Polyimide fiber and preparation method thereof

A technology of polyimide fiber and polyamic acid, applied in the field of fibers, can solve the problem of insufficient mechanical properties, and achieve the effects of orderly molecular chain structure, good mechanical properties, good high temperature resistance and chemical corrosion resistance.

Active Publication Date: 2011-05-04
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the mechanical properties of the above-mentioned polyimide fibers

Method used

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  • Polyimide fiber and preparation method thereof
  • Polyimide fiber and preparation method thereof

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preparation example Construction

[0038] The present invention also provides a kind of preparation method of polyimide fiber described in above-mentioned technical scheme, comprises the following steps:

[0039] Mix p-phenylenediamine, 4,4'-diaminodiphenyl ether and 3,3',4,4'-biphenyltetraacid dianhydride in an organic solvent, and perform polycondensation reaction to obtain polyamic acid spinning stock solution , the ratio of the moles of p-phenylenediamine to the total moles of p-phenylenediamine and 4,4'-diaminodiphenyl ether is 0.8-0.95;

[0040] Spinning the polyamic acid spinning stock solution to obtain a polyamic acid precursor;

[0041] Carrying out imidization treatment to the polyamic acid precursor to obtain polyimide spun fibers;

[0042] The polyimide primary fiber is subjected to thermal drawing treatment to obtain polyimide fiber.

[0043]The invention uses p-phenylenediamine, 4,4'-diaminodiphenyl ether and 3,3',4,4'-biphenyltetraacid dianhydride as raw materials, and adopts a two-step method...

Embodiment 1

[0065] Dissolve 51.33g (0.475mol) of p-phenylenediamine and 5.00g (0.025mol) of 4,4'-diaminodiphenyl ether in 1000mL of N, N'-dimethylacetamide, and add 152.90g (0.520 mol) 3,3',4,4'-biphenyltetraacid dianhydride, after reacting at -5°C to 30°C for 5 hours, a viscous polyamic acid spinning stock solution is obtained, and the mass concentration of the polyamic acid is about 18.2%;

[0066] After the polyamic acid spinning stock solution is filtered, vacuum degassed, extruded from the spinneret, it enters the solidification process composed of N,N'-dimethylacetamide and water with a volume ratio of 40:60 through the air layer. coagulated in a bath, and then washed and dried to obtain polyamic acid precursors. The spinneret of the spinneret is 30 holes, the aperture is 0.12mm, the spray draw ratio is 3.0 times, the spinneret speed is 30m / min, and the air layer height is 70mm;

[0067] The polyamic acid precursor is sent into a gradient heating heat treatment furnace for thermal...

Embodiment 2

[0073] Dissolve 48.63g (0.45mol) of p-phenylenediamine and 10.00g (0.05mol) of 4,4'-diaminodiphenyl ether in 1000mL of N,N'-dimethylacetamide, and add 152.90g (0.520 mol) 3,3',4,4'-biphenyltetraacid dianhydride, after reacting at -5°C to 40°C for 8 hours, a viscous polyamic acid spinning stock solution is obtained, and the mass concentration of the polyamic acid is about 17.9%;

[0074] After the polyamic acid spinning stock solution is filtered and vacuum degassed, it is extruded from the spinneret and enters the solidification process composed of N,N'-dimethylacetamide and water with a volume ratio of 1:1 through the air layer. coagulated in a bath, and then washed and dried to obtain polyamic acid precursors. The spinneret of the spinneret is 150 holes, the aperture is 0.1mm, the spray draw ratio is 4.0 times, the spinneret speed is 100m / min, and the air layer height is 50mm;

[0075]The polyamic acid precursor is sent into a gradient heating heat treatment furnace for th...

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Abstract

The invention provides a polyimide fiber comprising a polymer with a structure shown in a formula (I) in the specification, wherein m is the proportion of a repeat unit with a structure shown in a formula (II), in the structure of the polymer, and is more than and equal to 0.8 and less than and equal to 0.95. The invention also provides a preparation method of the polyimide fiber, comprising the following steps of: mixing p-phenylenediamine, 4,4'-diaminodiphenyl ether and 3,3',4,4-biphenyltetracarboxylic dianhydride in an organic solvent to carry out condensation polymerization so as to obtain a polyamic acid spinning solution, wherein proportion of the mole number of the p-phenylenediamine to the total mole number of the p-phenylenediamine and the 4,4'-diaminodiphenyl ether is 0.8-0.95; spinning to obtain polyamic acid protofilaments by using the polyamic acid spinning solution; carrying out imidization processing on the polyamic acid protofilaments to obtain polyimide nascent fibers; and carrying out hot stretching processing on the polyimide nascent fibers to obtain the polyimide fiber.

Description

technical field [0001] The invention relates to the field of fiber technology, in particular to a polyimide fiber and a preparation method thereof. Background technique [0002] Polyimide fiber is a new type of special fiber, which refers to the fiber containing aramid in the molecular chain. Polyimide fiber has the advantages of high strength, high modulus, high temperature resistance, flame retardancy, radiation protection, and chemical corrosion resistance. , sports equipment, new energy, environmental industry and protective equipment and other fields have good application prospects. [0003] The preparation method of existing polyimide fiber comprises two kinds of one-step method and two-step method, and one-step method refers to adopting polyimide solution to directly carry out spinning to prepare polyimide fiber, and the raw silk of this method spinning There is no need for amidation, the process is short, and the obtained polyimide fiber has high mechanical propert...

Claims

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Application Information

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IPC IPC(8): D01F6/78D01F11/08C08G73/10D01D1/02D01D1/10D01D5/06D01D5/04D01D5/14D01D10/02
Inventor 黄森彪邱雪鹏高连勋丁孟贤李国民
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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