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Method of preparing polyacrylonitrile-based carbon raw fibers by dry-wet method

A polyacrylonitrile-based carbon fiber, dry and wet technology, applied in wet spinning, fiber chemical characteristics, stretch spinning, etc., can solve the problem of easily disturbed coagulation bath level, inconsistent residence time, and insufficient coagulation of silk strands. It can solve the problem of atmospheric disturbance of the coagulation bath, improve the uniformity and adhesion problems, and facilitate stable and continuous effects.

Active Publication Date: 2019-12-20
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are also the following common problems in the above patented methods and actual production process: (1) After spinning, the filaments enter the coagulation bath vertically, and turn to pull out of the coagulation bath after being bundled by the steering roller
This makes the filaments at the edge of the spinneret and the filaments at the center inconsistent due to the inconsistency of the residence time of the convergence in the dry section, and the resulting raw filaments are not uniform; The adhesion between monofilaments affects the performance of the final carbon fiber; (2) the atmosphere in the dry section is highly required, which makes it difficult to implement the process or easily disturbs the coagulation bath liquid level, which is not conducive to the preparation of stable raw silk; (3) hot water washing The drawn filaments enter the oiling tank directly or after being rolled for oiling. The large amount of hot water entrained in the filaments causes the oiling agent to be unstable, making the filaments oiled unevenly

Method used

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  • Method of preparing polyacrylonitrile-based carbon raw fibers by dry-wet method
  • Method of preparing polyacrylonitrile-based carbon raw fibers by dry-wet method
  • Method of preparing polyacrylonitrile-based carbon raw fibers by dry-wet method

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Effect test

Embodiment 1

[0032] A dry-wet method for preparing polyacrylonitrile-based carbon fiber precursors, comprising the following steps:

[0033] (1) Preparation of spinning stock solution: spinning stock solution is composed of acrylonitrile copolymer and solvent dimethyl sulfoxide, wherein the acrylonitrile copolymer is a binary copolymer of acrylonitrile and itaconic acid, and the structural formula is as follows:

[0034]

[0035] In the formula: R1 is H; R2 is H; R 3 for CH 3 ; R4 is CH 3 CH 2 ;x=99.5mol%, y=0.5mol%, z=0;

[0036] The dynamic viscosity of the above-mentioned spinning dope is 50 Pa·s, the intrinsic viscosity of the acrylonitrile copolymer is 1.6 dL / g, and the temperature is 80°C.

[0037] (2) Spinning: the spinning dope is sent to the spinneret assembly through a primary filter and a secondary filter by a metering pump and a booster pump. The jacket water of the spinneret assembly is kept at a constant temperature of 30°C, and the distance between the spinneret and t...

Embodiment 2

[0048] A dry-wet method for preparing polyacrylonitrile-based carbon fiber precursors, comprising the following steps:

[0049] (1) Preparation of spinning stock solution: spinning stock solution is composed of acrylonitrile copolymer and solvent dimethyl sulfoxide, wherein the acrylonitrile copolymer is a terpolymer of acrylonitrile, itaconic acid derivatives, and acrylic acid derivatives, and the structural formula As follows:

[0050]

[0051] In the formula: R1 is NH 4 ; R2 is CH 3 CH 2 ; 3 Is H; R4 is H; x=97.6mol%, y=0.4mol%, z=2mol%;

[0052] The dynamic viscosity of the above-mentioned spinning dope is 250 Pa·s, the intrinsic viscosity of the acrylonitrile copolymer is 5 dL / g, and the temperature is 45°C.

[0053] (2) Spinning: The spinning dope is sent to the spinneret assembly through a primary filter and a secondary filter by a metering pump and a booster pump. The jacket water of the spinneret assembly is kept at a constant temperature of 50°C, and the dist...

Embodiment 3

[0064] A dry-wet method for preparing polyacrylonitrile-based carbon fiber precursors, comprising the following steps:

[0065] (1) Preparation of spinning stock solution: spinning stock solution is composed of acrylonitrile copolymer and solvent dimethyl sulfoxide, wherein the terpolymer of acrylonitrile copolymer acrylonitrile and itaconic acid derivatives and acrylic acid derivatives has the following structural formula Shown:

[0066]

[0067] In the formula: R1 is H; R2 is CH 3 ; 3 for CH 3 ; R4 is CH3; x=90mol%, y=9mol%, z=1mol%;

[0068] The dynamic viscosity of the above-mentioned spinning dope is 150 Pa·s, the intrinsic viscosity of the acrylonitrile copolymer is 3.5 dL / g, and the temperature is 55°C.

[0069] (2) Spinning: the spinning dope is sent to the spinneret assembly through a primary filter and a secondary filter by a metering pump and a booster pump. The jacket water of the spinneret assembly is kept at a constant temperature of 40°C, and the distance...

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Abstract

The invention particularly relates to a method of preparing polyacrylonitrile-based carbon raw fibers by a dry-wet method. Firstly, dimethyl sulfoxide is used as a solvent, a spinning dope of an acrylonitrile binary or ternary copolymer is prepared, and then oblique spinning, solidification, water washing and hot drawing, air drying, oiling and drying, steam drawing, and relaxation and setting areconducted to prepare the polyacrylonitrile-based carbon raw fibers. By adopting the method of preparing the polyacrylonitrile-based carbon raw fibers by the dry-wet method, a control method of a drysection is simplified, the uniformity of the fibers is improved, the problem of sticking is overcome, and the uniformity of oiling is improved by air-drying. The method of preparing the polyacrylonitrile-based carbon raw fibers by the dry-wet method has a simple process, easy process control and high production efficiency, and can be used for continuously preparing uniform and stable high-performance polyacrylonitrile-based carbon raw fibers. The general formula of the copolymer adopted by the method of preparing the polyacrylonitrile-based carbon raw fibers by the dry-wet method is shown as follows.

Description

technical field [0001] The invention belongs to the technical field of carbon fiber preparation, and in particular relates to a method for preparing polyacrylonitrile-based carbon fiber precursors by a dry-wet method. Background technique [0002] Polyacrylonitrile-based carbon fiber has a series of excellent properties such as high specific strength, high specific modulus, high temperature resistance, corrosion resistance, fatigue resistance, electrical conductivity, and heat transfer. Equipment and other military and civilian industries have a wide range of applications. The dry-wet spinning is characterized by high-speed spinning, improving equipment utilization efficiency and reducing costs, and the carbon fiber produced by dry-wet spinning has fewer surface defects, which is conducive to the preparation of high-performance carbon fibers, and is an important direction for the development of carbon fiber preparation technology. . The preparation of high-performance prec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01D5/06D01D5/12D01D10/06
CPCD01D5/06D01D5/12D01D10/06D01F9/22
Inventor 张兴华张寿春王宏宝经德齐赵振波
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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