# US 11,305,995 B2 · Method of preparing carbon particles from oil ash

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- Number: US 11,305,995 B2
- Document ID: US11305995B2
- Status: Granted
- Kind: B2
- Application number: 16/812,798
- Filed: 2020-03-09
- Published: 2021-09-09
- Granted: 2022-04-19
- Earliest claimed: 2020-03-09
- Assignees: King Fahd University of Petroleum and Minerals
- Applicants: King Fahd University of Petroleum and Minerals
- Inventors: Md. Abdul Aziz; Shaik Inayath Basha; Abbas Saeed Hakeem; Mohammed Maslehuddin; Shamsad Ahmad
- Web page: https://patentgrep.com/patent/US11305995B2

## CPC

- C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
- C10B 53/00: Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form (wet carbonising of peat C10F)
- C10B 57/005: {After-treatment of coke, e.g. calcination desulfurization}
- C01P 2002/82: by IR- or Raman-data
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C10B: DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS (cracking oils C10G; underground gasification of minerals E21B43/295)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## 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).

## Claims

### Claim 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.

### Claim 2 (depends on 1)

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

### Claim 3 (depends on 2)

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

### Claim 4 (depends on 2)

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.

### Claim 5 (depends on 1)

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.

### Claim 6 (depends on 1)

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.

### Claim 7 (depends on 1)

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

### Claim 8 (depends on 1)

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.

### Claim 9 (depends on 1)

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

### Claim 10 (depends on 1)

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

### Claim 11 (depends on 10)

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.

### Claim 12 (depends on 1)

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.

### Claim 13 (depends on 1)

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.

### Claim 14 (depends on 1)

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.

### Claim 15 (depends on 1)

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

### Claim 16 (depends on 1)

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.

### Claim 17 (depends on 1)

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.

### Claim 18 (depends on 1)

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.

### Claim 19 (depends on 1)

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.

### Claim 20 (depends on 1)

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.