Preparation method of polyacrylonitrile pre-oxidation fiber and carbon fiber

A technology of polyacrylonitrile-based pre-oxidation fiber and polyacrylonitrile, which is applied to the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of limiting the production efficiency of carbon fibers, complicated pre-oxidation process, etc., so as to improve the generation efficiency and shorten the heat treatment time. , the effect of rapid pre-oxidation

Active Publication Date: 2012-10-03
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

In most reports, the pre-oxidation process is complicated and the reaction time is more than

Method used

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  • Preparation method of polyacrylonitrile pre-oxidation fiber and carbon fiber

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Experimental program
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Example Embodiment

[0015] Example 1

[0016] The polyacrylonitrile raw silk was made to pass through two pre-oxidation temperature zones in sequence at a constant speed of 20 m / h in normal pressure and air medium, and the total time was 45 minutes. The first temperature zone is the cyclization stage, the reaction temperature is 230°C, the reaction time is set at 25 minutes in an air atmosphere, and a rigid draft of 3% is added. In the second temperature zone oxidative crosslinking stage, the reaction temperature was 265°C, the reaction time was 20 minutes, and a negative draft of 1.5% was added. Then, the conventional carbonization treatment was carried out in a nitrogen atmosphere for 5 minutes. First, it went through a low-temperature carbonization process in multiple temperature zones of 300 °C to 700 °C. At this time, 3% positive drafting was added, and then a high temperature carbonization of about 1300 °C was carried out. Add 3% negative draft.

[0017] The bulk density and mechanical pr...

Example Embodiment

[0019] Example 2

[0020] The polyacrylonitrile raw silk was made to pass through three pre-oxidation temperature zones in sequence at a constant speed of 20 m / h in normal pressure and air medium, and the total time was 33 minutes. The reaction temperature of the first temperature zone cyclization stage was 220°C, the reaction time was set to 15 minutes, and a rigid draft of 4.5% was added. The second temperature zone is the oxidative cyclization stage, the temperature is 245°C, and the reaction time is set as 6 minutes. The third temperature zone is the cross-linking aromatization stage, the temperature is 270°C, the reaction time is 12 minutes, and a negative draft of 1% is added. Then, the conventional carbonization treatment was carried out in a nitrogen atmosphere for 6 minutes. First, it went through a low-temperature carbonization process in multiple temperature zones of 300°C to 700°C. At this time, 3% positive drafting was added, and then a high temperature carboniza...

Example Embodiment

[0023] Example 3

[0024] The polyacrylonitrile raw silk was made to pass through four pre-oxidation temperature zones in turn at a constant speed of 20m / h in normal pressure and air medium, and the total time was 30 minutes. The reaction temperature of the initial cyclization stage in the first temperature zone was 210°C, the reaction time was set to 9 minutes, and a rigid draft of 6% was added. The second temperature zone is the mid-term cyclization stage, the temperature is 230°C, and the reaction time is 6 minutes, and the third temperature zone is the oxidative cyclization stage, the temperature is 250°C, and the reaction time is 6 minutes. The fourth temperature zone is the cross-linking aromatization stage, the temperature is 270°C, the reaction time is 9 minutes, and a negative draft of 1.5% is added. Then, the conventional carbonization treatment was carried out in a nitrogen atmosphere for 7 minutes. First, it went through a low-temperature carbonization process in ...

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Abstract

The invention discloses a preparation method of a polyacrylonitrile pre-oxidation fiber and a carbon fiber, belonging to the technical field of fiber preparation. The preparation method comprises the steps of: enabling polyacrylonitrile protofilament to pass through a continuous pre-oxidization device at a constant speed in a normal pressure and an air medium and carrying out pre-oxidization treatment, wherein the temperature rises by adopting 2-4 temperature zone gradients, and the total time is controlled within 30-45 min; in the low temperature stage of the pre-oxidization process, the reaction temperature is 200-240 DEG C, positive drafting accounting for 0%-8% of the total drafting is added, and the total time is 15-25 min; and in the high temperature stage, the reaction temperature is 240-275 DEG C, negative drafting accounting for 0%-3% of the drafting is added, the total time is 15-20min, the low temperature stage is divided into one or two temperature zones, and the high temperature stage is divided into one or two temperature zones, and the temperature of the 2-4 temperature zones rises in sequence, therefore the pre-oxidization fiber is obtained; furthermore, performing a regular carbonization treatment in the atmosphere of nitrogen for 5-8 min to obtain the carbon fiber. The preparation method of the polyacrylonitrile pre-oxidation fiber and the carbon fiber, disclosed by the invention, has the advantages of improving production efficiency of the pre-oxidization and shortening the pre-oxidization heat treatment time.

Description

technical field [0001] The invention relates to a high-efficiency pre-oxidation method of polyacrylonitrile-based carbon fiber precursors and a preparation method of carbon fibers. The invention mainly realizes the continuous and high-efficiency pre-oxidation of polyacrylonitrile fibers, and belongs to the technical field of fiber preparation. Background technique [0002] Due to its excellent mechanical properties, heat resistance, electrical and thermal conductivity, creep resistance, and corrosion resistance, polyacrylonitrile-based carbon fibers are often used as reinforcements for advanced composite materials and are widely used in aerospace and major areas of the national economy. The pre-oxidation of polyacrylonitrile precursor is the longest link in the whole carbon fiber production process, and it is also a key step in the process of carbon fiber preparation. Improving the production efficiency of pre-oxidation means shortening the pre-oxidation reaction time and rea...

Claims

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Application Information

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IPC IPC(8): D01F9/22
Inventor 徐樑华薛一萌童元建曹维宇赵振文李常清
Owner BEIJING UNIV OF CHEM TECH
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