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Coarse-denier high-strength medium-modulus polyacrylonitrile-based carbon fiber and preparation method thereof

A polyacrylonitrile-based carbon fiber and polyacrylonitrile spinning technology, which is applied in the fiber field, can solve the problems of difficult preparation of highly crystalline and oriented polyacrylonitrile precursors, limited crystallization, drafting and orientation, and difficult control of fiber surface defects. Achieve the effects of reducing fiber surface defects, reducing radial skin-core structure differences, and slowing down curing

Active Publication Date: 2021-06-01
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bottleneck in improving the strength of coarse denier fibers lies in the difficulty of controlling fiber surface defects and the difficulty in improving tensile properties
[0004] For the preparation of polyacrylonitrile fibers, the currently widely used methods are only wet spinning and dry spray wet spinning. The surface of the fiber rapidly forms a cortex structure due to the double diffusion behavior of the water phase system in the primary coagulation bath and the rapid solidification mechanism. It restricts its crystallization, drawing and orientation, and it is difficult to prepare polyacrylonitrile precursors with extremely low surface defects and high crystal orientation, which limits the mechanical properties of carbon fibers, especially the further improvement of Young's modulus

Method used

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  • Coarse-denier high-strength medium-modulus polyacrylonitrile-based carbon fiber and preparation method thereof
  • Coarse-denier high-strength medium-modulus polyacrylonitrile-based carbon fiber and preparation method thereof
  • Coarse-denier high-strength medium-modulus polyacrylonitrile-based carbon fiber and preparation method thereof

Examples

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preparation example Construction

[0037] A preparation method of polyacrylonitrile-based carbon fiber, such as figure 1 shown, including the following steps:

[0038] S1: Prepare polyacrylonitrile spinning dope by mixing polyacrylonitrile powder with organic solvent;

[0039] S2: Extrude the polyacrylonitrile spinning stock solution through the spinneret hole, enter the non-aqueous solvent gel bath with a temperature of 0°C to -50°C, and then draw it to obtain the primary fiber;

[0040] S3: extracting the primary fiber, washing it with water, hot drawing at 40-95°C, drying and densifying, and oiling, to prepare the original silk;

[0041] S4: Pre-oxidize the obtained raw silk, carbonize at 500°C to 800°C, carbonize at 1100°C to 1600°C, electrochemically treat, wash with water, sizing, and dry and wind up.

Embodiment 1

[0043] (1) Preparation of polyacrylonitrile-methyl acrylate PAN-MA powder:

[0044] Using acrylonitrile (AN) as raw material, add methyl acrylate (MA) with a mass ratio of 96:4, add 20wt% of the total mass percentage into the water phase polymerization reactor, and use 0.3mol% water system oxidation-reduction initiation agent (ammonium persulfate-ammonium bisulfite) was polymerized at 40°C for 6 hours at a constant temperature, and the formed slurry was filtered, washed twice, and dried with hot air at 90°C until the water content was lower than 5wt%, and polyacrylonitrile-methyl acrylate PAN was obtained. - MA powder.

[0045] (2) Preparation of polyacrylonitrile spinning dope:

[0046] The polyacrylonitrile-methyl acrylate PAN-MA (3.4wt%) powder with a molecular weight of 150,000 was mechanically ground to below 100 mesh, mixed with DMSO at 19°C and mechanically stirred (speed 800rpm) to prepare a solid content of 20.5 The wt% dispersion liquid is vacuumed to 40KPa, slowly...

Embodiment 2

[0058] This embodiment is basically the same as Embodiment 1, the difference is:

[0059] (1) Preparation of polyacrylonitrile-itaconic acid PAN-IA powder

[0060] Acrylonitrile (AN) is used as raw material, and itaconic acid (IA) is added with a mass ratio of 98:2.

[0061] (2) Preparation of polyacrylonitrile spinning dope:

[0062] The polyacrylonitrile-itaconic acid PAN-IA (1.8wt%) powder with a molecular weight of 150,000 was mixed with DMF, and a dispersion liquid with a solid content of 24wt% was prepared by the same method as in Example 1, and the subsequent steps were the same as those in Example 1. 1, the polyacrylonitrile PAN spinning stock solution was obtained, and the viscosity of the polyacrylonitrile PAN spinning stock solution at room temperature was 112 Pa.s.

[0063] (3) Preparation of primary fibers

[0064] During the spinning process, the temperature of the polyacrylonitrile PAN spinning stock solution is kept at 50 °C, and it is transported to the met...

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Abstract

The invention relates to the technical field of fibers, in particular to a coarse-denier high-strength medium-modulus polyacrylonitrile-based carbon fiber and a preparation method thereof. The preparation method of the polyacrylonitrile-based carbon fiber comprises the following steps: S1, preparing a polyacrylonitrile spinning solution from polyacrylonitrile powder and dimethyl sulfoxide; S2, extruding the polyacrylonitrile spinning solution through spinneret orifices, passing through an air layer and entering a non-aqueous solvent gel bath with the temperature ranging from 0 DEG C to -50 DEG C to be positively drafted, and thus obtaining a nascent fiber; S3, extracting the nascent fiber, washing with water, then carrying out hot drafting, drying and densifying, and oiling to prepare a protofilament; and S4, pre-oxidizing the obtained protofilament, carbonizing at the low temperature of 500-800 DEG C, carbonizing at the high temperature of 1100-1600 DEG C, carrying out electrochemical treatment, washing with water, sizing, drying and rolling. According to the method, the coarse-denier high-strength medium-modulus carbon fiber based on dry-jet gel spinning is obtained, and the method meets the application requirements of composite materials in the fields of aviation, aerospace and the like.

Description

technical field [0001] The invention relates to the field of fiber technology, in particular to a coarse-denier high-strength medium-mode polyacrylonitrile-based carbon fiber and a preparation method thereof. Background technique [0002] Polyacrylonitrile is currently the only and most widely used precursor for preparing high-performance carbon fibers. Using polyacrylonitrile (PAN) with one or more comonomers, different specifications of carbon fibers can be prepared by dissolution, spinning, thermal oxidation, carbonization, and graphitization. Due to its low density and high mechanical properties, carbon fiber is widely used in aviation, aerospace, industry, sports equipment and other fields, and is an important structural reinforcement material. [0003] At present, the T300 and T700 grade coarse denier (7μm diameter) carbon fiber products on the market belong to the series of medium strength (≤5GPa) and low modulus (≤260GPa), while the T800 grade carbon fiber belongs t...

Claims

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Application Information

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IPC IPC(8): D01F9/22D01F11/14D01F11/12D01D5/00
CPCD01F9/225D01F11/14D01F11/12D01D5/00
Inventor 刘耀东吕春祥安锋周普查于毓秀滕娜
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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