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Polyacrylonitrile-based carbon fiber precursor pre-oxidation accelerator and using method thereof

A polyacrylonitrile-based carbon fiber, polyacrylonitrile spinning technology, applied in the direction of fiber chemical characteristics, fiber processing, fiber type, etc., can solve the corrosion of potassium permanganate aqueous solution, difficult to form a stable solution, and affect the performance of carbon fiber, etc. problems, to achieve the effect of low cost, shortened pre-oxidation time, and reduced energy consumption

Active Publication Date: 2021-06-08
BEIJING UNIV OF CHEM TECH +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Chinese patent 200910234656.9 discloses a method of dipping polyacrylonitrile precursors in potassium permanganate aqueous solution to reduce the pre-oxidation temperature and increase the degree of pre-oxidation, but the potassium permanganate aqueous solution is corrosive and has adverse effects on related equipment. At the same time, potassium ions may be introduced into the fibers to form defects, which will affect the performance of carbon fibers; Chinese patent 201010285139.7 discloses that polyacrylonitrile precursors are impregnated with ozone aqueous solution to speed up the pre-oxidation speed and reduce the pre-oxidation temperature, but ozone itself is a gas, which is very Easily decomposed into oxygen, difficult to form a stable solution in water, and itself has adverse effects on the environment

Method used

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  • Polyacrylonitrile-based carbon fiber precursor pre-oxidation accelerator and using method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0016] (1) Preparation of polyacrylonitrile spinning solution: by mass fraction, acrylonitrile: dimethyl sulfoxide: itaconic acid: azobisisobutyronitrile: cumene hydroperoxide = 22: 100: 0.2: 0.1 : 0.1 was added to the polymerization kettle, and the polymerization reaction was carried out at 63° C. for 24 hours under the condition of agitation; the singlet and defoaming were carried out for 8 hours under the conditions of vacuum degree of 0.01 MPa and temperature of 63° C. to obtain spinning solution.

[0017] (2) Spinning of raw silk: the spinning solution is transported to a 3K spinneret with a pore size of 65 microns through a metering pump for wet spinning, and is wound after coagulation, drafting, water washing, oiling, and heat setting to obtain a polyester fiber. Acrylonitrile filament.

[0018] (3) Pre-oxidation: The polyacrylonitrile precursor obtained in step 3 is subjected to gradient temperature pre-oxidation treatment in three temperature zones under an air atmosp...

Embodiment 2

[0020] (1) Preparation of polyacrylonitrile spinning solution: by mass fraction, acrylonitrile: dimethyl sulfoxide: itaconic acid: azobisisobutyronitrile = 22: 100: 0.2: 0.1 is added to the polymerization kettle and stirred Polymerization reaction at 63° C. for 24 hours under the conditions; desingling and defoaming at 63° C. for 8 hours under the conditions of vacuum degree of 0.01 MPa and temperature of 63° C. to obtain spinning solution.

[0021] (2) Configuration of immersion solution: tert-butyl hydroperoxide is configured into an aqueous solution with a mass concentration of 2%, and placed in an immersion tank.

[0022] (3) Spinning of raw silk: the spinning solution is transported to a 3K spinneret with a pore size of 65 microns through a metering pump for wet spinning, and is wound after coagulation, drafting, washing, dipping, oiling, and heat setting Obtain polyacrylonitrile precursor, the residence time of fiber in dipping tank is 4 seconds;

[0023] (4) Pre-oxidat...

Embodiment 3

[0025] (1) Preparation of polyacrylonitrile spinning solution: same as Example 2.

[0026] (2) Configuration of immersion solution: Dicumyl peroxide is configured into an acetone solution with a mass concentration of 3%, and placed in an immersion tank.

[0027] (3) Spinning of raw silk: the spinning solution is transported to a 3K spinneret with a pore size of 65 microns through a metering pump for wet spinning, and is wound after coagulation, drawing, washing, oiling, and heat setting to obtain a polyester fiber. Acrylonitrile filament.

[0028] (4) Pre-oxidation: the polyacrylonitrile precursor of step (3) is immersed in the dipping liquid of step (2) for 2 minutes; Zone gradient temperature pre-oxidation treatment, the pre-oxidation treatment temperature is 190, 220, 240, 270 °C respectively, the residence time of the fiber in each temperature zone is 10 minutes, and the total pre-oxidation treatment time is 40 minutes.

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Abstract

The invention relates to a polyacrylonitrile-based carbon fiber precursor pre-oxidation accelerator and its use method. The accelerator of the invention refers to dicumyl peroxide and cumene hydroperoxide with a half-life of 1 to 60 minutes at 200°C. , tert-butyl hydroperoxide, di-tert-butyl peroxide and other peroxides, through any one of the preparation of polyacrylonitrile spinning solution, spinning of raw silk and pre-oxidation treatment Or adding accelerators or dipping in accelerator solutions during any process, so that the pre-oxidation temperature of polyacrylonitrile precursors can be reduced by more than 10 ° C, and the pre-oxidation time can be reduced by more than 16.7%, which effectively reduces the energy consumption of the carbon fiber preparation process and improves the carbon fiber production process. Production efficiency, with the advantages of simple operation process, low cost, less investment, and compatibility with existing carbon fiber production equipment.

Description

technical field [0001] The invention relates to a polyacrylonitrile-based carbon fiber precursor pre-oxidation accelerator and a use method thereof, belonging to the field of carbon fiber preparation. Background technique [0002] Carbon fiber has the characteristics of high specific strength, high specific modulus, high temperature resistance, corrosion resistance, and good electrical and thermal conductivity. It is an important reinforcement of advanced composite materials and is widely used in aerospace, transportation, building energy, sports and leisure fields. . In the process of carbon fiber preparation, production and application, it is extremely important to accurately and timely characterize the mechanical properties of carbon fiber. The preparation process of polyacrylonitrile-based carbon fibers includes basic processes such as polymerization, spinning, pre-oxidation, and carbonization, among which pre-oxidation is a bridge for the transformation of fibers from ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/22D06M13/10D01F1/10D01F6/54D06M101/28
CPCD01F1/10D01F6/54D01F9/225D06M13/10D06M2101/28
Inventor 童元建徐樑华张月义李杨曹维宇李常清
Owner BEIJING UNIV OF CHEM TECH
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