# US 10,307,729 B2 · Carbide-derived carbons having incorporated metal chloride or metallic nanoparticles

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- Number: US 10,307,729 B2
- Document ID: US10307729B2
- Status: Granted
- Kind: B2
- Application number: 15/795,338
- Filed: 2017-10-27
- Published: 2018-05-03
- Granted: 2019-06-04
- Earliest claimed: 2015-04-24
- Assignees: Georgia Tech Research Corporation
- Applicants: Georgia Tech Research Corporation
- Inventors: Michael Charles Mangarella; Krista S. Walton
- Web page: https://patentgrep.com/patent/US10307729B2

## CPC

- B01J 20/20: comprising free carbon; comprising carbon obtained by carbonising processes
- B01D 53/02: by adsorption, e.g. preparative gas chromatography {(solid sorbent compositions B01J20/00, preparation of inorganic compounds or elements C01)}
- B01J 20/02: comprising inorganic material
- B01J 20/0218: {Compounds of Cr, Mo, W}
- B01J 20/0225: {Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt}
- B01J 20/0229: {Compounds of Fe}
- B01J 20/0248: {Compounds of B, Al, Ga, In, Tl (B01J20/08 takes precedence)}
- B01J 20/0288: {Halides of compounds other than those provided for in B01J20/046}
- B01J 20/06: comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J 20/28007: {with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like (carbon nanostructures B01J20/205)}
- B01J 20/28061: {being in the range 100-500 m2/g}
- B01J 20/28064: {being in the range 500-1000 m2/g}
- B01J 20/28071: {being less than 0.5 ml/g}
- B01J 20/28073: {being in the range 0.5-1.0 ml/g}
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- B01J 20/3204: {Inorganic carriers, supports or substrates}
- B01J 20/3236: {containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts}
- B01J 21/18: Carbon
- B01J 21/185: {Carbon nanotubes (carbon nanotubes per se C01B32/15)}
- B01J 23/28: Molybdenum
- B01J 23/74: Iron group metals
- B01J 23/745: Iron
- B01J 27/128: with iron group metals or platinum group metals
- B01J 27/132: with chromium, molybdenum, tungsten or polonium
- B01J 35/393: {Metal or metal oxide crystallite size}
- B01J 37/18: with gases containing free hydrogen
- B01J 37/24: Chlorinating
- B01D 2253/102: Carbon
- B01D 2253/25: Coated, impregnated or composite adsorbents
- B01D 2257/302: Sulfur oxides
- B01D 2257/304: Hydrogen sulfide
- B01D 2257/406: Ammonia
- B01D 2259/4541: for portable use, e.g. gas masks
- B01J 35/615: {100-500 m2/g}
- B01J 35/617: {500-1000 m2/g}
- B01J 35/618: {more than 1000 m2/g}
- B01J 35/633: {less than 0.5 ml/g}
- B01J 35/635: {0.5-1.0 ml/g}
- B01J 35/638: {more than 1.0 ml/g}
- B01J 35/643: {less than 2 nm}
- B01J 35/647: {2-50 nm}
- B01J 2220/42: Materials comprising a mixture of inorganic materials (materials coated or impregnated on a carrier B01J20/32)
- B01J 2235/00: Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
- B01J 2235/10: Infrared [IR]
- B01J 2235/15: X-ray diffraction
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)

## Abstract

Carbide-derived carbons are provided that have high dynamic loading capacity for high vapor pressure gasses such as H2S, SO2, or NH3. The carbide-derived carbons can have a plurality of metal chloride or metallic nanoparticles entrapped therein. Carbide-derived carbons are provided by extracting a metal from a metal carbide by chlorination of the metal carbide to produce a porous carbon framework having residual metal chloride nanoparticles incorporated therein, and annealing the porous carbon framework with H2 to remove residual chloride by reducing the metal chloride nanoparticles to produce the metallic nanoparticles entrapped within the porous carbon framework. The metals can include Fe, Co, Mo, or a combination thereof. The carbide-derived carbons are provided with an ammonia dynamic loading capacity of 6.9 mmol g−1 to 10 mmol g−1 at a relative humidity of 0% RH to 75% RH.

## Claims

### Claim 1

A carbide-derived carbon comprising a plurality of metal nanoparticles entrapped therein, the carbide derived carbon made by the steps of:
extracting a metal from a metal carbide by chlorination of the metal carbide at a temperature of 500° C. to 700° C. for a period of time from 0.25 hours to 2 hours to produce a porous carbon framework having residual metal chloride nanoparticles incorporated therein, and
annealing the porous carbon framework with H2 to remove residual chloride by reducing the metal chloride nanoparticles to produce the metallic nanoparticles entrapped within the porous carbon framework,
wherein the metal is selected from the group consisting of Fe, Mo, and a combination thereof,
wherein the carbide-derived carbon has a surface area of 300 m2 g−1 to 900 m2 g−1, and
wherein the carbide-derived carbon has a pore volume of 0.25 cc g−1 to 0.5 cc g−1.

### Claim 2 (depends on 1)

The carbide-derived carbon of claim 1, wherein the metal carbide is selected from the group consisting of Fe3C, CoC, Co2C, Co3C, MoC, and Mo2C.

### Claim 3 (depends on 1)

The carbide-derived carbon of claim 1, wherein the carbide is granular having a particle size of about −200/+275 mesh.

### Claim 4 (depends on 1)

The carbide-derived carbon of claim 1, further comprising a plurality of acidic functional groups covalently attached to the porous carbon framework, wherein the acidic functional groups are present at a concentration of about 3 mmol g−1 to 7 mmol g−1 based upon the weight of the carbide-derived carbon.

### Claim 5

A carbide-derived carbon comprising a porous carbon framework having a plurality of metal chloride or metallic nanoparticles entrapped therein,
wherein the nanoparticles comprise a metal selected from the group consisting of Fe, Co, Ni, Al, Mo, and a combination thereof.

### Claim 6 (depends on 5)

The carbide-derived carbon of claim 5, wherein the carbide-derived carbon has a surface area of 300 m2 g−1 to 900 m2 g−1.

### Claim 7 (depends on 5)

The carbide-derived carbon of claim 5, wherein the carbide-derived carbon has a pore volume of 0.2 cc g−1 to 0.8 cc g−1.

### Claim 8 (depends on 5)

The carbide-derived carbon of claim 5, wherein the nanoparticles have an average particle diameter of 1 nm to 10 nm.

### Claim 9 (depends on 5)

The carbide-derived carbon of claim 5, further comprising a plurality of acidic functional groups covalently attached to the porous carbon framework.

### Claim 10 (depends on 9)

The carbide-derived carbon of claim 9, wherein the acidic functional groups are present at a concentration of 2 mmol g−1 to 10 mmol g−1 based upon the weight of the carbide-derived carbon.

### Claim 11 (depends on 5)

The carbide-derived carbon of claim 5, wherein the carbide-derived carbon has an ammonia dynamic loading capacity of 1.5 mmol g−1 to 10 mmol g−1 at 0% RH.

### Claim 12 (depends on 5)

The carbide-derived carbon of claim 5, wherein the carbide-derived carbon has an ammonia dynamic loading capacity of 3 mmol g−1 to 15 mmol g−1 at 75% RH.

### Claim 13 (depends on 5)

The carbide-derived carbon of claim 5, wherein the carbide-derived carbon has an ammonia dynamic loading capacity of 6.9 mmol g−1 to 10 mmol g−1 at a relative humidity of 0% RH to 75% RH.

### Claim 14 (depends on 5)

The carbide-derived carbon of claim 5, wherein the metal is present in an amount from 2.0 wt % to 25.0 wt % based upon the weight of the carbide-derived carbon.

### Claim 15

A carbide-derived carbon comprising a plurality of metallic nanoparticles entrapped therein, the carbide derived carbon made by the steps of:
extracting a metal from a metal carbide by chlorination of the metal carbide to produce a porous carbon framework having residual metal chloride nanoparticles incorporated therein, and
removing residual chloride by reducing the metal chloride nanoparticles to produce the metallic nanoparticles entrapped within the porous carbon framework.

### Claim 16 (depends on 15)

The carbide-derived carbon of claim 15, wherein the metal is selected from the group consisting of Fe, Co, Ni, Al, Mo, and a combination thereof.

### Claim 17 (depends on 15)

The carbide-derived carbon of claim 15, wherein the carbide-derived carbon has a surface area of 300 m2 g−1 to 900 m2 g−1.

### Claim 18 (depends on 15)

The carbide-derived carbon of claim 15, wherein the carbide-derived carbon has a pore volume of 0.2 cc g−1 to 0.8 cc g−1.

### Claim 19 (depends on 15)

The carbide-derived carbon of claim 15, wherein the metallic nanoparticles have an average particle diameter of 1 nm to 10 nm.

### Claim 20 (depends on 15)

The carbide-derived carbon of claim 15, wherein the carbide-derived carbon has an ammonia dynamic loading capacity that is 300% to 1500% greater than the ammonia dynamic loading capacity of the otherwise same carbide-derived carbon except without the metallic nanoparticles,
wherein the ammonia dynamic loading capacities are measured under the same conditions and at the same relative humidity.