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Polyimide fiber and preparation method thereof

A polyimide fiber, polyamic acid spinning technology, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, textiles and papermaking, etc., can solve the problem of high cost, tensile strength needs to be further improved, etc. problems, to achieve the effect of reducing raw material cost, compact arrangement and good fluidity

Active Publication Date: 2012-09-05
吉林省亚安新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method modifies the polyimide fiber by adding 2-(4-aminophenyl)-5-aminobenzimidazole with higher cost, but the tensile strength of the polyimide fiber prepared by this method is The tensile properties, especially the tensile strength, need to be further improved

Method used

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

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preparation example Construction

[0033] The invention also discloses a preparation method of polyimide fiber, comprising:

[0034] Dissolve diamine compounds and biphenyl dianhydride in a solvent, and react at -5°C to 30°C for 5 to 20 hours to obtain a polyamic acid spinning solution. The molar ratio of the diamine compound to biphenyl dianhydride is 1:0.95~1.05, the diamine compounds are p-phenylenediamine and 2-(4-aminophenyl)-5-aminobenzimidazole with a molar ratio of 0.8~0.95:0.05~0.2; wherein, p-phenylene The structural formula of diamine is shown in formula I; the structural formula of 2-(4-aminophenyl)-5-aminobenzimidazole is shown in formula II; the structural formula of biphenyltetralic acid dianhydride is shown in formula III.

[0035]

[0036] Spinning the polyamic acid spinning solution to obtain polyamic acid fibers;

[0037] Carrying out imidization treatment to the polyamic acid fiber to obtain polyimide primary fiber;

[0038] The polyimide as-spun fiber is subjected to heat drawing treat...

Embodiment 1

[0059] Dissolve 0.475mol p-phenylenediamine and 0.025mol 2-(4-aminophenyl)-5-aminobenzimidazole in 1000ml N,N-dimethylacetamide, add 0.520mol 3,3' under stirring , 4,4'-biphenyltetraacid dianhydride, react at -5°C to 30°C for 10 hours to obtain a viscous polyamic acid spinning solution, and filter;

[0060] The above-mentioned filtered polyamic acid spinning solution is spun and formed by using the dry-jet wet spinning method, and the polyamic acid spinning solution at room temperature is accurately metered by a metering pump, and is extruded from the spinneret and enters through the air layer. In the coagulation bath of N,N'-dimethylacetamide and water with a volume ratio of 40:60, the spinneret has 30 holes, the hole diameter is Ф0.20mm, the spray ratio is 3.0 times, and the spinneret speed is 30m / min , the height of the air layer is 70mm, and the polyamic acid fiber is obtained;

[0061] After the polyamic acid fiber is heat-dried, it is treated in a gradient heating heat ...

Embodiment 2

[0066] Dissolve 0.45mol p-phenylenediamine and 0.05mol 2-(4-aminophenyl)-5-aminobenzimidazole in 1000ml N,N-dimethylacetamide, add 0.520mol 3,3' under stirring , 4,4'-biphenyltetraacid dianhydride, react at -5°C to 30°C for 10 hours to obtain a viscous polyamic acid spinning solution, and filter;

[0067] The above-mentioned filtered polyamic acid spinning solution is spun and formed by using a dry-wet method, and the spinning slurry at room temperature is accurately metered by a metering pump, and then extruded from the spinneret and entered through the air layer with a volume ratio of 40: In the coagulation bath of 60 N,N'-dimethylacetamide and water, the spinneret has 150 holes, the hole diameter is Ф0.10mm, the spinning speed is 100m / min, the spray ratio is 4.0 times, and the air layer height is 50mm to obtain polyamic acid fiber;

[0068] After heat-drying the polyamic acid fibers, they are treated in a gradient temperature-raising heat treatment furnace under a nitrogen...

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Abstract

The embodiment of the invention discloses a method for preparing polyimide fibers, and in the method, a fully rigid polyimide fiber with an aromatic heterocyclic structure is prepared by using biphenyltetracarboxylic dianhydride, p-phenylenediamine and 2-(4-Aminophenyl)-5-aminobenzimidazole as raw materials. In the invention, by using the asymmetry of the structure of the 2-(4-Aminophenyl)-5-aminobenzimidazole, the flexibility of the prepared polyimide fiber is improved, so that the polyimide fiber has a better liquidity in the subsequent processing procedures, which increases the draw ratio of the polyimide fiber, improves the degree of orientation of the polyimide fiber and is benefical to overcoming the defects produced in the process of preparing the polyimide fiber, therefore, the prepared polyimide fiber has a high tensile strength. Experimental results show that the tensile strength of the polyimide fiber prepared by using the method of the invention reaches 2.5 GPa.

Description

technical field [0001] The invention relates to the technical field of polymer fibers, in particular to a polyimide fiber and a preparation method thereof. Background technique [0002] Due to its good thermal stability, elastic modulus, good radiation resistance and low water absorption, polyimide fiber has received more and more attention from various countries, and has been widely used in atomic energy industry, space environment, rescue, aerospace, etc. , national defense construction, new construction, high-speed transportation, marine development, sports equipment, new energy, environmental industry and protective tools and other fields have been more and more widely used. [0003] The existing preparation methods of polyimide fibers mainly include two processes, one-step method and two-step method. Wherein, such as the Chinese patent document that the application number is 02112048.X, the U.S. patent document that the patent number is US4370290 and US5378420 has repo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78C08G73/10
Inventor 黄森彪邱雪鹏高连勋丁孟贤李国民
Owner 吉林省亚安新材料有限公司
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