Method for efficiently preparing petroleum asphalt-based mesocarbon microbeads
A technology of mesocarbon microspheres and petroleum pitch, applied in the field of carbon materials, can solve the problems of uneven particle size distribution and low yield, and achieve the effect of abundant sources and low price
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Embodiment 1
[0022] Mix petroleum pitch and carbon black N110 with a mass fraction of 2% and place it in a reactor, then raise the temperature to 300°C at a rate of 4°C / min, 2 Under the conditions of flow rate 60mL / min, mechanical stirring speed 150r / min, and constant temperature 2h preheating treatment, a sufficient mixture of petroleum pitch and carbon black N110 from which small molecules have been removed can be obtained. after N 2 Under protection, the temperature was raised to 400°C at a rate of 5°C / min, and under the conditions of a pressure of 1MPa and a mechanical stirring speed of 200r / min, the polymerization was carried out at a constant temperature for 4h to obtain polymerized petroleum pitch containing mesophase carbon microspheres. Use 2 times the mass of washing oil to stir, dissolve and filter the above-mentioned polymerized petroleum asphalt at 190°C, and extract the filtered filter cake with pyridine until the reflux liquid is colorless. Afterwards, the extracted filter ...
Embodiment 2
[0024] Mix petroleum pitch and rosin with a mass fraction of 2%, and then raise the temperature to 300°C at a rate of 4°C / min. 2 Under the conditions of flow rate 40mL / min, mechanical stirring speed 200r / min, constant temperature 2h preheating treatment, that is to obtain a sufficient mixture of petroleum pitch and rosin from which small molecules have been removed. after N 2 Under protection, the temperature was raised to 410°C at a rate of 5°C / min, under the conditions of a pressure of 1MPa and a mechanical stirring speed of 200r / min, the polymerization was carried out at a constant temperature for 5h to obtain polymerized petroleum pitch containing mesophase carbon microspheres. Use 3 times the mass of washing oil to mechanically dissolve and filter the above-mentioned polymerized petroleum asphalt at 180°C, and extract the filtered filter cake with toluene until the reflux liquid is colorless. Afterwards, the extracted filter cake was vacuum-dried at 60° C. and a vacuum d...
Embodiment 3
[0026] Mix petroleum pitch and rosin with a mass fraction of 5%, and then raise the temperature to 280°C at a heating rate of 5°C / min. 2 Under the conditions of flow rate 80mL / min, mechanical stirring speed 200r / min, constant temperature 2h preheating treatment, that is to obtain a sufficient mixture of petroleum pitch and rosin from which small molecules have been removed. after N 2 Under protection, the temperature was raised to 410°C at a rate of 6°C / min, and under the conditions of pressure 1MPa and mechanical stirring speed 200r / min, polymerization was carried out at a constant temperature for 4 hours to obtain polymerized petroleum pitch containing mesophase carbon microspheres. Then use 2 times the mass of washing oil to stir, dissolve and filter the above-mentioned polymerized petroleum asphalt at 170°C, and extract the filtered filter cake with tetrahydrofuran until the reflux liquid is colorless. Afterwards, the extracted filter cake was vacuum-dried at 90° C. and a...
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