Preparation method of low-dielectric polyimide fibers

A technology of polyimide fiber and nascent fiber, applied in the direction of fiber chemical characteristics, drawing spinning, single-component synthetic polymer rayon, etc., can solve problems such as unfavorable high-performance low-dielectric composite materials, and achieve expansion Application range, low dielectric constant, dimensionally stable effect

Active Publication Date: 2020-10-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the imide structure has a higher polarity, which means that this type of material has a higher molecular polarizability. Generally, the dielectric constant κ of polyimide materials is greater than 3.0 (such as the dielectric constant κ ≈ 3.4), which is not conducive to obtaining high-performance low-dielectric composite materials. Therefore, it is of great significance to develop polyimide fiber materials with low dielectric properties of κ<3.0

Method used

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  • Preparation method of low-dielectric polyimide fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Under nitrogen protection, in a three-necked flask, add 250 mL of NMP, 11.34 g (0.05 mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA), 4.42 g (0.017 mol) of 3,5-diaminobenzoyl-4-amine-benzocyclobutene (synthesis method such as U.S.Patent 6,534,250[P].2003-3-18.), after stirring for 1h, add 21.74g ( 0.067mol) of 3,3',4,4'-benzophenonetetraacid dianhydride, stirred and reacted at 15°C for 10h; then raised the temperature to 130°C, 145°C, and 155°C for 1h each, and finally raised the temperature to 190°C React at constant temperature for 12 hours to obtain a high-viscosity polyimide solution with a solid content of 13%.

[0041] (2) Take the polyimide solution prepared in step (1) as the spinning solution, let it stand for defoaming, and use solidification as the volume ratio of 1:1 NMP and deionized water as the coagulation bath, and deionized water as the water system bath, using wet spinning technology to prepare polyimide as-spun fibers, dried and set aside. ...

Embodiment 2

[0044](1) Under nitrogen protection, in a three-necked flask, successively add 300 mL of DMAc, 13.04 g (0.058 mol) of 2-(4-aminophenyl)-5-aminobenzoxazole (BOA), 3.66 g ( 0.014mol) of 3,5-diaminobenzoyl-4-amine-benzocyclobutene (synthesis method such as U.S. Patent 6,534,250[P].2003-3-18.), after stirring for 1h, add 32.14g (0.072 mol) of hexafluorodianhydride (6-FDA), stirred and reacted at 15°C for 10h; then raised the temperature to 130°C, 145°C, and 155°C for 1h each, and finally raised the temperature to 165°C and reacted at a constant temperature for 12h to obtain high-viscosity polyimide Amine solution with a solid content of 14%.

[0045] (2) Take the polyimide solution obtained in step (1) as the spinning solution, let it stand for defoaming, and prepare polyimide primary fibers by dry spinning technology, the tunnel temperature is 230 ° C, and the tunnel length is 10 m. The wire speed was 300 m / min.

[0046] (3) In a nitrogen atmosphere, the polyimide fiber obtaine...

Embodiment 3

[0049] (1) Under the protection of nitrogen, in a three-necked flask, successively add 300mL of NMP, 13.92g (0.062mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA), 3.92g (0.016mol) mol) of 3,5-diaminobenzoyl-3-amine-benzocyclobutene (synthesis method such as U.S. Patent 6,534,250[P].2003-3-18.), after stirring for 1h, add 25.0g (0.0776mol ) of 3,3',4,4'-benzophenonetetraacid dianhydride, stirred and reacted at 20°C for 10h; then raised the temperature to 130°C, 145°C, and 155°C for 1h each, and finally raised the temperature to 185°C for constant temperature reaction After 10 hours, a high-viscosity polyimide solution with a solid content of 12.5% ​​was obtained.

[0050] (2) Take the polyimide solution prepared in step (1) as the spinning solution, let it stand for defoaming, and take solidification as the volume ratio of 6:4 NMP and deionized water as the coagulation bath, and deionized water as the water system bath, adopt dry jet-wet spinning technology to prepare pol...

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Abstract

The invention relates to a preparation method of low-dielectric polyimide fibers. The preparation method comprises the steps that benzocyclobutene diamine, heterocyclic diamine and a polar aprotic solvent are mixed and stirred; aromatic dianhydride is added in to the mixture, and a polymerization reaction is conducted; and the obtained soluble polyimide solution is subjected to deaeration and spinning and then subjected to heat drawing treatment. The low-dielectric polyimide fibers obtained through the method have the characteristics of low dielectric constant, low water absorption rate, stable size and the like, and can be applied to the fields of wave-transparent composite materials, flexible electronic substrates, wearable devices and the like; and certain functionality is given to thefibers, and the application range of the material can be further expanded.

Description

technical field [0001] The invention belongs to the field of polyimide fiber preparation, in particular to a method for preparing low-dielectric polyimide fiber. Background technique [0002] The dielectric properties of materials directly affect the speed, accuracy and reliability of information transmission. Generally, high dielectric constant materials are easy to absorb electromagnetic waves and dissipate them in the form of heat, which is not conducive to information transmission and has great safety hazards. It has important application value. [0003] As an important class of high-performance fibers, polyimide (PI) fibers have a polar imide ring structure in their molecular chains, and have properties such as high temperature resistance, high specific strength, and UV resistance, and have been successfully applied. It is used in high-tech fields such as high-temperature filtration, aerospace, and marine equipment. However, the imide structure has a higher polarity,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/78C08G73/10D01D10/02D01D5/12
CPCC08G73/1007C08G73/1039C08G73/1067C08G73/1071D01D5/12D01D10/02D01F6/78
Inventor 董杰张清华甘锋赵昕郑森森
Owner DONGHUA UNIV
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