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A kind of 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 processing repeatability, large specific surface area of ​​nanoparticles, and poor heat aging resistance of organic small molecules.

Active Publication Date: 2021-02-05
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 the product’s UV resistance is affected; 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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  • A kind of polyimide fiber and preparation method thereof
  • A kind of polyimide fiber and preparation method thereof
  • A kind of polyimide fiber and preparation method thereof

Examples

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preparation example Construction

[0054] The invention provides a kind of preparation method of polyimide fiber, comprises the following steps:

[0055] a) Aromatic dianhydride monomers and diamine monomers are polymerized in a solvent to obtain polyamic acid spinning stock solution;

[0056] b) spinning the polyamic acid spinning stock solution to obtain polyamic acid fibers;

[0057] c) performing imidization treatment on the polyamic acid fibers to obtain polyimide fibers;

[0058] The diamine monomer comprises monomer A and monomer B;

[0059] The monomer A is selected from one or more of the structures shown in formula a-1 to formula a-3:

[0060]

[0061] Among them, R 1 selected from: alkyl, substituted or unsubstituted phenyl;

[0062] The monomer B is selected from one or more of the structures shown in formula b-1 to formula b-7:

[0063]

[0064] in,

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

[0066] X is selected from -O-, -S-, or -NH-;

[0067] D is selected from -O-, -S-, or -NH-...

preparation example 1

[0217] Raw material preparation example 1 Monomer A-(3,5-diaminophenyl)(2-hydroxy-4-hexyloxyphenyl)methanone

[0218] (1) 37.24 grams (0.30 moles) of 3-methoxyphenol, 54.47 grams (0.33 moles) of n-hexane bromide, 49.76 grams (0.36 moles) of potassium carbonate, 2.49 grams (0.015 moles) of potassium iodide and 275 grams of acetonitrile were added successively into the reaction bottle, and then heated the reaction system to 80 ° C for 6 hours. After being cooled to room temperature, it was added to 1500 milliliters of water, the product was extracted with dichloromethane, dried over anhydrous magnesium sulfate, the solvent was concentrated, and 53.74 grams of the representative compound 1-hexyloxy-3-methoxyl group of the structure shown in formula (II) was obtained through purification. The refined product of phenylbenzene, the yield is 86.0%.

[0219] 1 H NMR (400MHz, DMSO) δ = 7.152 (t, J = 8.0Hz, 1H), 6.445-6.510 (m, 3H), 3.920 (t, J = 6.4Hz, 2H), 3.718 (s, 3H), 1.735 -1.6...

preparation example 2

[0226] Raw material preparation example 2 Monomer A-(3,5-diaminophenyl)(2-hydroxy-4-(4-fluorophenoxy)phenyl)methanone

[0227] (1) 62.07 grams (0.50 moles) of 3-methoxyphenol, 78.75 grams (0.45 moles) of p-bromofluorobenzene, 4.76 grams (0.025 moles) of cuprous iodide, 82.93 grams (0.60 moles) of potassium carbonate and 420 grams N,N-dimethylformamide was sequentially added into the reaction flask, and the reaction system was heated to 150° C. for 8 hours under the protection of nitrogen. After being cooled to room temperature, it was added to 2500 milliliters of water, the product was extracted with dichloromethane, washed with dilute hydrochloric acid, dried over anhydrous magnesium sulfate, the solvent was concentrated, and 77.58 grams of the representative compound 1-(4-fluoro The refined product of phenoxy)-3-methoxybenzene, the yield is 79.0%.

[0228] 1 H NMR (400MHz, DMSO) δ=7.295–7.175(m,3H),7.105–7.025(m,2H),6.703(dd,J=8.4Hz,2.2Hz,1H),6.557(t,J=2.2Hz , 1H), 6.504 ...

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Abstract

The invention provides a polyimide fiber and a preparation method thereof. The preparation method of the polyimide fiber provided by the present invention comprises: a) polymerizing the aromatic dianhydride monomer and the diamine monomer in a solvent to obtain a polyamic acid spinning stock solution; b) making the polyamic acid spinning stock solution Spinning to obtain polyamic acid fibers; c) imidizing the polyamic acid fibers to obtain polyimide fibers; the diamine monomers include monomer A and monomer B; wherein, Monomer A is selected from one or more of the structures of formula a-1 to formula a-3 shown below; monomer B is selected from one or more of the structures of formula b-1 to formula b-7 shown below kind. In the present invention, the specific monomer A and the monomer B that contain the o-hydroxybenzophenone structural unit in the side chain are matched as the diamine monomer, and are polymerized together with the dianhydride monomer and obtained polyimide fiber through spinning, which can improve the The UV aging resistance of polyimide fiber still maintains good breaking strength after long-term UV irradiation.

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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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78C08G73/10
CPCC08G73/1039C08G73/1042C08G73/1046C08G73/105C08G73/1071D01F6/78
Inventor 董志鑫姚海波代学民刘芳芳李国民蔡艳春邱雪鹏
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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