Preparation method of mesocarbon microbeads

Abstract

This invention provides a method for preparing mesophase carbon microspheres, comprising: step (A): preparing asphalt raw material, wherein the asphalt raw material has a QI content of 1.5 to 3.0 wt% and a TI content of 20 to 30 wt%; step (B): placing the asphalt raw material in a thermal reactor and performing a heat treatment process under a nitrogen atmosphere or an air atmosphere to obtain a carbonaceous matrix containing mesophase carbon microspheres; step (C): performing a separation process on the carbonaceous matrix containing mesophase carbon microspheres with a separation solvent to collect a crude product of mesophase carbon microspheres; wherein the separation solvent is an organic solvent obtained by first cooling and removing precipitates from a component of coal tar distilled at a temperature of 240°C to 250°C; and step (D): performing a washing process on the crude product of mesophase carbon microspheres using an aromatic hydrocarbon solvent, followed by a drying process to obtain the mesophase carbon microspheres.

Claims

1. A method for preparing mesophase carbon microspheres, comprising: Step (A): preparing an asphalt raw material, wherein the asphalt raw material has a quinoline insoluble content of 1.5% to 3.0% by weight and a toluene insoluble content of 20% to 30% by weight; Step (B): placing the asphalt raw material in a thermal reactor and subjecting the asphalt raw material to a heat treatment process under a nitrogen atmosphere or an air atmosphere to obtain a carbonaceous matrix containing mesophase carbon microspheres; wherein, The heat treatment process involves heating from 200°C to a final temperature and holding it at that temperature for 5 to 7 hours, where the final temperature is 420°C to 460°C. In this heat treatment process, the heat treatment temperature is increased from 320°C to 370°C at a heating rate of 0.4°C / min to 0.7°C / min, and the heat treatment temperature is increased from 410°C to the final temperature at a heating rate of 0.1°C / min to 0.2°C / min. Step (C): The carbonaceous matrix containing mesophase carbon microspheres is separated using a separation solvent to collect the crude product of mesophase carbon microspheres; wherein the separation solvent is an organic solvent obtained by cooling a component of coal tar distilled at a temperature of 240°C to 250°C to 6°C to 8°C and then removing the precipitates after cooling by filtration; and Step (D): The crude product of mesophase carbon microspheres is washed using an aromatic hydrocarbon solvent and then dried to obtain the mesophase carbon microspheres.

2. The manufacturing method as described in claim 1, wherein, The thermal reactor has a cylindrical reaction chamber with a length-to-diameter ratio of 1.9 to 2.

4.

3. The manufacturing method as described in claim 1, wherein, In step (C), the separation process is carried out at 170°C to 240°C.

4. The manufacturing method as described in claim 3, wherein, Based on the total weight of the separating solvent, the separating solvent contains acenaphthene at a weight percentage greater than or equal to 0% and less than 1% by weight, naphthalene at a weight percentage greater than or equal to 0% and less than 1% by weight, fluorene at a weight percentage greater than or equal to 0% and less than 1% by weight, phenanthrene at a weight percentage greater than or equal to 0% and less than 1% by weight, and anthracene at a weight percentage greater than or equal to 0% and less than 1% by weight.

5. The manufacturing method as described in claim 3, wherein, In this separation process, the ratio of the amount of separation solvent used to the weight of the asphalt raw material in step (A) is 1.2 to 2.

0.

6. The manufacturing method as described in claim 5, wherein, Step (C) includes steps (C1) and (C2), and the separation process includes a washing procedure and a filtration procedure; Step (C1): The carbonaceous matrix containing mesophase carbon microspheres is subjected to a first washing procedure and a first filtration procedure with the separation solvent to obtain a filter cake containing mesophase carbon microspheres. And step (C2): The filter cake containing mesophase carbon microspheres is subjected to a second washing process and a second filtration process with the separation solvent to collect the crude product of the mesophase carbon microspheres.

7. The manufacturing method as described in any one of claims 1 to 6, wherein, The aromatic hydrocarbon solvent includes toluene, benzene, xylene, or combinations thereof.

8. The manufacturing method as described in any one of claims 1 to 6, wherein, In the heat treatment process of step (B), the heat treatment temperature is increased from 200°C to 320°C at a heating rate of 0.8°C / min to 1.0°C / min.

9. The manufacturing method as described in any one of claims 1 to 6, wherein, In the heat treatment process of step (B), the heat treatment temperature is increased from 370°C to 390°C at a heating rate of 0.3°C / min to 0.6°C / min, and the heat treatment temperature is increased from 390°C to 410°C at a heating rate of 0.3°C / min to 0.4°C / min.

10. The manufacturing method as described in any one of claims 1 to 6, wherein, In step (D), the temperature of the drying process is 120°C to 170°C.

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