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Prepn of polyacrylonitrile-base high-performance raw carbon fiber

A polyacrylonitrile-based, high-performance technology, applied in fiber chemical characteristics, textiles and papermaking, etc., can solve the problem of uneven heating of filaments, affecting the uniformity of the microstructure of the original silk, and the increase in the coefficient of variation of the mechanical properties of the original silk, etc. problem, achieve the effect of avoiding uneven heating, reducing the probability of occurrence, and reducing the solvent content

Inactive Publication Date: 2003-05-14
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of such a process can easily lead to uneven heating of the filaments, thereby affecting the uniformity of the microstructure of the precursor filaments, which in turn leads to an increase in the coefficient of variation of the mechanical properties of the precursor filaments

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Preparation of spinning dope

[0024] Acrylonitrile, itaconic acid, and methyl methacrylate are blended at a weight ratio of 96:1:3 and then added to the reactor. Using dimethyl sulfoxide as a solvent, the temperature of the polymerization reaction is controlled at 75°C. The reaction time is 10 hours, and the PAN resin with a molecular weight of 140,000 and a molecular weight distribution of 3.5 is obtained by continuous polymerization, and the weight content of the PAN resin in the spinning dope is 20%.

[0025] 2. Filtration of silk stock solution The spinning stock solution is precisely filtered through a 5 μm filter material.

[0026] 3. The solidification of the silk stock solution is spun by dry-jet wet spinning. After the fiber leaves the spinneret hole, it enters the first-stage coagulation bath. The temperature of the first-stage coagulation bath is 0°C. The content of dimethyl sulfoxide in the coagulation bath It is 45wt%, and coagulation time is 2min. Aft...

Embodiment 2

[0037] 1. Preparation of silk stock solution

[0038]Acrylonitrile, itaconic acid, and methyl methacrylate are blended in a weight ratio of 92:2:6 and added to the reactor. By solution polymerization, using dimethyl sulfoxide as a solvent, the temperature of the polymerization reaction is controlled at 70°C. The reaction time is 20 hours, and the PAN resin with a molecular weight of 200,000 and a molecular weight distribution of 3.0 is obtained by continuous polymerization, and the weight content of the PAN resin in the silk stock solution is 23%.

[0039] 2. Filtration of spinning dope

[0040] The spinning dope is finely filtered through a 2.0μm filter material.

[0041] 3. Solidification and molding of the original solution

[0042] Adopt dry-jet wet-spinning method spinning, after fiber leaves spinneret orifice, enters first-stage coagulation bath, and first-stage coagulation bath temperature is 20 ℃, and the content of dimethyl sulfoxide in the coagulation bath is 65wt...

Embodiment 3

[0062] 1. Preparation of spinning dope

[0063] Acrylonitrile, itaconic acid, and methyl methacrylate are blended at a weight ratio of 93.5:0.7:4.8 and added to the reactor. By solution polymerization, using dimethyl sulfoxide as a solvent, the temperature of the polymerization reaction is controlled at 60°C. The reaction time was 40 hours, and the PAN resin with a molecular weight of 180,000 and a molecular weight distribution of 2.5 was obtained by continuous polymerization. The weight content of PAN resin in the spinning dope is 18%.

[0064] 2. Filtration of spinning dope

[0065] The spinning dope is finely filtered through a 3μm filter material.

[0066] 3. The solidification of the spinning stock solution is spun by dry-jet wet spinning. After the fiber leaves the spinneret hole, it enters the first-stage coagulation bath. The temperature of the first-stage coagulation bath is 10°C. The content is 50wt%, and the coagulation time is 1.5min. After the coagulated filam...

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Abstract

The present invention relates to the preparation of high-performance polyacrylonitrile-based carbon fiber. Acrylonitrile, itaconic acid and methyl methacrylate in a certain weight proportion are reacted to obtain spinning dope, and the spinning dope is made into greign fiber of high-performance carbon fiber through filtering, solidification, water washing, drafting in hot water, oiling, drying and densifying, re-oiling, drying and densifying for the second time, steam drafting and drying setting. The present invention has the advantages of high drafting rate, homogeneous fibre structure, and small mechanical performance variation coefficient.

Description

[0001] Field: The invention belongs to a method for preparing fiber precursors, in particular to a method for preparing polyacrylonitrile-based high-performance carbon fiber precursors. Background technique: [0002] In the usual polyacrylonitrile raw silk spinning process, filter cloth of about 400 mesh and ordinary absorbent cotton are generally used to filter the spinning stock solution. Although such a filtration method can filter out the impurity particles in the stock solution, it is powerless for the gel particles below 5 μm, and if these gel particles are not removed, they will cause tiny defects in the original silk, thus affecting the performance of the original silk . [0003] The coagulation bath process is the most important process step that affects the properties of the precursor. Among them, the temperature and concentration of the coagulation bath are two important process parameters. Increasing the concentration of the coagulation bath and reducing the temp...

Claims

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Application Information

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IPC IPC(8): D01F9/22
Inventor 凌立成梁晓怿贺福杨永岗吕永根
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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