Polyimide fibre containing benzimidazole structure and preparation method thereof

A technology of polyimide fiber and benzimidazole is applied in the field of polyimide fiber containing benzimidazole structure and its preparation field, which can solve the problem of low mechanical properties of PMDA-ODA type polyimide fiber, and achieves Improved mechanical strength, improved heat resistance, and easy control

Inactive Publication Date: 2008-06-18
SINOSELEN HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned result shows that the mechanical property of the obtained PMDA-ODA type polyimide fiber is not high

Method used

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  • Polyimide fibre containing benzimidazole structure and preparation method thereof
  • Polyimide fibre containing benzimidazole structure and preparation method thereof
  • Polyimide fibre containing benzimidazole structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The synthesis of polyamic acid solution is by PMDA: ODA: PABZ=10: 9: 1 molar ratio, first ODA and PABZ two kinds of diamine monomers are added in the solvent N-methylpyrrolidone of metering, make its total solid content be 12%, then stirred under the protection of nitrogen to dissolve all ODA and PABZ, then added PMDA and stirred, and continued to react at 15°C for 10 hours in a nitrogen atmosphere to obtain a viscous polyamic acid homogeneous solution. Its intrinsic viscosity is 3.16dL / g.

[0032] Polyamic acid fiber spinning The obtained polyamic acid solution is filtered, defoamed, and polyamic acid fiber is obtained according to the conventional dry / wet spinning process, wherein the number of spinneret holes used is 30 to 100 holes, and the hole diameter is 0.1 mm; the coagulation bath used is a mixture of ethanol and water, its weight ratio is 50:50, and the draw ratio of the fiber in the spinning stage is 1.5. In addition, the conventional wet spinning process ca...

Embodiment 2

[0037] The synthesis of polyamic acid solution is by PMDA: ODA: PABZ=10: 7: 3 molar ratio, first ODA and PABZ two kinds of diamine monomers are added in the solvent N-methylpyrrolidone of metering, make its total solid content be 12%, and then stirred under the protection of nitrogen to dissolve all ODA and PABZ, and then added PMDA and stirred to make it continue to react at 30°C for 15 hours in a nitrogen atmosphere to obtain a viscous polyamic acid homogeneous solution. Its intrinsic viscosity is 2.73dL / g.

[0038] Since the processes of polyamic acid fiber spinning and polyamic acid fiber imidization are exactly the same as those in Example 1, they are omitted here.

[0039] The structural formula of gained polyimide fiber is as shown in embodiment 1, and n in the formula: m=7: 3, and its tensile strength is 0.92GPa, and initial modulus is 56.6GPa, and elongation at break is 6.6%; The glass transition temperature is 410°C.

Embodiment 3

[0041] The synthesis of polyamic acid solution presses PMDA: ODA: PABZ=10: 5: 5 molar ratio, first adds ODA and PABZ two kinds of diamine monomers in the solvent N-methylpyrrolidone of metering, makes its solid content be 10 %, then stirred under the protection of nitrogen to completely dissolve ODA and PABZ, then added PMDA and stirred, and continued to react at 40° C. for 24 hours in a nitrogen atmosphere to obtain a viscous polyamic acid homogeneous solution. Its intrinsic viscosity is 2.35dL / g.

[0042] Since the processes of polyamic acid fiber spinning and polyamic acid fiber imidization are exactly the same as those in Example 1, they are omitted here.

[0043] The structural formula of gained polyimide fiber is as shown in embodiment 1, and n in the formula: m=5: 5, and its tensile strength is 1.26GPa, and initial modulus is 130.7GPa, and elongation at break is 5.8%; The glass transition temperature is 425°C.

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Abstract

The invention discloses polyimide fiber with benzimidazole structure, which is characterized in that the infrared spectrum of the fiber is provided with character absorption peaks of imide ring of 1776-1774cm<-1>, 1726-1722cm<-1> and 1378-1373cm<-1> within the wave number range of 1300-1800cm<-1> and N-H functional group absorption wide peaks in the imidazole structure within the wave number range of 3000-3750cm<-1>. The tensile strength is 0.73-1.53GPa. The initial modulus is 45.2-220GPa. The invention also provides a preparation method of the fiber. The fiber disclosed by the invention contains the benzimidazole structure with secondary amine hydrogen. Therefore, compared with PMDA-ODA polyimide fiber prepared with the same process, the tensile strength can be improved by nearly three times at the most, the initial modulus can be improved by more than twenty times at the most, and the heat resistance is further improved. The preparation method provided by the invention has the advantages of mature technology and easy control. The cost can be kept at a relative low level.

Description

technical field [0001] The invention belongs to the technical field of polyimide fibers and preparation methods thereof, and in particular relates to a polyimide fiber containing a benzimidazole structure and a preparation method thereof. Background technique [0002] Compared with other high-performance fibers, polyimide fiber (PI) is expected to be used in the atomic energy industry, space and It has been widely used in very harsh research in the fields of environment, rescue needs, aerospace, national defense construction, new construction, high-speed transportation, marine development, sports equipment, new energy, environmental industry and protective equipment. [0003] The preparation method of existing polyimide fiber generally comprises one-step method and two-step method technology, and its technological process is as follows figure 1 shown. One-step method is to use polyimide solution to directly spin to prepare polyimide fiber. Such as Chinese invention patent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F6/78
Inventor 刘向阳顾宜叶光斗高冠群董亮朱蓉琪盛兆碧
Owner SINOSELEN HI TECH
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