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A kind of polyimide film and its preparation method and application

A polyimide film, polyimide technology, applied in chemical instruments and methods, synthetic resin layered products, layered products, etc., can solve the problems of poor mechanical properties, poor heat resistance, and complex processes of polyimide. And other issues

Active Publication Date: 2022-04-26
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the existing problems in the prior art: low dielectric loss polyimide with fluororesin added has poor mechanical properties, poor high temperature bonding performance, complex process and low dielectric loss polyimide containing aliphatic chains At least one of the problems of low molecular weight, poor heat resistance, etc.

Method used

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  • A kind of polyimide film and its preparation method and application
  • A kind of polyimide film and its preparation method and application
  • A kind of polyimide film and its preparation method and application

Examples

Experimental program
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preparation example Construction

[0049] The synthesis method of the above-mentioned diamine monomer structural formula Ⅱ-1~Ⅱ-7 is similar, reference: J.Chem.Soc.,1958,3298-3313, the following formula Ⅱ-1 is taken as an example, the synthesis steps are as follows:

[0050] Mix 1mol of potassium p-nitro(phenyl)phenate and 0.5mol of 3,4-dibromocyclobutene in 400mL of anhydrous carbon tetrachloride and 400mL of anhydrous acetone, heat at 50°C and reflux for 6-8h, then filter , and the filtrate was evaporated in vacuo. The residue was dissolved in ether, washed successively with water, dilute aqueous sodium hydroxide solution, and water, then the ether solution was dried and evaporated, and crystallized from petroleum ether to obtain 3,4-bis(4-nitrophenoxy)cyclobutane- 1-ene.

[0051] Dissolve 0.5 mol of 3,4-bis(4-nitrophenoxy)cyclobut-1-ene in 200 mL of aqueous acetic acid (85%), add 50 g of iron for reduction, boil the suspension for 3 min, and Filtrate hot, cool, and slowly treat with 200 mL of concentrated h...

Embodiment 1

[0054] (1) Add 13.4060g (0.050mol) 4,4'-(cyclobutyl-3-ene-1,2-diyldioxy)diphenylamine (CBDA) monomer into a dry and clean 500mL three-neck flask, add After 225 g of N-methylpyrrolidone (NMP) was completely dissolved, 10.9060 g (0.050 mol) of pyromellitic dianhydride (PMDA) was added, and under the protection of nitrogen, react at 25°C for 12 hours to obtain a polyamic acid solution;

[0055] (2) above-mentioned polyamic acid solution is coated on dry and clean copper foil and glass flake respectively to form a film;

[0056] (3) Under a nitrogen atmosphere, dry the coated copper foil and glass sheet at 80°C for 6h; then heat to 150°C and keep it for 1h; then heat it to 200°C and keep it for 1h; then heat it to 250°C and keep it for 1h ; Finally, heat to 350°C, keep warm for 1h and then cool to room temperature. The film coated on the glass plate was boiled with boiling water until the polyimide film was removed from the glass plate to obtain a polyimide film with a thickness ...

Embodiment 2

[0058] (1) Add 14.1070g (0.050mol) 4,4'-(cyclopentyl-3-ene-1,2-diyldioxy)diphenylamine (CPDA) monomer into a dry and clean 500mL three-neck flask, add After 225 g of N-methylpyrrolidone (NMP) was completely dissolved, 10.9060 g (0.050 mol) of pyromellitic dianhydride (PMDA) was added, and under the protection of nitrogen, react at 25°C for 12 hours to obtain a polyamic acid solution;

[0059] (2) above-mentioned polyamic acid solution is coated on dry and clean copper foil and glass flake respectively to form a film;

[0060] (3) Under a nitrogen atmosphere, dry the coated copper foil and glass sheet at 80°C for 6h; then heat to 150°C and keep it for 1h; then heat it to 200°C and keep it for 1h; then heat it to 250°C and keep it for 1h ; Finally, heat to 350°C, keep warm for 1h and then cool to room temperature. The film coated on the glass plate was boiled with boiling water until the polyimide film was removed from the glass plate to obtain a polyimide film with a thickness...

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Abstract

The invention provides a polyimide film and its preparation method and application. The polyimide film is obtained by polymerizing a diamine monomer containing a cycloolefin structure and an aromatic dianhydride monomer, followed by imidization. The basicity of the diamine monomer containing the cyclic olefin structure is relatively weak, and the prepared polyimide has a high molecular weight, and in the high-temperature imidization process, the double bonds in the cyclic olefin structure are prone to crosslinking, which greatly improves the Heat resistance of polyimide film. In the polyimide film provided by the present invention, the cyclic hydrocarbon and the benzene ring are non-coplanar, the dielectric loss is significantly reduced, and no fluororesin is added to the film, so that the high-temperature adhesion between the film and the substrate is good, and the tensile strength of the film is good. The high tensile strength solves the problem that the traditional polyimide film cannot balance the dielectric properties, thermal properties and mechanical properties, and the preparation process is simple, so it is suitable for copper clad laminates.

Description

technical field [0001] The invention relates to the field of polyimide films, in particular to a polyimide film and its preparation method and application. Background technique [0002] Due to its excellent heat resistance, mechanical, electrical insulation and chemical resistance, polyimide is widely used in the manufacture of flexible copper clad laminates, which play a role in mechanical support and insulation of electronic circuits. The dielectric constant of common polyimide films is about 3.0, and the dielectric loss tangent is about 0.020. With the rapid development of electronic equipment in recent years and the arrival of the 5G era, the signal frequency band in the 5G era is higher than that in the 4G era, resulting in higher signal loss during circuit board transmission. Therefore, in the 5G era, higher requirements are put forward for the dielectric loss and heat resistance of polyimide. For example, when the signal frequency is higher than 10GHz, the dielectric...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08J5/18C08G73/10B32B15/08B32B15/20B32B27/06B32B27/28B32B33/00B32B37/06
CPCC08J5/18C08G73/1071C08G73/1042C08G73/1064C08G73/1039B32B15/08B32B15/20B32B27/06B32B27/281B32B33/00B32B37/06C08J2379/08B32B2307/204B32B2307/306B32B2307/50
Inventor 李义涛程堂剑云晧邓永茂陈志钊林丽平杨刚张凌飞
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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