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Preparation method of cross-linked poly(arylene ether nitrile) dielectric film with high temperature resistance

A technology of polyarylether nitrile and cross-linking type, which is applied in the field of synthesis of cross-linked polyarylether nitrile, which can solve the problems of metal salts affecting product performance, poor catalyst dispersion, and reducing resin performance, etc., and achieve excellent thermal performance. Performance, excellent heat resistance and mechanical properties, performance-enhancing effect

Active Publication Date: 2019-12-31
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The cross-linking of phthalonitrile-terminated polyarylether nitrile can be mainly through the following three methods: one is to use transition metals and transition metal salts as catalysts, but the poor dispersion of such catalysts is likely to cause incomplete curing , and the residual metal salt also has a certain impact on the performance of the product; the second is to use organic compounds containing polar groups such as organic amines as catalysts, but the introduction of small molecule curing agents will reduce the performance of the resin to a certain extent
The third is heat treatment at high temperature for a long time, but this condition is too harsh

Method used

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  • Preparation method of cross-linked poly(arylene ether nitrile) dielectric film with high temperature resistance
  • Preparation method of cross-linked poly(arylene ether nitrile) dielectric film with high temperature resistance
  • Preparation method of cross-linked poly(arylene ether nitrile) dielectric film with high temperature resistance

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0030] Biphenyl-type polyarylether nitrile end-capped with phthalonitrile containing amino groups in the side chain:

[0031] (1) Add potassium carbonate (0.12mol), biphenol (0.0918mol), 4-aminophenylhydroquinone (0.0102mol) to a reaction flask containing 50ml of dehydrating agent toluene and 75ml of N-methylpyrrolidone , heat the reaction at 130°C to reflux for 2 hours, then remove the water generated by the reaction, and control the reaction temperature between 130-140°C;

[0032] (2) Add 2,6-dichlorobenzonitrile (0.1mol) to the system, keep the reaction between 130-140°C for 1h, then slowly raise the temperature, raise the temperature to 170°C in about 2h, maintain the reaction at 170°C for 2h, react The system reaches the maximum viscosity;

[0033] (3) Lower the system temperature to 100°C, add 4-nitrophthalonitrile (0.02mol), potassium carbonate (0.02mol) and N-methylpyrrolidone (30ml), and then continue the reaction for 4h;

[0034] (4) Pour the obtained crude product...

experiment example 2

[0040] Bisphenol A type polyarylether nitrile end-capped by phthalonitrile containing amino groups in the side chain:

[0041] (1) Add potassium carbonate (0.12mol), bisphenol A (0.0918mol), and 4-aminophenylhydroquinone (0.0102mol) to a reaction flask containing 50ml of dehydrating agent toluene and 75ml of N-methylpyrrolidone , heating the reaction at 130°C to reflux for 2 hours, then removing the water generated by the reaction, and controlling the reaction temperature between 130-140°C;

[0042] (2) Add 2,6-dichlorobenzonitrile (0.1mol) to the system, keep the reaction between 130-140°C for 1h, then slowly raise the temperature, raise the temperature to 170°C in about 2h, maintain the reaction at 170°C for 2h, react The system reaches the maximum viscosity;

[0043] (3) Lower the system temperature to 100°C, add 4-nitrophthalonitrile (0.02mol), potassium carbonate (0.02mol) and N-methylpyrrolidone (20ml), and continue the reaction for 3h;

[0044] (4) Pour the obtained c...

experiment example 3

[0050] Side chain amino-containing phthalonitrile-terminated bisphenol AF type polyarylether nitrile:

[0051] (1) Add potassium carbonate (0.12mol), bisphenol AF (0.0918mol), 4-aminophenylhydroquinone (0.0102mol) to a reaction flask containing 50ml of dehydrating agent toluene and 75ml of N-methylpyrrolidone , heating the reaction at 130°C to reflux for 2 hours, then removing the water generated by the reaction, and controlling the reaction temperature between 130-140°C;

[0052] (2) Add 2,6-dichlorobenzonitrile (0.1mol) to the system, keep the reaction between 130-140°C for 1h, then slowly raise the temperature, raise the temperature to 170°C in about 2h, maintain the reaction at 170°C for 2h, react The system reaches the maximum viscosity;

[0053] (3) Lower the temperature of the system to 100°C, add 4-nitrophthalonitrile (0.02mol), potassium carbonate (0.02mol) and N-methylpyrrolidone (20ml), and then continue the reaction for 4h;

[0054] (4) Pour the obtained crude pr...

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Abstract

The invention relates to a synthesis method for cross-linked poly(arylene ether nitrile) and a preparation method of a high-temperature-resistant dielectric film thereof, belonging to the field of special high-polymer materials. Starting from the main molecular structure design of poly(arylene ether nitrile), hydroxyl-terminated poly(arylene ether nitrile) is synthesized by using hydroquinone withan amino-containing side chain as one of reaction monomers, and then phthalonitrile is introduced to the tail end of a molecular main chain to synthesize the cross-linkable poly(arylene ether nitrile). A cross-linked poly(arylene ether nitrile) film can be obtained by adopting curtain-coating film forming and low-temperature self-cross-linking strategies. The obtained film has excellent thermal properties, mechanical properties and dielectric properties, and can be used as a high-temperature-resistant dielectric film. The preparation method disclosed by the invention is simple in process andeasy for industrial operation, and the application range of the poly(arylene ether nitrile) can be widened.

Description

technical field [0001] The invention relates to a method for synthesizing cross-linked polyarylether nitrile and a method for preparing a high-temperature-resistant dielectric film, belonging to the field of special polymer materials. The cross-linked polyarylether nitrile can be used as a high temperature resistant dielectric film. Background technique [0002] Polyarylether nitrile (PEN) is a kind of polyarylether polymer with cyano group in its side chain. As a special thermoplastic resin, it has attracted widespread attention because of its advantages such as high temperature resistance, chemical corrosion resistance, high strength and high modulus, and easy molding and processing. Compared with polyarylether nitrile, polyarylether ketone, polyarylether sulfone, etc., due to the introduction of molecular side chain cyano functional groups, it has excellent heat resistance and mechanical properties and has more excellent processing performance, which is more important I...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08G65/40C08J5/18C08L71/12
CPCC08G65/4031C08G65/485C08J5/18C08J2371/12
Inventor 黄宇敏开媛林健刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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