Method for preparing pitch-based carbon fiber
A pitch-based carbon fiber and pitch technology, applied in fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of high production equipment and process level, narrow application range of viscose base, high equipment precision requirements, etc., and meet the requirements of raw materials Rich, avoid line breakage, good yield and quality
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[0020] A preparation method of pitch-based carbon fiber, comprising the following steps:
[0021] 1. Use the molecular distillation method to distill medium-temperature pitch for 0.5-2 hours to obtain low-QI coal tar pitch.
[0022] In this step, medium-temperature asphalt is used as raw material, the medium-temperature asphalt has a QI value of less than 0.3%, a softening point of 80-120°C, a coking value of more than 46%, a TI value of more than 12%, and no sodium ions. The specific process of the molecular distillation method is: add a certain quality of medium-temperature asphalt into the molecular still through the circulation pump, the circulation rate is 400-600ml / min, the vacuum negative pressure is 0.01-0.1MPa, and the initial distillation temperature is 130- Distillation is carried out at 180°C and the temperature difference between distillation and condensation is 40-80°C. During the distillation process, the temperature is continuously raised at a rate of 2-6°C / min...
Embodiment 1
[0029] (1) Add a certain amount of medium-temperature asphalt to the molecular still through a circulation pump, the circulation rate is 450ml / min, distill under a vacuum negative pressure of 0.099MPa, the distillation start temperature is 140°C, and the heating rate is 2°C / min , The temperature difference between distillation and condensation is 70°C. When the temperature rises to 310°C, there is no obvious distillate after about 85 minutes. The distillation stops and the residue is removed to obtain low QI coal tar pitch.
[0030] (2) Under the condition of 220°C, use air as the oxidant to oxidize the low-QI coal tar pitch, and the oxidation time is 5 hours;
[0031] (3) Under the conditions of 280°C and 0.08MPa, the oxidized bitumen is subjected to thin film distillation for 2 hours to remove light components;
[0032] (4) Under the condition of 310°C, melt-spin the bitumen after removing light components;
[0033] (5) Use air to pre-oxidize the as-spun fibers at 280°C for...
Embodiment 2
[0036] (1) Add a certain amount of medium-temperature asphalt to the molecular still through a circulation pump, the circulation rate is 450ml / min, distill under a vacuum negative pressure of 0.099MPa, the distillation start temperature is 140°C, and the heating rate is 2°C / min , The temperature difference between distillation and condensation is 70°C. When the temperature rises to 310°C, there is no obvious distillate after about 85 minutes. The distillation stops and the residue is removed to obtain low QI coal tar pitch.
[0037] (2) Under the condition of 240°C, use air as the oxidant to oxidize the asphalt, and the oxidation time is 6 hours;
[0038] (3) Under the conditions of 290°C and 0.09MPa, the oxidized bitumen is subjected to thin-film distillation for 2.5 hours to remove light components;
[0039] (4) Under the condition of 320°C, melt-spin the bitumen after removing light components;
[0040] (5) Use air to pre-oxidize the as-spun fiber at 300°C, and the oxidati...
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