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Mesophase pitch material for preparing high-performance carbon fibers and preparation method of mesophase pitch material

A mesophase pitch and carbon fiber technology, applied in fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of molecular weight distribution measurement and monitoring difficulties, catalyst recovery and recycling, and increased carbon fiber manufacturing costs, etc., to ensure long-term continuous Stable operation, conducive to industrial operation, and beneficial to the effect of control

Inactive Publication Date: 2014-12-10
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solid catalysts such as aluminum trichloride and alumina are difficult to separate from the reaction system, so there is a disadvantage that the catalyst is difficult to recycle and reuse. This not only increases the cost of carbon fiber manufacturing, but the more fatal disadvantage is that even if only a small amount remains in the pitch fiber The catalyst will also lead to a serious decrease in fiber strength in the subsequent pre-oxidation, carbonization, and graphitization projects
Therefore, it brings many difficulties to the measurement and monitoring of molecular weight distribution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:1:0.2, react at 300°C for 60 minutes, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them for use. Then, the temperature of the reactor was raised to 450° C., and nitrogen gas was continuously flowed in for 1 hour to remove low-boiling point products, and the temperature was lowered to obtain mesophase pitch. The mesophase content of the asphalt is 100% as measured by polarizing microscopy, the softening point is 250°C as measured by capillary rheometer, and the temperature difference between the flow point and softening point is 25°C. The mesophase pitch was melt-spun at 325° C., the spinning performance was good, there was no broken filament, and the process operation was stable. The obtained pitch fibers are pre-oxidized in an air atmosphere at a heating rate of 3 °C / min to 275 °C; then carbonized in a nitrogen atmosphere at a heatin...

Embodiment 2

[0032] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:0.60:0.2, and react at 250° C. for 4 hours, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them. Then, the temperature of the reactor was raised to 350° C., nitrogen gas was continuously fed for 20 hours to remove low-boiling point products, and the temperature was lowered to obtain mesophase pitch. The mesophase content of the asphalt is 100% measured by polarizing microscope, the softening point is 224°C measured by capillary rheometer, and the temperature difference between flow point and softening point is 21°C. The mesophase pitch was melt-spun at 298° C., the spinning performance was good, there was no broken filament, and the process operation was stable. The obtained pitch fibers are pre-oxidized in an air atmosphere at a heating rate of 3 °C / min to 275 °C; then carbonized in a nitrogen atmosphere at a heating rate of 10 °C / min ...

Embodiment 3

[0034] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:15:0.2, react at 280°C for 2 hours, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them for use. Then, the temperature of the reactor was raised to 360° C., nitrogen gas was continuously fed for 12 hours to remove low-boiling point products, and the temperature was lowered to obtain mesophase pitch. The mesophase content of the asphalt is 100% measured by polarizing microscope, the softening point is 241°C measured by capillary rheometer, and the temperature difference between flow point and softening point is 22°C. The mesophase pitch was melt-spun at 316° C., the spinning performance was good, there was no broken filament, and the process operation was stable. The obtained pitch fibers are pre-oxidized in an air atmosphere at a heating rate of 3 °C / min to 275 °C; then carbonized in a nitrogen atmosphere at a heating rate of 10 °C / min ...

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Abstract

The invention relates to a mesophase pitch material for preparing high-performance carbon fibers and a preparation method of the mesophase pitch material. Measured by use of a polarizing microscope, the mesophase content of the mesophase pitch material is 100%; measured by use of a capillary rheometer, the softening point of the mesophase pitch material is 190-270 DEG C and the temperature difference between the flow point and the softening point of the mesophase pitch material is lower than 28 DEG C. The mesophase pitch material is prepared from naphthalene compounds such as methylnaphthalene in the presence of a hydrogen fluoride-boron trifluoride as a catalyst under the control of polymerization conditions and low-boiling point product separation conditions. Compared with the prior art, the mesophase pitch material has the characteristics of excellent spinnability, narrow molecular weight distribution, and good orientation property depending on good melt fluidity, and is advantageous for the control and the operations of a spinning process and also advantageous for preparing the high-performance pitch-based carbon fibers.

Description

technical field [0001] The invention relates to the field of carbon industry, in particular to a mesophase pitch raw material required for the manufacture of high-strength and high-modulus high-performance pitch-based carbon fibers and a preparation method. Background technique [0002] High-performance carbon fiber is light, has high strength and high elastic modulus, and plays a huge role as a high-value material in the fields of defense industry, aerospace, cutting-edge technology, pillar industry, and daily life. The demand for high-performance carbon fiber is increasing. The rate of greater than 10% has increased significantly year by year. [0003] According to the classification of raw materials used, carbon fiber can be divided into polyacrylonitrile-based (PAN) carbon fiber, pitch-based carbon fiber and viscose-based carbon fiber. At present, carbon fiber products are mainly the first two types, of which PAN-based carbon fiber accounts for about 70% and pitch-based...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/145
Inventor 杨斌王新灵刘媛袁角亮张媛媛
Owner SHANGHAI JIAO TONG UNIV
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