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Chemical imidization accelerant of polyamide acid and polyimide thin film manufacturing method

A technology of polyimide chemical imide and polyamic acid glue, applied to polyimide film, chemical imidization of polyimide film, catalyst and dehydration for chemical imidization of polyamic acid In the field of pharmaceuticals, it can solve the problems of low production efficiency, poor performance of finished products, and lack of market competitiveness, and achieve the effects of good dimensional stability, low linear expansion coefficient, and small residual internal stress

Active Publication Date: 2013-06-12
HUAWEI POLYIMIDE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to overcome the disadvantages of poor product performance, low production efficiency, and lack of market competitiveness in the polyamic acid thermal imidization method in the prior art, and provide a polyamic acid chemical imidization process. Dehydrating agent and catalyst composition, and imidization method

Method used

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  • Chemical imidization accelerant of polyamide acid and polyimide thin film manufacturing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 200kg of N,N-dimethylformamide, 45kg of N,N-dicyclohexylcarbodiimide, 41kg of benzoic anhydride, 10kg of quinoline and diisopropyl Ethylamine 65kg, after stirring and mixing evenly, mix it with the polyamic acid solution with a solid content of 20% and a viscosity of 245,100 centipoise at a mass ratio of 1:6, filter and vacuum degassing, and then extrude The die device drool is coated on the endless stainless steel belt with a folded diameter of 6-15m in a closed clean system, and the chemical imidization is carried out in three stages at 75°C, 130°C, and 175°C at a speed of 16m / min, and then The partially chemically imidized gel film with a solid content of 28-32% is peeled off the endless steel strip through the peeling roller, and sent in with a rubber roller, or sent to 300°C, 400℃, 450℃, 475℃ and 250℃ high-temperature furnaces with five temperature sections for complete imidization treatment, so that the residual solvent content in the film is 2.8% to 3%, and f...

Embodiment 2

[0039] Add 180kg of N,N-dimethylformamide, 100kg of acetic anhydride, 35kg of benzoic anhydride, 60kg of isoquinoline, 1,8-di(N,N-dimethyl Amino)naphthalene 16kg, after stirring and mixing evenly, mix it with polyamic acid solution with a solid content of 18.5% and a viscosity of 236,600 centipoise at a mass ratio of 1:7, filter, vacuum debubble, and squeeze The die head device drool is coated on the endless stainless steel belt with a folded diameter of 6-15m in a closed clean system, and the chemical imidization is carried out in three stages at 65°C, 125°C, and 165°C at a speed of 18m / min. Then the partially chemically imidized gel film with a solid content of 28 to 35% is peeled off the endless steel strip through the peeling roller, and sent in with a rubber roller, or sent to 300°C after being biaxially stretched with a stretch ratio of 1.2. , 400°C, 450°C, 475°C and 250°C five-temperature high-temperature furnace for complete imidization treatment, so that the residual ...

Embodiment 3

[0041] Add 200kg of N,N-dimethylformamide, 30kg of acetic anhydride, 21kg of benzoic anhydride, 45kg of N,N-dicyclohexylcarbodiimide, and 15kg of isoquinoline into a storage tank at a temperature of -10±2°C , 10kg of quinoline and 45kg of diisopropylethylamine were stirred and mixed evenly, and mixed with a polyamic acid solution having a viscosity of 241,900 centipoise with a solid content of 19.1% in a mass ratio of 1:5, filtered, After vacuum defoaming, it is drool-coated on an endless stainless steel belt with a diameter of 6-15m in a closed clean system through the extrusion die device, at a speed of 20m / min, at 75°C, 130°C, and 175°C for three times. Sectional chemical imidization, and then the partially chemically imidized gel film with a solid content of 28-35% is peeled off the endless steel strip through the peeling roller, and is sent in with a rubber roller, or through a two-way stretching ratio of 1.2 After stretching, it is sent to a high-temperature furnace with...

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Abstract

The invention discloses a composition of a dehydrant and an accelerant for use in chemical imidization process of polyimide in the technical field of polymer thin film insulating material manufacture. The composition is composed of the dehydrant and the accelerant in the weight ratio of 7:1 to 1:1, wherein the dehydrant refers to an aliphatic anhydride, an aromatic anhydride, a halogenated lower aliphatic anhydride, or a thionyl halide and the like; the accelerant refers to a tertiary amine compound or a composition of the tertiary amine compounds; the tertiary amine compound can be heterocyclic tertiary amine, aliphatic tertiary amine, aromatic tertiary amine or composition thereof; 12-48 parts by weight of composition of the dehydrant and the accelerant is applied for each 100 parts by weight of polyamide acid glue solution. If the composition of the dehydrant and the accelerant provided by the invention is used for preparing a polyimide thin film material, the production efficiency is high, the imidization degree is high, residual internal tress inside the material is low, and the thin film is good in size stability and low in coefficient of linear expansion and therefore is very suitable for use as a flexible copper film-coated substrate material.

Description

technical field [0001] The invention relates to a chemical imidization catalyst of polyamic acid and its polyimide film, in particular to a catalyst and a dehydrating agent for chemical imidization of polyamic acid. The present invention also relates to a chemical imidization catalyst of polyimide film. The amination manufacturing technology belongs to the field of polymer materials. Background technique [0002] The main synthesis method of polyimide is a two-step method. Firstly, react an equimolar ratio of dibasic anhydrides and diamines in an aprotic polar solvent to generate the corresponding polyamic acid, and then use thermal imidization or chemical imidization to dehydrate and cyclize into the final polyimide amine. The thermal imidization method is currently used by all domestic polyimide film enterprises. This method is to coat polyamic acid solution and then conduct high-temperature heat treatment to form polyimide film. In the process of thermal imidization, t...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08L79/08
Inventor 黄渝鸿袁萍李晓敏邢涛黄樯
Owner HUAWEI POLYIMIDE
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