IP Library Granted Patent US 10,320,000
Granted Patent B2
US 10,320,000 · App. 15/056,184 · Granted Jun 11, 2019

Pyrolytic carbon black composite and method of making the same

Inventors: Amit K. Naskar (Knoxville, TN); Mariappan Parans Paranthaman (Knoxville, TN)
Assignee: UT-BATTELLE, LLC
H01M4/587C09C1/48C09C1/482H01M4/0471H01M4/133H01M4/1393H01M10/054H01M10/0525C01P2004/04C01P2006/12C01P2006/40H01M10/052H01M2004/027
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Quick Facts
Patent No.
US 10,320,000
App. No.
15/056,184
Granted
Jun 11, 2019
Kind
B2
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 (29)

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 m 2 /g.

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

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

4. The method of claim 1 , wherein the sulfonation bath comprises between 0.1-65 wt. % SO 3 .

5. The method of claim 1 , wherein the sulfonation bath comprises 2-30 wt. % SO 3 .

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

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

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

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

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

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

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

13. 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.

14. 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.

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

16. 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.

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

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

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

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

21. 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.

22. The method of claim 1 , wherein the carbon black containing product has a specific surface area of less than 2000 m 2 /g.

23. The method of claim 1 , wherein the carbon black containing product has a specific surface area of less than 1000 m 2 /g.

24. The method of claim 1 , wherein the carbon black containing product has a specific surface area of less than 100 m 2 /g.

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

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

Assignments (2)
CONFIRMATORY LICENSE Recorded Jul 18, 2016
From: UT-BATTELLE, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 039176/0992 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 6, 2016
From: NASKAR, AMIT K.; PARANTHAMAN, MARIAPPAN PARANS
To: UT-BATTELLE, LLC
Reel/Frame 038485/0893 →
Continuity (2)
Continuation In Part 13945239 · Jul 18, 2013
Related Publication 20160254543A1 · Sep 1, 2016