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

[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.

[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.

[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