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High-strength high modulus polyimide fiber and preparation method thereof

A technology of high-modulus polyimide fiber and high-modulus polyimide, which is applied in the direction of spinning solution preparation, fiber chemical characteristics, dry spinning method, etc., can solve the problems of not meeting the performance requirements of high-strength and high-modulus polyimide fiber, and improve the reliability Spinning performance, performance improvement, cost performance improvement effect

Active Publication Date: 2012-02-08
JIANGSU XIANNUO NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two methods all improve the mechanical properties of polyimide fibers by adding 2-(4-aminophenyl)-5-aminobenzimidazole, and make their mechanical properties greatly improved, but they have not yet reached The performance requirements of high-strength and high-modulus polyimide fibers require major breakthroughs and changes in synthesis methods and preparation processes

Method used

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  • High-strength high modulus polyimide fiber and preparation method thereof
  • High-strength high modulus polyimide fiber and preparation method thereof
  • High-strength high modulus polyimide fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Synthesis of polyamic acid solution: according to the molar ratio of BPDA: pPDA: BIA = 4.2: 3: 1, first place the two diamine monomers PPDA and BIA in a three-necked flask, and add a measured amount of solvent dimethylformamide (DMF), under the protection of nitrogen, stirred at 50°C to completely dissolve PPDA and BIA, then added BPDA in batches and stirred to make the solid content 10%, then stirred at 50°C for 2 hours under the protection of nitrogen, and then stirred at 10°C Stir for 1 hour, then stir for 2 hours at -5°C to obtain a viscous polyamic acid solution with an intrinsic viscosity of 3.0 dl / g.

[0049] Preparation of polyimide fiber: After the polyamic acid solution is filtered and defoamed, it is spun by a dry-wet process, and the spinning solution is pumped out by a metering pump and passed through a spinneret (number of holes: 100 holes, pore size: 0.15 mm) passes through the air layer (length: 50mm) and then enters the coagulation bath (composed of wat...

Embodiment 2

[0054] Synthesis of polyamic acid solution: according to the molar ratio of BPDA: pPDA: BIA = 21: 13: 7, first place the two diamine monomers PPDA and BIA in a three-necked flask, and add a measured amount of solvent dimethylacetamide (DMAc), under the protection of nitrogen, stirred at 70°C to completely dissolve PPDA and BIA, then added BPDA in batches and stirred to make the solid content 15%, then stirred at 70°C for 5 hours under the protection of nitrogen, and then stirred at 20°C Stir for 2 hours, then stir for 3 hours at 0°C to obtain a viscous polyamic acid solution. Its intrinsic viscosity is 2.5dl / g.

[0055] Preparation of polyimide fiber: After the polyamic acid solution is filtered and defoamed, it is spun by a wet process, and the spinning solution is pumped out by a metering pump and then passed through the spinneret (number of holes: 50 holes, hole diameter: 0.075mm ) into the coagulation bath (composed of water) to form polyamic acid fibers, and then washed ...

Embodiment 3

[0060] Synthesis of polyamic acid solution: according to the molar ratio of BPDA: pPDA: BIA = 4.75: 2: 3, two diamine monomers, PPDA and BIA, are placed in a three-necked flask, and a measured amount of solvent dimethylacetamide is added (DMAc), under the protection of nitrogen, stirred at 75°C to completely dissolve PPDA and BIA, then added BPDA in batches and stirred to make the solid content 20%, then stirred at 75°C for 2 hours under the protection of nitrogen, and then stirred at 30°C Stir for 3 hours, then stir at 0°C for 10 hours to obtain a viscous polyamic acid solution. Its intrinsic viscosity is 2.3dl / g.

[0061] Preparation of polyimide fiber: After the polyamic acid solution is filtered and defoamed, it is spun by a wet process, and the spinning solution is pumped out by a metering pump and passed through a spinneret (number of holes: 500 holes, pore size: 0.045mm ) into the coagulation bath (composed of water and DMAc, with a volume ratio of 7:3) to form polyami...

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Abstract

The invention relates to high-strength high modulus polyimide fiber and a preparation method thereof, which belongs to the high performance organic fiber technical field. The fiber comprises the polyimide fiber which is prepared by biphenyltetracarboxylic dianhydride (BPDA), para-phenylene diamine (pPDA) and 2-(4-aminophenyl)-5-aminobenzimidazoles (BIA), wherein the mol ratio of pPDA to BIA is 1:10-3:1, other di-amine and di-anhydride monomers are added in the synthesis process, a gradient temperature reaction method and a one step continuous preparation method are used in the preparation process, so that the difficulties for synthesizing and processing due to the content increase of 2-(4-aminophenyl)-5-aminobenzimidazoles are solved, the problems of poor homogeneity and stability of thefiber performance can be solved, and the high-strength high modulus polyimide fiber can be obtained, the strength can reach 4.5GPa, the modulus can reach 201GPa, and the raw material source is wide, the spinning process can be continuously performed, the method has low cost and high efficiency which is capable of realizing the industrial production.

Description

technical field [0001] The invention belongs to the technical field of high-performance organic fibers, and in particular relates to a high-strength and high-modulus polyimide fiber and a preparation method thereof. Background technique [0002] As a variety of high-performance fibers, polyimide (PI) fibers have high strength and high modulus, high temperature resistance, low temperature resistance and radiation resistance, and also have good biocompatibility and dielectric properties. It is widely used in nuclear energy industry, space environment, rescue needs, aerospace, national defense construction, new construction, high-speed transportation, marine development, sports equipment, new energy, environmental industry and protective equipment. [0003] At present, the preparation of polyimide fibers mainly includes one-step method and two-step method. The one-step technical route is: use polyimide solution as spinning slurry, spin polyimide fiber by wet method or dry-wet ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/78C08G73/10D01D1/02D01D5/04D01D5/06D01D5/12D01D10/02
CPCD01D10/02C08L79/04C08G73/1042D01D5/06D01D1/02D01F6/78C08L79/08D01D5/04C08G73/18C08G73/1003D01D5/12C08G73/1085C08G73/10
Inventor 武德珍牛鸿庆齐胜利韩恩林闫晓娜赵昕吴战鹏
Owner JIANGSU XIANNUO NEW MATERIAL TECH
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