ACTIVATED CARBON CRYOGELS AND RELATED METHODS

• US 20100331179A1
• Filed: 03/26/2010
• Published: 12/30/2010
• Est. Priority Date: 11/21/2005
• Status: Active Grant

• Current Assignee: BASF SE
• Original Assignee: Aaron Feaver, Guozhong Cao
• Inventors: Feaver, Aaron, Cao, Guozhong
• Granted Patent: US 8,158,556 B2
• Time in Patent Office: Days
• US Class Current: 502/416
• CPC Class Codes: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes
• CPC Class Codes: B01J 20/28011 Other properties, e.g. density, crush strength
• CPC Class Codes: B01J 20/28047 Gels
• CPC Class Codes: B01J 20/28057 Surface area, e.g. B.E.T specific surface area
• CPC Class Codes: B01J 20/28076 being more than 1.0 ml/g
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 3/0021 Carbon, e.g. active carbon, carbon nanotubes, fullerenes; Treatment thereof
• CPC Class Codes: C01B 32/00 Carbon; Compounds thereof C01B21/00, C01B23/00 take precedence; percarbonates C01B15/10; carbon black C09C1/48
• CPC Class Codes: F17C 11/005 for hydrogen
• CPC Class Codes: F17C 11/007 for hydrocarbon gases, such as methane or natural gas, propane, butane or mixtures thereof [LPG]
• CPC Class Codes: Y02E 60/32 Hydrogen storage

Abstract

Carbon cryogels, methods for making the carbon cryogels, methods for storing a gas using the carbon cryogels, and devices for storing and delivering a gas using the carbon cryogels.

Claims

1-25. -25. (canceled)

26. A carbon material comprising a surface area of from about 1500 to about 3000 m²/g, wherein the carbon material comprises a pore size distribution comprising:

a) a peak for pores having a diameter less than 2 nm;

b) a peak for pores having a diameter of about 3 nm; and

c) a peak for pores having a diameter between 7 and 8 nm.

27. A carbon material comprising a gravimetric methane storage capacity of 15-20%, a surface area of from about 2400 to about 2600 m²/g and a total pore volume of from about 1.0 to about 1.5 cm³/g.

28. A carbon material comprising a peak pore volume greater than about 0.1 cm³/g for pores comprising a diameter less than about 2 nm and comprising a peak pore volume greater than about 0.1 cm³/g for pores comprising a diameter of about 5 to about 12 nm.

29. The carbon material of claim 28 further comprising a peak pore volume greater than about 0.04 cm³/g for pores comprising a diameter of about 2 to about 4 nm.

30. A carbon material comprising a gravimetric methane storage capacity of about 0.009 to about 0.013 mol/g at room temperature and 500 psi, a surface area of from about 1500 to about 2500 m²/g and a total pore volume of from about 1.2 to about 1.5 cm³/g.

31. The carbon material of claim 30, wherein the total pore volume is from about 1.4 to about 1.5 cm³/g.

32. The carbon material of claim 30, wherein the pore volume is from about 1.2 to about 1.4 cm³/g.

33. The carbon material of claim 30 comprising mesopores comprising a diameter of about 5 to about 12 nm.

34. The carbon material of claim 30 comprising mesopores comprising a diameter of about 2 to about 4 nm.

35. The carbon material of claim 30, wherein the surface area is from about 1500 to about 2000 m²/g.

36. The carbon material of claim 30, wherein the surface area is from about 2000 to about 2500 m²/g.

39. A method for making the carbon material of claim 30, the method comprising:

(a) preparing a sol by mixing resorcinol, formaldehyde, and a catalyst in water;

(b) gelling the sol by heating at a temperature and for a time sufficient to provide a gel;

(c) washing the gel with acid to provide an acid-washed gel comprising an aqueous solvent;

(d) washing the acid-washed gel with a suitable organic solvent to exchange the aqueous solvent for an organic solvent to provide a solvent-exchanged gel;

(e) freeze drying the solvent-exchanged gel; and

(f) pyrolyzing the solvent-exchanged gel to provide a carbon material.

40. The method of claim 39, wherein the molar ratio of resorcinol to catalyst is from about 10 to about 300.

41. The method of claim 39, wherein the catalyst is sodium carbonate.

42. The method of claim 39, wherein the weight ratio of resorcinol to water is from about 0.01 to about 2.0.

43. The method of claim 39, wherein gelling the sol comprises heating at a temperature and for a period of time sufficient to convert the sol to a crosslinked gel.

44. The method of claim 39, wherein gelling the sol comprises heating at about 900°

C. for from about 1 to about 7 days.

45. The method of claim 39, wherein washing the gel with acid comprises washing the gel with aqueous trifluoroacetic acid.

46. The method of claim 39, wherein washing the acid-washed gel comprises washing the gel with t-butanol.

47. The method of claim 39, wherein pyrolyzing the solvent-exchanged gel comprises heating at a temperature and for a period of time sufficient to convert the gel to a carbon material.

48. The method of claim 39, wherein pyrolyzing the solvent-exchanged gel comprises heating at about 1050°

C. for about 4 hours under nitrogen.

49. The method of claim 39, wherein heating at a temperature and for a time sufficient to provide an activated carbon material comprises heating at about 900°

C. under carbon dioxide.

50. The method of claim 39, further comprising heating the carbon material at a temperature and for a time sufficient to provide an activated carbon material.

51. The method of claim 50, wherein the temperature is about 900°

C., and the time is from about 10 to about 120 minutes.

52. The method of claim 50, wherein the activation is from about 5 to about 90%.

37. A gas storage vessel, comprising a vessel and a carbon material, the carbon material comprising a gravimetric methane storage capacity of about 0.009 to about 0.013 mol/g at room temperature and 500 psi, a surface area of from about 1500 to about 2500 m²/g, and a total pore volume of from about 1.2 to about 1.5 cm³/g.

38. The gas storage vessel of claim 37, further comprising a gas adsorbed on the carbon material, wherein the gas is selected from the group consisting of methane, hydrogen, nitrogen, carbon monoxide, fluorine, nitric oxide, nitrogen trifluoride, silane, ethylene, boron trifluoride, phosphine, arsine, disilane, and carbon tetrafluoride.