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Polyamide acid and preparation method thereof, polyimide and preparation method of polyimide film

A polyimide film and polyimide technology are applied in the field of intermediate polyamic acid and preparation, polyimide and polyimide film preparation, and can solve the problem of poor solubility, poor solubility and difficult processing. Polyimide materials and other problems, to achieve the effect of improving solubility, good processability, simple and reliable production process

Active Publication Date: 2019-05-10
武汉柔显科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of polyimide has the problem of poor solubility. When it is used in the production of polyimide film materials, the technical problems of poor solubility and difficult processing often limit the application of polyimide materials.

Method used

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  • Polyamide acid and preparation method thereof, polyimide and preparation method of polyimide film
  • Polyamide acid and preparation method thereof, polyimide and preparation method of polyimide film
  • Polyamide acid and preparation method thereof, polyimide and preparation method of polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Polyimide film embodiment 1 (PMDA / p-ABO / ODA)

[0057] In a three-neck flask (100ml) equipped with a stirring rod and a nitrogen inlet, add 4,4-diaminodiphenyl ether (ODA) (1.001g, 0.005mol), Y1-NH 2 6-amino-2-(4-(4-aminophenyl) phenyl)-benzoxazole (p-ABO) (1.587g, 0.005mol) and N-methylpyrrolidone (30ml ), wherein the sum of the molar weights of ODA and AAB is 0.01mol. Under the protection of nitrogen, after mechanical stirring at 0~50° C. to be completely dissolved, add pyromellitic anhydride (PMDA) (2.181 g, 0.01 mol) to the solution, keep the temperature of the reaction system constant, react 1 to 24 hours to obtain a polyamic acid solution with a viscosity of 10.7Pa·s; after the above polyamic acid solution is decompressed to eliminate air bubbles, it is coated on a clean glass plate with a wet film thickness of 1 to 300μm, and then heated at 80°C After drying in a vacuum oven for 5 hours, it was cured in a nitrogen oven at 150° C. for 1 hour, 350° C. for 1 hour, ...

Embodiment 2

[0058] Polyimide film embodiment 2 (PMDA / m-ABO / ODA)

[0059] Except for Y2-NH 2 6-amino-2-(3-(4-aminophenyl)phenyl)-benzoxazole (m-ABO) (1.587g, 0.005mol) of Experimental Example 1 replaced 6-amino-2-(4- Except for (4-aminophenyl)phenyl)-benzoxazole (p-ABO), the others were the same as in Example 1 to obtain a polyimide film 2. However, the obtained polyamic acid solution had a viscosity of 5.42 Pa·s.

Embodiment 3

[0060] Polyimide film embodiment 3 (s-BPDA / p-ABO / PPD)

[0061] In a three-neck flask (100ml) equipped with a stirring rod and a nitrogen inlet, add p-phenylenediamine (PPD) (0.541g, 0.005mol), Y1-NH 2 6-amino-2-(4-(4-aminophenyl) phenyl)-benzoxazole (p-ABO) (1.587g, 0.005mol) and N-methylpyrrolidone (30ml ), wherein the sum of the molar weights of PPD and AAB is 0.01mol. Under the protection of nitrogen, stir mechanically at 0~50°C and after the solution is completely dissolved, add 3,3′,4,4′-biphenyltetracarboxylic dianhydride (s-BPDA) (2.942g , 0.01mol), keep the temperature of the reaction system constant, and react for 1-24 hours to obtain a polyamic acid solution with a viscosity of 5.67Pa·s; decompress the above polyamic acid solution to eliminate air bubbles, and then coat it on a clean glass plate , with a wet film thickness of 1-300 μm, followed by drying in a vacuum oven at 80°C for 5 hours, followed by curing in a nitrogen oven at 150°C for 1 hour, 350°C for 1 hou...

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Abstract

The invention discloses polyamide acid and a preparation method thereof, polyimide and a preparation method of polyimide film. The preparation method of the polyamide acid comprises: mixing polyphosphoric acid, 2,4-diaminophenol dihydrochloride, 4-(4-aminophenoxy)benzoic acid or 3-(4-aminophennoxy)benzoic acid, and tin powder, and dissolving by stirring to obtain a homogenous solution; adding phosphorus pentoxide, allowing to react to obtain a reaction product, precipitating the reaction product, filtering, and washing to an ether bond-modified diamine with benzoxazole structure; mixing an aromatic diamine and the ether bond-modified diamine with benzoxazole structure, adding the mixture to a polar organic solvent, and dissolving by stirring to obtain a diamine monomer mixed solution; adding an aromatic dianhydride, and allowing to react to obtain polyamide acid solution; coating the surface of a substrate with the polyamide acid solution, and drying and solidifying to obtain the polyimide film. The polyimide film herein has good solubility, good mechanical properties and high heat resistance.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular, the invention relates to an intermediate polyamic acid and a preparation method thereof, a polyimide and a preparation method of a polyimide film. Background technique [0002] Polyimides, especially aromatic polyimides, are widely used in electric / electronic devices and semiconductors due to their excellent physical and chemical properties, including thermal stability, resistance to dissolution, excellent insulation properties, and radiation resistance and other fields. For example, copper-clad laminate substrate materials in flexible printed wiring boards. In recent years, with the development of the display field, light and flexible polymer materials have been used instead of glass substrates for display screens. Therefore, higher performance polymer materials are required. [0003] It is the direction that those skilled in the art are committed to research by intro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 颜枫肖桂林鲁丽萍朱双全
Owner 武汉柔显科技股份有限公司
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