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Prepn. of polyacrylonitrile-base high-performance raw carbon fiber

A polyacrylonitrile-based, high-performance technology, which is applied in the field of preparation of polyacrylonitrile-based high-performance carbon fiber precursors, can solve problems such as increasing the concentration of the coagulation bath, the core-skin structure of the precursor, and the difficulty of large-scale drafting. Achieve the effects of avoiding uneven heating, small coefficient of variation of filaments, and reducing solvent content

Inactive Publication Date: 2004-09-22
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

Among them, the temperature and concentration of the coagulation bath are two important process parameters. Increasing the concentration of the coagulation bath and lowering the temperature of the coagulation bath are conducive to slowing down the double diffusion process of the primary filaments in the coagulation bath to obtain densified coagulation filaments, which is beneficial to The acquisition of high-performance raw silk. Increasing the concentration of the coagulation bath will inevitably lead to a higher solvent content in the coagulated silk, which increases the concentration difference between the coagulated silk and the washing tank, which will easily cause the skin-core structure of the raw silk and destroy the original silk. Homogenization degree of silk
[0005] The usual polyacrylonitrile raw silk spinning process generally adopts a 1-2 stage boiling water drawing process, and the primary filaments are drawn at a high rate of 3 to 4 times in boiling water. However, for high molecular weight and high viscosity spinning dope , it is difficult to carry out large-scale drafting
[0006] The usual polyacrylonitrile raw silk spinning process generally uses a hot air drying oven or an infrared hot plate to dry and densify the fiber after drawing. However, such a process is likely to cause uneven heating of the filaments, thereby affecting the microstructure of the raw silk. Uniformity, which in turn leads to an increase in the coefficient of variation of the mechanical properties of the precursor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Preparation of spinning dope

[0038] Acrylonitrile, itaconic acid, and methyl methacrylate are blended at a weight ratio of 96:1:3 and 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%.

[0039] 2. Filtration of silk stock solution

[0040] The spinning dope is finely filtered through a 5μm filter material.

[0041] 3. Solidification and molding of silk stock solution

[0042] Adopt dry spray wet spinning method spinning, after fiber leaves spinneret hole, enters the coagulation bath of the first stage, and the coagulation bath temperature of the first stage is 0 ℃, and the content of dimethyl sulfoxide in the coagulation bath is 45wt%, and coagulation...

Embodiment 2

[0061] 1. Preparation of silk stock solution

[0062] Acrylonitrile, itaconic acid, and methyl methacrylate are added to the reactor after being blended in a weight ratio of 92:2:6. By solution polymerization, using dimethyl sulfoxide as a solvent, the temperature of the polymerization reaction is controlled at 70 DEG C. The reaction time is 20 hours, continuous polymerization to obtain a PAN resin with a molecular weight of 200,000 and a molecular weight distribution of 3.0, and the weight content of the PAN resin in the silk stock solution is 23%.

[0063] 2. Filtration of spinning dope

[0064] The spinning dope is finely filtered through a 2.0μm filter material.

[0065] 3. Solidification and molding of the original solution

[0066] 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 65w...

Embodiment 3

[0086] 1. Preparation of spinning dope

[0087] Acrylonitrile, itaconic acid, and methyl methacrylate are added to the reactor after being blended at a weight ratio of 93.5: 0.7: 4.8. 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%.

[0088] 2. Filtration of spinning dope

[0089] The spinning dope is finely filtered through a 3μm filter material.

[0090] 3. Solidification and molding of spinning dope

[0091] Adopt dry-jet wet-spinning method spinning, after fiber leaves spinneret orifice, enters first stage coagulation bath, and first stage coagulation bath temperature is 10 ℃, and the content of dimethyl sulfoxide in the coagulation bath is 50wt%, coagula...

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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: [0002] 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: [0003] In the usual polyacrylonitrile raw silk spinning process, a filter cloth of about 400 meshes and ordinary absorbent cotton are generally used to filter the spinning stock solution. Although this filtering method can filter out the impurity particles in the stock solution, it is not suitable for gels below 5 μm The particles are helpless, and these gel particles, if not removed, will cause tiny defects in the precursor, which will affect the performance of the precursor. [0004] 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 lower...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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