Manufacturing methods for the production of carbon materials

• US 8,293,818 B2
• Filed: 04/08/2010
• Issued: 10/23/2012
• Est. Priority Date: 04/08/2009
• Status: Active Grant

• Current Assignee: BASF SE
• Original Assignee: EnerG2 Technologies, Incorporated
• Inventors: Costantino, Henry R., Feaver, Aaron, Scott, William D.
• Primary Examiner(s): Cain, Edward
• Application Number:
  US12/756,668
• Publication Number:
  US 20110028599A1
• Time in Patent Office: 929 Days
• Field of Search: 523/309, 523/307
• US Class Current: 523/309
• 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 32/336 characterised by gaseous activating agents
• CPC Class Codes: C08G 8/22 Resorcinol
• CPC Class Codes: C08G 8/28 Chemically modified polycondensates
• CPC Class Codes: C08J 3/12 Powdering or granulating
• CPC Class Codes: C08K 5/04 Oxygen-containing compounds C08K5/0091 takes precedence
• CPC Class Codes: H01G 11/34 characterised by carbonisation or activation of carbon
• CPC Class Codes: H01M 4/96 Carbon-based electrodes
• CPC Class Codes: H01M 8/0234 Carbonaceous material
• CPC Class Codes: Y02E 60/13 Energy storage using capacitors
• CPC Class Codes: Y02E 60/32 Hydrogen storage
• CPC Class Codes: Y02E 60/50 Fuel cells
• CPC Class Codes: Y02P 70/50 Manufacturing or production processes characterised by the final manufactured product
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]

Abstract

The present application is generally directed to activated carbon materials and methods for making the same. The disclosed methods comprise rapidly freezing synthetically prepared polymer gel particles. The methods further comprise drying, pyrolyzing, and activating steps to obtain an activated carbon material of high porosity. The disclosed methods represent viable manufacturing processes for the preparation of activated carbon materials.

Claims

1. A method for making frozen polymer gel particles, the method comprising rapidly freezing polymer gel particles, wherein the polymer gel particles have been generated from a polymer gel, and wherein the polymer gel has been prepared by reaction of one or more polymer precursors, wherein rapidly freezing the polymer gel particles comprises immersing the polymer gel particles in a liquid having a temperature below about −

10°

C.

2. The method of claim 1, wherein rapidly freezing the polymer gel particles comprises immersing the polymer gel particles in a liquid having a temperature below about −

30°

C.

3. The method of claim 1, wherein the polymer gel particles are generated by grinding or milling the polymer gel.

4. The method of claim 1, wherein the liquid is liquid nitrogen.

5. The method of claim 1, wherein the liquid is ethanol.

6. The method of claim 1, wherein the polymer gel particles have an average particle size of less than about 30 mm.

7. The method of claim 6, wherein the polymer gel particles have an average particle size of about 0.5 mm to about 10 mm.

8. The method of claim 1, wherein the polymer gel particles are immersed in the liquid at a rate of about 5 grams/min.

9. A method for making frozen polymer gel particles, the method comprising rapidly freezing polymer gel particles, wherein the polymer gel particles have been generated from a polymer gel, and wherein the polymer gel has been prepared by reaction of one or more polymer precursors, wherein rapidly freezing the polymer gel particles comprises:

a) admixing the polymer gel particles with a cold solid;

b) admixing the polymer gel particles with a gas having a temperature below about −

10°

C.;

or

c) grinding or milling the polymer gel in the presence of a cold solid.

10. The method of claim 9, wherein the cold solid is solid carbon dioxide.

11. The method of claim 9, wherein the gas is nitrogen.

12. The method of claim 9, wherein the cold solid is solid carbon dioxide.

13. A method for making frozen polymer gel particles, the method comprising rapidly freezing polymer gel particles, wherein the polymer gel particles have been generated from a polymer gel, and wherein the polymer gel has been prepared by reaction of one or more polymer precursors, wherein rapidly freezing the polymer gel particles comprises:

a) contacting the polymer gel particles with an atomized liquid having a temperature below about −

10°

C.;

b) contacting sprayed droplets comprising the polymer gel particles with a cold medium having a temperature below about −

10°

C. to obtain frozen droplets comprising the frozen polymer gel particles;

or

c) rapidly pulling a vacuum on the polymer gel particles.

14. The method of claim 13, wherein rapidly freezing the polymer gel particles comprises contacting the polymer gel particles with an atomized liquid having a temperature below about −

30°

C.

15. The method of claim 13, wherein the atomized liquid is liquid nitrogen.

16. The method of claim 13, wherein the cold medium has a temperature below about −

30°

C.

17. The method of claim 13, wherein the sprayed droplets comprise a suspension of the polymer gel particles.

18. The method of claim 13, wherein the polymer gel particles comprise polymer gel having a viscosity of less than about 1000 cP.

19. The method of claim 13, wherein the polymer gel particles comprise incompletely polymerized polymer gel.

20. The method of claim 19, wherein polymerization of the polymer gel is completed after the sprayed droplets are contacted with the cold medium (i.e. after the freezing step).

21. The method of claim 20, further comprising lyophilizing the frozen droplets to obtain freeze-dried particles and completing the polymerization reaction within the freeze-dried particle.

22. The method of claim 20, further comprising completing the polymerization of the polymer gel within the frozen droplets.

23. The method of claim 13, wherein the sprayed droplets further comprise microspheres comprising the polymer gel particles.

24. The method of claim 23, wherein the microspheres comprise an emulsion selected from a water-in-oil (w/o) emulsion, oil-in-water (o/w) emulsion, oil-in-water-oil (o/w/o) emulsion, water-in-oil-in-water (w/o/w) emulsion, and water-in-oil-in-oil (w/o/o) emulsion.

25. The method of claim 24, wherein the emulsion comprises a surfactant selected from non-ionic, cationic, non-ionic polymeric, and non-ionic polymeric fluorinated surfactants.

26. The method of claim 13, wherein the cold medium is liquid nitrogen or ethanol.

27. A polymer cryogel comprising less than about 1000 ppm of t-butanol, wherein the polymer cryogel has a tap density of between about 0.15 cc/g and about 0.25 cc/g.