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Preparation method of polyacrylonitrile carbon fiber

A polyacrylonitrile-based carbon fiber and polyacrylonitrile technology, which is applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of complex equipment, high cost, unsuitable temperature control, etc., and achieve the effect of reducing process and low cost.

Inactive Publication Date: 2011-04-27
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patents 02136722.1 and 200810036189.4 indicate that the production process of layered thermal stabilization furnace with heating and drawing in 6-12 zones can be used. This method can prepare high-quality pre-oxidized fibers. However, the method is extremely complicated and the temperature is not suitable for control. and costly

Method used

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  • Preparation method of polyacrylonitrile carbon fiber
  • Preparation method of polyacrylonitrile carbon fiber
  • Preparation method of polyacrylonitrile carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 1-butyl-3-methylimidazolium chloride salt type ionic liquid and polyacrylonitrile powder into the reactor with mechanical stirring device, and add catalyst KMnO after the polymer is completely dissolved 4, to promote the cyclization of polyacrylonitrile. The mass fractions of the added raw materials are: polyacrylonitrile is 5%, and solvent is 95%. QUR 4 The mass accounts for 0.05% of polyacrylonitrile. The mixture was stirred and reacted at 170°C, and a certain flow of oxygen was introduced to control the temperature and time of the pre-oxidation reaction, and samples were taken at 20 min, 40 min, 60 min, and 90 min to obtain polyacrylonitrile spinning solutions with different pre-oxidation degrees. diagram 2-1 IR spectra of PAN / IL pre-oxidized at 170°C for different times.

Embodiment 2

[0046] Add 1-butyl-3-methylimidazolium chloride salt type ionic liquid and polyacrylonitrile into the reactor with mechanical stirring device, and add the catalyst KMnO after the polymer is completely dissolved 4 , to promote the cyclization of polyacrylonitrile. The mass fractions of the added raw materials are: polyacrylonitrile is 5%, and solvent is 95%. QUR 4 The mass accounts for 0.05% of polyacrylonitrile. The mixture was stirred and reacted at 160°C, and an oxygen-containing gas was introduced at a rate of 5ml / min to control the temperature and time of the pre-oxidation reaction, and samples were taken at 20min, 40min, 60min, 90min, 120min, and 150min to obtain different oxidation Degree of polyacrylonitrile spinning solution. Figure 2-2 IR spectra of PAN / IL preoxidized at 160℃ for different times

Embodiment 3

[0048] Add DMSO and polyacrylonitrile into the reactor with a mechanical stirring device, and add the catalyst KMnO after the polymer is completely dissolved 4 , to promote the cyclization of polyacrylonitrile. The mass fractions of the added raw materials are: polyacrylonitrile is 10%, and DMSO is 90%. QUR 4 The mass accounts for 0.05% of polyacrylonitrile. The mixture was stirred and reacted at 175° C., and an oxygen-containing gas was introduced at a rate of 5 ml / min to control the temperature and time of the pre-oxidation reaction. The time was about 4-5 hours to obtain a polyacrylonitrile spinning solution. image 3 IR spectra of PAN / DMSO preoxidized at 175°C for different times.

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Abstract

The invention relates to a making method of polyacrylonitrile carbon fiber, comprising: (1) mixing polyacrylonitrile and solvent according to the solid content of 0.1%-25% in a reactor, heating and stirring to completely dissolve the polyacrylonitrile and solvent; (2) after dissolving completely, adding KMnO4, then adding gas with oxide, processing pre-oxidation for the spinning solution; pre-oxidizing at temperature of 90-250 DEG C for 1-2h; reaching different pre-oxidation effect under different pre-oxidation temperatures and different pre-oxidation time; (3) spinning the spinning solution in the step (2) in a spinning machine, then obtaining pre-oxidation filaments with good pre-oxidation degree after water washing, drafting and heat forming; then obtaining high-property carbon fiber through carbonization. The method in the invention carries out innovation for pre-oxidation stage of carbon fiber with convenient operation, simple equipment but rarely pollution for the environment; low-cost controllable pre-oxidation of polyacrylonitrile is implemented and the skin-core structures are reduced, thereby being capable of producing high-property carbon fiber; and the preparation method greatly reduces the production cost of carbon fiber.

Description

technical field [0001] The invention belongs to the field of carbon fiber preparation, in particular to a preparation method of polyacrylonitrile-based carbon fiber. Background technique [0002] Carbon fiber has a series of excellent properties such as high specific strength, high specific modulus, and high temperature resistance. It is widely used in high-tech industrial fields, especially in the field of aerospace, and has great application prospects. It is known as the most vital in the 21st century. of new materials. The preparation of PAN-based carbon fibers generally goes through the processes of polymerization, spinning, pre-oxidation and carbonization. Among them, pre-oxidation is a very critical and time-consuming process in the whole process, and the structural transformation of the pre-oxidation process largely determines the structure and performance of the final carbon fiber. Since the pre-oxidation process is a period of severe structural transformation, def...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/22
Inventor 余木火荣怀苹韩克清王兆华张毅炜滕翠青董勤礼
Owner DONGHUA UNIV
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