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Polyimide fiber and its preparing method

A technology of polyimide fiber and polyimide, which is applied in the field of polymer fiber and its preparation, can solve the problems that the mechanical properties need to be improved, and achieve the effect of prolonging the solidification time, optimizing the solidification conditions and ideal mechanical properties

Inactive Publication Date: 2006-08-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that the mechanical properties need to be improved

Method used

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  • Polyimide fiber and its preparing method

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Experimental program
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Effect test

Embodiment 1

[0014] The synthesis reaction of polyamic acid is carried out in a three-necked flask, which is stirred by a stirrer with a multi-stage speed governor, and nitrogen gas is passed through one side of the three-necked flask to keep the reactants from being oxidized. The used three-necked flask was dried in an oven at 130° C. for 3 hours before use. Accurately weigh 14.592 g of 4,4'-diaminodiphenyl ether (ODA) and 16.212 g of pyromellitic dianhydride (PMDA) with an electronic balance, first add the weighed diamine into the three-necked flask, and add the solvent DMAC ( Finally add 160mL) and make it completely dissolve into a transparent liquid under stirring. While stirring, use the freezing bath of the low-temperature cooling liquid circulation pump to cool it to 0°C, and then add the dianhydride powder in four times while stirring, each time 1 hour apart. Then use the metered DMAc to wash the remaining dianhydride on the bottle wall into the bottle, and stir and react under n...

Embodiment 2-5

[0016] The reaction process is the same as in Example 1, and other conditions are shown in Table 1.

[0017] implement

Embodiment 6

[0019] The polyamic acid solution obtained in Example 1 was spun and shaped using the wet process route shown in Figure 2. After filling about 150mL of polyamic acid spinning solution into a special storage tank with a spinneret, inject the circulating fluid at 0°C from the low-temperature cooling liquid circulation pump into the jacket of the slurry storage tank to make the spinning solution Keep at 0°C, stand under normal pressure for defoaming for 15 hours, and then perform spinning operation. Use nitrogen to add a pressure of 0.3MPa to the slurry, and the spinning solution passes through a 1000-mesh filter cloth, and is sprayed out through the spinneret into the vertical coagulation bath. The extrusion speed of the spinning slurry is 11.90m / min, and the vertical coagulation bath The length of the wire is 0.75m. In the coagulation bath, the thread is properly solidified and enters the water bath through the godet roller. The length of the water bath is 1.85m. The speed of t...

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Abstract

The present invention discloses a kind of polyimide fiber and its preparation process. The preparation process includes the following steps: 1. reacting 4, 4í»-diamino diphenyl ether and pyromellitic dianhydride in the weight ratio of 1 to 1.02 with N, N-dimethyl acetylamide solution of 15-20 % concentration at 0-5 deg.c to obtain polyamic acid solution; 2. wet spinning the polyamic acid solution and imidation reaction of the polyamic acid fiber to obtain polyimide fiber through dewatering and cyclization; and 3. mixing the polyimide fiber with acetic anhydride and triethylamide, flushing with acetone, soaking and drying to obtain the polyimide fiber. The present invention has positive effects of optimized synthesis condition of spinning solution, prolonged solidification period of initially formed fiber in the solidification bath, and fiber with ideal mechanical performance.

Description

technical field [0001] The invention relates to a polymer fiber and a preparation method thereof, in particular to a polyimide fiber and a preparation method thereof. Background technique [0002] Polyimide fiber has unique chemical, physical, mechanical and electrical properties, especially its excellent thermal stability and good mechanical properties. At the same time, polyimide fiber has high radiation resistance, which is unmatched by other fibers, so it is one of the preferred materials for aerospace, and it is also a filter material for high-temperature media and radioactive substances. [0003] There are generally two ways to synthesize and spin polyimide fibers. One is to synthesize polyimide solution first, and then directly spin it into polyimide fibers. The main disadvantage is the use of phenolic solvents, which are highly toxic and have a large amount of residue in the fibers. The second is a two-step method, first preparing polyamic acid solution, and then s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74
Inventor 李焱刘兆峰于俊荣胡祖明
Owner DONGHUA UNIV
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