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Polyimide fiber and preparation method thereof

A polyimide fiber, imidization technology, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, textiles and papermaking, etc., can solve the problems of polyimide fiber development difficulties and other issues

Active Publication Date: 2021-04-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, there are many types of polyimide products, such as polyimide films, fibers and resins, among which the preparation of polyimide fibers has the highest requirements on the structure and purity of monomers, which makes the development of polyimide fibers more difficult

Method used

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  • Polyimide fiber and preparation method thereof
  • Polyimide fiber and preparation method thereof
  • Polyimide fiber and preparation method thereof

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Experimental program
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preparation example Construction

[0058] The invention provides a kind of preparation method of polyimide fiber, comprises the following steps:

[0059] a) Aromatic dianhydride monomers and diamine monomers are polymerized in a solvent to obtain a polyamic acid solution;

[0060] b) spinning the polyamic acid spinning solution to obtain polyamic acid fibers;

[0061] c) performing imidization treatment on the polyamic acid fibers to obtain polyimide fibers;

[0062] The diamine monomer is monomer A, or a mixture of monomer A and other diamine monomers;

[0063] The monomer A is selected from one or more of the compounds shown in the formulas A1-A4:

[0064]

[0065] The present invention uses a specific diamine monomer A containing a pyridazine structure or a pyrazine structure to react with dianhydride to form a polyamic acid precursor, which can prepare high-performance polyimide fibers and effectively improve the resistance of polyimide fibers. heat aging properties.

[0066] Regarding step a): the a...

preparation example 1

[0139] Raw material preparation example 1 Monomer A4—2,5-bis(4-aminophenyl)pyrazine

[0140] Under nitrogen protection, 4-aminophenylboronic acid pinacol ester (0.066mol, 14.46g), 2,5-dibromopyrazine (0.03mol, 5.80g), tetrakis (triphenylphosphine) palladium (0.001mol , 1.16g), anhydrous potassium carbonate (0.3mol, 41.46g), 50mL toluene and 50mL deionized water were successively added into a 250mL round-bottomed flask, and the reaction system was stirred and refluxed at 120°C, monitored by TLC until 2,5-di The bromopyrazine disappeared completely, and the reaction was stopped. After cooling to room temperature, a large amount of solids precipitated. After the solids were filtered and washed with deionized water, toluene and methanol for several times, the crude product was obtained by vacuum drying; after purification, a yellow 7.01 g of crystals, namely 2,5-bis(4-aminophenyl)pyrazine, with a yield of 89%.

[0141] 1 H NMR (400MHz, DMSO-d 6 ) 8.96 (s, 2H), 7.84 (d, J = 8.7H...

preparation example 2

[0144] Raw material preparation example 2 Monomer A2-3,6-bis(4-aminophenyl)pyridazine

[0145] Under the protection of nitrogen, 4-aminophenylboronic acid pinacol ester (0.456mol, 100.00g), 3,6-dibromopyridazine (0.21mol, 50.00g), tetrakis (triphenylphosphine) palladium (0.01mol , 12.00g), anhydrous potassium carbonate (1.81mol, 250.00g), 350mL toluene and 350mL deionized water were successively added into a 1000mL three-necked flask, and then the reaction was stirred and refluxed at 130°C, monitored by TLC until 3,6-dibromo Pyridazine completely disappeared, the reaction was stopped, cooled to room temperature, a large amount of solids were precipitated and filtered, and then washed with deionized water, toluene and methanol for several times, and dried in vacuum to obtain a crude product; after purification, a yellow crystal 47.93 g, namely 3,6-bis(4-aminophenyl)pyridazine, the yield is 87%.

[0146] 1 H NMR (400MHz, DMSO-d 6 ) δ 7.94 (s, 2H), 7.89 (d, J = 8.4 Hz, 4H), 6....

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Abstract

The invention provides a polyimide fiber and a preparation method thereof. According to the preparation method, a specific diamine monomer A containing a pyridazine structure or a pyrazine structure reacts with dianhydride to form a polyamide acid precursor spinning solution, so that the high-performance polyimide fiber can be prepared. Specifically, the mechanical property of the fiber can reach the standard of high strength and high modulus, and meanwhile, the fiber can still keep relatively high mechanical property after being thermally aged at the constant temperature of 300 DEG C for 400 hours, and has excellent thermal aging resistance.

Description

technical field [0001] The invention relates to the field of organic materials, in particular to a polyimide fiber and a preparation method thereof. Background technique [0002] Organic fibers refer to fibers made of organic materials, such as polyester, acrylic, nylon, and polypropylene, which are widely used in national production and life because of their light weight, low cost, chemical stability, and easy manufacturing. Among them, organic fibers with high mechanical properties and high thermal stability are required in many fields. As an important category of organic fibers, polyimide fibers have the characteristics of flame retardancy, high temperature resistance, chemical corrosion resistance, electrical insulation, and excellent mechanical properties. They are used in aerospace, national defense, marine development, high-speed transportation, and environmental protection. fields have a very wide range of applications. [0003] Compared with traditional organic fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/78C08G73/10
CPCD01F6/78C08G73/1067C08G73/1007
Inventor 邱雪鹏鲍峰代学民戚福玲董志鑫姚海波蔡艳春
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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