Large tow polyacrylonitrile pre-oxidized fiber, large tow carbon fiber, and preparation methods of large tow polyacrylonitrile pre-oxidized fiber and large tow carbon fiber

A technology of polyacrylonitrile pre-oxidized yarn and polyacrylonitrile fiber, which is applied in fiber treatment, ultrasonic/sonic fiber treatment, textiles and papermaking, etc., and can solve the problem of reducing the heat release of large tow polyacrylonitrile fibers and pre-oxidized silk skin. The core structure is serious and the pre-oxidation temperature is lowered to achieve the effect of reducing the pre-oxidation time, solving the difficulty of oxygen diffusion, and lowering the pre-oxidation temperature

Inactive Publication Date: 2018-08-14
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the large heat release, large energy consumption, high reaction temperature and long reaction time in the preparation process of the existing large-tow polyacrylonitrile pre-oxidized yarn, and the pre-oxidized yarn sheath-core produced Defects such as severe structure, provide a large-tow polyacrylonitrile pre-oxidized yarn, large-tow carbon fiber and its preparation method
The preparation method of the present invention significantly reduces the heat release of the large-tow polyacrylonitrile fiber during the pre-oxidation process, reduces the pre-oxidation temperature, and reduces the Energy consumption, while introducing oxygen elements, solving the problem of oxygen diffusion, and reducing pre-oxidation time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation method of large tow polyacrylonitrile pre-oxidized silk is as follows:

[0038] (1) Open the electron accelerator, the electron beam energy is 0.5MeV, make the large tow polyacrylonitrile fiber (with the sample of comparative example 1) follow a track (the track passes directly below the irradiation window of the electron accelerator), reciprocate Movement, to pass through the electron beam back and forth for irradiation reaction; the radiation absorbed dose rate is 30Gy / s, the total irradiation time is 1000s, and the total radiation absorbed dose is 30kGy; the reciprocating motion speed is 0.2m / min;

[0039] (2) After the irradiation reaction is finished, pre-oxidize the irradiated large-tow polyacrylonitrile fiber to obtain the product; there are 4 pre-oxidation temperature zones, and the temperatures are 210°C, 225°C, 245°C, and 265°C, respectively. The pre-oxidation time is 45 minutes, and the draft ratio in the pre-oxidation temperature range is 1:1...

Embodiment 2

[0043] The preparation method of large tow polyacrylonitrile preoxygenated silk is the same as embodiment 1, and the difference is only in:

[0044] The electron beam energy is 8.0MeV, the radiation absorbed dose rate is 200Gy / s, the total irradiation time is 2000s, and the total radiation absorbed dose is 400kGy; the reciprocating motion speed is 30m / min; there are 3 pre-oxidation temperature zones, and the pre-oxidation temperature 210°C, 240°C, 268°C, pre-oxidation time is 35min, and the draw ratio in the pre-oxidation temperature range is 1:1.1:0.95.

[0045] The cyclization exothermic heat of the obtained polyacrylonitrile pre-oxidized yarn is 512.03J / g, and the density before pre-oxidation is 1.18g / cm -3 , the density after preoxidation is 1.34g / cm -3 .

[0046] Carry out carbonization treatment on the polyacrylonitrile pre-oxidized yarn: low-temperature carbonization temperature is 500-700°C, carbonization time is 12s; high-temperature carbonization temperature is 900...

Embodiment 3

[0048] The preparation method of large tow polyacrylonitrile preoxygenated silk is the same as embodiment 1, and the difference is only in:

[0049] The electron beam energy is 2MeV, the radiation absorbed dose rate is 1000Gy / s, the total irradiation time is 1000s, and the total radiation absorbed dose is 1000kGy; the reciprocating motion speed is 15m / min; there are 5 pre-oxidation temperature zones, and the pre-oxidation temperature is 205°C, 225°C, 240°C, 255°C, 270°C, the pre-oxidation time is 75 minutes, and the draft ratio in the pre-oxidation temperature range is 1:1:1:1.1:0.98.

[0050] The cyclization exothermic heat of gained polyacrylonitrile preoxidation silk is 424.15J / g, and the density before preoxidation is 1.18g / cm -3 , the density after preoxidation is 1.37g / cm -3 .

[0051] Carry out carbonization treatment on the polyacrylonitrile pre-oxidized yarn: low-temperature carbonization temperature is 500-700°C, carbonization time is 12s; high-temperature carboniz...

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Abstract

The invention discloses large tow polyacrylonitrile pre-oxidized fiber, large tow carbon fiber, and preparation methods of the large tow polyacrylonitrile pre-oxidized fiber and the large tow carbon fiber. The preparation method of the large tow polyacrylonitrile pre-oxidized fiber comprises: 1, after an electron accelerator is turned on, carrying out an intermittent irradiation reaction on largetow polyacrylonitrile fiber, wherein the irradiation absorption dose rate is 0.5-5*10<4> Gy/s, and the total irradiation absorption dose is 20-5000 kGy; and 2, carrying out pre-oxidation on the irradiated large tow polyacrylonitrile fiber for 15-75 min at a temperature of 180-270 DEG C after completing the irradiation reaction so as to obtain the large tow polyacrylonitrile pre-oxidized fiber, wherein the large tow polyacrylonitrile pre-oxidized fiber is carbonized to obtain the carbon fiber. According to the present invention, with the preparation method, the heat release during the pre-oxidation of the fiber can be significantly reduced, the pre-oxidation temperature can be reduced, the energy consumption can be reduced, and the oxygen is introduced so as to solve the oxygen diffusion problem and reduce the pre-oxidation time; and the large tow polyacrylonitrile pre-oxidized fiber has advantages of high density and high strength, and the subsequently-prepared carbon fiber material has excellent performance.

Description

technical field [0001] The invention relates to a large tow polyacrylonitrile preoxidized yarn, a large tow carbon fiber and a preparation method thereof. Background technique [0002] Electron beam radiation processing technology is an important technology that can adjust the chemical structure and physical properties of polymers through electron beams. Polymer materials can undergo chemical reactions such as radiation cross-linking, radiation degradation, and radiation oxidation after being irradiated by electron beams. In an aerobic environment, they can also undergo oxidative cross-linking reactions with oxygen. Polyacrylonitrile fibers can undergo oxidative crosslinking or oxidative degradation after electron beam irradiation in an aerobic environment. At present, there are many related documents and patents on the application of irradiation technology in the production of carbon fiber industry (Huang Yudong, Xu Zhiwei, Zhang Chunhua, a method for improving the strengt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M10/02D01F9/22
CPCD01F9/22D06M10/025
Inventor 张文礼吴国忠王谋华刘伟华张文发李诚
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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