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Polyimide copolymer precursor, polyimide and preparation method of polyimide film

A polyimide and copolymer technology, which is used in the preparation of polyimide copolymer precursors, polyimide and polyimide films to achieve excellent low moisture absorption, improved adhesion, and production processes. Simple and reliable process

Active Publication Date: 2019-05-31
武汉柔显科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Polyimide copolymer precursor, polyimide and preparation method of polyimide film
  • Polyimide copolymer precursor, polyimide and preparation method of polyimide film
  • Polyimide copolymer precursor, polyimide and preparation method of polyimide film

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Embodiment 1

[0055] Polyimide film embodiment 1 (PMDA / HBOA / ODA)

[0056] In a three-neck flask (100ml) equipped with a stirring rod and a nitrogen inlet, add 4,4-diaminodiphenyl ether (ODA) (1.001g, 0.005mol), Y1-NH 2 5,5'-diamino-2-trifluoromethyl-2'-hydroxy-phenyl-benzodiimidazole HBOA (2.122g, 0.005mol) and N-methylpyrrolidone (30ml) prepared in Experimental Example 1, Wherein, the sum of the moles of ODA and AAB is 0.01 mol. Under the protection of nitrogen, after mechanical stirring at 0-50°C until completely dissolved, add pyromellitic anhydride (PMDA) (2.181g, 0.01mol) to the solution, keep the temperature of the reaction system constant, and react 1 to 24 hours to obtain a polyimide precursor solution with a viscosity of 4.6 Pa s; after the above polyimide precursor solution is decompressed to eliminate air bubbles, it is coated on a clean glass plate with a wet film thickness of 1 ~ 300 μm, followed by drying in a vacuum oven at 80° C. for 5 hours, followed by curing in a nitrog...

Embodiment 2

[0057] Polyimide film embodiment 2 (s-BPDA / HBOA / PPD)

[0058] In a three-neck flask (100ml) equipped with a stirring rod and a nitrogen inlet, add p-phenylenediamine (PPD) (0.541g, 0.005mol), Y1-NH 2 5,5'-diamino-2-trifluoromethyl-2'-hydroxy-phenyl-benzodiimidazole HBOA (2.122g, 0.005mol) and N-methylpyrrolidone (30ml) prepared in Experimental Example 2, Wherein, the sum of the moles of PPD and AAB is 0.01 mol. Under the protection of nitrogen, stir mechanically at 0-50°C until completely dissolved, then add 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA) (2.942g , 0.01mol), keep the temperature of the reaction system constant, and react for 1 to 24 hours to obtain a polyimide precursor solution with a viscosity of 4.78Pa·s; after reducing the pressure of the above polyimide precursor solution to eliminate bubbles, apply Covered on a clean glass plate with a wet film thickness of 1-300 μm, and then dried in a vacuum oven at 80°C for 5 hours, then cured in a nitrogen o...

Embodiment 3

[0059] Polyimide film embodiment 3 (BTDA / HBOA / PPD)

[0060] In a three-neck flask (100ml) equipped with a stirring rod and a nitrogen inlet, add p-phenylenediamine (PPD) (0.541g, 0.005mol), Y1-NH 2 5,5'-diamino-2-trifluoromethyl-2'-hydroxy-phenyl-benzodiimidazole HBOA (2.122g, 0.005mol) and N-methylpyrrolidone (30ml) prepared in Experimental Example 3, Wherein, the sum of the moles of PPD and AAB is 0.01 mol. Under the protection of nitrogen, stir mechanically at 0-50°C until completely dissolved, then add 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) (3.222g, 0.01mol), keep the temperature of the reaction system constant, and react for 1 to 24 hours to obtain a polyimide precursor solution with a viscosity of 6.25Pa s; after decompressing the above polyimide precursor solution to eliminate bubbles, coating On a clean glass plate, the wet film thickness is 1-300 μm, and then dried in a vacuum oven at 80 °C for 5 h, then cured in a nitrogen oven at 150 °C for 1 h, ...

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Abstract

The invention discloses a polyimide copolymer precursor, polyimide and a preparation method of a polyimide film. Preparation of the polyimide copolymer precursor comprises mixing polyphosphoric acid,2-hydroxy-4-nitrobenzoic acid and 4,5-dinitro-o-phenylenediamine, stirring to allow dissolving and reacting, adding Pd / C and hydrazine hydrate to allow reducing, adding 4-amino-2-trifluoromethylbenzoic acid, mixing to allow reacting, precipitating the reaction product, filtering, and washing to obtain a hydroxy- and trifluoromethyl-modified diamine with benzimidazole structure; mixing an aromaticdiamine with the hydroxy- and trifluoromethyl-modified diamine with benzimidazole structure, adding the mixture into a polar organic solvent to obtain a diamine monomer mixed solution, adding an aromatic dianhydride, allowing to react to obtain a polyimide copolymer precursor solution, coating the surface of a substrate with the solution, and drying and solidifying to obtain the polyimide film. The polyimide film herein has good adhesive power, good mechanical properties and low water absorption rate.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a polyimide copolymer precursor, a polyimide and a method for preparing a polyimide film. Background technique [0002] Aromatic polyimides are widely used in aerospace materials and high-performance composite materials due to their excellent mechanical properties, outstanding thermo-oxidative stability, superior chemical resistance and good dielectric properties. However, most aromatic polyimides have disadvantages of poor adhesion and high coefficient of linear thermal expansion. In order to overcome these shortcomings, different structural modification methods have been adopted to adjust, including the introduction of oxygen-containing ether bonds and other polar groups. However, the introduction of these groups often sacrifices the mechanical and thermal properties of polyimide. Therefore, a controlled approach is required to balance these properties. [0003] Ge...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 颜枫肖桂林鲁丽萍朱双全
Owner 武汉柔显科技股份有限公司
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