Preparation method of polyacrylonitrile carbon fiber with evenly distributed copolymerization sequence

A polyacrylonitrile carbon fiber, uniform distribution technology, applied in the direction of spinning solution preparation, fiber chemical characteristics, wet spinning method, etc., can solve the problems of large viscosity changes, poor mixing uniformity, concentrated reaction heat, etc.

Active Publication Date: 2015-02-25
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Organic solvent polymerization systems have problems such as large ...

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  • Preparation method of polyacrylonitrile carbon fiber with evenly distributed copolymerization sequence
  • Preparation method of polyacrylonitrile carbon fiber with evenly distributed copolymerization sequence
  • Preparation method of polyacrylonitrile carbon fiber with evenly distributed copolymerization sequence

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Embodiment 1～13

[0061] 1) Acrylonitrile is used as the first comonomer, the second and third comonomers are methyl methacrylate and itaconic acid respectively, and the weight ratio of acrylonitrile and methyl methacrylate is 97:3. The concentration of the total monomer of the material is 22.5wt%, the oxidizing agent is sodium chlorate, and the reducing agent is sodium pyrosulfite. In terms of the total amount of all polymerization monomers charged, the initiator consumption is 0.37% (wherein the mol ratio between the reducing agent and the oxidizing agent is 1.5:1), the reaction temperature is controlled at 53.5°C for copolymerization reaction, the reaction residence time in each series tank is 15-40min, the total reaction time is controlled at 1.0-3.0 hours, the feeding of the third comonomer itaconic acid solution See Table 1 for the ratio and partition ratio, and see Table 1 for the number of series tanks in the polymerization reactor. The polymer overflowed from the last tank passes throu...

Embodiment 14～26

[0080] 1) Acrylonitrile is used as the first comonomer, the second and third comonomers are ethyl acrylate and itaconic acid respectively, the weight ratio of acrylonitrile and ethyl acrylate is 97:3, and the total monomers fed The concentration of the oxidizing agent is 25wt%, the oxidant is sodium chlorate, and the reducing agent is sodium pyrosulfite. The amount of the initiator is 0.40% (wherein the molar ratio between the reducing agent and the oxidizing agent is 1.5:1) based on the total amount of all polymerized monomers charged. Control the reaction temperature to 54.0°C for the copolymerization reaction, the reaction residence time in each series tank is 15-40min, and the total reaction time is controlled to be 1.0-3.0 hours. For the feeding ratio and partition ratio of the third comonomer itaconic acid solution, see Table 4, the number of tanks in series in the polymerization reactor is shown in Table 4; the polymer overflowed from the last tank passes through the con...

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Abstract

The invention relates to a preparation method of a polyacrylonitrile carbon fiber with an evenly distributed copolymerization sequence. The preparation method comprises the following steps: determining the number of serially connected reactors; determining the ratio of fed materials of different areas in the third co-monomer zone; carrying out precipitation polymerization by taking water as the medium, drying so as to obtain polyacrylonitrile powder; dissolving the polyacrylonitrile powder to prepare a spinning solution, removing the bubbles from the solution, filtering, spraying, and curing to form primary fibers, washing and subjecting the primary fibers to a post treatment so as to obtain polyacrylonitrile-based carbon precursor fibers; and finally subjecting the precursor fibers to pre-oxidation, carbonation, and a post treatment so as to obtain the high performance carbon fiber. The preparation method adopts multi-grade serially-connected stirred tank polymerization reactors, and raw materials are supplemented in the third co-monomer zone according to a certain ratio in different areas so as to obtain a PAN copolymer with evenly distributed copolymerization sequence. Because the distribution uniformity of the copolymerization sequence of polyacrylonitrile precursor fibers is high, the possibility that fibers with a shell-core structure appear during the pre-oxidation process is small. Moreover, the diffusion of oxygen gas in the radical direction of fibers is also promoted, thus the pre-oxidation reactions can be stably carried out and the heat dissipation can be controlled so as to obtain carbon fiber with an excellent performance.

Description

technical field [0001] The present invention relates to a preparation method of polyacrylonitrile carbon fiber with uniform distribution of copolymerization sequence, in particular to polyacrylonitrile resin prepared by aqueous phase precipitation polymerization process as spinning raw material, and polyacrylonitrile with uniform sequence distribution produced by solution spinning process Raw silk, and then obtain the preparation method of polyacrylonitrile high-performance carbon fiber through suitable pre-oxidation, carbonization and post-treatment process. Background technique [0002] The R&D and industrialization of polyacrylonitrile-based carbon fibers, including polymerization, spinning, pre-oxidation, carbonization and post-treatment, etc., is a system engineering involving multiple complex processes and highly interrelated. How to control the molecular structure of polyacrylonitrile through the polymerization process is a prerequisite for the preparation of high-per...

Claims

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Application Information

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IPC IPC(8): D01F9/22C08F220/44C08F2/10C08F2/01C08F4/40D01D1/02D01D5/06D01D10/02
Inventor 宋文迪顾文兰夏永辉吴嵩义季春晓冯林明张捷
Owner CHINA PETROLEUM & CHEM CORP
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