IP Library Granted Patent US 8,366,979
Granted Patent B2
US 8,366,979 · App. 13/011,554 · Granted Feb 5, 2013

Robust carbon monolith having hierarchical porosity

Inventors: Sheng Dai (Knoxville, TN); Georges A. Guiohon (Farragut, TN); Chengdu Liang (Knoxville, TN)
Assignees: UT-Battelle, LLC; University of Tennessee Research Foundation
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Quick Facts
Patent No.
US 8,366,979
App. No.
13/011,554
Granted
Feb 5, 2013
Kind
B2
Abstract

A carbon monolith includes a robust carbon monolith characterized by a skeleton size of at least 100 nm, and a hierarchical pore structure having macropores and mesopores.

Claims (16)

1. A method of preparing a monolithic chromatography column comprising the step of:

providing a carbon monolith precursor having a particulate, porosity-generating fugitive phase dispersed therein, said precursor comprising at least one carbonizable polymer, and said fugitive phase comprising mesoparticles and macroparticles;

carbonizing said carbon monolith precursor to form a carbon monolith comprising said fugitive phase;

removing said fugitive phase from said carbon monolith by dissolution to form a robust, porous carbon monolith characterized by a skeleton size having a wall thickness of at least 100 nm and a hierarchical pore structure having macropores and mesopores, said macropores having a size ranging from 0.05 μm to 100 μm, and said mesopores having a size ranging from 18 Å to 50 nm; and

encapsulating said porous carbon monolith within a cladding material which conforms to the shape of the resulting carbon monolith to form a chromatographic column.

2. A method in accordance with claim 1 wherein said porosity-generating fugitive phase comprises a material that is soluble in a solvent that does not harm said porous carbon monolith.

3. A method in accordance with claim 1 wherein said porosity-generating fugitive phase comprises silica.

4. A method in accordance with claim 1 further comprising, after said removing step, an additional step of graphitizing said porous carbon monolith.

5. A method according to claim 1 wherein the carbon monolith precursor is prepared by admixing the porosity-generating fugitive phase with an iron (III) complex of resorcinol and formaldehyde to form an admixture, and polymerizing said admixture to form said carbon monolith precursor.

6. A method in accordance with claim 1 wherein said wall thickness is 100 nm to 20 μm.

7. A method in accordance with claim 6 wherein said wall thickness is 200 nm to 10 μm.

8. A method in accordance with claim 7 wherein said wall thickness is 400 nm to 1 μm.

9. A method in accordance with claim 1 wherein said macropores are of a size range of 0.1 μm to 50 μm.

10. A method in accordance with claim 9 wherein said macropores are of a size range of 0.8 μm to 10 μm.

11. A method in accordance with claim 1 wherein said mesopores are of a size range of 0.5 nm to 40 nm.

12. A method in accordance with claim 11 wherein said mesopores are of a size range of 5 nm to 30 nm.

Continuity (3)
Continuation 12145927 · Jun 25, 2008
Continuation 10770734 · Feb 3, 2004
Related Publication 20110140296A1 · Jun 16, 2011