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Method for preparing polyimide film by adopting chemical imidization in combined mode

A technology of polyimide film and chemical imidization, which is applied in the field of polyamic acid chemical imidization manufacturing and combined chemical imidization manufacturing of polyamic acid, which can solve the problems of poor performance of finished products, low production efficiency, Lack of market competitiveness and other issues, to achieve the effect of small internal stress, good dimensional stability, and small linear expansion coefficient

Active Publication Date: 2014-06-18
HUAWEI POLYIMIDE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose 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 combined chemical imidization method for polyamic acid Manufacturing method

Method used

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  • Method for preparing polyimide film by adopting chemical imidization in combined mode

Examples

Experimental program
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Effect test

Embodiment 1

[0030]Take 600kg of polyamic acid solution with a solid content of 20% and a viscosity of 245,100 centipoise, and keep the temperature below 0°C, quickly mix it with dehydrating agent and catalyst (dehydrating agent: thionyl chloride 11kg, 1,3-dichlorohexyl Carbodiimide 17kg, catalyst: N,N-dimethylaminopyridine 19kg, triethylenediamine 25kg), after mixing and defoaming, cast the film immediately, pay attention to the casting die lip During the whole process of the mouth, the temperature of the glue solution is always kept below 0°C. When the extrusion die device flows from the gap of the casting nozzle to the closed clean system running below it, the endless stainless steel belt running at a speed of 18m / min is cast into a film of uniform thickness, and the chemical sublimation is carried out at 75°C. Amination, after one week of circulation, the preliminary chemically imidated gel film is peeled off the endless steel strip by the peeling roller, and then sent to the bath tank...

Embodiment 2

[0032] Take 650kg of a polyamic acid solution with a solid content of 21% and a viscosity of 255,300 centipoise, and keep the temperature below 0°C, and quickly mix it with a dehydrating agent and a catalyst (dehydrating agent: 18kg of acetic anhydride, 1,3-dichlorohexyl carbonization Diimine 22kg, catalyst: N,N-dimethylaminopyridine 21kg, triethylenediamine 24kg), after mixing and defoaming, cast the film immediately, pay attention to the casting die lip During the whole process, the glue temperature is always kept below 0°C. When the extrusion die device flows from the gap of the casting nozzle to the closed clean system running below it, it is cast on the endless stainless steel belt running at a speed of 25m / min to form a film of uniform thickness, and the chemical sublimation is carried out at 65°C. Amination, after one week of circulation, the preliminary chemically imidated gel film is peeled off the endless steel strip by the peeling roller, and then sent to the bath t...

Embodiment 3

[0034] Take 600kg of a polyamic acid solution with a solid content of 19% and a viscosity of 233,600 centipoise, and keep the temperature below 0°C, quickly mix it with a dehydrating agent and a catalyst (dehydrating agent: thionyl chloride 11kg, N,N-dicyclohexyl Carbodiimide 30kg, catalyst: quinoline 15kg, triethylenediamine 31kg), after mixing and defoaming, cast the film immediately, pay attention to the glue in the whole process of entering the lip of the casting die The temperature is always kept below 0°C. When the extrusion die device flows from the gap of the casting nozzle to the closed clean system running below it, the endless stainless steel belt running at a speed of 10m / min is cast into a film of uniform thickness, and the chemical sublimation is carried out at 85°C. Amination, after one week of circulation, the preliminary chemically imidated gel film is peeled off the endless steel strip by the peeling roller, and then sent to the bath tank with a length of 5 m...

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Abstract

The invention discloses a polyamic acid imidization catalyst composite and a method for preparing an electronic-grade polyimide film by adopting chemical imidization in a combined mode, and belongs to the technical field of the manufacture of electronic film insulating materials. The novel chemical imidization method of polyimide mainly comprises the following steps of: storing polyamic acid at a low temperature, and stretching to form a film in a casting way; and then producing high-quality electronic-grade polyimide film through a mixing type and bath type combined high-efficiency imidization method. Compared with a method firstly adopting thermal imidization, the method disclosed by the invention outstandingly improves the linear expansion coefficient, the mechanical property, and the like of the obtained polyimide film and is high in production efficiency, lower in preparation cost and suitable for large-scale chemical industrial production of the high-property polyimide film.

Description

technical field [0001] The invention relates to a polyamic acid chemical imidization manufacturing technology, in particular to a polyamic acid combined chemical imidization manufacturing method, which belongs to the field of special polymer materials. Background technique [0002] At present, the vast majority of polyimide manufacturers in China use the thermal imidization method to produce polyimide. This method is to coat polyamic acid solution and then perform high-temperature heat treatment to form polyimide. The heating process of imidization is divided into two stages, the first stage is a heat treatment section below 150°C, and the second stage is an imidization section higher than the glass transition temperature of polyimide. The imidization process in production should be carried out in stages while gradually raising the temperature, and the temperature can be raised to about 400 degrees, which has higher requirements for production equipment and process condition...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J7/00C08J5/18C08L79/08C08G73/10
Inventor 黄渝鸿袁萍李晓敏邢涛黄樯
Owner HUAWEI POLYIMIDE
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