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High-speed preparation method for producing large-tow carbon fibers

A technology of tow carbon fiber and large tow, which is applied in the field of high-speed preparation of large tow carbon fiber, can solve the problems of lack of large tow carbon fiber technology, discrete fiber indicators, and difficult pre-oxidation, etc., to improve the scale of enterprises Production efficiency, reduce unit production consumption, and ensure performance effects

Active Publication Date: 2020-04-17
CHANGCHUN UNIV OF TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyacrylonitrile fiber (precursor) is the main raw material for preparing large-tow carbon fiber; large-tow carbon fiber has the advantage of low cost compared with small-tow fiber, and large-tow carbon fiber is more conducive to the development of low-cost, general-purpose However, in the foreign market, large-scale production of large-tow carbon fiber is mainly carried out by Mitsubishi, Toho, SGL, Aksa, Formosa Plastics, etc. Foreign blockade and domestic large-tow raw silk production and large-tow carbon fiber carbonization production technology, equipment, environment and other factors restrict the development; domestic large-scale production capacity of large-tow carbon fiber is currently only Jilin Carbon Valley Carbon Fiber Co., Ltd. and Jilin Jinggong Carbon Fiber Co., Ltd. (Jilin Carbon Valley mainly produces large tow carbon fiber precursors, Jilin Jinggong mainly carbonizes), and there are also enterprises that are developing and planning construction, such as Shanghai Petrochemical, Weihai Development, Kangdexin, Xinjiang Carbon Valley New Material Co., Ltd., Zhongfu Shenying Carbon Fiber, etc. Among them, the ZL201610517888.5 developed by Weihai discloses the pre-oxidation method for preparing large-tow carbon fibers. The 24K polyacrylonitrile copolymer fiber is pre-oxidized and heat-treated in an air atmosphere for 60-90 minutes , the circulating wind speed of the oxidation furnace is controlled at 6±2m / s, the carbonization time needs to be 6±1.5min, the tensile strength of the obtained carbon fiber is 4.5-4.7GPa, and the modulus is about 240GPa
[0003] While vigorously developing large tow carbon fibers, the main problems in the production of large tow carbon fibers are as follows: 1. During the pre-oxidation process, the heat released by the oxidation of large tow polyacrylonitrile fibers (precursor filaments) is not easy to dissipate heat, resulting in that the heat cannot be timely Discharge, and then fiber breakage, roll winding, etc. will affect stable production and cause excessive dispersion of fiber indicators; 2. The pre-oxidation of large-tow polyacrylonitrile fibers (precursors) is more difficult, and large-tow polyacrylonitrile fibers With more tows, the inside of the fiber is less likely to be oxidized, resulting in obvious skin-core structure, and low-temperature carbonization is difficult to pass through, etc.

Method used

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  • High-speed preparation method for producing large-tow carbon fibers
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Examples

Experimental program
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Effect test

Embodiment 1

[0019] Choose the 25K large-tow polyacrylonitrile copolymer fiber (precursor) produced by Jilin Carbon Valley Company produced by wet spinning, the PAN copolymer fiber containing more than 90% acrylonitrile monomer components, in the air medium, the speed is 12m / Under the conditions of 230°C, 238°C, 247°C, 255°C, 261°C, and 270°C, six-stage pre-oxidation furnaces were used for treatment under the condition of 270°C. The oxidation time was 50 minutes, and the draw ratio was 1.01, resulting in a density of 1.3844g / cm 3 Then, under the protection of nitrogen, the pre-oxidized wire was carbonized at 800°C for 63s at a low temperature, with a draft ratio of 1.01; at a high temperature of 1200°C, with a draft ratio of 0.97, and a high temperature carbonization time of 63s, and then passed through the surface Processing, sizing, and drying to obtain 25K large-tow carbon fibers.

[0020] The prepared large-tow carbon fiber was prepared with Beihua resin A / Beihua resin B / acetone (1:0....

Embodiment 2

[0022] Choose the 25K large tow polyacrylonitrile copolymer fiber (precursor) produced by Jilin Carbon Valley Company produced by wet spinning, the PAN copolymer fiber containing more than 90% acrylonitrile monomer components, in air medium, the speed is 13m / Under the condition of 235°C, 243°C, 252°C, 260°C, 264°C, and 273°C, six gradient pre-oxidation furnaces were used for treatment, the oxidation time was 45min, the draw ratio was 1.01, and the density was 1.3850g / cm 3 Then, under the protection of nitrogen, the pre-oxidized wire was carbonized at 800°C for 63s at a low temperature, with a draft ratio of 1.01; at a high temperature of 1200°C, with a draft ratio of 0.97, and a high temperature carbonization time of 63s, and then passed through the surface Processing, sizing, and drying to obtain 25K large-tow carbon fibers.

[0023] The prepared large-tow carbon fiber was prepared with Beihua resin A / Beihua resin B / acetone (1:0.34:12) to prepare a mixed resin, dipped and cu...

Embodiment 3

[0025] Choose the 25K large tow polyacrylonitrile copolymer fiber (precursor) produced by the Jilin Carbon Valley Company produced by wet spinning, the PAN copolymer fiber containing more than 90% acrylonitrile monomer components, in the air medium, the speed is 14m / Under the condition of 240°C, 248°C, 256°C, 266°C, 269°C, and 276°C, the six-stage gradient pre-oxidation furnace was used for treatment under the condition of 240°C, the oxidation time was 42.9min, the draw ratio was 1.01, and the density was 1.3812g / cm 3 Then, under the protection of nitrogen, the pre-oxidized wire was carbonized at 800°C for 63s at a low temperature, with a draft ratio of 1.01; at a high temperature of 1200°C, with a draft ratio of 0.97, and a high temperature carbonization time of 63s, and then passed through the surface Processing, sizing, and drying to obtain 25K large-tow carbon fibers.

[0026] The prepared large-tow carbon fiber was prepared with Beihua resin A / Beihua resin B / acetone (1...

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Abstract

The invention provides a high-speed preparation method for producing large-tow carbon fibers, and belongs to the technical field of preparation of large-tow carbon fiber materials. The method comprises the following steps of pre-oxidizing large-tow polyacrylonitrile copolymer fibers in an air atmosphere at the temperature of 220-300 DEG C, and performing heat treatment in an oxidation furnace in asix-gradient temperature rising mode for 45-90 minutes to obtain pre-oxidized filaments of tow carbon fibers, wherein the temperature gradient is 9+ / -3 DEG C, the production speed is 12-15m / min, andthe draw ratio is 0.98-1.20; performing low-temperature carbonization treatment on the pre-oxidized filaments; and performing high-temperature carbonization treatment on the carbon fibers subjected tolow-temperature carbonization treatment to obtain the large-tow carbon fibers. The tensile strength of the prepared carbon fibers is over 5,000 MPa, and the modulus is 240-250 GPa.

Description

technical field [0001] The invention belongs to the technical field of large-tow carbon fiber material preparation, and in particular relates to a high-speed preparation method for producing large-tow carbon fiber. Background technique [0002] Polyacrylonitrile-based carbon fiber reinforced fiber is the main material of composite materials, and high-efficiency and low-cost carbon fiber plays an important role in promoting the lightweight of composite materials. Polyacrylonitrile fiber (precursor) is the main raw material for preparing large-tow carbon fiber; large-tow carbon fiber has the advantage of low cost compared with small-tow fiber, and large-tow carbon fiber is more conducive to the development of low-cost, general-purpose However, in the foreign market, large-scale production of large-tow carbon fiber is mainly carried out by Mitsubishi, Toho, SGL, Aksa, Formosa Plastics, etc. Foreign blockade and domestic large-tow raw silk production and large-tow carbon fiber ...

Claims

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Application Information

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IPC IPC(8): D01F9/22
CPCD01F9/225
Inventor 敖玉辉庄海林尚垒杜巍峰宁臣李红龙马岩
Owner CHANGCHUN UNIV OF TECH
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