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Wet-spinning preparation method for polyacrylonitrile-based carbon fiber precursor

A polyacrylonitrile-based carbon fiber, wet spinning technology, applied in wet spinning, fiber chemical characteristics, textiles and papermaking, etc., to achieve the effects of stabilizing production efficiency, improving fiber separation, and reducing surface defects

Inactive Publication Date: 2016-07-13
ZHONGFU SHENYING CARBON FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention mainly overcomes the need to improve the coagulation and forming conditions of wet spinning in the wet spinning process, and provides a wet spinning method for reducing surface defects of polyacrylonitrile-based carbon fibers through a high-temperature, low-concentration coagulation bath forming method. Silk method, mainly by controlling higher coagulation bath concentration and lower coagulation bath temperature to improve the groove depth and straightness of the surface of polyacrylonitrile-based carbon fiber during coagulation molding, thereby improving the performance of carbon fiber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The temperature of the spinning stock solution of polyacrylonitrile-based carbon fiber precursors (polyacrylonitrile solution with a solid content of 15% and an intrinsic viscosity of 1.5 using dimethyl sulfoxide as a solvent) was controlled at 60°C by heat preservation water, and after 12000 The hole spinneret is extruded into a concentration of 30%, the temperature is 60 ° C, and the pH value is 7.0 in the coagulation bath (the coagulation bath is an aqueous solution of dimethyl sulfoxide), the negative draft is -25%, and the circulation volume (unit root 12K primary fiber) under 1000L / h for wet spinning, after washing, water drawing, oiling, drying, steam drawing, heat setting, and winding processes, the polyacrylonitrile-based carbon fiber precursor is obtained. In the process of the preparation method, there are slightly entangled and broken filaments, and hairy filaments are produced. The stability is general. It is 5.5CN / dtex, and the strength of the fired carbon...

Embodiment 2

[0014] The temperature of the spinning stock solution of polyacrylonitrile-based carbon fiber precursors (polyacrylonitrile solution with a solid content of 20% and an intrinsic viscosity of 1.7 using dimethyl sulfoxide as a solvent) was controlled at 80°C by heat preservation water, and after 12000 The hole spinneret is extruded into a coagulation bath with a concentration of 48%, a temperature of 62°C, and a pH value of 7.5 (the coagulation bath is an aqueous solution of dimethyl sulfoxide), the negative draft is -30%, and the circulation volume (single 12K primary fiber) is wet-spun at 1500L / h, and after washing, water drawing, oiling, drying, steam drawing, heat setting, and winding processes, polyacrylonitrile-based carbon fiber precursors are obtained. In the preparation method process, there are slightly entangled and broken filaments, and hairy filaments are produced, the stability is general, the fineness of the precursor is 1.16dtex, the spinning speed of the polyacry...

Embodiment 3

[0016] The temperature of the spinning stock solution of polyacrylonitrile-based carbon fiber precursors (polyacrylonitrile solution with a solid content of 26% and an intrinsic viscosity of 1.7 using dimethyl sulfoxide as a solvent) was controlled at 65°C by heat preservation water, and after 12000 The hole spinneret is extruded into a concentration of 35%, a temperature of 65°C, and a coagulation bath (the coagulation bath is an aqueous solution of dimethyl sulfoxide) of 8 at a temperature of 65°C. The negative draft is -50%. Root 12K as-spun fiber) is carried out wet spinning under 1800L / h, after washing, water pulling, oiling, drying, steaming pulling, after heat-setting process, obtain polyacrylonitrile-based carbon fiber precursor, in this preparation method During the process, there is a slight phenomenon of entanglement and broken filaments, no hairy filaments are produced, and the stability is good. The fineness of the precursor is 1.16dtex, the spinning speed of polya...

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Abstract

The invention relates to a preparation method of a carbon fiber precursor, and in particular to a wet-spinning preparation method for a polyacrylonitrile-based carbon fiber precursor. The preparation method comprises the following steps: 1) metering a spinning solution of polyacrylonitrile-based carbon fiber by using a metering pump, ejecting from a 12000 spinning nozzle to form fine yarns, and feeding the yarns into a coagulating bath, wherein the coagulating bath is a dimethyl sulfoxide solution of which the temperature is 60-80 DEG C, the concentration is 30-50% and the pH value is 7.0-9.0; 2) performing wet-spinning at minus drafting of minus 80% to minus 25% and coagulating bath circulation volume of 1000-2000L / h, and performing water washing, water holding, oiling, drying, steaming drafting, thermal molding, and winding, thereby obtaining the polyacrylonitrile-based carbon fiber precursor, wherein the final spinning speed is up to 120-150m / min. According to the preparation method, in the wet-spinning process, curing molding conditions of wet-spinning are improved, and a high-temperature and low-concentration coagulating bath molding method is provided, so that surface defects of the polyacrylonitrile-based carbon fiber can be reduced, and the spinning speed of the wet-spinning method can be increased.

Description

technical field [0001] The invention relates to a method for preparing carbon fiber precursors, in particular to a method for preparing polyacrylonitrile-based carbon fiber precursors by wet spinning. Background technique [0002] In the preparation process of polyacrylonitrile-based carbon fiber precursors, coagulation molding is a key link in production, so the molding quality of primary fibers directly affects the comprehensive performance of precursors and carbon filaments. In wet spinning, coagulation forming mainly relies on double diffusion as the forming power, so that the spinning fine flow reaches a critical concentration, coagulation and precipitation to form nascent fibers. This molding method will generate surface grooves. The presence of appropriate surface grooves can improve the fiber splitting between fiber filaments and increase the specific surface area of ​​fibers, which is beneficial to improve the shear strength of composite materials. If the groove is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01D5/06
CPCD01F9/22D01D5/06
Inventor 金亮刘芳夏新强张克勤
Owner ZHONGFU SHENYING CARBON FIBER
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