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Method for effectively preparing polyimide fiber

A technology of polyimide fiber and polyamic acid, which is applied in the direction of fiber chemical characteristics, dry spinning method, stretch spinning method, etc., can solve the problems of increased fiber production cost, low production efficiency, long time, etc., and achieve improved production Efficiency, reducing the effect of thermal or chemical cyclization procedures and equipment

Active Publication Date: 2011-10-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disclosed polyimide fiber dry spinning route is relatively complicated, especially the thermal or chemical cyclization of the precursor fiber takes a long time, consumes a lot of energy, and has low production efficiency, which leads to an increase in the production cost of the fiber; Moreover, polyamic acid is sensitive to water and temperature, and it is prone to degradation behavior during intermediate storage and degassing processes, which affects the performance of the fiber.

Method used

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  • Method for effectively preparing polyimide fiber
  • Method for effectively preparing polyimide fiber
  • Method for effectively preparing polyimide fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 0.226kg of 3,4'-diaminodiphenyl ether into 2L of dimethylacetamide and stir until completely dissolved. Afterwards, 0.245 kg of pyromellitic dianhydride was added to the solution in batches, and stirred at room temperature for 6 hours to obtain a pale yellow viscous polyamic acid solution. Add 58g of acetic anhydride and equimolar pyridine into the polyamic acid solution, stir and react for 2-4 hours to obtain the spinning dope.

[0019] The above-prepared spinning stock solution is degassed and then dry-spun on a dry-spinning machine. The length of the tunnel is 10 meters. The temperature of the upper section of the tunnel is 255° C., and the temperature of the lower section is 285° C. Then, it is wound and formed to obtain fibers. The fiber is stretched twice at 430° C. to obtain a high-performance polyimide fiber with a breaking strength of 5.5 cN / dtex and a breaking elongation of 32%.

Embodiment 2

[0021] Add 2.246kg of 4,4'-diaminodiphenylmethane into 20L of dimethylacetamide and stir until completely dissolved. Afterwards, 2.471 kg of pyromellitic dianhydride was added to the solution in batches, and stirred at room temperature for 8 hours to obtain a pale yellow viscous polyamic acid solution. Add 578g of acetic anhydride and equimolar triethylamine into the polyamic acid solution, stir and react for 2-4 hours to obtain the spinning dope.

[0022] The above-prepared spinning stock solution is degassed and then dry-spun on a dry-spinning machine. The length of the tunnel is 12 meters. The temperature of the upper section of the tunnel is 280 ° C, and the temperature of the lower section is 320 ° C. After that, it is wound and formed to obtain fibers. The fiber is stretched 7 times at 500° C. to obtain a high-performance polyimide fiber with a breaking strength of 17 cN / dtex and a breaking elongation of 5%.

Embodiment 3

[0024] Add 0.689kg of phenylenediamine into 10L of N-methylpyrrolidone and stir until completely dissolved. Afterwards, 1.876 kg of biphenyl dianhydride was added to the solution in batches, and stirred at room temperature for 10 hours to obtain a light yellow viscous polyamic acid spinning stock solution.

[0025] The above-prepared spinning stock solution is degassed and then dry-spun on a dry-spinning machine. The length of the tunnel is 9 meters. The temperature of the upper section of the tunnel is 290 ° C, and the temperature of the lower section is 320 ° C. After that, it is wound and formed to obtain fibers. The fiber was stretched 5 times at 510° C. to obtain a high-performance polyimide fiber with a breaking strength of 10.3 cN / dtex and a breaking elongation of 8%.

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Abstract

The invention discloses a method for effectively preparing polyimide fiber, wherein a dry-process spinning device is used for directly preparing polyimide fiber; the method comprises the following steps of: (1) condensing dianhydride and diamine monomers to form precursor spinning solution used for spinning, adding chemical cyclizing agent or not; (2) spinning the fiber at a high temperature in a drying manner; (3) and hot-stretching the polyimide fiber. The polyimide fiber prepared in the invention has good high-temperature resistance, corrosion resistance, mechanical performance, and the like, and the production efficiency is greatly improved and the manufacturing procedure of cyclization reaction is omitted; and the polyimide fiber prepared in the invention can be widely applied to composite material reinforcing fiber, cable reinforcing core, car and ship mooring rope, filter material of high-temperature or radioactive substance, etc.

Description

technical field [0001] The invention relates to a preparation method for polyimide fiber production, which is characterized in that the polyimide fiber is directly produced by passing the polyamic acid spinning slurry through a high-temperature spinning tunnel, and the polyimide fiber is produced after thermal stretching. Amine fiber. Background technique [0002] Polyimide fiber is a high-performance fiber with many superior properties such as high strength, high modulus, high temperature resistance, flame resistance, radiation resistance, and chemical corrosion resistance. There are many ways to prepare polyimide fibers: One is the one-step technical route: firstly, polyimide solution is synthesized, used as raw material for direct spinning, and polyimide fibers are obtained after thermal stretching. It is relatively simple, but the choice of solvent is relatively difficult and often has high toxicity, so the type of polyimide is greatly restricted. The national invention...

Claims

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Application Information

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IPC IPC(8): D01F6/74C08G73/10D01D5/04D01D5/12
Inventor 张清华夏清明徐圆陈大俊
Owner DONGHUA UNIV
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