Process method for preparing intermediate phase lignin and carbon fibers thereof
A process method, lignin technology, applied in the field of high-performance mesophase lignin and carbon fiber production and manufacturing process, can solve the problems of limited use, only reachable, no fluidity and spinnability, and achieve low modulation cost Effect
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Embodiment 1
[0035] Select ethanol lignin, the weight-average molecular weight is 2000-10000, the dispersion coefficient is 1.8, and the ash content is ≤0.025%. Take 500g of lignin and add it to the reaction kettle, and add 1000g of anthracene oil to feed nitrogen, blow out the air in the kettle, and then pass Heat the reactor in a salt bath to 380°C, keep the pressure not exceeding 3.5MPa for 5 hours, take it out after cooling, add it to a salt bath glass reactor, feed nitrogen, stir and heat at 400°C, and evaporate excess After anthracene oil and light components were kept for 7 hours, mesophase lignin was obtained after cooling. Observed under a polarizing microscope, its mesophase content reaches 75% by mass, and the measured softening point is 272°C. It is spun in a single-hole melt spinning machine, the diameter of the spinneret hole is 0.3mm, and the spinning temperature is 305°C. Afterwards, the raw silk is placed in a pre-oxidation furnace, and the temperature is programmed to ris...
Embodiment 2
[0037]Select ethanol lignin, the weight-average molecular weight is 2000-10000, the dispersion coefficient is 1.8, and the ash content is ≤0.025%. Take 500g of lignin, add it to the reaction kettle, and add 500g of naphthol to feed nitrogen, blow out the air in the kettle, and then pass Heat the reactor in a salt bath to 400°C, keep the pressure not exceeding 3.5MPa for 4 hours, take it out after cooling, put it into a salt bath glass reactor, feed nitrogen, stir and heat at 400°C, and evaporate the light components After that, it was kept for 3 hours, and the mesophase lignin was obtained after cooling. Observed under a polarizing microscope, the mesophase content reaches 90% by mass, and the measured softening point is 282°C. It is spun in a single-hole melt spinning machine, the diameter of the spinneret hole is 0.3mm, and the spinning temperature is 312°C. Afterwards, the raw silk was placed in a pre-oxidation furnace, and the temperature was programmed to rise to a maximu...
Embodiment 3
[0039] Select ammonia lignin, the weight-average molecular weight is 2000-5000, the dispersion coefficient is 1.4, and the ash content is ≤0.01%. Take 500g of lignin, add it to the reaction kettle, and add 150g of fluoranthene to feed nitrogen, blow out the air in the kettle, and then pass Heat the reactor to 420°C in a salt bath, keep the pressure not exceeding 3MPa for 10 hours, take it out after cooling, put it into a salt bath glass reactor, feed nitrogen, stir and heat at 420°C, and evaporate the light components , kept for 5 hours, and obtained mesophase lignin after cooling. Observed under a polarizing microscope, the mesophase content reaches 100% by mass, and the measured softening point is 265°C. Spinning in a single-hole melt spinning machine, the diameter of the spinneret hole is 0.3mm, and the spinning temperature is 298°C. Afterwards, the raw silk was placed in a pre-oxidation furnace, and the temperature was programmed to rise to a maximum temperature of 300°C, ...
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