1) Under nitrogen protection, in a three-necked flask, sequentially add 300 mL of NMP, 12.74 g (0.057 mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA, Changzhou Sunshine Pharmaceutical Co., Ltd., analytically pure), 11.17g (0.038mol) of 3,3'-dichloro-4,4'-diaminobenzoic anilide (Changzhou Sunshine Pharmaceutical, analytically pure), 25.1g (0.095mol) of 3,3 ',4,4'-benzophenone tetracarboxylic dianhydride (Beijing Malmo Technology Co., Ltd., analytical grade), stirred at 5 °C for 12 h; then heated to 120 °C, 140 °C, and 160 °C for 1 h each, and finally heated up The high-viscosity polyimide solution was obtained by reacting at a constant temperature of 190°C for 16h.

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

Example Embodiment

[0032] Example 3

[0033](1) Under nitrogen protection, in a three-necked flask, sequentially add 400 mL of NMP, 17.4 g (0.078 mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA, Changzhou Sunshine Pharmaceuticals, analytically pure), 13.5g (0.052mol) of 3-chloro-4,4'-diaminobenzamide (Changzhou Sunshine Pharmaceutical, analytically pure), 41.66g (0.129mol) of 3,3',4, 4'-benzophenone tetracarboxylic dianhydride (Beijing Malmo Technology Co., Ltd., analytically pure), stirred at 8 °C for 12 h; then heated to 120 °C, 140 °C, and 160 °C for 1 h, and finally heated to a constant temperature of 190 °C The reaction was carried out for 18h to obtain a high viscosity polyimide solution.

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

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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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