Method for preparing polyimide fiber

A polyimide fiber and polyimide technology, applied in the field of polyimide fiber preparation, can solve the problems of inaccurate temperature control, unfavorable operation, etc., to overcome inaccurate temperature control, high limit oxygen index, Ease of continuous production

Active Publication Date: 2009-01-07
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

However, the imidization process generally adopts two-stage furnace technology, the temperature control is not accurate, and it is not conducive to operation.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: 35.14g (0.325mol) p-phenylenediamine and 352.32g (1.100mol) 2,2'-bis(trifluoromethyl)4,4'-biphenylenediamine were dissolved in 4470ml N,N- In the dimethylacetamide, 327.18 g (1.500 mol) pyromellitic dianhydride was added under stirring state, and reacted at room temperature for 10 hours to obtain a pale yellow viscous polyamic acid spinning solution. The solution is directly used as spinning slurry after filtration.

[0017] The above-mentioned polyamic acid slurry is spun and formed by the dry-jet wet spinning method, and the spinning slurry at room temperature is accurately metered by a metering pump, and then extruded from the spinneret and enters the N,N-dimethyl In a coagulation bath of acetamide and water (1:1 volume ratio). The spinneret has 100 holes, the hole diameter is Φ0.08mm, the spray ratio is 3.0 times, the spinneret speed is 60m / min, and the air layer height is 30mm. The nascent polyamic acid fiber is treated in a gradient temperature-raisin...

Embodiment 2

[0018] Example 2: Dissolve 300.36g (1.500mol) of 4,4'-diaminodiphenyl ether in 3707ml of N,N-dimethylformamide, and add 218.12g (1.000mol) of pyromellitic dianhydride under stirring React with 147.11 g (0.500 mol) of 3,4'-biphenyldianhydride at -5°C for 10 hours to obtain a light yellow viscous polyamic acid spinning solution. The solution is directly used as spinning slurry after filtration.

[0019] The above-mentioned polyamic acid slurry is used for spinning and forming in the wet process technology route. After the spinning slurry at room temperature is accurately metered with a metering pump, it is extruded from the spinneret and enters ethanol and water (1:2 volume ratio) through the air layer. ) in the coagulation bath. The spinneret has 150 holes, the hole diameter is Φ0.10mm, the spinning speed is 100m / min, the spray ratio is 7.0 times, and the air layer height is 50mm. The nascent polyamic acid fiber is treated in a gradient temperature-raising heat treatment furn...

Embodiment 3

[0020] Example 3: 315.38g (1.575mol) of 3,4'-diaminodiphenyl ether was dissolved in 1264ml of N-methylpyrrolidone, and 218.12g (1.000mol) of pyromellitic dianhydride and 147.11g of pyromellitic dianhydride were added under stirring (0.500mol) 3,4'-biphenyldianhydride, reacted at -10°C for 10 hours to obtain a light yellow viscous polyamic acid spinning solution. The solution is directly used as spinning slurry after filtration.

[0021] The above-mentioned polyamic acid slurry is spun and formed by dry-jet wet spinning method, and the spinning slurry at room temperature is accurately metered by a metering pump, extruded from the spinneret, and then enters N-methylpyrrolidone and ethanol through the air layer. and water (1:1:6 volume ratio) coagulation bath. The spinneret has 30 holes, the hole diameter is Φ0.20mm, the spray ratio is 1 times, the spinneret speed is 30m / min, and the air layer height is 70mm. The nascent polyamic acid fiber is treated in a gradient temperature-...

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Abstract

The invention relates to a preparation method of polyimide fiber. The procedures and conditions of the preparation method are as follows: (1) precursor acid polyamine solution used for spinning is made by fasculating diamine and dianhydride monomer; (2) the preparation of the polyimide fiber adopts dry-wet spinning process; (3) the polyimide fiber is imidized; and (4) the polyimide fiber undergoes the heat drawing under the temperature of 300 to 500 DEG C, and the drawing multiple of the fiber is 1 to 7 times. Imide process adopts a gradient heating-up thermal treatment furnace so as to overcome the defects of the inaccurate temperature control and the non-feasibility of the prior double thermal furnace process. The preparation method has simple process and is easy for continuous production. The prepared polyimide fiber has stronger strength and high modulus and can be used under the temperature of over 300 DEG C. In addition, the polyimide fiber has UV irradiating resistance property, a higher limited oxygen index and corrosion resistance, so the polyimide fiber can be widely applicable for the reinforced fiber of composite materials, a cable sheath, a cable reinforcing core, the mooring rope of vehicle and vessel and the filtering materials of high temperature or radioactive substance, etc.

Description

technical field [0001] The invention relates to a preparation method of polyimide fiber. Background technique [0002] Polyimide fiber is a new type of special fiber with many excellent properties such as high strength, high modulus, high temperature resistance, flame retardancy, radiation protection, and chemical corrosion resistance. There are generally two preparation routes for polyimide fibers: one is to directly spin polyimide as a raw material, and obtain polyimide fibers after hot drawing. This method is simple in process, but difficult to choose a solvent. The toxicity of the solvent is higher, and the structure of polyimide is more restricted. U.S. Patent No. 4,370,290 and U.S. Patent No. 5,378,420 all disclose this method to prepare polyimide fibers. Another method is to use polyamic acid as raw material to obtain polyamic acid fiber by wet spinning, and then obtain polyimide fiber through imidization and thermal drawing. A variety of polyimide fibers can be pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F6/60D01F11/08
Inventor 邱雪鹏高连勋丁孟贤刘芳芳
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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