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Method for preparing polyacrylonitrile carbon fiber protofilament by dry and wet methods

A technology of polyacrylonitrile carbon fiber, dry and wet method, applied in the direction of fiber treatment, fiber chemical characteristics, single-component synthetic polymer rayon, etc., can solve problems such as difficult to ensure uniformity, and achieve stable spinning process and wool The effect of less, less gel content

Inactive Publication Date: 2012-12-12
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the patent CN02130023.2 adopts the method of feeding ammonia into the reaction system after polymerization to improve the hydrophilicity of the spinning solution, but for the polymer solution with high viscosity, it is difficult to ensure the homogeneity of this gas-solid phase reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Copolymerize 10kg of acrylonitrile, 0.2kg of itaconic acid, 0.4kg of methyl acrylate, 0.07kg of azobisisoheptanonitrile and 36kg of dimethyl sulfoxide at 50°C to obtain a binary copolymer with a viscosity average molecular weight of 17 Ten thousand, the molecular weight distribution is 2.3. After the polymer is degassed by a defoaming tank with a vacuum degree of -95KPa to remove air bubbles, residual monomers and part of the solvent, the spinning stock solution with a temperature of 55°C and a solid content of 20.5% is obtained, and passed through a 2-stage candle wick filter Filtration and metering pump metering, using a 1000-hole spinneret with a nozzle size of Φ0.15mm for dry-jet wet spinning, the air layer height is 5mm, the temperature of the sprayed stream is 0°C, and the concentration of DMSO is 55% by weight %, solidify and form in an aqueous solution of dimethyl sulfoxide containing 0.1% by mass of ammonia water with a concentration of 17% by mass, and at the ...

Embodiment 2

[0050] 10.5kg of acrylonitrile, 0.3kg of itaconic acid, 0.4kg of methyl acrylate, 0.065kg of azobisisoheptanonitrile and 36kg of dimethyl sulfoxide were copolymerized at 50°C, and the obtained binary copolymer had a viscosity-average molecular weight of 220,000, the molecular weight distribution is 2.2. After the polymer is degassed by a defoaming tank with a vacuum degree of -95KPa to remove air bubbles, residual monomers and part of the solvent, the spinning stock solution with a temperature of 55°C and a solid content of 21.5% is obtained, and passed through a 2-stage candle wick filter Filtration and metering pump metering, using a 1000-hole spinneret with a nozzle size of Φ0.15mm for dry-jet wet spinning, the air layer height is 7mm, the temperature of the jet stream is 10°C, and the DMSO concentration is 60 wt. %, solidify and form in an aqueous solution of dimethyl sulfoxide containing 0.05% by weight of ammonia water with a concentration of 20% by mass, and at the same...

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Abstract

The invention discloses a method for preparing polyacrylonitrile carbon fiber protofilament by dry and wet methods. The method comprises the steps of polymerization, demonomerization and defoaming, filtration, coagulation, washing and drafting, oiling densification, steam drafting, heat setting and drying. Three-level coagulating baths at the temperature of between 10 DEG C below zero and 70 DEG C and with dimethyl sulfoxide with concentration of 10 to 60 mass percent are adopted in the coagulation step, and the first coagulating bath contains aqueous ammonia accounting for 0.05 to 1 percent of the mass of the first coagulating bath; and a spinning head is subjected to 1.5 to 5 times positive drafting in the first coagulating bath, and the drafting is 0 in the second and third coagulatingbathes. According to the method for preparing the polyacrylonitrile carbon fiber protofilament, the spinning process is stable, the broken filament is little, the spinning speed is high, the spinningis stable, the prepared protofilament has few defects, the density is not less than 1.180g / cm<3>, and the tensile strength is not less than 7cN / dtex. The protofilament can be prepared into a high-performance carbon fiber with tensile strength of more than 4.9GPa and elastic modulus of between 260 and 280GPa by high-temperature carbonization.

Description

technical field [0001] The invention relates to the field of polyacrylonitrile fiber preparation, in particular to a method for preparing polyacrylonitrile carbon fiber precursors by a dry-wet method. Background technique [0002] Carbon fiber has the advantages of high specific strength, high specific modulus, high temperature resistance, creep resistance, and certain electrical conductivity. It has been widely used in various fields such as aerospace, transportation, medical equipment, sports, and new energy. [0003] High-quality raw silk is a prerequisite for the preparation of high-performance carbon fibers, which has been recognized by the industry. The production of polyacrylonitrile precursors prepared by the wet spinning process widely used at present is low, and there are many grooves and other defects on the surface of the fibers due to the solidification method, which seriously restricts the further improvement of the performance of carbon fibers, so the spinning...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F11/06D01F9/22D01D5/00D01D10/02D01D10/06C08F220/46
Inventor 马雷辛伟黄险波宋威曾祥斌叶丹滢蔡彤旻
Owner KINGFA SCI & TECH CO LTD
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