Asphalt-base carbon fiber prepared by coal directly liquefied residues and preparation method thereof

A pitch-based carbon fiber and coal direct liquefaction technology, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, etc., to achieve the effect of low price and abundant raw material sources

Active Publication Date: 2009-12-02
CHNA ENERGY INVESTMENT CORP LTD +1
2 Cites 57 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0008] The main documents about the utilization of coal direct liquefaction residue are: CN 1827697A, CN1807715A, Fuel Processing Technology (2000, 62: 109-118), Coal Conversion (2001, 24 (1): 15-19), Combustion Science and Tech...
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Abstract

The invention discloses a method for preparing asphalt-base carbon fiber by taking coal directly liquefied residues as a raw material. The method comprises the following steps that: mixed solution of coal directly liquefied residue powder and tetrahydroquinoline solvent is filled into a high pressure autoclave, and is heated to a temperature of between 150 and 400 DEG C after air in the autoclave is replaced by nitrogen; hydrogen is introduced into the autoclave while pressure is increased to 2 to 50MPa; most elements, such as sulfur, oxygen, nitrogen and the like, contained in original residues are removed through distilling under reduced pressure; removing tetrahydroquinoline insoluble substance through filtering under reduced pressure, reclaiming the tetrahydroquinoline solvent through distilling under reduced pressure, and recycling the tetrahydroquinoline solvent; and the obtained tetrahydroquinoline soluble substance can be produced into the asphalt-base carbon fiber through melt spinning, pre-oxidation, low temperature carbonization, high temperature carbonization, superficial treatment, post treatment and other processes.

Application Domain

Fibre chemical features

Technology Topic

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  • Asphalt-base carbon fiber prepared by coal directly liquefied residues and preparation method thereof
  • Asphalt-base carbon fiber prepared by coal directly liquefied residues and preparation method thereof

Examples

  • Experimental program(3)

Example Embodiment

[0033] Example 1
[0034]Grind 10 kg of coal directly liquefied residue into powder with a particle size of 0.01-0.3 microns. The coal direct liquefaction residue powder is thoroughly mixed with 20 kg of tetrahydroquinoline to obtain a mixed solution. Put the mixed solution into an autoclave, replace the air in the autoclave with nitrogen, and then heat and pressurize while passing in hydrogen gas for hydrogenation; vacuum distillation removes most of the sulfur, oxygen, nitrogen, etc. contained in the original residue The elements are filtered under reduced pressure to remove the tetrahydroquinoline insoluble matter, and the tetrahydroquinoline solvent is recovered by vacuum distillation and recycled. The pitch raw material produced in the pitch preparation process is heated and melted and melt-spinned by a spinning machine. During the spinning process, the raw material viscosity is controlled to 10 Pa·S and the spinning temperature is 350° C. The raw yarn is obtained by melt spinning. The three-stage temperature of the raw silk introduced into the air and the furnace is 210°C in the first stage, 260°C in the second stage, 300°C in the third stage, and 2.5 hours of reaction time to obtain the pre-oxidized wire. Under the protection of nitrogen, the pre-oxygenated wire is carbonized at a temperature of 600°C, a time of 30 minutes, and a time of 1000°C, and a time of 30 minutes, respectively, to obtain a carbon wire; the carbon wire is subjected to surface treatment to obtain a pitch-based carbon fiber. The performance is shown in Table 1.

Example Embodiment

[0035] Example 2
[0036] Grind 10 kg of coal directly liquefied residue into powder with a particle size of 0.01-0.3 microns. The coal direct liquefaction residue powder is thoroughly mixed with 30 kilograms of tetrahydroquinoline to obtain a mixed solution. Put the mixed solution into an autoclave, replace the air in the autoclave with nitrogen, and then heat and pressurize while passing in hydrogen gas for hydrogenation; vacuum distillation removes most of the sulfur, oxygen, nitrogen, etc. contained in the original residue The elements are filtered under reduced pressure to remove the tetrahydroquinoline insoluble matter, and the tetrahydroquinoline solvent is recovered by vacuum distillation and recycled. The pitch raw material produced in the pitch preparation process is heated and melted and melt-spinned by a spinning machine. During the spinning process, the raw material viscosity is controlled to 15 Pa·S, the spinning temperature is 380° C., and the raw yarn is obtained by melt spinning. The three-stage temperature of the raw silk is introduced into the air and the furnace is respectively: the temperature of the first stage is 200°C, the temperature of the second stage is 250°C, the temperature of the third stage is 280°C, and the reaction time is 2 hours to obtain the pre-oxidized wire. Under the protection of nitrogen, the pre-oxygenated wire is carbonized at a temperature of 700°C, a time of 20 minutes, and a time of 900°C, and a time of 30 minutes to obtain a carbon wire; the carbon wire is subjected to surface treatment to obtain a pitch-based carbon fiber. The performance is shown in Table 1.

Example Embodiment

[0037] Example 3
[0038] Grind 10 kg of coal directly liquefied residue into powder with a particle size of 0.01-0.3 microns. The coal direct liquefaction residue powder is thoroughly mixed with 40 kilograms of tetrahydroquinoline to obtain a mixed solution. Put the mixed solution into an autoclave, replace the air in the autoclave with nitrogen, and then heat and pressurize while passing in hydrogen gas for hydrogenation; vacuum distillation removes most of the sulfur, oxygen, nitrogen, etc. contained in the original residue The elements are filtered under reduced pressure to remove the tetrahydroquinoline insoluble matter, and the tetrahydroquinoline solvent is recovered by vacuum distillation and recycled. The pitch raw material produced in the pitch preparation process is heated and melted and melt-spinned by a spinning machine. During the spinning process, the raw material viscosity is controlled to 18 Pa·S, the spinning temperature is 400° C., and the raw yarn is obtained by melt spinning. The three-stage temperature of the raw silk introduced into the air and the furnace is 210°C in the first stage, 270°C in the second stage, 300°C in the third stage, and 3 hours of reaction time to obtain the pre-oxidized wire. The pre-oxygenated wire is carbonized under the conditions of a temperature of 800°C, a time of 30 minutes and a time of 900°C, and a time of 30 minutes, respectively, under the protection of nitrogen, so as to obtain a carbon wire; the carbon wire is subjected to surface treatment to obtain a pitch-based carbon fiber. The performance is shown in Table 1.
[0039] Table 1 shows the properties of the prepared pitch and carbon fiber
[0040] Performance
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PUM

PropertyMeasurementUnit
Particle size0.01 ~ 0.3µm
Monofilament diameter10.0 ~ 30.0µm
Tensile strength900.0 ~ 1800.0MPa
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

  • Abundant sources of raw materials
  • Low price
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