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Polyamide acid slurry, preparation method thereof and polyimide film

A technology of polyamic acid and slurry, which is applied in the fields of polyamic acid slurry and its preparation, polyimide precursor polyamic acid, and polyimide film, can solve the problem that the performance of polyimide film is greatly affected. , The preparation process is difficult to control, the polymerization reaction speed is fast, etc., to solve the difficulty of filtration, reduce the large particles of agglomeration or encapsulation, and improve the yield.

Active Publication Date: 2021-06-01
武汉柔显科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the problems that the polymerization reaction speed is fast in the preparation process of polyamic acid, the preparation process is difficult to control, and the feeding process and polymerization conditions have a great influence on the characteristics of polyamic acid slurry and the performance of polyimide film; in order to solve the above problems, the present invention provides A polyamic acid slurry with a high degree of polymerization and uniform stability, which greatly improves the bonding force between the polyimide resin and the coated substrate, and the overall performance of the cured polyimide film is excellent

Method used

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  • Polyamide acid slurry, preparation method thereof and polyimide film
  • Polyamide acid slurry, preparation method thereof and polyimide film
  • Polyamide acid slurry, preparation method thereof and polyimide film

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[0036] The present invention provides a method for preparing a polyamic acid slurry applied to a substrate and a film thereof, the method comprising the following steps:

[0037] A first aspect of the present invention provides a method for preparing a polyamic acid slurry, comprising the following steps:

[0038] (1) diamine A1 is dissolved in polar organic solvent E at a certain temperature to obtain diamine A1 solution, and diamine A2 is dissolved in polar organic solvent E at a certain temperature to obtain diamine A2 solution;

[0039] (2) adding dianhydride B1 to organic solvent E, and uniformly distributing B1 in organic solvent E by high-speed dispersing equipment to obtain slurry H1; adding dianhydride B2 to organic solvent E, and uniformly distributing B2 by high-speed dispersing equipment In the organic solvent E, a slurry H2 is obtained; wherein, the state of the dianhydrides B1 and B2 in the organic solvent E is a dissolved or suspended state.

[0040] (3) Add pa...

Embodiment 1

[0097] 1L three-necked flask, 5L constant temperature oil bath, digital display mechanical stirring, high-purity nitrogen pipeline, spherical condenser, liquid-sealed tube and addition funnel, set up the reaction device, continue to feed high-purity nitrogen, first add 6.7278g APBA (0.03mol) and 62.55g NMP, stir in an oil bath at 30°C for about 8min to completely dissolve the diamine APBA, then add 14.1223g BPDA (0.048mol) powder directly and quickly at one time, and add 1.54g methanol, use 86.22g Washed with NMP, the mixed system was reacted at 60°C for 6 hours. Then, the reaction temperature was lowered to 30°C, 54.0621g ODA (0.27mol) and 34.10g NMP were added to the system, the reaction was continued for 6h, and 74.1423g BPDA (0.252mol), 0.2g isoquinoline, 0.5g of triphenyl phosphate and dianhydride BPDA powder were added quickly at one time, and 264.29g of NMP solvent was rinsed.

[0098] The obtained polyamic acid slurry viscosity and solid content results are shown in T...

Embodiment 2

[0100] 1L three-necked flask, 5L constant temperature oil bath, digital display mechanical stirring, high-purity nitrogen pipeline, spherical condenser, liquid-sealed tube and addition funnel, set up the reaction device, continue to feed high-purity nitrogen, first add 6.7278g APBA and 62.55 g of NMP, and stirred in an oil bath at 30° C. for 8-10 min to completely dissolve the diamine APBA. 88.2646g BPDA powder of dianhydride was dispersed in 291.27g NMP at high speed, the temperature of the dispersing kettle was set at 30°C, the stirring rate was 5000rpm, and the dispersion time was 2h, to prepare a uniform dianhydride suspension H1 for later use. Then, the homogeneous suspension of 16% H1 (0.048mol BPDA) in mass ratio was slowly and uniformly added to the above diamine solution, and 1.54 g of methanol was added, and the mixed system was reacted at 60° C. for 6 hours. Next, the reaction temperature was lowered to 30°C, 54.0621g ODA and 34.10g NMP were added to the system, the...

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Abstract

The invention discloses polyamide acid slurry, a preparation method thereof and a polyimide film, excessive dianhydride reacts with diamine containing an imidazole structure, and then alcohol is added to obtain an ester-terminated polyamide acid composition; by adding a second part of dianhydride monomer and diamine monomer into the solution, a polyamide acid solution in which the molar weight of the dianhydride monomer is basically close to the molar weight of the diamine monomer is obtained; when the first part of dianhydride or diamine monomer and the second part of dianhydride or diamine monomer are different in type, polyamic acid of a block structure can be obtained, the polyamic acid is further cured to obtain the polyimide film of the block structure, the viscosity is small and controllable in the reaction process, the ratio of the dianhydride to the diamine monomer can be increased, batch solution feeding is achieved, a high-molecular-weight low-viscosity imidazole structure-containing block type polyamide acid solution is prepared, and due to the action of an imidazole structure, a substrate hydrogen bond and the like, a film cured at a high temperature is excellent in comprehensive performance, and the adhesive force of the film and a coated substrate is greatly improved.

Description

technical field [0001] The invention relates to polyimide precursor polyamic acid and polyimide film, in particular to a polyamic acid slurry and a preparation method thereof and a polyimide film. Background technique [0002] Polyimides are generally prepared from polyamic acid precursors. In order to obtain a polyimide resin or film with excellent comprehensive properties, it is generally required that the molecular weight of the polyimide be as high as possible, so the molecular weight of the polyamic acid precursor is required to be as high as possible. However, with the increase of the molecular weight of the polyamic acid, the viscosity of the polyamic acid solution increases greatly, which deteriorates the processing characteristics and film-forming characteristics of the polyamic acid solution, and at the same time increases the difficulty of synthesis. The optimization of the preparation of the feeding process and the synthesis conditions is very meaningful. [00...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1085C08G73/1007C08J5/18C08J2379/08
Inventor 肖桂林阮敏付华鲁丽平朱双全
Owner 武汉柔显科技股份有限公司
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