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Preparation method of high-temperature-resistant polyimide film

A technology of polyimide film and high temperature resistance, which is applied in the field of preparation of high temperature resistant polyimide film, can solve problems affecting the mechanical properties of composite films, achieve energy saving and environmental protection in the production process, solve agglomeration, and simple methods

Inactive Publication Date: 2018-09-14
HUBEI DINGLONG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The present invention provides a preparation method of high temperature resistant polyimide film, by using surface-modified nano-silica or aluminum oxide particles, it solves the problem of nano-particles in polyimide mentioned in the background above. Agglomeration affects the mechanical properties of the composite film, and a composite film material with excellent thermal stability, processability and mechanical properties has been prepared

Method used

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  • Preparation method of high-temperature-resistant polyimide film
  • Preparation method of high-temperature-resistant polyimide film
  • Preparation method of high-temperature-resistant polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] S1. Dissolve 1.08 g (0.01 mol) of p-phenylenediamine in 30 ml of dry N-methylpyrrolidone at room temperature, under nitrogen protection, mechanically stir until completely dissolved, then add 3.24 g (0.011 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, continue to stir for 1h;

[0036]S2. Add 0.16 g (0.001 mol) of norbornene diacid anhydride, which is the end-capping agent NA anhydride, fully stir at 50 ° C, and react for 8 hours to obtain a polyamic acid solution with a solid content of about 15 wt %;

[0037] S3. Disperse hydrophobic silicon dioxide powder with a particle size not greater than 100nm in N-methylpyrrolidone solvent, and stir for 1 h to fully disperse to a macroscopically clear and transparent 1 wt% colloidal solution. Then the colloid solution and the polyamic acid solution were mixed according to 1:20 (mass ratio), and stirred for 2 h to make them evenly mixed;

[0038] Among them, the modification method of hydrophobic silica is: add 5.0g of ...

Embodiment 2

[0041] S1. Dissolve 1.08 g (0.01 mol) of p-phenylenediamine in 30 ml of dry N-methylpyrrolidone at room temperature, under nitrogen protection, mechanically stir until completely dissolved, then add 3.24 g (0.011 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, continue to stir for 1h;

[0042] S2. Add 0.16 g (0.001 mol) of end-capping agent NA anhydride, fully stir at 50 °C, and react for 8 hours to obtain a polyamic acid solution with a solid content of about 15 wt%.

[0043] S3. Disperse the hydrophobic silica powder in N-methylpyrrolidone solvent, stir for 1 h to fully disperse to a macroscopically clear and transparent 1 wt% colloidal solution. Then the colloid solution and the polyamic acid solution were mixed according to 1:10 (mass ratio), and stirred for 2 h to make them evenly mixed.

[0044] S4. After the above-mentioned polyamic acid solution containing nanoparticles is decompressed to eliminate bubbles, it is coated on a clean glass plate with a film thickn...

Embodiment 3

[0046] S1. Dissolve 1.08 g (0.01 mol) of p-phenylenediamine in 30 ml of dry N-methylpyrrolidone at room temperature, under nitrogen protection, mechanically stir until completely dissolved, then add 3.24 g (0.011 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, continue to stir for 1h;

[0047] S2. Add 0.16 g (0.001 mol) of end-capping agent NA anhydride, fully stir at 50 °C, and react for 8 hours to obtain a polyamic acid solution with a solid content of about 15 wt%.

[0048] S3. Disperse the hydrophobic silica powder in N-methylpyrrolidone solvent, stir for 1 h to fully disperse to a macroscopically clear and transparent 1 wt% colloidal solution. Then the colloid solution and the polyamic acid solution were mixed according to 1:5 (mass ratio), and stirred for 2 h to make them evenly mixed.

[0049] S4. After the above-mentioned polyamic acid solution containing nanoparticles is decompressed to eliminate bubbles, it is coated on a clean glass plate with a film thickne...

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Abstract

The invention discloses a preparation method of a high-temperature-resistant polyimide film. Polyimide is prepared from aromatic dianhydride, aromatic diamine and hydrophobic modified silicon dioxideor aluminum oxide nanometer particles through compounding. The uniform scattering of nanometer particles in the polyimide can be realized through hydrophobic modification. The obtained polyimide filmhas the advantages of high thermal stability, low linear thermal expansion coefficient and excellent mechanical performance. The process is simple; the energy is saved; the environmental-friendly effect is achieved; the economic benefits are high.

Description

technical field [0001] The invention relates to the technical field of polymer materials. More specifically, the present invention relates to a preparation method of high temperature resistant polyimide film. Films are suitable for substrates in flexible printed circuit boards. Background technique [0002] Polyimide is one of the engineering plastics with the best heat resistance among polymer materials at present, and because of its corrosion resistance, solvent resistance, good thermal stability, outstanding dielectric properties and radiation resistance, and Widely used in aerospace, microelectronics, liquid crystal, separation membrane and other fields. However, most polyimides, especially aromatic polyimides, have disadvantages such as insolubility and infusibility, high molding pressure, high reaction temperature, and harsh process. For a long time, people have improved the process performance and mechanical properties of polyimide through various methods, and furt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08K9/06C08K3/36C08J5/18C08L79/08
CPCC08G73/1007C08G73/1067C08J5/18C08J2379/08C08K3/36C08K9/06C08K2201/011
Inventor 朱双全颜枫肖桂林鲁丽萍
Owner HUBEI DINGLONG CO LTD
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