A core-shell type low-dielectric flame-resistant polyimide-based fiber material and its preparation method

A technology for burning polyimide-based and polyimide fibers is applied in the field of core-shell low-dielectric flame-retardant polyimide-based fiber materials and their preparation, and can solve the problem of aminopropyl-polysilsesquioxane The alkane raw materials are not easy to obtain, the flame retardant properties of the material are not considered, and it is difficult to develop and apply on a large scale, so as to achieve the effects of improving mechanical properties, reducing dielectric constant and high mechanical properties.

Active Publication Date: 2022-03-08
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This invention requires high pressure and the raw material of aminopropyl-polysilsesquioxane as the cross-linking node is not easy to obtain, and the mechanical properties cannot be guaranteed, nor is it considered to improve the flame retardancy of the material, so it is difficult to develop and apply on a large scale

Method used

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  • A core-shell type low-dielectric flame-resistant polyimide-based fiber material and its preparation method
  • A core-shell type low-dielectric flame-resistant polyimide-based fiber material and its preparation method
  • A core-shell type low-dielectric flame-resistant polyimide-based fiber material and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A preparation method of a core-shell type low-dielectric flame-resistant polyimide-based fiber material is as follows:

[0045] a) At room temperature, N 2 Add 1.7g of aminoethylheptyl-polysilsesquioxane, 0.4g of 2,4,6-trimethylbenzaldehyde and 20g of acetone into the reaction kettle in an atmosphere, react at 55°C for 10h, then lower the temperature to 10°C, add 1.1g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 10g of absolute ethanol, mix well and add dropwise 15g of sodium carbonate solution (dissolved in 10mL of water ), after 0.5h of dripping, adjust the temperature to 55°C, react for 4h, distill under reduced pressure at 50°C for 0.5h, extract with 30mL of anhydrous methanol, wash with 60mL of petroleum ether for 3 times, and finally place it at 50°C for 20h , cooled to room temperature to obtain phosphate-based aminopolysilsesquioxane;

[0046] b) At room temperature, N 2 Add 1.0g of 4,4'-diaminodiphenyl ether, 8g of N,N-dimethylacetamide aromatic...

Embodiment 2

[0052] A preparation method of a core-shell type low-dielectric flame-resistant polyimide-based fiber material is as follows:

[0053] a) At room temperature, N 2 In the atmosphere, 2.8g of aminoethylfluoromethyl-polysilsesquioxane, 0.8g of 3,4,5-trihydroxybenzaldehyde and 40g of pentane were added to the reaction kettle, and reacted at 110°C for 4h, then the temperature Adjust to 25°C, then add 1.7g 3-fluoro-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 18g absolute ethanol, mix well and add dropwise 16g potassium carbonate solution (dissolved in 11mL of water), after 0.6h of dripping, adjust the temperature to 55°C, react for 10h, distill under reduced pressure at 55°C for 0.5h, extract with 45mL of anhydrous methanol, wash with 65mL of petroleum ether and filter three times, and finally Place it at 50°C for 14 hours, and cool to room temperature to prepare phosphate-based aminopolysilsesquioxane;

[0054] b) At room temperature, N 2 Add 1.2g of 4,4'-diaminodiphe...

Embodiment 3

[0060] A preparation method of a core-shell type low-dielectric flame-resistant polyimide-based fiber material is as follows:

[0061] a) At room temperature, N 2 In the atmosphere, 3.4g of aminopentylheptyl-polysilsesquioxane, 1g of 2,4,6-trimethylbenzaldehyde and 44g of chloroform were added to the reaction kettle, and reacted at 75°C for 8h, then the temperature Adjust to 15°C, add 2.3g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 20g of absolute ethanol, mix well and add dropwise 14g of sodium carbonate (dissolved in 11mL of water ), after 1 hour of dripping, adjust the temperature to 60°C, react for 6 hours, distill under reduced pressure at 55°C for 0.8h, extract with 70mL of anhydrous methanol, wash with 90mL of petroleum ether for 3 times, and place at 55°C for 18 hours , cooled to room temperature to obtain phosphate-based aminopolysilsesquioxane;

[0062] b) At room temperature, N 2 In the atmosphere, add 1.2g 4,4'-diaminodiphenyl ether, 10g N,N-dimet...

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Abstract

The invention discloses a core-shell type low-dielectric flame-resistant polyimide-based fiber material and a preparation method thereof. Firstly, Kabachnik-Fields is carried out by using a phosphate-based compound, a symmetrical aromatic aldehyde compound and amino polysilsesquioxane. Phosphate-based amino polysilsesquioxane is prepared by reaction, and then aromatic diamine and aromatic dianhydride amide are reacted to obtain polyamic acid, and modified polyamic acid is prepared by reacting phosphoric acid ester-based amino polysilsesquioxane and polyamic acid amide. Then use the coaxial electrospinning method to spin the modified polyamic acid solution and the polyamic acid solution in different paths in the micro-syringe pump to obtain the core-shell modified polyamic acid fiber material, and finally After heat treatment, the core-shell low-dielectric flame-resistant polyimide-based fiber material is obtained. The core of the material is polyimide fiber, and the outer shell is modified polyimide. The dielectric constant is lower than 2.2, and the oxygen index LOI is higher than 35%, has excellent dielectric and flame retardant properties, and has good application prospects in the preparation of 5G, printed circuit boards, optoelectronics, aerospace and other related materials.

Description

technical field [0001] The invention relates to the field of fiber materials and their preparation, in particular to a core-shell type low-dielectric flame-resistant polyimide-based fiber material and a preparation method thereof. Background technique [0002] As a high-performance polymer fiber, aramid fiber is widely used as a matrix material for electronic products and structural material for aerospace vehicles because of its excellent dielectric properties, thermal stability, mechanical properties and optical properties. With the advent of the Internet era, the development and use of 5G and even higher-frequency communication technologies have greatly increased the social demand for electronic products. High-frequency communication technology has raised higher requirements for the performance of packaging materials for electronic products. requirements. [0003] Due to high-frequency electromagnetic waves, the dielectric constant of the dielectric material of the interc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F8/16C08G81/00D01D5/00D01D5/34D01D10/02
CPCD01F8/16C08G81/00D01D5/003D01D5/34D01D10/02
Inventor 周钰明徐健行鲍杰华卜小海张一卫孙伯旺王明亮
Owner SOUTHEAST UNIV
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