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Preparation method of polyacrylonitrile based heat stabilized fiber

A polyacrylonitrile-based heat and heat stabilization technology, which is applied in the fields of fiber chemical characteristics, chemical post-treatment of synthetic polymer artificial filaments, textiles and papermaking, etc., can solve the problems of insufficient polycondensation reaction and affecting the performance of carbon fibers, etc. Achieve the effects of reducing structural defects, improving compactness, and good application prospects

Active Publication Date: 2017-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] What the present invention aims to solve is the problem that the polyacrylonitrile fiber molecular chains in the prior art cannot fully undergo polycondensation reaction during the thermal stabilization process, which will affect the performance of the final carbon fiber. chemical fiber process

Method used

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  • Preparation method of polyacrylonitrile based heat stabilized fiber

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] First, the polyacrylonitrile precursors are sequentially heat-treated in three air thermal stabilization furnaces at 230°C, 250°C, and 270°C. The constant temperature zone of each air heat stabilization furnace is the same length, and the total heat treatment time is 60min. The total draft of the five air heat stabilization furnaces is 6%. Then, the obtained fiber is heat-treated in a nitrogen stabilization furnace at a temperature of 270° C., the stabilization furnace time is 12 minutes, and the draft is -2% to obtain a polyacrylonitrile thermally stabilized fiber.

[0015] The obtained thermally stabilized fiber is subjected to low-temperature carbonization and high-temperature carbonization treatments. The low temperature carbonization temperature is 350-700°C, the heat treatment time is 3 minutes, and the draft is 3%; the high temperature carbonization temperature is 1350°C, the heat treatment time is 3 minutes, and the draft is -3.5%. The results of the mechanical p...

Embodiment 2

[0017] First, the polyacrylonitrile precursors are sequentially heat-treated in five air thermal stabilization furnaces at 190°C, 218°C, 240°C, 260°C, and 270°C. The constant temperature zone of each air heat stabilization furnace is the same length, and the total heat treatment time is 60min. The total draft of the five air heat stabilization furnaces is 6%. Then, the obtained fiber is heat-treated in a nitrogen stabilization furnace at a temperature of 270° C., the stabilization furnace time is 12 minutes, and the draft is -2% to obtain a polyacrylonitrile thermally stabilized fiber.

[0018] The obtained thermally stabilized fiber is subjected to low-temperature carbonization and high-temperature carbonization treatments. The low temperature carbonization temperature is 350-700°C, the heat treatment time is 3 minutes, and the draft is 3%; the high temperature carbonization temperature is 1350°C, the heat treatment time is 3 minutes, and the draft is -3.5%. The results of the...

Embodiment 3

[0020] Firstly, the polyacrylonitrile precursor is heat-treated in five air thermal stabilization furnaces in sequence at 200°C, 215°C, 230°C, 255°C, and 265°C. The constant temperature zone of each air heat stabilization furnace is the same length, and the total heat treatment time is 60min. The total draft of the five air heat stabilization furnaces is 6%. Then, the obtained fiber is heat-treated in a nitrogen stabilization furnace at a temperature of 265° C., the stabilization furnace time is 12 minutes, and the draft is -2% to obtain a polyacrylonitrile thermally stabilized fiber.

[0021] The obtained thermally stabilized fiber is subjected to low-temperature carbonization and high-temperature carbonization treatments. The low temperature carbonization temperature is 350-700°C, the heat treatment time is 3 minutes, and the draft is 3%; the high temperature carbonization temperature is 1350°C, the heat treatment time is 3 minutes, and the draft is -3.5%. The results of the ...

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Abstract

The invention relates to a preparation method of a polyacrylonitrile based heat stabilized fiber, and mainly solves the problem that the polyacrylonitrile heat stabilization process in the prior art affects the performance of heat stabilized fiber. Polyacrylonitrile precursors are subjected to heat treatment for not less than 40min in at least three ordinary pressure heat stabilization furnaces of oxygen-containing gas atmosphere, and the total draft is not higher than 6%. The heat treated fiber passes through at least one ordinary pressure heat stabilization furnace of inert gas atmosphere to undergo heat treatment at 240-270DEG C for not less than 5min, and the draft ranges from -2 to 0%, thus obtaining the polyacrylonitrile based heat stabilized fiber. The technical scheme well solves the problem, and can be used for the heat stabilized industrial production of polyacrylonitrile precursors.

Description

Technical field [0001] The invention relates to a preparation method of polyacrylonitrile-based heat stabilized fiber, and belongs to the technical field of polyacrylonitrile carbon fiber preparation. Background technique [0002] Improving the compactness of the polyacrylonitrile thermally stabilized fiber structure and reducing structural defects are conducive to improving the mechanical properties of the final carbon fiber. In the process of thermal stabilization, the polyacrylonitrile molecular chain will combine with oxygen in the air to form an oxygen-containing structure. This kind of oxygen-containing structure can further undergo polycondensation in an inert atmosphere, making the polyacrylonitrile fiber form a denser network structure. It is beneficial to improve the mechanical properties of carbon fiber. Part of the polycondensation reaction is carried out in the subsequent carbonization process, and the polyacrylonitrile carbon fiber has a series of excellent propert...

Claims

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Application Information

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IPC IPC(8): D01F11/06D01F9/22D02J13/00D02J1/22
Inventor 肖士洁沈志刚李磊史纪友
Owner CHINA PETROLEUM & CHEM CORP
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