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Polyamic acid, preparation method thereof, polyimide thermal-conducting film and preparation method of film

A technology of polyamic acid and polyimide, which is applied in the fields of polyamic acid and its preparation, polyimide thermal conductive film and its preparation, can solve the problems of limited effect of increasing thermal conductivity and few reactive sites, and the like, Achieve the effect of improving the effect, facilitating large-scale production, and enhancing the thermal conductivity

Active Publication Date: 2019-09-10
黑龙江英创新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the silane coupling agent only reacts with the end group of the polyamic acid in the process of combining with the organic resin, and can only play the role of capping, so there are fewer reactive sites on the resin matrix. For carbon-based fillers / polyimides The thermal conductivity of amine composites has a limited effect on the enhancement of thermal conductivity

Method used

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  • Polyamic acid, preparation method thereof, polyimide thermal-conducting film and preparation method of film

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preparation example Construction

[0054] The present invention provides the preparation method of polyamic acid described in above-mentioned technical scheme, comprises the following steps:

[0055] Mix diamine, dianhydride and polar organic solvent for copolymerization to obtain polyamic acid;

[0056] The diamine includes diamine A and diamine B, and the diamine A includes 3,3'-diaminodiphenyl ether, 3,4'-diaminodiphenyl ether, 4,4'-diaminodiphenyl ether ether, 2,3-diaminotoluene, 4,4'-diaminodiphenylsulfone, 4,4'-diaminobiphenyl or 1,1-bis(4-aminophenyl)cyclohexane, 4,4 One or more of '-diaminodiphenylmethane and 4,4'-diaminobenzophenone; the diamine B includes 4-dimethyl (ethoxy) silylbenzene-1,2 -diamine, 5-(triethoxysilyl)-1,3-phenylenediamine, 4-(4-aminophenoxy)-3-trimethoxysilyl)aniline, 3,5-diamino -N-(4-trimethoxysilyl)phenyl)benzamide, 3,5-diamino-N-(4-dimethoxy(methyl)silyl)phenyl)benzamide and 3 , one or more of 5-diamino-N-(3-(4-(triethoxysilyl)phenyl)propyl)benzamide;

[0057] The dianhydrid...

Embodiment 1

[0089] Weigh 0.1500 g of hydroxylated single-walled carbon nanotubes (20 μm in length and 1 nm in diameter) and place them in a three-necked flask filled with 92.08 mL of N,N-dimethylacetamide (DMAc) solution, and heat them at 40 kHz, 250 W Ultrasonic treatment for 2 hours under the condition of ultrasonic dispersion, the three-necked flask was connected to the inlet of nitrogen gas, and the tetrafluoro stirring blade was added to the reaction kettle successively. g (3.59mmol) 4-dimethyl (ethoxy) silylbenzene-1,2-diamine, start stirring, and stir fully at a speed of 2000r / min until the added diamine is completely dissolved; then add 10.5596g (35.89mmol) 3,3',4,4'-biphenyltetracarboxylic dianhydride, stirring constantly, and controlling the temperature at 20°C for copolymerization for 12h (during the copolymerization, when the solution viscosity increases significantly When the rod is climbed, the stirring rate is appropriately reduced until the phenomenon of climbing the rod i...

Embodiment 2

[0091] Weigh 0.7500g of hydroxylated double-walled carbon nanotubes (10 μm in length and 2nm in diameter) and place them in a three-necked flask containing 86.86mL of N-methylpyrrolidone (NMP) solution, and disperse them under ultrasonic dispersion conditions of 40kHz and 250W. Under the ultrasonic treatment for 2h, the three-neck flask was connected to the inlet of nitrogen gas, and the tetrafluoro stirring blade was added to the reaction kettle successively. ) 5-(triethoxysilyl)-1,3-phenylenediamine, start stirring, fully stir at a speed of 2000r / min until the added diamine is completely dissolved; then add 9.6952g (31.25mmol) at one time 3,3',4,4'-Diphenyl ether tetra-acid dianhydride, stirring continuously, and controlling the temperature at 20°C for copolymerization for 12h, (during the copolymerization, when the solution viscosity increases significantly to the Appropriately reduce the stirring rate until the rod-climbing phenomenon is not obvious, continue to maintain t...

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Abstract

The invention belongs to the technical field of nano composite materials, and particularly relates to a polyamic acid, a preparation method thereof, a polyimide thermal-conducting film and a preparation method of the film. The polyamic acid provided by the invention contains a siloxane group on the side chain, the side chain containing the siloxane group can be hydrolyzed into a hydroxyl group andfurther connected to a hydroxyl group on the surface of a carbon-based filler by a covalent bond, so that an interface of the carbon-based filler can be greatly improved, the interfacial bonding ability between the polyamic acid and the carbon-based filler is strong, and the effect of improving the carbon-based filler is remarkable; and when the polyamic acid prepared by the method is used for preparing the polyimide thermal-conducting film, the carbon-based filler can effectively form a thermal-conducting passage in a polyimide substrate, so that the thermal conductivity of the polyimide isimproved, and the effect of increasing the thermal conductivity of the polyimide composite material is obvious.

Description

technical field [0001] The invention relates to the technical field of nanocomposite materials, in particular to a polyamic acid and a preparation method thereof, a polyimide heat-conducting film and a preparation method thereof. Background technique [0002] With the rapid development of electronic information technology in recent years, the microelectronics industry is in a state of high-density and high-speed operation, making most electronic components and electrical equipment continue to move towards high-power, thin-layer, multi-functional, high-performance and miniaturized In the direction of development, it is difficult to avoid the problem of heating of electronic components and electrical equipment. Therefore, the development of device materials with excellent thermal conductivity is a major topic in the current development of information technology. [0003] Polyimide (PI) is a high-temperature insulating material with competitive advantages due to its outstandin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08K3/04C08L79/08C08J5/18
CPCC08G73/1039C08G73/1042C08G73/1046C08G73/105C08G73/1064C08G73/1067C08G73/1071C08G73/1078C08J5/18C08J2379/08C08K3/041C08K3/042C08K2201/011
Inventor 赵晓刚赵君禹王春博王大明陈春海
Owner 黑龙江英创新材料有限公司
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