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Method for spinning polyimide fiber by utilizing dry-process spinning technology

A polyimide fiber, dry spinning technology, applied in the direction of spinning solution preparation, dry spinning method, fiber chemical characteristics, etc., to achieve large output, improve mechanical properties and stability, and improve performance

Active Publication Date: 2015-01-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the technology of preparing polyimide fibers by the two-step dry method has been applied in industrialization, due to the autocatalytic cracking of the ortho carboxyl group in the polyamic acid precursor-polyamic acid in this process, resulting in The anhydride is hydrolyzed by the water in the solvent, which puts forward higher requirements for the spinning process

Method used

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  • Method for spinning polyimide fiber by utilizing dry-process spinning technology
  • Method for spinning polyimide fiber by utilizing dry-process spinning technology
  • Method for spinning polyimide fiber by utilizing dry-process spinning technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Under the protection of nitrogen deoxygenation, add 1.84L of N-methylpyrrolidone, 69.95g of lithium chloride, and 307.17g of 4,4-diaminodiphenyl ether into a 3L polymerization kettle, and add 1 after it is completely dissolved. 115.54 g of 4-dimethyl-2,5-diacyl chloride and 13.99 g of isoquinoline were reacted at 0° C. for 2.5 h to obtain a spinning dope. (2) After degassing the spinning stock solution, dry spinning on the spinning machine, wherein the spinneret temperature is 60-70°C, the hot air temperature is 200°C, the tunnel temperature is 280°C, and the spinning air volume is 28m 3 / min, the air volume ratio of the upper and lower outlets of the tunnel is 70 / 30, and the winding speed is 150m / min; (3) the oxygen content of the spun fibers is in a mixed gas atmosphere of 35% at 200°C, and the temperature is kept for 1h, and then Raise the ambient temperature to 350°C, keep the temperature constant for 3 hours, and finally raise the temperature of the fiber to 40...

Embodiment 2

[0027] (1) Under the protection of nitrogen deoxygenation, add 2.56L of N-methylpyrrolidone, 100.23g of lithium chloride, and 4,4'-diamino-2,2'-bis(trifluoromethyl ) biphenyl 320.23g, add 281.13g of 2,6-dimethyl-1,5-diacylchloronaphthalene and 20.05g of isoquinoline after completely dissolving, and react at 5°C for 3h to obtain spinning stock solution. (2) Degas the spinning dope and dry-spin it on the spinning machine, wherein the spinneret temperature is 60°C, the hot air temperature is 190°C, the tunnel temperature is 220°C, and the spinning air volume is 28m 3 / min, the air volume ratio of the upper and lower outlets of the tunnel is 70 / 30, and the winding speed is 150m / min. (3) Keep the oxygen content of the spun fibers at 200°C in a 35% mixed gas atmosphere, keep the temperature constant for 1 hour, then increase the ambient temperature to 350°C, keep the temperature constant for 3.5 hours, and finally raise the temperature of the fibers to 450°C in a nitrogen atmosphere...

Embodiment 3

[0029] (1) Under the protection of nitrogen deoxygenation, add 1.83L of dimethylformamide, 161.48g of calcium chloride, and 108.07g of p-phenylenediamine into a 3L polymerization kettle, and add 4,4'-dimethylformamide after it is completely dissolved. Base-3,5'-diacyl chloride biphenyl 307.17g, isoquinoline 11.53g, react at 0°C for 3h to obtain spinning dope. (2) After degassing the spinning stock solution, dry spinning on the spinning machine, wherein the spinneret temperature is 60-70°C, the hot air temperature is 150°C, the tunnel temperature is 180°C, and the spinning air volume is 28m 3 / min, the air volume ratio of the upper and lower outlets of the tunnel is 70 / 30, and the winding speed is 150m / min. (3) Keep the oxygen content of the spun fibers at 200°C in a 35% mixed gas atmosphere, keep the temperature constant for 1 hour, then increase the ambient temperature to 350°C, keep the temperature constant for 5 hours, and finally raise the temperature of the fibers to 450°...

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Abstract

The invention relates to a method for spinning a polyimide fiber by utilizing a dry-process spinning technology. The method comprises the following steps: (1) adding diamine and dimethyl oxalyl chloride monomer into 1-methyl-2-pyrrolidinone, N,N-dimethylformamide and N,N-dimethylacetamide to synthesize into an O-methyl polyamide spinning solution; (2) performing dry-process spinning, namely extruding the polyamide solution by spinneret orifices, and then winding through a high-temperature channel to obtain a polyamide nascent fiber; and (3) carrying out staged temperature rising on the obtained O-methyl polyamide nascent fiber for dewatering and ring formation, thus obtaining the polyimide fiber with imide rings. The method is a new path for preparing polyimide by adopting the O-methyl polyamide fiber as a precursor through dry-process spinning and carrying out high-temperature oxidation and ring formation and provides a wholly-new idea for preparing polyimide.

Description

technical field [0001] The invention belongs to the field of man-made fiber preparation, in particular to a method for spinning polyimide fibers by dry spinning technology. Background technique [0002] As a high-performance fiber, polyimide fiber has become a hot spot in industrial development due to its excellent thermal stability, solvent resistance, chemical stability and outstanding radiation resistance, and has been widely used in recent years. Civil aviation and other businesses. At present, polyimide fibers are usually spun by a two-step method, that is, dianhydride and diamine are mixed in an aprotic polar solvent such as DMF (dimethylformamide), DMAc (dimethylacetamide) and NMP (N-formaldehyde). Based pyrrolidone) in low temperature polymerization to obtain polyimide precursor polyamic acid solution, and then through dry, wet or dry spray wet spinning spinning into fibers, and then through chemical cyclization or thermal cyclization dehydration Finally, polyimide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01D5/04D01D1/02D01D10/02
Inventor 张清华谭文军张殿波赵昕李振涛董杰尹朝青陈大俊
Owner DONGHUA UNIV
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