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Heat treatment method of polyacrylonitrile-based fibers

A technology of polyacrylonitrile-based fiber and heat treatment method, which is applied in the directions of fiber treatment, radiation wave/microwave fiber treatment, fiber type, etc., can solve the problems of long thermal stabilization process time, reduce thermal stabilization process time, etc. Thermal stabilization time, improving mechanical properties, optimizing the effect of combined processes

Active Publication Date: 2021-01-15
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] One of the technical problems to be solved by the present invention is that the thermal stabilization process of polyacrylonitrile in the prior art takes a long time, and the fiber is prone to the influence of skin-core structure In order to solve the problem of final carbon fiber performance, a new method of heat treatment of microwave-strengthened polyacrylonitrile-based fibers is provided. The heat treatment method effectively reduces the heat stabilization process time, reduces the influence of the skin-core structure, and improves the mechanical properties of the final carbon fiber

Method used

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  • Heat treatment method of polyacrylonitrile-based fibers

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Effect test

Embodiment 1

[0026] First, polyacrylonitrile precursors were mixed with 10% KMnO 4 After immersing in the solution for 30 minutes, the modified raw silk was heat-treated in an air-atmosphere microwave oven at a temperature of 230°C for 20 minutes and a draft of 3%. Then the fiber is placed in 3 normal pressure heat stabilization furnaces with air atmosphere for heat treatment, the temperature is 250°C and 260°C respectively, the constant temperature zones of each air heat stabilization furnace are equal in length, the total heat treatment time is 20min, and the total pull Stretch is 0%. Finally, the obtained thermally stabilized fibers are subjected to low-temperature carbonization and high-temperature carbonization treatment. The low-temperature carbonization temperature is 690°C, the heat treatment time is 3min, and the draft is 3%; the high-temperature carbonization temperature is 1450°C, the heat treatment time is 3min, and the draft is -3.5%. The mechanical properties of the obtaine...

Embodiment 2

[0028] First, polyacrylonitrile precursors were mixed with 10% KMnO 4 After immersing in the solution for 30min, the modified raw silk was heat-treated in an air atmosphere microwave oven at a temperature of 210°C for 20min and a draft of 3%. Then the fiber is placed in 3 normal pressure heat stabilization furnaces with air atmosphere for heat treatment, the temperature is 250°C and 260°C respectively, the constant temperature zones of each air heat stabilization furnace are equal in length, the total heat treatment time is 20min, and the total pull Stretch is 0%. Finally, the obtained thermally stabilized fibers are subjected to low-temperature carbonization and high-temperature carbonization treatment. The low-temperature carbonization temperature is 690°C, the heat treatment time is 3min, and the draft is 3%; the high-temperature carbonization temperature is 1450°C, the heat treatment time is 3min, and the draft is -3.5%. The results of mechanical properties of the obtain...

Embodiment 3

[0030] First, polyacrylonitrile precursors were mixed with 10% KMnO 4 After immersing in the solution for 30 minutes, the modified raw silk was heat-treated in an air-atmosphere microwave oven at a temperature of 210°C for 12 minutes and a draft of 3%. Then the fiber is placed in 3 normal pressure heat stabilization furnaces with air atmosphere for heat treatment, the temperature is 250°C and 260°C respectively, the constant temperature zones of each air heat stabilization furnace are equal in length, the total heat treatment time is 20min, and the total pull Stretch is 0%. Finally, the obtained thermally stabilized fibers are subjected to low-temperature carbonization and high-temperature carbonization treatment. The low-temperature carbonization temperature is 690°C, the heat treatment time is 3min, and the draft is 3%; the high-temperature carbonization temperature is 1450°C, the heat treatment time is 3min, and the draft is -3.5%. The results of mechanical properties of ...

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Abstract

The invention relates to a heat treatment method of polyacrylonitrile-based fibers, and mainly solves the problems that in the prior art, the time of a polyacrylonitrile heat stabilization process islong, and the performance of final carbon fibers is influenced by a sheath-core structure easily generated by the fibers. According to the heat treatment method of the polyacrylonitrile-based fibers,the method comprises the following steps of carrying out microwave heat treatment on polyacrylonitrile precursor in a microwave heating furnace in an air atmosphere and carrying out thermal stabilization treatment in a normal-pressure thermal stabilization furnace in the air atmosphere; and the method is characterized in that the polyacrylonitrile precursor is subjected to modification pretreatment in a strong oxidizing solution before microwave heat treatment, so that the problems are better solved, and the method can be used in industrial production of polyacrylonitrile precursor thermal stabilization and carbonization processes.

Description

technical field [0001] The invention relates to a microwave-strengthened method for preparing polyacrylonitrile-based thermally stabilized fibers, and belongs to the technical field of polyacrylonitrile-based carbon fiber preparation. Background technique [0002] The preparation of polyacrylonitrile carbon fiber mainly includes processes such as polymerization, spinning, thermal stabilization and carbonization. The thermal stabilization of polyacrylonitrile is to convert the linear macromolecular chain of polyacrylonitrile precursor into a heat-resistant ladder polymer structure, so that it will not melt or burn in the subsequent carbonization process, and maintain a thermodynamic stable state. A critical step in performance carbon fiber. Scholars at home and abroad have conducted a lot of research on the thermal stabilization process of polyacrylonitrile. At present, the thermal stabilization process commonly used is: the polyacrylonitrile raw silk is subjected to gradien...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M10/00D01F9/22D06M101/28
CPCD06M10/003D01F9/225D06M2101/28
Inventor 肖士洁沈志刚陈辉
Owner CHINA PETROLEUM & CHEM CORP