Activated graphitic carbon and metal hybrids thereof

• US 20050196336A1
• Filed: 03/07/2005
• Published: 09/08/2005
• Est. Priority Date: 03/05/2004
• Status: Abandoned Application

• Current Assignee: Anthony Michael Woolf, Arup Kumar Chatterjee
• Original Assignee: Anthony Michael Woolf, Arup Kumar Chatterjee
• Inventors: Chatterjee, Arup Kumar, Woolf, Anthony Michael
• Application Number:
  US11/072,425
• Publication Number:
  US 20050196336A1
• Time in Patent Office: Days
• US Class Current: 423/448
• CPC Class Codes: B01J 20/02 comprising inorganic material
• CPC Class Codes: B01J 20/041 Oxides or hydroxides
• CPC Class Codes: B01J 20/06 comprising oxides or hydroxides of metals not provided for in group B01J20/04
• CPC Class Codes: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes
• CPC Class Codes: B01J 20/205 Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs carbon nanotubes per se C01B32/15
• CPC Class Codes: B01J 20/28004 Sorbent size or size distribution, e.g. particle size
• CPC Class Codes: B01J 20/28016 Particle form
• CPC Class Codes: B01J 20/2805 Sorbents inside a permeable or porous casing, e.g. inside a container, bag or membrane
• CPC Class Codes: B01J 20/28057 Surface area, e.g. B.E.T specific surface area
• CPC Class Codes: B01J 20/28061 being in the range 100-500 m2/g
• CPC Class Codes: B01J 20/2808 being less than 2 nm, i.e. micropores or nanopores
• CPC Class Codes: B01J 20/28083 being in the range 2-50 nm, i.e. mesopores
• CPC Class Codes: B01J 20/28097 being coated, filled or plugged with specific compounds
• CPC Class Codes: B01J 20/3078 Thermal treatment, e.g. calcining or pyrolizing
• CPC Class Codes: B01J 20/3204 Inorganic carriers, supports or substrates
• CPC Class Codes: B01J 20/3236 containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
• CPC Class Codes: B01J 2220/4825 Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
• CPC Class Codes: B01J 2220/485 Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
• CPC Class Codes: C01B 3/0015 Organic compounds; Solutions thereof
• CPC Class Codes: C01B 32/21 After-treatment
• CPC Class Codes: C01B 32/324 : from waste materials, e.g. tyres or spent sulfite pulp liquor
• CPC Class Codes: C01B 32/342 : characterised by non-gaseous activating agents
• CPC Class Codes: Y02E 60/32 : Hydrogen storage

Abstract

A graphitized activated carbon and a method for the preparation thereof is disclosed. The material is comprised of bundles of aligned tubes that share a common wall and range from 10 to 500 micrometeres in length. Individual particle diameters range from 5 to 150 micrometers, and individual tube diameters are 1 to 10 micrometers. The shared walls are no thicker than 3 micrometers, and preferably less than 1 micrometer thick. Embedded within said walls are pores and channels of a diameter in a range of less than 1 to 50 nanometers, preferably less than 5 nanometers. When the carbonaceous particles are combined with metallic species including oxides, alloys, and/or multi-metal combinations, the hybrid material is useful for reversible storage of gas, including hydrogen, and do not require reaction of the metal components with hydrogen prior to combination with the carbon component.

Claims

1. The structure of an activated graphitic carbon that is comprised of bundles of longitudinally aligned tubes that share common walls and wherein the said wall structures are predominantly comprised of graphitic carbon and contain pores leading to channels within the tube walls.

2. The structure of claim 1 wherein the diameter of the longitudinally aligned tubes is from 0.5 to 10 micrometers.

3. The structure of claim 1 wherein the thickness of said graphitic tube walls is no more than 3 micrometers.

4. The structure of claim 1 wherein the pores within the walls of the tubes have an opening diameter smaller than 50 nanometers and lead to internal channels which branch successively, and wherein each internal branch may have successively smaller diameter.

5. The structure of claim 1 wherein the surface area by BET methodology using Nitrogen gas is greater than 250 m{circumflex over ( 

)}2 per gram.

6. A method to produce the structure of claim 1.

7. The material of claim 1 wherein particles of metal, multi metal, alloy, metal oxide, or combination thereof are associated with the tube walls, pores and/or channels described, and the graphite sheets which comprise said walls, channels and pores.

8. A structure in accordance with claim 7 wherein the metal, multi metal, alloy, and/or metal-oxide particles or combination thereof, include at least one element from Group IA, IIA, IIIA, IVB, VB, VIB, VIIB, VIII, IB or IIB of the Periodic Table of Elements.

9. A Process in accordance with claim 8 wherein the particles of metal, multi metal, alloy, metal oxide or combination thereof are incorporated into the carbon material by solution chemistry, electrodepositon, chemical vapor deposition with or without energetic augmentation, or by thermal decomposition of a metal salt placed in solution with the carbon and an energetic material such as urea or glycerine, such that the size of each metallic particle species may be controlled as desired and range from small angstrom scale clusters of several atoms, having diameters from 5 to 150 angstroms, to larger nanometer scale accumulations of metallic atoms comprised of hundreds to thousands of atoms and having diameters from 1 to 150 nanometers.

10. The method of claim 6 wherein the precursor material is derived from plant material such as plant stalks and contains a plurality of plant xylem and/or phloem tissue.

11. The method of claim 6 wherein the plant precursor material is sugar cane bagasse, corn stalks, and/or rice straw that has been dried and ground to the desired particle size.

12. A process in accordance with claim 6 wherein the precursor material is treated with Potassium or Sodium Hydroxide prior to pyrolysis.

13. A process in accordance with claim 6 wherein pyrolysis is completed at temperatures between 800 and 1200 C under an inert atmosphere for a period of time ranging from 15 to 60 minutes.

14. A process in accordance with claim 6 wherein the material is purified and activated by refluxing in a solution of nitric acid for a period of up to 12 hours.

16. A process in accordance with claim 6 wherein the pyrolyzed carbon is activated by a known chemical or physical methodology.

17. A process wherein the materials of claims 1 and/or claim 7 are compacted under pressure.

18. A process for reversibly sorbing hydrogen, methane, other light gases, to the structures of claim 1 and/or claim 7 using known pressure swing, temperature swing, combination pressure and temperature swing methods and apparatus.

20. A method for the use of the material of claim 1 as a charge separation material for use as the electrode in an electric double layer capacitor.

15. A process to remove amorphous carbon from highly structured and nanostructured graphitic carbon materials without removing metals that are associated with the graphitic carbon by placing the unpurified carbon into a standard mixing device with a neutral solution of potassium permanganate and stirring over mild heat or using a known reflux apparatus to treat the material until the desired purity is attained.

19. A process wherein a given sorbent material is packaged into a thin, lightweight container, such as a polymer or metal vessel or bag, that is permeable to the desired sorbent gas and has a conformation so as to promote heat transfer to and from the sorbent material, and to facilitate ready removal of the sorbent material from the adsorption/desorption apparatus.