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Polyamide acid dispersion liquid and preparation method thereof as well as polyimide film

A polyamic acid and dispersion technology, applied in the field of nanomaterials, can solve the problems of molecular chain embrittlement, material shrinkage stress, poor corona resistance, etc., and achieve good corona resistance and good mechanical properties

Active Publication Date: 2013-06-26
株洲时代华鑫新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the corona resistance effect of polyimide is poor. When it is applied to the variable frequency motor, because the variable frequency motor adopts the pulse width modulation driving pulse speed regulation technology, it will cause partial discharge phenomenon, that is, the generation of corona, and the polyimide used Imide film insulation materials have poor corona resistance, which will cause local high-temperature oxidation in the motor insulation materials, resulting in decomposition of insulation materials, embrittlement of molecular chains, and fractures, eventually causing insulation breakdown, making the insulation system of the motor The service life is greatly reduced, and may even cause the motor to be damaged during the trial run. Therefore, to prolong the service life of the motor, it is necessary to improve the corona resistance of its insulating material, that is, the polyimide film
[0004] At present, the method of adding corona-resistant nanoparticles in polyimide films is often used to improve the corona resistance of polyimide films. The prior art discloses the use of sol-gel methods to prepare nano-metal oxide dispersions, and then make However, this method is complicated and not suitable for large-scale industrial production, and during the gel drying process, the volatilization of solvents and small molecules may cause shrinkage stress inside the material, affecting the mechanical and mechanical properties of the material; There is also the technology of directly dispersing nanoparticles in polyamic acid solution to prepare polyimide film with corona resistance, but due to the large specific surface area and surface energy of nanoparticles, there is a strong interaction between the particles , easy to agglomerate, and the polyamic acid solution itself has a high viscosity, it is difficult to achieve the ideal nanoscale composite of nanoparticles and polyamic acid, and finally the mechanical properties of the prepared polyimide film are poor.

Method used

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  • Polyamide acid dispersion liquid and preparation method thereof as well as polyimide film

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preparation example Construction

[0020] The invention provides a kind of preparation method of polyamic acid dispersion liquid, comprising:

[0021] A) dispersing the metal oxide nanoparticles whose surface is modified by a coupling agent into an organic solvent to obtain a nanoparticle dispersion;

[0022] B) Mixing and reacting the nanoparticle dispersion obtained in step A) with dianhydride and diamine to obtain a polyamic acid dispersion.

[0023] The present invention firstly modifies the surface of the metal oxide nanoparticles, and then disperses the nanoparticles in an organic solvent with a low viscosity, so that the nanoparticles can be uniformly and stably dispersed, and avoids the problem of the high viscosity of the polyamic acid solution causing the Disadvantage of inhomogeneous dispersion, the final polymerization reaction is carried out to prepare polyamic acid dispersion liquid, and the polyimide film prepared by it not only has good corona resistance performance, but also has good mechanical...

Embodiment 1

[0038] Disperse 9 g of zirconia nanoparticles with a particle size of 10 nm in 20 mL of ethanol, heat to 30 ° C, then add 1 g of silane coupling agent to react for 5 h, then filter the reaction product, wash the solid with ethanol for 3 times, and the obtained The solid is dried to obtain zirconia nanoparticles whose surface is modified by a silane coupling agent.

[0039] At room temperature (25°C), 5 g of zirconia nanoparticles whose surface was modified by a silane coupling agent were uniformly dispersed in 40 g of N-methylpyrrolidone to obtain a zirconia nanoparticle dispersion, and then pyromellitic dianhydride was added 7.8g and 7.2g of 4,4'-diaminodiphenyl ether, the temperature of the reaction system was raised to 30°C, after the dianhydride and diamine were fully dissolved, the reaction was continued for 2h, and the reaction system was cooled to room temperature to obtain poly Amic acid dispersion.

[0040] Add the prepared polyamic acid dispersion into a casting mac...

Embodiment 2

[0043] Disperse 5 g of zinc oxide nanoparticles with a particle size of 30 nm in 20 mL of ethanol, heat to 50 ° C, then add 1 g of silane coupling agent to react for 3 h, then filter the reaction product, wash the solid with ethanol for 3 times, and the obtained The solid is dried to obtain zinc oxide nanoparticles whose surface is modified by a silane coupling agent.

[0044] At room temperature (25°C), uniformly disperse 1 g of zinc oxide nanoparticles whose surface is modified by a silane coupling agent in 83 g of N-methylpyrrolidone to obtain a zinc oxide nanoparticle dispersion, and then add pyromellitic dianhydride 14.6g and 13.4g of 4,4'-diaminodiphenyl ether, the temperature of the reaction system was raised to 40°C, after the dianhydride and diamine were fully dissolved, the reaction was continued for 5h, and the reaction system was cooled to room temperature to obtain poly Amic acid dispersion.

[0045] Add the prepared polyamic acid dispersion into a casting machin...

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Abstract

The invention provides a preparation method of a polyamide acid dispersion liquid. The preparation method comprises the following steps: dispersing metal oxide nanoparticles with the surfaces modified by a coupling agent into an organic solvent, thereby obtaining a nanoparticle dispersion liquid; and mixing the obtained nanoparticle dispersion liquid with dianhydride and diamine and reacting, thereby obtaining the polyamide acid dispersion liquid. According to the preparation method, the surfaces of the metal oxide nanoparticles are modified firstly; and then the nanoparticles are dispersed into the organic solvent with the low viscosity, so that the nanoparticles are dispersed evenly and stably, and therefore, the defect that the nanoparticles are not dispersed evenly because the polyamide acid solution is high in viscosity is overcome. Finally, the polyamide acid dispersion liquid is obtained by performing a polymerization reaction. A polyimide film prepared by the polyamide acid dispersion liquid is good in corona-resistant performance and mechanical performance.

Description

technical field [0001] The invention relates to the technical field of nanometer materials, in particular to a polyamic acid dispersion liquid, a preparation method thereof and a polyimide film. Background technique [0002] Polyimide film is a new type of high-temperature-resistant organic polymer film. It is the best film insulating material in the world. Since it was first introduced to the market in 1966, it has been known for its excellent electrical properties, flame High temperature resistance and radiation resistance, as a high-performance insulating material, it is used in various fields such as aerospace industry, electronic and electrical industry, and information industry. [0003] However, the corona resistance effect of polyimide is poor. When it is applied to the variable frequency motor, because the variable frequency motor adopts the pulse width modulation driving pulse speed regulation technology, it will cause partial discharge phenomenon, that is, the gen...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08K9/06C08K9/04C08K3/22C08L79/08
Inventor 廖波张步峰王文进田苗周升
Owner 株洲时代华鑫新材料技术有限公司
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