Pyrolytic carbon black composite and method of making the same

Patent metadata

Field	Value
Publication number	US-9441113-B2
Application number	US-201313945239-A
Country	US
Kind code	B2
Filing date	Jul 18, 2013
Priority date	Jul 18, 2013
Publication date	Sep 13, 2016
Grant date	Sep 13, 2016

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. A method of making a battery electrode is also disclosed.

First claim

We 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, wherein the sulfonation bath comprises sulfonation agent is chlorosulfonic acid in 1,2 dichloroethane solution; and,
pyrolyzing the sulfonated material to produce a carbon black containing product comprising a glassy carbon matrix phase having carbon black dispersed therein.

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 between 0.1-65 wt. % SO 3 .

4. The method of claim 1 , wherein pyrolysis step is conducted at a temperature that is greater than 1000° C.

5. The method of claim 1 , wherein pyrolysis step is conducted at a temperature that is between 200-1000° C.

6. The method of claim 1 , further comprising the steps of reducing the carbonaceous source material to a powder prior to contacting the carbonaceous source material with the oleum bath.

7. The method of claim 6 , wherein the powder has an average maximum dimension of less than 100 nm to 10 cm.

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

9. The method of claim 8 , wherein the carbon reinforcing agent is at least one selected from the group consisting of carbon black, carbon particles, nanoparticles, mesoparticles and fibers.

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

11. The method of claim 10 , wherein the waste material is rubber tires.

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

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

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

15. 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,
pyrolyzing the sulfonated material to produce a carbon black containing product comprising a glassy carbon matrix phase having carbon black dispersed therein; and
wherein the carbon black product has an average pore size of less than 8 nm.

16. The method of claim 15 , wherein the sulfonation bath is an oleum bath.

17. The method of claim 15 , wherein the sulfonation bath comprises between 0.1-65 wt. % SO 3 .

18. The method of claim 15 , wherein pyrolysis step is conducted at a temperature that is greater than 1000° C.

19. The method of claim 15 , wherein pyrolysis step is conducted at a temperature that is between 200-1000° C.

20. The method of claim 15 , further comprising the steps of reducing the carbonaceous source material to a powder prior to contacting the carbonaceous source material with the oleum bath.

21. The method of claim 20 , wherein the powder has an average maximum dimension of less than 100 nm to 10 cm.

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

23. The method of claim 22 , wherein the carbon reinforcing agent is at least one selected from the group consisting of carbon black, carbon particles, nanoparticles, mesoparticles and fibers.

24. The method of claim 15 , wherein the carbonaceous source material is a waste material.

25. The method of claim 24 , wherein the waste material is rubber tires.

26. The method of claim 15 , wherein the carbon black containing product has a specific surface area of less than 1000 m 2 /g.

27. The method of claim 15 , wherein the pyrolyzing step occurs after the contacting step.

28. The method of claim 15 , wherein the pyrolyzing step occurs before the contacting step.

29. 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,
pyrolyzing the sulfonated material to produce a carbon black containing product comprising a glassy carbon matrix phase having carbon black dispersed therein; and
wherein the carbon black product has an average pore size of between 2 and 120 nm.

30. The method of claim 29 , wherein the sulfonation bath is an oleum bath.

31. The method of claim 29 , wherein the sulfonation bath comprises between 0.1-65 wt. % SO 3 .

32. The method of claim 29 , wherein pyrolysis step is conducted at a temperature that is greater than 1000° C.

33. The method of claim 29 , wherein pyrolysis step is conducted at a temperature that is between 200-1000° C.

34. The method of claim 29 , further comprising the steps of reducing the carbonaceous source material to a powder prior to contacting the carbonaceous source material with the oleum bath.

35. The method of claim 34 , wherein the powder has an average maximum dimension of less than 100 nm to 10 cm.

36. The method of claim 29 , wherein the carbonaceous source material comprises carbon reinforced composites.

37. The method of claim 36 , wherein the carbon reinforcing agent is at least one selected from the group consisting of carbon black, carbon particles, nanoparticles, mesoparticles and fibers.

38. The method of claim 29 , wherein the carbonaceous source material is a waste material.

39. The method of claim 38 , wherein the waste material is rubber tires.

40. The method of claim 29 , wherein the carbon black containing product has a specific surface area of less than 1000 m 2 /g.

41. The method of claim 29 , wherein the pyrolyzing step occurs after the contacting step.

42. The method of claim 29 , wherein the pyrolyzing step occurs before the contacting step.

43. 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,
pyrolyzing the sulfonated material to produce a carbon black containing product comprising a glassy carbon matrix phase having carbon black dispersed therein; and
wherein the carbon black product is further surface activated and the carbon black product has an average pore size between 1 and 20 nm and a density of pores having an average pore size between 1 and 20 nm is increased.

44. The method of claim 43 , wherein the sulfonation bath is an oleum bath.

45. The method of claim 43 , wherein the sulfonation bath comprises between 0.1-65 wt. % SO 3 .

46. The method of claim 43 , wherein pyrolysis step is conducted at a temperature that is greater than 1000° C.

47. The method of claim 43 , wherein pyrolysis step is conducted at a temperature that is between 200-1000° C.

48. The method of claim 43 , further comprising the steps of reducing the carbonaceous

Assignees

• Ut Battelle Llc

Inventors

• Naskar Amit K
• Paranthaman Mariappan Parans
• Bi Zhonghe

Classifications

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2006/12

  Surface area · CPC title

• H01M4/587

  for inserting or intercalating light metals · CPC title

• C09C1/482 Primary

  Preparation from used rubber products, e.g. tyres (recovery of plastics or other constituents of waste material containing plastics B29B17/00) · CPC title

• C01P2006/40

  Electric properties · CPC title