Pre-oxidation method for preparation of large-tow carbon fiber

A large-tow carbon fiber and pre-oxidation technology, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, can solve the problems of less research on key technologies of large-tow carbon fiber processing, and achieve a good guiding effect

Active Publication Date: 2016-12-14
WEIHAI TUOZHAN FIBER
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Some domestic carbon fiber manufacturers and colleges and universities have broken through the key technology of dry spray wet processi

Method used

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  • Pre-oxidation method for preparation of large-tow carbon fiber

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Example Embodiment

[0008] Example 1:

[0009] The PAN copolymer fiber (the tow is 24K, the copolymer composition (wt%)) is: acrylonitrile (AN): Methyl acrylate (MA): Itaconic acid (IA)=96:2.0:2.0), in air medium, using 225℃, 240℃, 255℃ three-stage pre-oxidation furnace treatment, temperature gradient 15℃, oxidation furnace The internal circulation wind speed is 6m / s, the residence time is 80min, the draft ratio is 0%, and the density is 1.35g / cm 3 For pre-oxidized fiber, the pre-oxidized fiber is carbonized at 300~900℃ for 3min at low temperature under the protection of nitrogen, and +1% draft ratio is applied; at 1000~1500℃, 4% draft ratio is applied, high temperature Carbonize for 3 minutes to obtain large tow carbon fiber. The prepared carbon fiber was glued and cured into strips with epoxy resin E44 / acetone / triethylenetetramine (10:15:1) liquid, and then the mechanical properties of the corresponding carbon fiber samples were tested according to the national standard GB / T3362-2005. The results...

Example Embodiment

[0010] Example 2:

[0011] Adopt 24KPAN copolymer fiber produced by Weihai Expansion Fiber Co., Ltd., adopt three-stage pre-oxidation furnace treatment at 230℃, 243℃, and 256℃. The temperature gradient is 13℃. The circulating air velocity in the oxidation furnace is 7m / s and the residence time is 65min. The draft ratio is 1%, and the density is 1.36g / cm 3 The other process parameters and operations of the pre-oxidized fiber are the same as in Example 1, and large tow carbon fibers are obtained. The results are shown in Table 1.

Example Embodiment

[0012] Example 3:

[0013] The 24KPAN copolymer fiber produced by Weihai Expansion Fiber Co., Ltd. is processed in a three-stage pre-oxidation furnace at 220°C, 237°C, and 254°C. The temperature gradient is 17°C, the circulating air velocity in the oxidation furnace is 4m / s, and the residence time is 75min. The draft ratio is 0%, and the density is 1.34g / cm 3 The other process parameters and operations of the pre-oxidized fiber are the same as in Example 1, and large tow carbon fibers are obtained. The results are shown in Table 1.

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Abstract

The invention specifically relates to a pre-oxidation method for preparation of a large-tow carbon fiber, belonging to the field of organic polymers. The pre-oxidation method comprises the following steps: pre-oxidizing a large-tow polyacrylonitrile copolymer fiber at 180 to 280 DEG C in an air atmosphere and carrying out heat treatment for 60 to 90 min by using a three-stage gradient heating manner under the conditions that temperature gradient is 15 +/- 2 DEG C, the speed of recirculation air in an oxidation furnace is controlled to be 6 +/- 2 m/s and a draw ratio is -2 to 2%, thereby preparing a pre-oxidized fiber with a density of 1.35 +/- 0.02 g/cm<3>; and under conventional carbonization conditions, subjecting the pre-oxidized fiber to low-temperature carbonization at 300 to 900 DEG C for 3 +/- 1.5 min under the protection of nitrogen and the condition of a draw ratio of -2 to 2%, and the subjecting the obtained fiber to high-temperature carbonization at 1000 to 1500 DEG C for 3 +/- 1.5 min under the condition of a draw ratio of -5 to 0%. According to the invention, the pre-oxidized fiber with a complete structure is prepared by controlling the pre-oxidation temperature gradient, the speed of recirculation air in the oxidation furnace and the density of the obtained pre-oxidized fiber, so the high-performance large-tow carbon fiber is prepared.

Description

technical field [0001] The invention relates to the technical field of carbon fibers, in particular to a pre-oxidation method for preparing large tow carbon fibers. Background technique [0002] We know that reinforcing fiber is the main material of composite materials, and high-efficiency and low-cost carbon fibers play an important role in promoting the lightweight of composite materials. There are two ways to reduce the cost of carbon fiber, one is to use dry spray wet process to increase the spinning speed; the other is to use large tow carbon fiber. Some domestic carbon fiber manufacturers and colleges and universities have broken through the key technology of dry spray wet processing through independent research and development, but there are few researches on the key technology of large tow carbon fiber processing. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a pre-oxidation met...

Claims

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Application Information

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IPC IPC(8): D01F9/22
CPCD01F9/22
Inventor 张月义丛宗杰李松峰曹明海王文义
Owner WEIHAI TUOZHAN FIBER
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