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Polyimide film and production process thereof

A polyimide film and production process technology, applied in the field of plastic film manufacturing, can solve the problems of poor alkali resistance and moisture resistance, affecting applications, high imide group content, etc., to achieve improved alkali resistance and moisture resistance, The effect of performance improvement and content reduction

Active Publication Date: 2011-02-02
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of product has high imide group content, so the alkali resistance and moisture resistance are poor, which affects its application in some special fields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] I. Weighing

[0022] Weigh 14.3kg of 4,4'-bis(4-aminophenoxy)diphenyl ether and 11kg biphenyltetracarboxylic dianhydride; solvent N,N'-dimethylacetamide 75kg;

[0023] II. Preparation of resin solution

[0024] Using a reactor with cooling water circulation, first put 4,4'-bis(4-aminophenoxy)diphenyl ether into the N,N'-dimethylacetamide, stir to make it completely dissolved; then batch Put in biphenyltetracarboxylic dianhydride and stir, and control the reaction temperature between 20°C and 70°C; put in 5.5kg of biphenyltetracarboxylic dianhydride for the first time, and add 2.8kg at intervals of 50 minutes for the second time. The third input in 50 minutes, the input amount is 1.4kg, the fourth input at an interval of 50 minutes, the input amount is 0.7kg, the fifth input at an interval of 50 minutes, the input amount is 0.3kg, and finally 0.4kg biphenyltetraic acid Dianhydride is used to adjust the viscosity, that is, a small amount of input at the beginning, the s...

Embodiment 2

[0031] I. Weighing

[0032] Weigh 11.3kg of 4,4'-bis(4-aminophenoxy)diphenyl ether and 8.7kg biphenyltetracarboxylic dianhydride; solvent N,N'-dimethylacetamide 80kg;

[0033] II. Preparation of resin solution

[0034] Using a reactor with cooling water circulation, first put 4,4'-bis(4-aminophenoxy)diphenyl ether into N,N'-dimethylacetamide, stir to dissolve it completely; then put it in batches Biphenyltetracarboxylic dianhydride and stir, and control the reaction temperature between 20°C and 70°C; the first input of biphenyltetracarboxylic dianhydride is 4.4kg, and the second input is 40 minutes apart. The input amount is 2.3kg, and the interval is 30 minutes. The third input in minutes, the input amount is 1.1kg, and the fourth input at an interval of 30 minutes, the input amount is 0.6kg, and the remaining 0.3kg biphenyltetracarboxylic dianhydride is used to adjust the viscosity, and the fifth input at an interval of 30 minutes, The input amount is 0.1kg, and after stir...

Embodiment 3

[0041] I. Weighing

[0042] Take by weighing 5.65kg of 4,4'-bis(4-aminophenoxy) diphenyl ether and 4.35kg biphenyltetracarboxylic dianhydride; solvent N,N'-dimethylacetamide 90kg;

[0043] II. Preparation of resin solution

[0044] Using a reactor with cooling water circulation, first put 4,4'-bis(4-aminophenoxy)diphenyl ether into the N,N'-dimethylacetamide, stir to make it completely dissolved; then batch Put in biphenyltetracarboxylic dianhydride and stir, and control the reaction temperature between 20°C and 70°C; put in 2.2kg of biphenyltetracarboxylic dianhydride for the first time, and add 1.1kg for the second time at intervals of 30 minutes. The third input in 40 minutes, the input amount is 0.55kg, the remaining 0.5kg biphenyltetracarboxylic dianhydride is used to adjust the viscosity, the fourth input is 20 minutes apart, the input amount is 0.1kg, and the resin viscosity is measured after stirring for 20 minutes , did not meet the requirements, the fifth input, th...

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Abstract

The invention relates to a polyimide film and a production process thereof. The polyimide film is mainly formed by the polymerization of material A 4,4'-bis(4-aminophenoxy)diphenylether and material B biphenyl tetracarboxylic acid dianhydride, wherein the ratio of the number of imide groups to the molecular weight of chain links is 2 / 678. The production process comprises the following steps: weighing the material A and the material b according to a weight ratio of 1.3:(0.99-1.0), and using N,N'-dimethyl acetamide as a solvent; throwing the material A into the solvent, stirring until the material A is dissolved, throwing the material B into the solvent in multiple times at a time interval of 20-50 minutes, and stirring, wherein the temperature is limited to 20-70 DEG C, and the weight of the solvent is 3-9 times of the total weight of the material A and the material B; and stopping throwing the material B when the resin viscosity reaches the reaction end point (4.0-7.0*10<5> centipoises) at 30 DEG C, continuing to stir for 4-6 hours to obtain a polyamic acid resin solution, casting into a film, and carrying out imidization; and regulating the viscosity when the material B remains 0.3-0.5 kilogram, wherein 0.03-0.1 kilogram of the material B is thrown each time, and the throwing amount is gradually reduced. The imide group content of the film is greatly reduced, and the alkali resistance and the moisture resistance of the film are greatly improved.

Description

(1) Technical field [0001] The invention relates to a plastic film manufacturing technology, in particular to a polyimide film and a production process thereof. (2) Background technology [0002] Polyimide film is an insulating material with excellent heat resistance, which is widely used in electronics, electrical engineering, aerospace and other industries; the traditional product is mainly isophthalic polyimide film, and its market share is over 80%. , the weight ratio of pyromellitic dianhydride to 4,4'-diaminodiphenyl ether in the raw material is 218 to 200, and the ratio of the number of imide groups to the molecular weight of chain members is 2 / 418. Using N,N'-dimethylacetamide as a solvent, polycondensation reaction is carried out to synthesize a polyamic acid resin solution, and then the obtained resin solution is salivated into a film and undergoes processes such as imidization to obtain a homophenylene polyimide film products. This type of product has high imide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
Inventor 李耀星冯俊杰
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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