# US 10,320,000 B2 · Pyrolytic carbon black composite and method of making the same

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- Number: US 10,320,000 B2
- Document ID: US10320000B2
- Status: Granted
- Kind: B2
- Application number: 15/056,184
- Filed: 2016-02-29
- Published: 2016-09-01
- Granted: 2019-06-11
- Earliest claimed: 2013-07-18
- Assignees: UT-Battelle, LLC
- Applicants: UT-Battelle, LLC
- Inventors: Amit K. Naskar; Mariappan Parans Paranthaman
- Web page: https://patentgrep.com/patent/US10320000B2

## CPC

- H01M 4/587: for inserting or intercalating light metals
- C09C 1/48: Carbon black
- C09C 1/482: {Preparation from used rubber products, e.g. tyres (recovery of plastics or other constituents of waste material containing plastics B29B17/00)}
- H01M 4/0471: {involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis}
- H01M 4/133: Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/1393: of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- H01M 10/054: Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2006/12: Surface area
- C01P 2006/40: Electric properties
- H01M 10/052: Li-accumulators
- H01M 2004/027: {Negative electrodes}
- Y02E 60/10: Energy storage using batteries
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method of recovering carbon black includes the step of providing a carbonaceous source material containing carbon black. The carbonaceous source material is contacted with a sulfonation bath to produce a sulfonated material. The sulfonated material is pyrolyzed to produce a carbon black containing product comprising a glassy carbon matrix phase having carbon black dispersed therein. The pyrolysis can be conducted at a temperature from 1100° C. to 1490° C. A method of making a battery electrode and a lithium ion or sodium ion battery is also disclosed.

## Claims

### Claim 1

A method of recovering carbon black, comprising the steps of:
providing a carbonaceous source material containing carbon black;
contacting the carbonaceous source material with a sulfonation bath to produce a sulfonated material; and,
pyrolyzing the sulfonated material at a temperature of from 1400 to 1600° C. without any activation to produce a layered carbon black containing product comprising a glassy carbon matrix phase having carbon black dispersed therein, the layered carbon black containing product having an interlayer spacing of from 0.4 to 0.5 nm and pores of from 1 to 20 nm, and the carbon black containing product having a specific surface area less than 100 m2/g.

### Claim 2 (depends on 1)

The method of claim 1, wherein the sulfonation bath is an oleum bath.

### Claim 3 (depends on 1)

The method of claim 1, wherein the sulfonation bath comprises sulfonation agent is chlorosulfonic acid in 1,2 dichloroethane solution.

### Claim 4 (depends on 1)

The method of claim 1, wherein the sulfonation bath comprises between 0.1-65 wt. % SO3.

### Claim 5 (depends on 1)

The method of claim 1, wherein the sulfonation bath comprises 2-30 wt. % SO3.

### Claim 6 (depends on 1)

The method of claim 1, wherein the sulfonation bath has a temperature of between −20° C. to 200° C.

### Claim 7 (depends on 1)

The method of claim 1, wherein pyrolysis step is conducted at a temperature that is greater than 1200° C.

### Claim 8 (depends on 1)

The method of claim 1, wherein pyrolysis step is conducted at a temperature that is greater than 1300° C.

### Claim 9 (depends on 1)

The method of claim 1, wherein the pyrolysis step is conducted at a temperature from 1200-1400° C.

### Claim 10 (depends on 1)

The method of claim 1, wherein pyrolysis step is conducted at a temperature from 1250-1350° C.

### Claim 11 (depends on 1)

The method of claim 1, wherein the pyrolysis step is conducted at a temperature from 1100-1400° C.

### Claim 12 (depends on 1)

The method of claim 1, wherein the duration of the pyrolysis step is from 1 minute to 12 hours.

### Claim 13 (depends on 1)

The method of claim 1, further comprising the steps of reducing the carbonaceous source material to at least one selected from the group consisting of powder and shredded rubber pieces prior to contacting the carbonaceous source material with the oleum bath.

### Claim 14 (depends on 13)

The method of claim 13, wherein the powder and/or shredded rubber pieces has an average maximum dimension of less than 100 nm to 10 cm.

### Claim 15 (depends on 1)

The method of claim 1, wherein the carbonaceous source material comprises carbon reinforced composites.

### Claim 16 (depends on 15)

The method of claim 15, wherein the carbon reinforcing agent is at least one selected from the group consisting of carbon black, carbon particles, nanoparticles, mesoparticles and fibers.

### Claim 17 (depends on 1)

The method of claim 1, wherein the carbonaceous source material is a waste material.

### Claim 18 (depends on 17)

The method of claim 17, wherein the waste material is rubber tires.

### Claim 19 (depends on 1)

The method of claim 1, wherein the average pore size of the carbon black product is less than 8 nm.

### Claim 20 (depends on 1)

The method of claim 1, wherein the average pore size of the carbon black product is between 2 and 120 nm.

### Claim 21 (depends on 1)

The method of claim 1, wherein the isolated carbon is further surface activated and the density of average pore size of the carbon black product between 1 and 20 nm is increased.

### Claim 22 (depends on 1)

The method of claim 1, wherein the carbon black containing product has a specific surface area of less than 2000 m2/g.

### Claim 23 (depends on 1)

The method of claim 1, wherein the carbon black containing product has a specific surface area of less than 1000 m2/g.

### Claim 24 (depends on 1)

The method of claim 1, wherein the carbon black containing product has a specific surface area of less than 100 m2/g.

### Claim 25 (depends on 1)

The method of claim 1, wherein the pyrolyzing step occurs after the contacting step.

### Claim 26 (depends on 1)

The method of claim 1, wherein the pyrolyzing step occurs before the contacting step.