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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

Method used

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

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Experimental program
Comparison scheme
Effect test

Embodiment 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 the air medium, using a three-stage pre-oxidation furnace at 225°C, 240°C, and 255°C, with a temperature gradient of 15°C, the oxidation furnace The wind speed of the internal circulation is 6m / s, the residence time is 80min, the draft ratio is 0%, and the density is 1.35g / cm 3 Under the protection of nitrogen, the pre-oxidized fiber is carbonized at a low temperature of 300-900°C for 3 minutes, and the draft ratio of +1% is applied; the draft ratio of -4% is applied at a temperature of 1000-1500°C, and the high temperature Carbonize for 3 minutes to obtain large tow carbon fibers. The prepared carbon fibers were glued and cured into strips with epoxy resin E44 / acetone / triethylenetetramine (10:15:1), and then the mechanical properties of the corresponding carbon fiber samples were tested according to the national st...

Embodiment 2

[0011] The 24KPAN copolymer fiber produced by Weihai Kaizhan Fiber Co., Ltd. is used, and it is treated in a three-stage pre-oxidation furnace at 230°C, 243°C, and 256°C. The temperature gradient is 13°C. The circulating wind speed in the oxidation furnace is 7m / s, and the residence time is 65min. The draw ratio is 1%, resulting in a density of 1.36g / cm 3 The preoxidized fiber, other process parameters and operation are the same as embodiment 1, obtains large tow carbon fiber, and the results are shown in Table 1.

Embodiment 3

[0013] The 24KPAN copolymer fiber produced by Weihai Kaizhan Fiber Co., Ltd. is used, and it is treated in a three-stage pre-oxidation furnace at 220°C, 237°C, and 254°C. The temperature gradient is 17°C. The circulating wind speed in the oxidation furnace is 4m / s, and the residence time is 75min. The draw ratio is 0%, resulting in a density of 1.34g / cm 3 The preoxidized fiber, other process parameters and operation are the same as embodiment 1, obtains large tow carbon fiber, and 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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