Intermediate-phase asphalt stock with superior spinning performance and preparation method
A mesophase pitch, mesophase technology, applied in the processing of tar pitch/petroleum pitch/natural pitch, processing tar pitch/petroleum pitch/natural pitch by distillation, and chemically processing tar pitch/petroleum pitch/natural pitch, etc. , can solve the problems of high volatile content, decreased fiber strength, affecting carbon fiber strength, etc., to achieve the effects of excellent spinnability, simple and convenient operation and control, and less low-molecular-weight volatiles.
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Embodiment 1
[0029] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:0.5:0.6, react at 270°C for 180 minutes, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them for use. Then the product is distilled under reduced pressure at a temperature of 400° C. and 0.5 KPa to separate low-boiling point products to obtain mesophase pitch. The mesophase content of the asphalt is 100% as measured by polarizing microscopy, the softening point is 190°C as measured by capillary rheometer, and the weight loss rate at spinning temperature as measured by thermogravimetric analysis is 0.46wt%. The mesophase bitumen is melt-spun at 260° C., and it runs continuously for more than 3 hours without any broken filaments. The spinning performance is excellent and the operation is stable. The obtained pitch fibers were pre-oxidized in an air atmosphere at a heating rate of 5 °C / min to 260 °C; then carbonized in a nitrogen atmospher...
Embodiment 2
[0031] Add methylnaphthalene, hydrogen fluoride and boron trifluoride into the reactor at a molar ratio of 1:8.0:0.6. After reacting at 270°C for 180 minutes, the catalyst hydrogen fluoride and fluorine triboride are discharged and recycled. Then the product is distilled under reduced pressure at a temperature of 400° C. and 0.5 KPa to separate low-boiling point products to obtain mesophase pitch. The mesophase content of the asphalt is 100% as measured by polarizing microscopy, the softening point is 223°C as measured by capillary rheometer, and the weight loss rate at spinning temperature as measured by thermogravimetric analysis is 0.63wt%. The mesophase pitch is melt-spun at 293° C., and it runs continuously for more than 4 hours without any broken filaments. The spinning performance is excellent and the operation is stable. Then, the same conditions as in Example 1 were used to pre-oxidize and carbonize the pitch fibers to obtain high-performance pitch-based carbon fibers...
Embodiment 3
[0033] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:15.0:0.6. After reacting at 270°C for 180 minutes, the catalyst hydrogen fluoride and fluorine triboride are discharged and recycled. Then the product is distilled under reduced pressure at a temperature of 400° C. and 0.5 KPa to separate low-boiling point products to obtain mesophase pitch. The mesophase content of the pitch is 100% as measured by polarizing microscopy, the softening point is 250°C as measured by capillary rheometer, and the weight loss rate at spinning temperature as measured by thermogravimetric analysis is 0.80wt%. The mesophase bitumen is melt-spun at 320° C., and it runs continuously for more than 4 hours without broken filaments. The spinning performance is excellent and the operation is stable. Then, the same conditions as in Example 1 were used to pre-oxidize and carbonize the pitch fibers to obtain high-performance pitch-based carbon ...
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