Method of preparing carbon fiber by using coal to directly liquefy residue-based asphalt vinyl material
A coal direct liquefaction and asphaltene-based technology, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, can solve the problems of low added value, environmental pollution, waste of resources, etc., and achieve the effects of conventional equipment, environment-friendly, and resource utilization
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Embodiment 1
[0020] Weigh about 10.0105g of asphaltenes (with a particle size of about 100 mesh) obtained by extracting coal direct liquefaction residue with N-methylpyrrolidone in a porcelain boat, put it into a high-temperature tube furnace, seal it, and purge it with nitrogen. Raise the temperature to 380°C at a heating rate of 2.5°C / min, keep the temperature at 380°C for 10 hours, and then cool down naturally. During the process of heating up, constant temperature and cooling down, 60ml / min of nitrogen gas was introduced for protection. 6.1344g of solid product was prepared, namely the mesophase, the yield was about 61.28%, the H / C was about 0.57, the S content was about 0.36%, and the softening point was about 235°C. The prepared mesophase is used to spin a raw filament under the condition of heating at 275° C. through a melt spinning machine. The raw silk was pre-oxidized in an air atmosphere at 280°C, and then carbonized in a nitrogen atmosphere at 1000°C to prepare carbon fibers. ...
Embodiment 2
[0022] Weigh about 10.0617g of asphaltenes (with a particle size of about 100 mesh) obtained by extracting coal direct liquefaction residue with N-methylpyrrolidone in a porcelain boat, put it into a high-temperature tube furnace, seal it, and blow it with nitrogen. Raise the temperature to 390°C at a heating rate of 2.5°C / min, keep the temperature at 390°C for 10 hours, and then cool down naturally. During the process of heating up, constant temperature and cooling down, 50ml / min of nitrogen gas was introduced for protection. 5.3659g of solid product was prepared, namely the mesophase, the yield was about 53.33%, the H / C was about 0.52, the S content was about 0.08%, and the softening point was about 225-235°C. Use the prepared mesophase to spin a precursor under the condition of heating at 280° C. through a melt spinning machine. The raw silk was pre-oxidized in an air atmosphere at 280°C, and then carbonized in a nitrogen atmosphere at 1000°C to prepare carbon fibers. The...
Embodiment 3
[0024] Weigh about 10.0130g of asphaltenes (particle size about 100 mesh) obtained by extracting coal direct liquefaction residue with N-methylpyrrolidone, put it into the autoclave in the glove box, seal it and take it out. Raise the temperature to 400°C at a heating rate of 2°C / min, keep the temperature at 400°C for 8 hours, and then cool down naturally. 7.9012g of solid product was prepared, namely the mesophase, with a yield of about 78.91%, H / C of about 0.73, S content of about 0.42%, and a softening point of about 182°C.
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