Method for accelerating oxidation stabilization of mesophase pitch fiber

A mesophase pitch and oxidation stabilization technology, applied in fiber chemical characteristics, textiles and papermaking, etc., can solve problems such as insufficient correlation between production and application of mesophase pitch-based carbon fibers, fiber debonding or pulling out, poor fiber infiltration, etc. , to achieve the effects of improving interface interaction and interface bonding strength, increasing reactivity, and accelerating oxidation reaction

Inactive Publication Date: 2019-04-12
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mesophase pitch-based carbon fiber is obtained after the non-melting fiber is subjected to subsequent high-temperature treatment. Usually, the surface of the obtained mesophase pitch-based carbon (graphite) fiber is regular, flat, and smooth, and there may be problems such as fiber infiltration during the application and use of composite materials. Not good, fiber debonding or pulling out, low interfacial interaction and other deficiencies, which are the result of insufficient correlation between the production and application of mesophase pitch-based carbon fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A method for accelerating the oxidative stabilization of mesophase pitch fibers. The specific process is as follows:

[0019] (1) The mesophase pitch fibers are soaked and dissolved in toluene solution at 60°C for 120 minutes, the amount of toluene is 60 times the mass of the mesophase pitch fibers, and 10vol.% of the amount of 25% concentration of hydrogen peroxide is added for activation;

[0020] (2) Take out the mesophase pitch fiber obtained in (1) with a filter screen, then wash it with deionized water for 3 times, just immerse the fiber sample in the amount of water, and then dry it at 50°C for 12 hours;

[0021] (3) The mesophase pitch fibers obtained in (2) were oxidized at 260° C. for 4 hours by air to obtain infusible mesophase pitch fibers.

[0022] Compared with the traditional gas-phase oxidation process, the non-melting time of the mesophase pitch fibers in this example can be shortened by 1 to 2 hours; the non-melting mesophase pitch fibers obtained in ...

Embodiment 2

[0024] A method for accelerating the oxidative stabilization of mesophase pitch fibers. The specific process is as follows:

[0025] (1) Soak and dissolve the mesophase pitch fiber with pyridine solution at 50° C. for 80 minutes, the amount of pyridine is 30 times the mass of the mesophase pitch fiber, and add 12% hydrogen peroxide in an amount of 8 vol.% to activate;

[0026] (2) Take out the mesophase pitch fiber obtained in (1) with a filter screen, then wash it with deionized water for 3 times, just immerse the fiber sample in the amount of water, and then dry it at 50°C for 12 hours;

[0027] (3) Oxidize the mesophase pitch fiber obtained in (2) at 315° C. for 3 h with air to obtain an infusible mesophase pitch fiber.

[0028] Compared with the traditional gas-phase oxidation process, the non-melting time of the mesophase pitch fibers in this example can be shortened by 2 to 3 hours; the non-melting mesophase pitch fibers obtained in this example are carbonized at 1000 °...

Embodiment 3

[0030] A method for accelerating the oxidative stabilization of mesophase pitch fibers. The specific process is as follows:

[0031] (1) Soak and dissolve the mesophase pitch fiber with quinoline solution for 30min at 40°C, the amount of quinoline is 25 times of the quality of the mesophase pitch fiber, and add 3vol.% of 10% concentration of hydrogen peroxide for activation;

[0032] (2) Take out the mesophase pitch fiber obtained in (1) with a filter screen, then wash it with deionized water for 3 times, just immerse the fiber sample in the amount of water, and then dry it at 50°C for 12 hours;

[0033] (3) Oxidize the mesophase pitch fibers obtained in (2) at 345° C. for 1 h with air to obtain infusible mesophase pitch fibers.

[0034] Compared with the traditional gas-phase oxidation process, the non-melting time of the mesophase pitch fibers in this example can be shortened by 3 to 4 hours; the non-melting mesophase pitch fibers obtained in this example are carbonized at ...

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PUM

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Abstract

The invention relates to a method for accelerating oxidation stabilization of a mesophase pitch fiber. The method comprises the steps as follows: 1) immersing and dissolving the mesophase pitch fiberin an organic solvent at a low temperature, and adding hydrogen peroxide for activation; 2) removing the mesophase pitch fiber obtained in the step 1) by a filter screen, then washing with deionized water 3 times, and then drying at 50 DEG C for 12 hours; 3) subjecting the mesophase pitch fiber obtained in the step 2) to oxidation stabilization by air to obtain the oxidation stabilized mesophase pitch fiber. By adopting the method, the stabilizing time of the mesophase pitch fiber is shortened, and the production cost of a mesophase pitch-based carbon fiber is significantly reduced.

Description

technical field [0001] The invention belongs to the technical field of mesophase pitch-based carbon fibers, and in particular relates to a method for accelerating the oxidation stabilization of mesophase pitch fibers. Background technique [0002] Mesophase pitch-based carbon fibers are prepared from spinnable mesophase pitch raw materials through hot-melt spinning, oxidation stabilization, high-temperature carbonization and graphitization processes. Oxidative stabilization refers to the use of oxidants (such as air) to carry out chemical crosslinking reactions on mesophase asphalt macromolecules to make them insoluble (solubilized) and non-melted (melted) to complete the transformation from thermoplastic to thermosetting, so as to maintain the fiber shape and internal structure. Oxidative stabilization is an important process in the production of mesophase pitch-based carbon fibers (polyacrylonitrile-based carbon fibers are no exception), and has an important impact on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/14
CPCD01F9/145
Inventor 袁观明颜凤崔正威董志军李轩科丛野张江李艳军朱辉
Owner WUHAN UNIV OF SCI & TECH
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