Method for regulating and controlling homogenization degree of polyacrylonitrile preoxidized fiber

A technology of polyacrylonitrile fiber and pre-oxidized fiber, which is applied in fiber processing, textile and papermaking, etc., can solve the problems of affecting the modification effect, demulsification of oil agent, affecting the oiling effect of raw silk, etc., so as to improve the homogenization degree, the effect of improving the modification effect

Inactive Publication Date: 2017-05-10
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem caused by this approach is that the pH value of the oil agent is generally about 6.7 (Sun Xiuhua. Master’s Thesis of Changchun University of Technology, 2012), while the pH value of 0.1% boric acid solution is about 5.0 (Zhao Jingjing et al. Anhui Chemical Industry ,2014,40:87), which changes the pH value of the oil agent, which will destroy the stability of the oil agent, cause the oil agent to break, affect the oiling effect of the raw silk, and finally affect the performance of the carbon fiber
Xie Huaiyu (CN103572411A) directly modified the PAN fiber by impregnating oxygen-rich substances, siloxane, and borate solution to improve the homogenization degree of the pre-oxidized fiber. The disadvantage of this method is that the PAN fiber was not removed before modification. Fiber surface oil, will significantly affect the modification effect

Method used

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  • Method for regulating and controlling homogenization degree of polyacrylonitrile preoxidized fiber
  • Method for regulating and controlling homogenization degree of polyacrylonitrile preoxidized fiber
  • Method for regulating and controlling homogenization degree of polyacrylonitrile preoxidized fiber

Examples

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Effect test

Embodiment 1

[0031] At room temperature, impregnate 2g of 1KPAN fiber in an Erlenmeyer flask filled with 200ml of xylene, then place the Erlenmeyer flask in an ultrasonic oscillator of the model YH-320DH for 5 minutes, and use ultrasonic vibration to increase The removal efficiency and effect of PAN fiber surface oil agent. After removing the PAN fiber surface oil agent, the PAN fiber with the surface oil agent removed is immersed in a boric acid solution with a mass fraction of 0.5% for 1 min, and the temperature is raised from room temperature to 260 °C at a heating rate of 9 °C / min, and then heated at 260 °C. Stay for 30min. Weigh 1g of the resulting pre-oxidized fiber, cut it into 3cm short filaments, dip it in a flask filled with sulfuric acid solution, the sulfuric acid solution concentration is 40wt%, the sulfuric acid solution is heated to boiling, and treated under boiling conditions for 0.8h, then use Stir and wash with deionized water until neutral, filter through filter paper,...

Embodiment 2

[0035] At room temperature, impregnate 2g of 3KPAN fiber in a conical flask filled with 200ml of xylene, then place the conical flask in an ultrasonic oscillator of the model YH-320DH for 8 minutes, and use ultrasonic vibration to increase The removal efficiency and effect of PAN fiber surface oil agent. After removing the PAN fiber surface oil agent, the PAN fiber with the surface oil agent removed is immersed in a boric acid solution with a mass fraction of 1% for 2 minutes, and the temperature is raised from room temperature to 280°C at a heating rate of 8°C / min, and then heated at 280°C. Stay for 25min. Take by weighing 1g of the gained preoxidized fiber, cut it into 3cm long short filaments, adopt the same treatment and sample preparation method as in Example 1, scan the preoxidized fiber cross-section with SEM, as shown in the attached Figure 4 shown.

Embodiment 3

[0039] At room temperature, impregnate 6KPAN fibers with a weight of 2g in an Erlenmeyer flask containing 200ml of xylene, and then place the Erlenmeyer flask in an ultrasonic oscillator of the model YH-320DH for 10 minutes, and use ultrasonic vibration to increase The removal efficiency and effect of PAN fiber surface oil agent. After removing the PAN fiber surface oil agent, the PAN fiber with the surface oil agent removed is immersed in a boric acid solution with a mass fraction of 2% for 3 minutes, and the temperature is raised from room temperature to 300°C at a heating rate of 7°C / min, and then heated at 300°C. Stay for 20min. Take by weighing 1g of the gained preoxidized fiber, cut it into 3cm long short filaments, adopt the same treatment and sample preparation method as in Example 1, scan the preoxidized fiber cross-section with SEM, as shown in the attached Figure 6 shown.

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Abstract

The invention relates to a method for regulating and controlling the homogenization degree of a polyacrylonitrile preoxidized fiber. The method comprises the steps of dipping a polyacrylonitrile fiber into xylene at the room temperature, carrying out oscillation for 5-15 minutes in an ultrasonic oscillation instrument, removing an oil agent from the surface of the PAN fiber, carrying out dipping modification on the polyacrylonitrile fiber by virtue of a 0.5%-4% boric acid solution for 0.5 second to 6 minutes, heating the boric acid-modified polyacrylonitrile fiber in air from the room temperature to 260-340 DEG C at a heating speed of 5 -9 DEG / min, and carrying out pre-oxidation for 10-30 minutes. The method has the advantages that the homogenization degree of the PAN preoxidized fiber can be regulated and controlled and the strength of carbon fibers can be increased.

Description

technical field [0001] The invention belongs to a method for increasing the strength of carbon fibers, in particular to a method for regulating the homogenization degree of polyacrylonitrile (PAN) preoxidized fibers. Background technique [0002] The carbon content of carbon fiber is more than 90%, which not only has the characteristics of general carbon materials, such as corrosion resistance, high temperature resistance, friction resistance, thermal conductivity, electrical conductivity, etc., but also has the machinability characteristics of general fibers, such as softness and anisotropy , easy processing, and high strength along the fiber axis, so that carbon fiber can be used not only as a reinforcing base for structural materials to carry loads, but also as a functional material in aerospace, sports, construction, automobiles, new energy and other fields. [0003] In the production process of PAN-based carbon fiber, pre-oxidation treatment is one of the key links affe...

Claims

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Application Information

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IPC IPC(8): D01F9/22D06M11/82D06M101/28
CPCD01F9/225D06M11/82D06M2101/28
Inventor 吕春祥孙同庆李永红邵伟
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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