A preparation method of polyacrylonitrile carbon fiber with uniform distribution of copolymerization sequences

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

Active Publication Date: 2018-03-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Organic solvent polymerization systems have problems such as large viscosity changes, poor mixing uniformity, and concentrated reaction heat

Method used

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  • A preparation method of polyacrylonitrile carbon fiber with uniform distribution of copolymerization sequences
  • A preparation method of polyacrylonitrile carbon fiber with uniform distribution of copolymerization sequences
  • A preparation method of polyacrylonitrile carbon fiber with uniform distribution of copolymerization sequences

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Experimental program
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Effect test

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 method for preparing polyacrylonitrile carbon fibers with uniform distribution of copolymerization sequences, comprising: determining the number N of cascaded reactors; determining the feed ratio of the third comonomer in different zones; using water as a medium to carry out precipitation polymerization and drying to obtain polypropylene Nitrile powder; then dissolved to prepare spinning stock solution, after removing air bubbles and filtering, spinning, solidification and forming into primary fibers, washing and post-treatment to make polyacrylonitrile-based carbon fiber precursors; finally pre-oxidation, carbonization and post-treatment Process made of high-performance carbon fiber. The invention adopts a multi-stage series-connected stirred tank type polymerization reactor, and obtains a PAN copolymer with uniform distribution of copolymerization sequences through the strategy of supplementing the third comonomer partitions in proportion. The better the distribution uniformity of the copolymerization sequence of the polyacrylonitrile precursor, the greater the degree of avoidance of the fiber "skin-core" structure during the pre-oxidation process, which is conducive to the diffusion of oxygen in the radial direction of the fiber, maintaining the smooth progress of the pre-oxidation reaction and heat dissipation control, and finally produce carbon fibers with 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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Patent Type & Authority Patents(China)
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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