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Polyimide fiber and preparation method thereof

A technology of polyimide fiber and polyamic acid fiber, applied in the fiber field, can solve the problems of poor heat aging resistance, large specific surface area of ​​nanoparticles, and poor mechanical properties of materials, etc.

Active Publication Date: 2020-03-06
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

The main problem of the method of adding anti-ultraviolet nanoparticles is that the nanoparticles have a large specific surface area and are easy to agglomerate, so the dispersion of the nanoparticles in the matrix is ​​difficult to control, the processing repeatability is poor, and it affects the product's resistance to ultraviolet radiation; the method of adding small organic molecules The main problem is that organic small molecules have poor thermal aging resistance, and they will decompose and lose under high temperature conditions, resulting in poor mechanical properties of materials, reducing or even losing the anti-ultraviolet radiation performance of materials.

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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preparation example Construction

[0053] The invention provides a kind of preparation method of polyimide fiber, comprises the following steps:

[0054] a) Aromatic dianhydride monomers and diamine monomers are polymerized in a solvent to obtain polyamic acid spinning stock solution;

[0055] b) spinning the polyamic acid spinning stock solution to obtain polyamic acid fibers;

[0056] c) performing imidization treatment on the polyamic acid fibers to obtain polyimide fibers;

[0057] The diamine monomer comprises monomer A and monomer B;

[0058] The monomer A is selected from one or more of the structures shown in formula a-1 to formula a-8:

[0059]

[0060] The monomer B is selected from one or more of the structures shown in formula b-1 to formula b-7:

[0061]

[0062] in,

[0063] M is selected from -O-, -S-, or -NH-;

[0064]X is selected from -O-, -S-, or -NH-;

[0065] D is selected from -O-, -S-, or -NH-;

[0066] E is selected from -O-, -S-, -SO 2 -, -CH 2 -, -C(CF 3 ) 2 -, -CO-, ...

preparation example 1

[0203] Raw material preparation example 1 Preparation of diamine shown in monomer A-formula a-1

[0204] (1) 69.52 grams (0.56 moles) of 3-methoxyphenol, 88.23 grams (0.56 moles) of p-nitrochlorobenzene, 85.14 grams (0.616 moles) of potassium carbonate and 200 grams of dimethyl sulfoxide were added to the reactor in sequence , heated to 160°C for 6 hours; cooled to 60°C, added to 2000 ml of water, the crude product was precipitated, filtered out, washed with water, dissolved in dichloromethane, dried over anhydrous magnesium sulfate, and concentrated to obtain the crude product , 114.23 grams of refined product of compound (II-1) shown in formula (II) were obtained through recrystallization; yield 83.2%.

[0205] Utilize nuclear magnetic resonance to characterize the structural compound (II-1) shown in the formula (II) that obtains, the proton nuclear magnetic resonance spectrum result that obtains is: 1 H NMR (400MHz, DMSO) δ = 8.280–8.205 (m, 2H), 7.389 (t, J = 8.2Hz, 1H), 7....

preparation example 2

[0212] Raw material preparation example 2 Preparation of diamine shown in monomer A-formula a-2

[0213] (1) 62.07 grams (0.50 moles) of 3-methoxyphenol, 101.0 grams (0.50 moles) of m-bromonitrobenzene, 4.76 grams (0.025 moles) of cuprous iodide, 76.02 grams (0.55 moles) of potassium carbonate and 200 Add grams of N,N-dimethylformamide to the reaction flask in turn, heat the reaction system to 150°C under nitrogen protection and react for 12 hours; after cooling to 60°C, add it to 2000 ml of water, precipitate the crude product, filter it out, and wash with water Afterwards, it was dissolved in dichloromethane, dried over anhydrous magnesium sulfate, the solvent was concentrated, and purified to obtain 90.59 g of the refined product of the structural compound (II-2) shown in formula (II); the yield was 73.9%.

[0214] (2) 89.07 grams (0.48 moles) of 4-nitrobenzoyl chloride, 69.34 grams (0.52 moles) of aluminum trichloride, 1000 milliliters of dichloromethane and 105.45 grams (...

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Abstract

The invention provides a polyimide fiber and a preparation method thereof. The preparation method includes the steps: a) polymerizing an aromatic anhydride monomer and a diamine monomer to obtain polyamide acid spinning solution; b) spinning the polyamide acid spinning solution to obtain a polyamide acid fiber; c) performing imidization treatment on the polyamide acid fiber to obtain a polyimide fiber. The diamine monomer includes a monomer A and a monomer B, the monomer A is selected from one or more of structures from a formula a-1 to a formula a-8 as shown in the specification, and the monomer B is selected from one or more of structures from a formula b-1 to a formula b-7 as shown in the specification. According to the polyimide fiber, special monomer A and special monomer B are matched to serve as a diamine monomer, main chains of the monomer A and the monomer B contain o-hydroxybenzophenone structure units, the monomer A, the monomer B and aromatic anhydride monomer are polymerized and spun to obtain a polyimide fiber, special monomers are introduced, and the ultraviolet resistance and the ageing resistance of polyimide can be improved.

Description

technical field [0001] The invention relates to the field of fiber technology, in particular to a polyimide fiber and a preparation method thereof. Background technique [0002] Polyimide fiber material is a new type of special fiber with excellent comprehensive properties. The molecular chain contains imide rings. It has many excellent properties such as high strength, high modulus, high temperature resistance, flame retardancy, chemical corrosion resistance, and low temperature resistance. Performance, widely used in aerospace, weapons and equipment, transportation and other high-tech fields. [0003] During the use of polyimide fiber materials, its performance will be affected by the environment, especially after ultraviolet radiation, chemical reactions will occur on the surface of the fiber, resulting in a decrease in the performance of the fiber. In particular, polyimide fiber materials used in aerospace vehicles, without the barrier of the high-altitude atmosphere (e...

Claims

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Application Information

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IPC IPC(8): D01F6/78C08G73/10
CPCC08G73/1042C08G73/1071D01F6/78
Inventor 姚海波董志鑫刘芳芳代学民李国民王汉夫邱雪鹏
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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