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Mesophase pitch raw material as well as preparation method and application of mesophase pitch raw material in preparing high-performance carbon fiber

A mesophase pitch and raw material technology, applied in the chemical characteristics of fibers, chemical processing of tar pitch/petroleum pitch/natural pitch, textiles and papermaking, etc., can solve the problems of increasing carbon fiber manufacturing costs, decreasing fiber strength, and difficulty in recycling catalysts Reuse and other issues to achieve the effect of low cost, simple preparation process, and favorable industrial operation

Inactive Publication Date: 2014-10-08
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
However, there is currently a lack of specific indicators about the molecular structure of mesophase pitch with good preoxidation performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add methylnaphthalene, hydrogen fluoride, and boron trifluoride to the reactor at a molar ratio of 1:0.63:0.24, react at 2.5 MPa and 260°C for 2 hours, release the pressure to atmospheric pressure, and discharge hydrogen fluoride and fluorine triboride in the gas phase , Nitrogen gas is introduced into the reactor to remove the low-boiling point product to obtain the product pitch. The mesophase content of the asphalt measured by polarizing microscopy is 100%, the softening point temperature is 218° C., the H / C is 0.67, and the naphthenic carbon content is 14%. The mesophase pitch was spun at 280°C and 500m / min traction speed, the spinning performance was good, no broken filaments, and the process was stable, and pitch fibers with a diameter of 12.5 μm were obtained. The obtained pitch fibers were pre-oxidized at 230° C. for 30 minutes in an oxygen atmosphere, and then carbonized at 2500° C. in a nitrogen atmosphere to obtain high-performance pitch-based carbon fibers. ...

Embodiment 2

[0031] Add methylnaphthalene, hydrogen fluoride, and boron trifluoride to the reactor in a molar ratio of 1:0.77:0.37, react at 3.1MPa and 270°C for 2 hours, release the pressure to atmospheric pressure, and discharge hydrogen fluoride and fluorine triboride in the gas phase , Nitrogen gas is introduced into the reactor to remove the low-boiling point product to obtain the product pitch. The measured mesophase content of the pitch is 100%, the softening point temperature is 239° C., the H / C is 0.55, and the naphthenic carbon content is 13%. The mesophase pitch was spun at 280°C and 500m / min traction speed, the spinning performance was good, no broken filaments, and the process was stable, and a pitch fiber with a diameter of 12 μm was obtained. The obtained pitch fibers were pre-oxidized at 250° C. in an oxygen atmosphere for 30 minutes, and then carbonized at 2500° C. in a nitrogen atmosphere to obtain high-performance pitch-based carbon fibers. The fiber diameter is 10.4 μm...

Embodiment 3

[0033] Add methylnaphthalene, hydrogen fluoride, and boron trifluoride into the reactor at a molar ratio of 1:0.52:0.20, react at 2.5 MPa and 250°C for 2 hours, release the pressure to atmospheric pressure, and discharge hydrogen fluoride and fluorine triboride in the gas phase , Nitrogen gas is introduced into the reactor to remove the low-boiling point product to obtain the product pitch. The measured mesophase content of the pitch is 100%, the softening point temperature is 203° C., the H / C is 1.0, and the naphthenic carbon content is 9%. The mesophase pitch was spun at 280°C and 500m / min traction speed, the spinning performance was good, no broken filaments, and the process was stable, and pitch fibers with a diameter of 13.5 μm were obtained. The obtained pitch fibers were pre-oxidized at 215°C in an oxygen atmosphere for 30 minutes, and then carbonized at 2500°C in a nitrogen atmosphere to obtain high-performance pitch-based carbon fibers. The fiber diameter is 13 μm, t...

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Abstract

The invention relates to a mesophase pitch raw material as well as a preparation method and an application of the mesophase pitch raw material in preparing a high-performance carbon fiber. By virtue of measurement based on an elemental analysis method for the mesophase pitch raw material, the molar ratio H / C of hydrogen atoms to carbon atoms in the molecular structure of the mesophase pitch raw material is 0.55-1.0; the molar ratio of the naphthenic carbon content to the total carbon content in the molecular structure measured by virtue of a nuclear magnetic resonance method is greater than 9%; the softening point temperature, measured by an insertion method, of the mesophase pitch raw material is 200-240 DEG C; the content, measured by a polarizing microscope method, of the mesophase is 100%. The preparation method comprises the following step: polymerizing naphthalene-based compounds such as methylnaphthalene used as raw materials in the presence of a mixture of hydrogen fluoride and boron trifluoride as a catalyst by virtue of controlling the polymerization conditions. Compared with the prior art, the mesophase pitch raw material has the advantages of good spinning stability and high pre-oxidation activity, and is conductive to the control and operation of the carbon fiber spinning and pre-oxidation processes, the operation process is simple and the mesophase pitch raw material is conducive to preparing a high-performance pitch-based carbon fiber.

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 method for preparing high-performance carbon fibers using the raw materials. 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-...

Claims

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Application Information

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IPC IPC(8): C10C3/02D01F9/145
Inventor 杨斌王新灵刘媛张媛媛宋晨晨
Owner SHANGHAI JIAO TONG UNIV
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