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Method for preparing carbon fiber precursor by employing sodium thiocyanate through dry and wet spinning process

A carbon fiber precursor, dry-wet spinning technology, applied in the direction of spinning solution preparation, fiber chemical characteristics, textiles and papermaking, etc., can solve the problem that it is difficult to meet the requirements of high concentration and high viscosity of spinning stock solution, low viscosity of stock solution , low solvency and other problems, to achieve the effect of high quality, high strength, and small dispersion of the original silk

Active Publication Date: 2016-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solubility of sodium thiocyanate aqueous solution is lower than that of organic solvents such as DMSO, DMF, and DMAc, and the viscosity of the stock solution is low, so it has a tendency to separate out gel at a lower composition content, and the concentration (solid content) of the spinning stock solution is generally between Between 12wt% and 13wt%, it is difficult to meet the requirements of high concentration and high viscosity of dry and wet spinning dope

Method used

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  • Method for preparing carbon fiber precursor by employing sodium thiocyanate through dry and wet spinning process
  • Method for preparing carbon fiber precursor by employing sodium thiocyanate through dry and wet spinning process
  • Method for preparing carbon fiber precursor by employing sodium thiocyanate through dry and wet spinning process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~8

[0028] With 51.5wt% aqueous sodium thiocyanate as solvent, the polymerized monomers include acrylonitrile (AN), the second monomer methyl acrylate (MA) and the third monomer itaconic acid (ITA). The feed mass ratio is 97:2:1. In the system, azobisisobutyronitrile is used as the initiator, and the addition amount is 0.25wt% of the total mass of polymerized monomers. Isopropanol is used as a molecular weight regulator, and the added amount is 4.5 wt% of the total mass of polymerized monomers. With thiourea dioxide as the light coloring agent, the addition amount is 0.3wt% of the total mass of polymerized monomers. The above mixture is polymerized at 78-80°C, and the reaction time is 2 hours. The obtained polymerization stock solution enters the vacuum falling-film type high-efficiency single-removal column for single removal. The crude stock solution after single removal is preheated After reaching 80°C, the order was removed for the second time. The original liquid after the ...

Embodiment 9~16

[0043] The spinning dope of Examples 1 to 8 were respectively spun, and the specific steps were as follows:

[0044] (1) The stock solution obtained in Examples 1 to 8 was adjusted in temperature and pressure, and supplied to the spinning assembly in the heat preservation for extrusion spinning. The adjusted temperature was 10-50℃, the pressure was 1.0-2.0MPa, and the spinning The heat preservation temperature of the components is the same as the temperature of the spinning dope, which is 10~50℃;

[0045] (2) The spinning dope is extruded from the spinneret, passes through an air layer of about 1-10 mm, and then enters into a NaSCN aqueous solution with a concentration of 0-10% by weight and a temperature of 0-10°C to solidify and form. The thin stream of raw liquid extruded from the spinneret is stretched 0.2-1.1 times in the air layer;

[0046] (3) The thread from the coagulation bath is air drawn, washed with water, drawn in boiling water, oiled, densified, steam drawn, dried, an...

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Abstract

The invention discloses a method for preparing carbon fiber precursor by employing sodium thiocyanate through a dry and wet spinning process. The method comprises the following steps: taking a sodium sulfocyanate aqueous solution as a solvent for polymerization to obtain a polymerization stock solution, passing the polymerization stock solution through a first demonomerization tower for removing an unreacted monomer in the polymerization stock solution, then preheating the material to the temperature of 75-85 DEG C and introducing the material into a second demonomerization tower, and wherein content of a residual monomer is controlled at less than or equal to 0.1%, preheating the demonomerized polymerization stock solution to the temperature of 70-95 DEG C, defoaming the polymerization stock solution under a pressure reduction state and then dehydrating, then performing multistage cyclic preheating, defoaming and dehydrating to obtain the high-density (high solid content) spinning stock solution which satisfies the dry and wet spinning requirements, and spinning to obtain the carbon fiber precursor. The method is simple, the obtained carbon fiber precursor has good wire drawing capability, nozzle stretching is stable, breakage rate is little, precursor dispersion is little, and intensity is high.

Description

Technical field [0001] The invention relates to a method for preparing a carbon fiber precursor by a polyacrylonitrile-based carbon fiber dry-wet spinning process, in particular to a method for preparing a polyacrylonitrile-based carbon fiber precursor by adopting a sodium thiocyanate aqueous solution dry-wet spinning process. Background technique [0002] The most commonly used spinning method of PAN precursor is wet spinning. With the continuous expansion of the application field of carbon fiber, the production cost and performance requirements of carbon fiber are getting higher and higher. The dry and wet raw yarn has less surface and internal defects, high density, easy to control cross section, and has a high-power spinneret. Stretching and high spinning speed (5-10 times that of wet spinning) are very beneficial to high-strength carbon fibers and greatly reducing production costs. It is the current development direction of carbon fiber precursor production. [0003] Dry-wet ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01D1/02C08F220/46C08F220/14C08F222/02C08F2/10C08F6/10
Inventor 顾文兰袁玉红夏永辉冯林明
Owner CHINA PETROLEUM & CHEM CORP
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