Method of preparing carbon particles from oil ash

Patent metadata

Field	Value
Publication number	US-11305995-B2
Application number	US-202016812798-A
Country	US
Kind code	B2
Filing date	Mar 9, 2020
Priority date	Mar 9, 2020
Publication date	Apr 19, 2022
Grant date	Apr 19, 2022

Abstract

A method of producing submicron carbon particles from oil ash. The method comprises pyrolyzing the oil ash to produce a pyrolyzed oil ash and milling the pyrolyzed oil ash to produce carbon particles having a mean particle size in the submicron regime. The method produces submicron carbon particles which have a very high carbon content (90 to 99 atom %) and a very low content of oxygen, the particles having a ratio of carbon to oxygen ratio of 10:1 to 99:1. The size of the particles may be controlled by the duration of the milling. The submicron carbon particles are devoid of functionalities containing carbon-oxygen double bonds as measured by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS).

First claim

The invention claimed is:

1. A method for producing submicron carbon particles, comprising:
pyrolyzing oil ash at 600 to 1000° C. for 1 to 6 hours to produce a pyrolyzed oil ash, and
milling the pyrolyzed oil ash for 1 to 24 hours to produce the submicron carbon particles,
wherein the submicron carbon particles have a ratio of carbon to oxygen of 10:1 to 99:1, and
wherein the submicron carbon particles are devoid of functional groups containing carbon-oxygen double bonds as determined by XPS or Raman spectroscopy.

2. The method of claim 1 , wherein the oil ash comprises carbon, oxygen, and sulfur.

3. The method of claim 2 , wherein the oil ash has a carbon to oxygen ratio of 3:1 to 15:1.

4. The method of claim 2 , wherein the oil ash further comprises at least one element selected from the group consisting of vanadium, iron, aluminum, silicon, magnesium, and calcium.

5. The method of claim 1 , wherein the oil ash has a carbon atomic % of 65 to 89 atom %, based on a total number of atoms in the oil ash.

6. The method of claim 1 , wherein the oil ash has a sulfur atomic % of less than 2 atom %, based on a total number of atoms in the oil ash.

7. The method of claim 1 , wherein the oil ash is a heavy oil ash.

8. The method of claim 1 , wherein the pyrolyzing is performed with a heating rate of 1° C./min to 15° C./min and a cooling rate of 1° C./min to 15° C./min.

9. The method of claim 1 , wherein the pyrolyzing is performed in an inert atmosphere.

10. The method of claim 1 , wherein the milling is ball milling.

11. The method of claim 10 , wherein the ball milling is performed at 1500 to 5000 rpm and with a ball-to-powder ratio of 50:1 to 5:1 by mass.

12. The method of claim 1 , wherein the submicron carbon particles have a carbon atomic % of 90 to 99 atom % based on a total number of atoms in the submicron carbon particles.

13. The method of claim 1 , wherein the submicron carbon particles have a sulfur atomic % of less than 5 atom % based on a total number of atoms in the submicron carbon particles.

14. The method of claim 1 , wherein the submicron carbon particles further comprise at least one element selected from the group consisting of vanadium, iron, aluminum, silicon, magnesium, and calcium.

15. The method of claim 1 , wherein the submicron carbon particles have a mean particle size of 100 to 500 nm.

16. The method of claim 1 , wherein the pyrolyzed oil ash is milled for 1 to less than 7.5 hours and the submicron carbon particles have a mean particle size of greater than 350 to 500 nm.

17. The method of claim 1 , wherein the pyrolyzed oil ash is milled for greater than 7.5 to less than 12.5 hours and the submicron carbon particles have a mean particle size of greater than 200 to less than 350 nm.

18. The method of claim 1 , wherein the pyrolyzed oil ash is milled for greater than 12.5 to 24 hours and the submicron carbon particles have a mean particle size of 100 to less than 200 nm.

19. The method of claim 1 , wherein the submicron carbon particles have a Raman spectrum that has a ratio of an intensity at 1520 to 1590 cm −1 to an intensity at 1275 to 1325 cm −1 of 1:1 to 3:1.

20. The method of claim 1 , wherein the submicron carbon particles have an XPS spectrum with a single signal in the region 280 to 292 eV with a maximum intensity at 283.5 to 285.5 eV.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Aziz Md Abdul
• Basha Shaik Inayath
• Hakeem Abbas Saeed
• Maslehuddin Mohammed
• Ahmad Shamsad

Classifications

• C10B57/005

  After-treatment of coke, e.g. calcination desulfurization · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01B32/05 Primary

  Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30 · CPC title

• C01P2002/85

  by XPS, EDX or EDAX data · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title