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Polyamic acid solution and preparation method thereof, polyimide, polyimide film

A polyamic acid and solution technology, applied in polyimide film, polyamic acid solution and its preparation, and polyimide field, can solve the problem that the molecular weight of the polymer cannot be reduced, the comprehensive performance of the polyimide is reduced, and the polyamide The problem of high viscosity of acid solution can achieve the effect of excellent dimensional stability, enhanced mechanical properties and heat resistance, and excellent mechanical properties

Active Publication Date: 2022-05-06
JILIN OPTICAL & ELECTRONICS MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the viscosity of polyamic acid solution is very high, and even gel will occur when the molecular weight reaches a certain level.
In order to meet the process requirements, the viscosity of the polyamic acid solution needs to be controlled without reducing the molecular weight of the polymer, otherwise the overall performance of the polyimide will be reduced

Method used

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  • Polyamic acid solution and preparation method thereof, polyimide, polyimide film
  • Polyamic acid solution and preparation method thereof, polyimide, polyimide film
  • Polyamic acid solution and preparation method thereof, polyimide, polyimide film

Examples

Experimental program
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Effect test

Embodiment 1

[0057] This embodiment provides a kind of polyamic acid solution and polyimide film, and concrete preparation method comprises the following steps:

[0058] S1. Under the protection of nitrogen, add 4.56g of p-phenylenediamine and 124.33g of N-methyl-2-pyrrolidone into the reactor with a stirring paddle and a thermometer. Dissolve diamine, add 10.00g pyromellitic dianhydride and 10.00g N-methyl-2-pyrrolidone, react for 2 hours, add 0.28g glycine and 10.00g N-methyl-2-pyrrolidone, react for 2 hours, add 4.96g p-Phenylenediamine and 10.00g N-methyl-2-pyrrolidone, after p-phenylenediamine is completely dissolved, add 9.20g pyromellitic dianhydride and 10.00g N-methyl-2-pyrrolidone, and react for 48h to obtain A polyamic acid solution with a solid content of 15%.

[0059] S2. Take the polyamic acid solution prepared above and filter it with a filter. The filter membrane size is 5 μm. The filtered solution is degassed under reduced pressure. Take 20 mL of the treated solution and ...

Embodiment 2

[0061] This embodiment provides a kind of polyamic acid solution and polyimide film, and specific preparation method comprises the following steps:

[0062] S1. Under the protection of nitrogen, add 3.23g of p-phenylenediamine and 64.08g of N-methyl-2-pyrrolidone into the reactor with a stirring paddle and a thermometer. Dissolve the diamine, add 10.00g 3,3',4,4'-biphenyltetracarboxylic dianhydride and 10.00g N-methyl-2-pyrrolidone, add 0.31g glycine and 10.00g N-methyl-2-pyrrolidone after reacting for 2 hours 2-pyrrolidone, react for 2 hours, add 3.68g p-phenylenediamine and 10.00g N-methyl-2-pyrrolidone, after p-phenylenediamine is completely dissolved, add 8.8g 3,3',4,4'-biphenyl Tetracarboxylic dianhydride and 10.00 g of N-methyl-2-pyrrolidone were reacted for 48 hours to obtain a polyamic acid solution with a solid content of 20%.

[0063] S2. The post-treatment and film-forming process of the polyamic acid solution are the same as in Example 1, and a polyimide film can ...

Embodiment 3

[0065] This embodiment provides a kind of polyamic acid solution and polyimide film, and specific preparation method comprises the following steps:

[0066] S1. Under the protection of nitrogen, add 5.68g of 4,4'-diaminodiphenyl ether and 86.28g of N-methyl-2-pyrrolidone into the reactor with a stirring paddle and a thermometer at a speed of 300rpm. Stir under conditions until 4,4'-diaminodiphenyl ether is dissolved, add 10.00g 4,4'-oxydiphthalic anhydride and 10.00g N-methyl-2-pyrrolidone, add 0.64g benzene after 2 hours of reaction Alanine and 10.00g N-methyl-2-pyrrolidone, react for 2h, add 6.45g 4,4'-diaminodiphenyl ether and 10.00g N-methyl-2-pyrrolidone, and wait for 4,4'-di After the aminodiphenyl ether was completely dissolved, 8.8g of 4,4'-oxydiphthalic anhydride and 10.00g of N-methyl-2-pyrrolidone were added and reacted for 48 hours to obtain a polyamic acid solution with a solid content of 20%.

[0067] S2. The post-treatment and film-forming process of the polyam...

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Abstract

The invention discloses a polyamic acid solution, a preparation method thereof, polyimide and a polyimide film, and belongs to the technical field of polymer materials. The polyamic acid solution includes repeating units of polyamic acid and amino acids and / or or its derivatives end-capped end unit; the structural formula of the repeating unit of the polyamic acid is: in the formula, X represents an alicyclic or aromatic ring quaternary organic group with 4 or more carbon atoms; Y represents a carbon An alicyclic or aromatic ring divalent organic group having 4 or more atoms, n represents a positive integer. The present invention introduces an amino acid and / or its derivatives carrying an amino group and a carboxyl group, and the carboxyl group reacts with the amino group at the end of the molecular chain during the thermal imidization process to realize the growth of the molecular chain, which can improve the efficiency of the polymerization process. The mechanical properties, heat resistance and dimensional stability of the polyimide prepared from the amic acid solution can reduce the viscosity of the polyamic acid solution under the premise of ensuring a certain solid content.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a polyamic acid solution and a preparation method thereof, polyimide, and a polyimide film. Background technique [0002] Because polyimide contains very stable aromatic rings and imide rings in its molecular chain, it is a kind of polymer material with the best temperature resistance among existing materials, and its performance is basically unchanged no matter in low temperature or high temperature environment. The maximum thermal decomposition temperature can reach 600°C, making it one of the most high-temperature-resistant polymers so far. In addition, polyimide also has excellent mechanical properties, dielectric properties, dimensional stability, flame retardancy, etc. [0003] Due to the outstanding comprehensive properties, polyimide has a wide range of uses. Film is the earliest application method of polyimide, which is mainly used for electrical insulation m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08L79/08C08J5/18
CPCC08G73/1067C08G73/1071C08G73/1007C08J5/18C08J2379/08
Inventor 马晓宇赵贺张求学吕庆龙杨天宇张雪
Owner JILIN OPTICAL & ELECTRONICS MATERIALS