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Low-thermal-expansion-coefficient thermoplastic polyimide, film, molding powder and preparation method

A low thermal expansion coefficient, polyimide film technology, used in the field of molding powder and preparation, film, low thermal expansion coefficient thermoplastic polyimide, can solve the problem of unsatisfactory improvement of the melt index of the product

Active Publication Date: 2021-03-09
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the unsatisfactory improvement of the melt index of the obtained product in the existing matrix resin molecular structure linearization method, and proposes a low thermal expansion coefficient thermoplastic polyimide, film and molding powder with good processability and high transparency and preparation method

Method used

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  • Low-thermal-expansion-coefficient thermoplastic polyimide, film, molding powder and preparation method
  • Low-thermal-expansion-coefficient thermoplastic polyimide, film, molding powder and preparation method
  • Low-thermal-expansion-coefficient thermoplastic polyimide, film, molding powder and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Preparation of low CTE thermoplastic polyamic acid resin

[0047] Add 30.41g 4,4-diaminodiphenyl ether and 900g N,N-dimethylacetamide to the three-necked flask, stir and mix for 1h, then add 69.59g p-phenylbis(trimellitate) to the three-necked flask ) dianhydride, stirred and reacted for 1h, then placed in a constant temperature oil bath and slowly raised to 60°C, stirred and reacted for 30min, then removed from the oil bath and cooled to room temperature, continued to stir for 8h, wherein the molar ratio of diamine and dianhydride was 1:1 to prepare low CTE thermoplastic polyamic acid resin with a solid content of 10%.

[0048] (2) Preparation of low CTE thermoplastic polyimide film

[0049] Apply the low CTE thermoplastic polyamic acid resin evenly on the smooth glass plate by scraping method, put it in the oven, follow the temperature of 130℃ / 0.5h+170℃ / 0.5h+260℃ / 0.5h+340℃ / 0.5 h temperature program to complete the imidization, the preparation of low CTE thermopl...

Embodiment 2

[0100] (1) Preparation of low CTE thermoplastic polyamic acid resin

[0101] Add 29.71g 4,4-diaminodiphenyl ether and 566g N,N-dimethylacetamide to the three-necked flask, stir and mix for 1h, then add 58.30g p-phenylbis(trimellitate ) dianhydride, stirred and reacted for 1 hour, then placed in a constant temperature oil bath and slowly raised to 60°C, stirred and reacted for 60 minutes, then removed from the oil bath and cooled to room temperature; then added 2.12g of 4,4-diaminodiphenyl ether, Stir the reaction for 1 hour; add 9.86g of 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride, and continue stirring for 8 hours, wherein the molar ratio of the total amount of diamine to the total amount of dianhydride is 1:1 to obtain low CTE Thermoplastic polyamic acid resin with a solid content of 15%.

[0102] (2) Preparation of low CTE thermoplastic polyimide film

[0103] Referring to Example 1. The color of the film is yellow and transparent.

[0104] (3) Preparation of l...

Embodiment 3

[0109] (1) Preparation of low CTE thermoplastic polyamic acid resin

[0110] Add 23.39g 4,4-diaminodiphenyl ether and 566g N,N-dimethylacetamide to the three-necked flask, stir and mix for 1h, then add 45.89g p-phenylbis(trimellitate ) dianhydride, stirred and reacted for 1 hour, then placed in a constant temperature oil bath and slowly raised to 60°C, stirred and reacted for 30 minutes, then removed from the oil bath and cooled to room temperature; then added 10.02g of 4,4-diaminodiphenyl ether, Stir the reaction for 1h; add 20.70g of 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride, and continue stirring for 8h, wherein the molar ratio of the total amount of diamine to the total amount of dianhydride is 1:1, and the low CTE thermoplastic polyamic acid resin with a solid content of 15%.

[0111] (2) Preparation of low CTE thermoplastic polyimide film

[0112] Referring to Example 1. The color of the film is yellow and transparent.

[0113] (3) Preparation of low CTE t...

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Abstract

The invention discloses low-thermal-expansion-coefficient thermoplastic polyimide, a film, molding powder and a preparation method, and belongs to the technical field of polyimide materials. The low-thermal-expansion-coefficient thermoplastic polyimide contains a structural unit shown as a formula (I), and preferably, the ratio of the structural unit shown as the formula (I) is 60-100 mol%. According to the present invention, by introducing the diester bond structure chain segment, the molecular chain straight chain degree is effectively improved, such that the obtained thermoplastic polyimidefilm has characteristics of low thermal expansion coefficient, low dielectric property and high transparency in the absence of the filler while the good processability is maintained, and can be usedin the fields of aerospace aircraft devices and optical communication. The structural unit shown in the formula (I) is shown in the specification;.

Description

technical field [0001] The invention relates to a thermoplastic polyimide material, in particular to a low thermal expansion coefficient thermoplastic polyimide, a film, molding powder and a preparation method. Background technique [0002] Thermoplastic polyimide (TPI) has become another polyimide material because of its good high-temperature melt fluidity, which can realize parts processing in high-temperature lamination, molding, injection molding, extrusion and other plastic molding processes. important direction. Good high-temperature fluidity is an important index to measure the processability of TPI. Improving high-temperature fluidity is mainly through the flexibility of polyimide molecular chains, reducing the interaction force between macromolecules, and breaking the regular molecular structure of polyimide. However, at the same time, the dimensional stability will be greatly reduced, resulting in a high coefficient of thermal expansion (CTE), usually 40-60ppm / K, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1071C08G73/105C08G73/1007C08J5/18C08L79/08C08J2379/08C08L2201/10C08L2201/08
Inventor 姬亚宁白小庆青双桂唐必连赵恒宇
Owner GUILIN ELECTRICAL EQUIP SCI RES INST