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Polyimide film with stable size and preparation method thereof

A technology for polyimide film and polyamic acid film, which is applied in the field of polyimide film and its preparation, can solve the problems of high thermal expansion coefficient of polyimide film, difficult process control, product quality decline, etc. Improve regularity and bulk density, achieve dimensional stability and overall performance, and reduce CTE

Active Publication Date: 2020-05-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the technical problems to be solved by the present invention is that the thermal expansion coefficient of the polyimide film in the prior art is high and the process is difficult to control, and the product quality declines. A polyimide film with stable dimensions and small thermal expansion coefficient is provided. Thin film, the precursor solution of the polyimide film is blended in the flexible structure to add the rigid segment can effectively reduce the CTE of the material, and the polyamic acid with a narrow molecular weight distribution and a very low gel particle content is used solution, it is easy to control stably during film processing, and the film is not easy to produce defects, and high-performance polyimide film products can be obtained

Method used

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  • Polyimide film with stable size and preparation method thereof
  • Polyimide film with stable size and preparation method thereof
  • Polyimide film with stable size and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] 1. Stock solution preparation

[0060] (1) Dissolve p-phenylenediamine in N,N-dimethylacetamide, 2 Stir under protection, after completely dissolving, continuously and uniformly add pyromellitic dianhydride (dianhydride, diamine molar ratio 0.98, solid content 15%), feed time is 3 hours, after pyromellitic dianhydride is added After fully reacting for 3 hours, add 4-phenylethynylphthalic anhydride capping agent to the above system, and continue stirring for 2 hours to obtain a polyamic acid A solution.

[0061] (2) Dissolve 4,4'-diaminodiphenyl ether in N,N-dimethylacetamide, 2 Stir under protection, after complete dissolution, continuously and uniformly add 3,3',4,4'-biphenyltetracarboxylic dianhydride (the molar ratio of dianhydride and diamine is 0.98, the solid content is 15%), and the feeding time is 3 hours After the dianhydride was added, the polyamic acid B solution was obtained after fully reacting for 3 hours.

[0062] (3) Mix the polyamic acid A solution a...

Embodiment 2

[0069] 1. Stock solution preparation

[0070] (1) Dissolve p-phenylenediamine in N,N-dimethylacetamide, 2 Stir under protection, after completely dissolving, add pyromellitic dianhydride (dianhydride to diamine molar ratio 0.95, solid content 25%) continuously and at a uniform speed, feed time is 6 hours, after pyromellitic dianhydride is added After fully reacting for 10 hours, add a phenylethynyl trimellitic anhydride capping agent to the above system, and continue stirring for 3 hours to obtain a polyamic acid A solution.

[0071] (2) Dissolve 4,4'-diaminodiphenyl ether in N,N-dimethylacetamide, 2 Stir under protection, after completely dissolving, continuously and uniformly add 3,3',4,4'-benzophenone tetracarboxylic dianhydride (dianhydride, diamine molar ratio 1.03, solid content 25%), the feeding time is After 4 hours, the polyamic acid B solution was obtained after fully reacting for 6 hours after adding the dianhydride.

[0072] (3) Mix the polyamic acid A solution ...

Embodiment 3

[0076] 1. Stock solution preparation

[0077] (1) Dissolve p-phenylenediamine in N,N-dimethylpyrrolidone, 2 Stir under protection, after completely dissolving, continuously and uniformly add pyromellitic dianhydride (dianhydride, diamine molar ratio 0.992, solid content 12%), feed time is 4 hours, after pyromellitic dianhydride is added After fully reacting for 2 hours, add a phenylethynyl trimellitic anhydride capping agent to the above system, and continue stirring for 2 hours to obtain a polyamic acid A solution.

[0078] (2) Dissolve diaminodiphenylmethane in N,N-dimethylpyrrolidone, stir at 20°C under N2 protection, after completely dissolving, add 3,3',4,4'-biphenyl tetra Formic acid dianhydride (dianhydride, diamine molar ratio 0.996, solid content 12%), the feeding time is 2 hours, after the dianhydride is added, fully react for 10 hours to obtain the polyamic acid B solution.

[0079] (3) Mix the polyamic acid A solution and the polyamic acid B solution at a mass ra...

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Abstract

The invention provides a polyimide film with a stable size and a preparation method thereof, and mainly solves the problems of poor size stability of polyimide films, difficult control of the technological process and unstable product quality in the prior art. The polyimide film is prepared from a precursor solution through film formation and thermal imidization, wherein the precursor solution comprises a mixture of a polyamic acid solution A and a polyamic acid solution B; the mass ratio of the polyamic acid solution A to the polyamic acid solution B is 1: (2-20) based on the mass of polyamicacid; the polyamic acid B is polyamic acid containing a flexible chain segment; and the structure of the polyamic acid A is shown as a formula (I). The problems are well solved, and the preparation method can be applied to industrial production of polyimide films.

Description

technical field [0001] The invention relates to a dimensionally stable polyimide film and a preparation method thereof. Background technique [0002] Polyimide is a kind of polymer with excellent comprehensive performance, which has excellent heat resistance, low temperature resistance, self-lubrication, radiation resistance and flame retardancy, as well as excellent mechanical properties and dielectric properties , Widely used in aerospace, microelectronics, solar cells, high temperature filtration, machinery, separation membranes and OLEDs and other fields. Polyimides used in high-end fields such as flexible circuit substrates, OLED substrates, etc. have high requirements on the dimensional stability of materials, and how to reduce the coefficient of thermal expansion (CTE) of polyimide materials and improve the dimensional stability of materials is An important research direction for the development of high-performance polyimide materials. [0003] The main chain of ord...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08J5/18C08G73/10
CPCC08J5/18C08G73/1067C08G73/1071C08J2379/08C08J2479/08Y02E10/549
Inventor 刘京妮孙旭阳崔晶陈雪
Owner CHINA PETROLEUM & CHEM CORP
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