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A kind of preparation method of polyimide fiber

A technology of polyimide fiber and polyamic acid, which is applied in the field of fiber, can solve the problems that cannot fully meet the needs of polyimide fiber, and achieve excellent durability and anti-aging performance

Active Publication Date: 2016-07-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, at present, there are few studies on polyimide fibers resistant to radiation radiation, which cannot fully meet the needs of polyimide fibers in spacecraft, shielding fabrics, flexible ropes and cables, nuclear industry, fire-resistant and flame-retardant materials, etc.

Method used

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  • A kind of preparation method of polyimide fiber
  • A kind of preparation method of polyimide fiber
  • A kind of preparation method of polyimide fiber

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preparation example Construction

[0033] The embodiment of the present invention discloses a kind of preparation method of polyimide fiber, comprises the following steps:

[0034] (A) dianhydride and diamine are polymerized in an aprotic polar solvent to obtain a polyamic acid spinning solution;

[0035] The dianhydride is one or more of the compounds represented by formulas (I) to (III):

[0036]

[0037] Among them, A in the formula (III) is -S-, -O-,

[0038] The diamine is one or more of 4,4'-diaminobenzophenone, 3,4'-diaminobenzophenone and 3,3'-diaminobenzophenone, or 4 , one or more of 4'-diaminobenzophenone, 3,4'-diaminobenzophenone and 3,3'-diaminobenzophenone with (IV)~(IX) One or more mixtures of the compounds shown;

[0039]

[0040] Among them, B is -O-, -S-, -SO 2 -, -CH 2 -,

[0041] D is N, S or O;

[0042] (B) spinning the polyamic acid spinning solution described in step A) to obtain polyamic acid fibers;

[0043] (C) subjecting the polyamic acid fiber described in step ...

Embodiment 1

[0066] Dissolve 150.18g (0.750mol) of 4,4'-diaminodiphenyl ether and 159.19g (0.750mol) of 3,4'-diaminobenzophenone in 3200ml of dimethyl sulfoxide, and add 310.82 g (1.425mol) pyromellitic dianhydride, react at 50°C for 4 hours to obtain a light yellow viscous polyamic acid spinning solution, which is directly used as spinning slurry after filtration.

[0067] The above-mentioned polyamic acid slurry is spun and formed by dry-jet wet spinning technology, and the spinning slurry at room temperature is accurately metered with a metering pump, extruded from the spinneret hole, and then enters dimethyl sulfoxide and water through the air layer. (1:4 volume ratio) in the coagulation bath. The spinneret has 200 holes, the hole diameter is Φ0.15mm, the spray ratio is 1.6 times, the spinning speed is 30m / min, and the air layer height is 10mm. The as-spun fibers were washed with water and then dried in a hot nitrogen tunnel to obtain polyamic acid fibers.

[0068] The polyamic acid ...

Embodiment 2

[0070] Dissolve 792.12g (2.150mol) of 4,4'-bis(3-aminophenoxy)biphenyl and 212.25g (1.000mol) of 4,4'-diaminobenzophenone in 137000ml of N-methylpyrrolidone, Add 196.31g (0.900mol) of pyromellitic dianhydride and 844.85g (2.100mol) of 3,3',4,4'-triphenylene ether tetracarboxylic dianhydride under stirring, and react at -10°C for 10h to obtain light Yellow viscous polyamic acid spinning solution, the solution is directly used as spinning slurry after filtration.

[0071] The above-mentioned polyamic acid slurry is spun and formed by dry-jet wet spinning technology, and the spinning slurry at room temperature is accurately metered by a metering pump, extruded from the spinneret hole, and then enters N-methylpyrrolidone and water through the air layer. (1:5 volume ratio) in the coagulation bath. The spinneret has 30 holes, the hole diameter is Φ0.12mm, the spray ratio is 2.0 times, the spinning speed is 30m / min, and the air layer height is 5mm. The as-spun fibers were washed wi...

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Abstract

The invention provides a preparation method of polyimide fiber. Dianhydride and diamine have a polymerization reaction in an aprotic polar solvent, so as to obtain a polyamide acid spinning solution, wherein the dianhydride is one or more than one of compounds shown in formulas (I) to (III); the diamine is one or more than one of 4,4'-diaminobenzophenone, 3,4'-diaminobenzophenone and 3,3'-diaminobenzophenone, or a mixture of 4,4'-diaminobenzophenone, 3,4'-diaminobenzophenone, 3,3'-diaminobenzophenone and one or more than one of the compounds shown in the formulas (IV) to (IX); the polyamide acid spinning solution is spun, so as to obtain polyamide acid fiber; the polyamide acid fiber is subjected to thermal imidization treatment, so as to obtain polyimide nascent fiber; the polyimide nascent fiber is subjected to hot drawing treatment, so as to obtain the polyimide fiber. The polyimide fiber obtained by the method has excellent tolerance and ageing resistance to rays.

Description

technical field [0001] The invention relates to the field of fibers, in particular to a preparation method of polyimide fibers. Background technique [0002] Polyimide is a class of polymers containing imide rings in the main chain, among which polymers containing phthalimide structures are the most important. Polyimide has outstanding characteristics in terms of performance and synthesis, and has broad application prospects whether it is used as a structural material or a functional material. At present, it is mainly used in aerospace, aviation, microelectronics, nano, liquid crystal, separation membrane, Laser lights and other fields. [0003] Polyimide fiber, also known as aromatic heterocyclic fiber, is a synthetic fiber. Polyimide fiber has excellent properties such as high strength, high modulus, high temperature resistance, flame retardancy, and chemical corrosion resistance. It has a wide range of applications and can be made into a variety of industrial products,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78C08G73/10D01D5/04D01D5/06D01D5/12
Inventor 邱雪鹏李国民丁祥董志鑫刘芳芳高连勋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI