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Polyimide precursor and preparation method and application thereof

A technology of polyimide precursor and polyamic acid, which is applied in the field of polyimide precursor and its preparation and application, can solve the problems of high thermal expansion coefficient of polyimide, difficult to control the decline of product quality, and reduce the CTE of materials , achieve excellent heat resistance, avoid precision and difficulty, and improve quality

Pending 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 the high coefficient of thermal expansion of polyimide in the prior art and the problem that the technical process is difficult to control the decline in product quality. A polyimide precursor is provided. The precursor of the polyimide The blending method of the polyamic acid solution in the flexible structure can effectively reduce the CTE of the material, and the polyamic acid solution with a narrow molecular weight distribution and a very low gel particle content is easy to control stably in the subsequent processing. And the product is not easy to produce defects, and high-performance polyimide products can be obtained

Method used

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  • Polyimide precursor and preparation method and application thereof
  • Polyimide precursor and preparation method and application thereof
  • Polyimide precursor and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] (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.

[0048] (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.

[0049] (3) Mix the polyamic acid A solution and the polyamic acid B solution at a mas...

Embodiment 2

[0051] (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.

[0052] (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.

[0053] (3) Mix the polyamic acid A solution and the polyamic acid B solution at a ma...

Embodiment 3

[0055] (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.

[0056] (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.

[0057] (3) Mix the polyamic acid A solution and the polyamic acid B solution at a mass ratio of 1:15. 2 After stirring for 1 hou...

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Abstract

The invention provides a polyimide precursor as well as a preparation method and application thereof, and mainly solves the problems of high thermal expansion coefficient, difficulty in control the technical process, and decreased product quality in the prior art. The polyimide precursor comprises a polyamic acid solution A and a polyamic acid solution B, wherein the mass ratio of the polyamic acid solution A to the polyamic acid solution B is 1: (2-20) based on the mass of the polyamic acid; the polyamic acid B is polyamic acid containing a flexible chain segment; 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 materials.

Description

technical field [0001] The invention relates to a precursor of polyimide and its preparation method and application. 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 ordina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08J5/18C08G73/10
CPCC08L79/08C08J5/18C08G73/1067C08G73/1071C08G73/1007C08J2379/08C08J2479/08C08L2205/025
Inventor 崔晶孙旭阳刘京妮陈雪
Owner CHINA PETROLEUM & CHEM CORP
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