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Polyamic acid, polyimide fiber thereof and preparation method of polyamide acid and polyimide fiber

A technology of polyimide fiber and polyamic acid, applied in the field of polyimide, can solve the problems of unfavorable continuous production and processing, low elongation at break, easy to break, etc., achieve good production continuity and improve mechanical properties , The effect of increasing the drafting ratio

Pending Publication Date: 2022-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention mainly solves one of the problems in the prior art. In the prior art, the high-strength and high-model polyimide fiber has high fiber brittleness during the imidization process, and the elongation at break is generally low, and it is prone to breakage, which is not conducive to continuous production and further processing issues

Method used

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  • Polyamic acid, polyimide fiber thereof and preparation method of polyamide acid and polyimide fiber
  • Polyamic acid, polyimide fiber thereof and preparation method of polyamide acid and polyimide fiber
  • Polyamic acid, polyimide fiber thereof and preparation method of polyamide acid and polyimide fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] [Example 1] BIA molar ratio 0.7

[0063] 1. Stock solution preparation: (1) 4.10Kg (18.28mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA) and 3.21Kg (7.83mol) of 2,2-bis[4 -(4-Aminophenoxy)phenyl]propane (BAPP) was dissolved in 85Kg N,N-dimethylacetamide (DMAc), at 25℃N 2 Stir under protection, after completely dissolving, add 7.68Kg (26.12mol) of 3,3'4,4'-biphenyltetracarboxylic dianhydride (BPDA), and continue stirring for 1h after the addition, to obtain a polymer with a solid content of 15%. Amic acid (PAA) spinning dope.

[0064] 2. Coagulation forming: After vacuum degassing, the spinning dope is filtered at 3 μm, and then extruded through the spinneret into the first coagulation bath. The temperature of the coagulation bath is 0°C, the concentration is 35%, and the draft ratio is -50%. The second coagulation bath is 30°C, the concentration is 20%, and the draft ratio is 110%, and the third coagulation bath is at 40°C, the concentration is 10%, and the draft...

Embodiment 2

[0070] [Example 2] BIA molar ratio 0.6

[0071] 1. Stock solution preparation: (1) 3.70Kg (16.49mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA) and 3.21Kg (10.99mol) of all-meta-triphenyl ether Diamine (1,3,3-APB) was dissolved in 85Kg N,N-dimethylacetamide (DMAc), at 25℃N 2 Stir under protection, after completely dissolving, add 8.08Kg (27.49mol) of 3,3'4,4'-biphenyltetracarboxylic dianhydride (BPDA), and continue stirring for 1h after the addition, to obtain a polymer with a solid content of 15%. Amic acid (PAA) spinning dope.

[0072] The rest of the steps were as in Example 1, and the monofilament strength of the obtained polyimide fiber was 3.3GPa, the modulus was 125GPa, and the elongation at break was 6.3%.

Embodiment 3

[0073] [Example 3] BIA molar ratio 0.9

[0074] 1. Stock solution preparation: (1) 5.81Kg (25.91mol) of 2-(4-aminophenyl)-5-aminobenzimidazole (BIA) and 0.71Kg (2.88mol) of 4,4'-diamino Diphenylsulfone (DDS) was dissolved in 85Kg N,N-dimethylacetamide (DMAc), at 25°C N 2 Stir under protection, after completely dissolving, add 8.47Kg (28.79mol) of 3,3'4,4'-biphenyltetracarboxylic dianhydride (BPDA), continue stirring for 1h after the addition, and obtain a polymer with a solid content of 15%. Amic acid (PAA) spinning dope.

[0075] The rest of the steps were according to Example 1, the monofilament strength of the obtained polyimide fiber was 3.2GPa, the modulus was 105GPa, and the elongation at break was 5.8%.

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Abstract

The invention relates to polyamic acid, polyimide fibers thereof and a preparation method of the polyamic acid and the polyimide fibers. The polyamic acid has a structure as shown in a formula 1, wherein Ar is an aromatic residue containing a bridging structure; m is the molar ratio of the repeating unit with the structure shown in the formula 2 in the polyamide acid, and m is larger than or equal to 0.6 and smaller than or equal to 0.9. The breaking strength of the polyimide fiber is larger than 3.0 GPa, the modulus is larger than 100 GPa, the elongation at break is larger than 4%, and the problems that in the prior art, in the imidization process of the high-strength and high-model polyimide fiber, brittleness is achieved, the elongation at break is generally low, and continuous production and further processing are not facilitated are solved.

Description

technical field [0001] The invention relates to the field of polyimide, in particular to a polyamic acid, its polyimide fiber and a preparation method thereof. Background technique [0002] As a high-performance organic fiber, polyimide (PI) fiber has excellent properties such as high strength, high modulus, high and low temperature resistance, and radiation resistance. It is suitable for use under extreme conditions such as high temperature and high heat. It is used in aerospace, marine engineering, advanced There are extremely important applications in fields such as rail transit and high-temperature filtration. [0003] With the development of science and technology, the scope of application of PI fiber continues to expand, and it has increasingly penetrated into various fields from civil, industrial to national defense. Higher strength and modulus have become an important and challenging goal to pursue. However, the global PI fiber technology is mainly concentrated abro...

Claims

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Application Information

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IPC IPC(8): C08G73/10D01F6/78
CPCC08G73/1067C08G73/1007C08G73/1071C08G73/1064C08G73/1039D01F6/78
Inventor 陈雪崔晶孙旭阳林程
Owner CHINA PETROLEUM & CHEM CORP
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