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Preparation method of high-strength high-temperature-resistant polyarylene ether nitrile film

A polyarylene ether nitrile and high temperature-resistant technology is applied in the field of preparation of high-strength and high-temperature-resistant polyarylene ether nitrile films, and can solve problems such as the catalyst is not easily dispersed uniformly, the process is cumbersome and complicated, and the performance of the polyarylene ether nitrile resin is reduced.

Active Publication Date: 2021-09-14
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, currently films with relatively high mechanical strength do not have a high glass transition temperature, and the mechanical strength of polyarylene ether nitrile films with a high glass transition temperature still cannot reach a high level, and technical difficulties have not yet been overcome, making it difficult to put into production The factory is industrialized and the output supply is insufficient, so it cannot meet the needs of today's aerospace high-temperature resistant fields and electronic high-tech industries. Therefore, in the case of reducing time and economic costs, a preparation method for high-strength and high-temperature resistant polyarylene ether nitrile films is developed. and its preparation method are particularly important
[0004] Patent CN110628014A discloses a method for preparing a cross-linked polyarylether nitrile high temperature resistant dielectric film. By introducing the amino group of active hydrogen into the polyarylether nitrile terminated by phthalonitrile, the catalytic effect of the amino group is used to improve the cross-linking The speed of the reaction, but the process is relatively cumbersome and complicated, and the amino group of active hydrogen needs to be introduced in the process method, which has stricter requirements on the matrix structure and experimental environment
In addition, there are currently studies using metal salts as catalysts to promote cross-linking reactions, but such catalysts are not easy to disperse uniformly, and the presence of metal ions will reduce the insulation of the system; there are also organic compounds containing active hydrogen atoms as catalysts to speed up cross-linking reactions. Link reaction, but it will reduce the original performance of polyarylether nitrile resin
There is also the use of temperature as an influencing condition to increase the glass transition temperature, but the glass transition temperature in this study is not raised much, and the range is not wide
[0005] The glass transition temperature of the existing polyarylether nitrile material is about 180°C, and it can be used for a long time under the pressure of 230°C. However, the degree of crosslinking of polyarylether nitrile gradually increases under the post-solid-state chemical reaction, and the brittleness will not be comparable. It can meet the processing and preparation process of electronic substrates; and the dielectric constant of the existing polyarylether nitrile film is between 3.5-4.0, and the dielectric loss is between 0.01-0.05, which cannot meet the dielectric properties of 5G electronic substrates Require

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  • Preparation method of high-strength high-temperature-resistant polyarylene ether nitrile film
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  • Preparation method of high-strength high-temperature-resistant polyarylene ether nitrile film

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Embodiment 1

[0034] The first embodiment of the present invention discloses a method of preparing high-strength high-temperature polyaryl ether nitrile films, and the specific steps are as follows:

[0035] S1, preparing an aromatic ether nitrile of a phtotrronlonitrile:

[0036] Additional phenol, biphenol, and 2,6-dichlorodylphenyl nitriles are added to the three-necked flask equipped with a thermometer, a moisture, a condensate reflow device, and a mechanical stirring device, and occurs under the catalysis of potassium carbonate. Nuclear reactive reactions gave mixtures, phenol, biphenol, and 2,6-dichlorobenzene and potassium molar ratio of 1: 4.1: 5: 6, press 3: 1 volume ratio to NMP and Toluene, mixed with the above mixture, the mixture and NMP solid-liquid mass ratio of 1: 1, heated to 180 ° C for polymerization, to obtain a hydroxy-block polyaryl ether nitrile; cool the reactor in all mixtures to 80 ° C, add Potassium carbonate, 4-nitroenenenidyl tetrane, NMP solvent, potassium carbonat...

Embodiment 2

[0045] The second embodiment of the present invention discloses a method of preparing high-strength high-temperature polyaryl ether nitrile films, and the specific steps are as follows:

[0046] S1, preparing an aromatic ether nitrile of a phtotrronlonitrile:

[0047] Additional phenol, biphenol, and 2,6-dichlorodylphenyl nitriles are added to the three-necked flask equipped with a thermometer, a moisture, a condensate reflow device, and a mechanical stirring device, and occurs under the catalysis of potassium carbonate. Nuclear reactive reactions gave mixtures, phenol, biphenol, and 2,6-dichlorobenzene and potassium molar ratio of 1: 4.1: 5: 6, press 3: 1 volume ratio to NMP and Toluene, mixed with the above mixture, the mixture and NMP solid-liquid mass ratio of 1: 1, heated to 180 ° C for polymerization, to obtain a hydroxy-block polyaryl ether nitrile; cool the reactor in all mixtures to 80 ° C, add Potassium carbonate, 4-nitroenenenidyl tetrane, NMP solvent, potassium carbona...

Embodiment 3

[0056] The present invention discloses a method for preparing high strength high temperature polyaryl ether nitrile films, and the specific steps are as follows:

[0057] S1, preparing an aromatic ether nitrile of a phtotrronlonitrile:

[0058] Additional phenol, biphenol, and 2,6-dichlorodylphenyl nitriles are added to the three-necked flask equipped with a thermometer, a moisture, a condensate reflow device, and a mechanical stirring device, and occurs under the catalysis of potassium carbonate. Nuclear reactive reactions gave mixtures, phenol, biphenol, and 2,6-dichlorobenzene and potassium molar ratio of 1: 4.1: 5: 6, press 3: 1 volume ratio to NMP and Toluene, mixed with the above mixture, the mixture and NMP solid-liquid mass ratio of 1: 1, heated to 180 ° C for polymerization, to obtain a hydroxy-block polyaryl ether nitrile; cool the reactor in all mixtures to 80 ° C, add Potassium carbonate, 4-nitroenenenidyl tetrane, NMP solvent, potassium carbonate, 4-nitrophenylene ter...

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Abstract

The invention discloses a preparation method of a high-strength high-temperature-resistant polyarylene ether nitrile film. The preparation method comprises the specific steps of preparing phthalonitrile-terminated polyarylene ether nitrile; preparing a biphenyl type bisphthalonitrile prepolymer; blending and dissolving the obtained phthalonitrile-terminated polyarylene ether nitrile powder and biphenyl bisphthalonitrile prepolymer powder in N-methyl pyrrolidone, and heating and stirring to obtain a transparent solution; and carrying out film forming by a tape casting method, heating, carrying out heat treatment, and naturally cooling to obtain the high-strength high-temperature-resistant polyarylene ether nitrile film. The film obtained by the invention not only has high glass transition temperature, high tensile strength and high modulus, but also has stable dielectric properties.

Description

Technical field [0001] The present invention relates to the technical findings of a polymer material processing process, and more particularly to a method of preparing a high strength high temperature resistant polyaryl ether nitrile film. Background technique [0002] Special high molecular materials are an indispensable military and civilian two-use strategic new materials for the development of air space, nuclear high-speed rail, new energy and other defense military and high-tech industries. R & D levels of advanced high performance polymer materials have become a key factor in reflecting national science and technology strength and technical levels. At present, the rapid development of international science and technology is more strict, and the production of light, small and fine, and large-scale production has put forward higher requirements for reducing material costs. High temperature polyorne ether resin, such as polyaryl ether sulfone, polyether ketone, polyaryl ether ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J3/24C08L71/10C08L79/04C08G65/40C08G65/48
CPCC08J5/18C08J3/24C08G65/4006C08G65/4093C08G65/48C08J2371/10C08J2479/04
Inventor 童利芬何亮刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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