# US 8,569,205 B2 · Media for removal of contaminants from fluid streams and method of making same

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- Number: US 8,569,205 B2
- Document ID: US8569205B2
- Status: Granted
- Kind: B2
- Application number: 12/830,684
- Filed: 2010-07-06
- Published: 2011-01-06
- Granted: 2013-10-29
- Earliest claimed: 2009-07-06
- Assignees: MAR Systems, Inc.
- Applicants: Anthony E. Kuhel; Harry A. Adams; Gina Sacco
- Inventors: Anthony E. Kuhel; Harry A. Adams; Gina Sacco
- Web page: https://patentgrep.com/patent/US8569205B2

## CPC

- B01J 20/20: comprising free carbon; comprising carbon obtained by carbonising processes
- B01J 20/02: comprising inorganic material
- B01J 20/0229: {Compounds of Fe}
- B01J 20/0237: {Compounds of Cu}
- B01J 20/0248: {Compounds of B, Al, Ga, In, Tl (B01J20/08 takes precedence)}
- B01J 20/0266: {Compounds of S}
- B01J 20/0281: {Sulfates of compounds other than those provided for in B01J20/045}
- B01J 20/0285: {Sulfides of compounds other than those provided for in B01J20/045}
- B01J 20/06: comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J 20/08: comprising aluminium oxide or hydroxide; comprising bauxite
- B01J 20/3204: {Inorganic carriers, supports or substrates}
- B01J 20/3236: {containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts}
- C02F 1/281: {using inorganic sorbents}
- C02F 1/288: {using composite sorbents, e.g. coated, impregnated, multi-layered}
- G21F 9/12: by absorption; by adsorption; by ion-exchange
- C02F 2101/20: Heavy metals or heavy metal compounds
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- G21F: PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR (radiation protection by pharmaceutical means A61K8/00, A61Q17/04; in cosmonautic vehicles B64G1/54; combined with a reactor G21C11/00; combined with X-ray tubes H01J35/16; combined with X-ray apparatus H05G1/02)

## Abstract

Sorption media for removal of contaminants from fluid streams are provided. The sorption media comprise an active compound bound or linked to a support substrate or matrix. Support substrates can include iron- and alumina-based materials. A method for making sorption media for the removal of contaminants from fluid streams is also described. The method includes selecting a support substrate, and, optionally, providing a doping mixture comprising an active compound. The selected support substrate can be contacted with the doping mixture to form a doped mixture. The doped mixture can be reacted at a predetermined temperature and atmospheric environment for a predetermined duration to form an active media, wherein the active compound is bound or linked to the support substrate.

## Claims

### Claim 1

A sorption media, comprising:
a support substrate, the support substrate comprising a porous metallic material; and
a sulfur species chemically bonded to the support substrate,
wherein the media includes at least 10 mol % aluminum species, and
wherein the sorption media further comprises an iron species.

### Claim 2 (depends on 1)

The sorption media of claim 1, wherein the sulfur species comprises at least 50 mol % sulfate.

### Claim 3 (depends on 2)

The sorption media of claim 2, wherein the sulfur species comprises at least 90 mol % sulfate.

### Claim 4 (depends on 1)

The sorption media of claim 1, wherein the sorption media has a sulfur content of at least 0.2 mol %.

### Claim 5 (depends on 1)

The sorption media of claim 1, wherein the bond between the sulfur species and support substrate reduces the amount of sulfur species removed from the support substrate when the media is in contact with a fluid relative to the amount of sulfur species that would be removed without said bond.

### Claim 6 (depends on 1)

The sorption media of claim 1, wherein the sorption media further comprises a copper species.

### Claim 7 (depends on 1)

The sorption media of claim 1, wherein the sulfur species is chemically bonded to the support substrate by at least one of an ionic bond and a covalent bond.

### Claim 8 (depends on 1)

The sorption media of claim 1, wherein the support substrate comprises alumina.

### Claim 9

A sorption media, comprising:
a support substrate, the support substrate comprising a porous metallic material; and
a sulfur species chemically bonded to the support substrate,
wherein the media includes at least 10 mol % aluminum species, and
wherein the sulfur species comprises at least 80 mol % sulfide.

### Claim 10

A sorption media, comprising:
a support substrate, the support substrate comprising a porous metallic material; and
a sulfur species chemically bonded to the support substrate,
wherein the media includes at least 10 mol % aluminum species, and
wherein the sorption media has a contaminant capacity of at least 113 mg-mercury/kg-media.

### Claim 11 (depends on 10)

The sorption media of claim 10, wherein the sorption media has a contaminant capacity of at least 2000 mg-mercury/kg-media.

### Claim 12 (depends on 11)

The sorption media of claim 11, wherein the sorption media has a contaminant capacity of at least 3000 mg-mercury/kg-media.

### Claim 13 (depends on 12)

The sorption media of claim 12, wherein the sorption media has a contaminant capacity of at least 10,000 mg-mercury/kg-media.

### Claim 14

A sorption media, comprising:
a support substrate, the support substrate comprising a porous metallic material; and
a sulfur species chemically bonded to the support substrate,
wherein the media includes at least 9 mol % iron species, and
wherein the media further comprises an aluminum species.

### Claim 15 (depends on 14)

The sorption media of claim 14, wherein the sulfur species comprises at least 70 mol % sulfide.

### Claim 16 (depends on 15)

The sorption media of claim 15, wherein the sulfur species comprises at least 80 mol % sulfide.

### Claim 17 (depends on 14)

The sorption media of claim 14, wherein the sorption media has a sulfur content of at least 1.7 mol %.

### Claim 18 (depends on 14)

The sorption media of claim 14, wherein the bond between the sulfur species and support substrate reduces the amount of sulfur species removed from the support substrate when the media is in contact with a fluid relative to the amount of sulfur species that would be removed without said bond.

### Claim 19 (depends on 14)

The sorption media of claim 14, wherein the sulfur species is chemically bonded to the support substrate by at least one of an ionic bond and a covalent bond.

### Claim 20 (depends on 14)

The sorption media of claim 14, wherein the support substrate comprises iron oxides.

### Claim 21 (depends on 14)

The sorption media of claim 14, wherein the support substrate comprises an iron-containing catalyst for the removal of sulfur compounds from a gas stream.

### Claim 22

A sorption media, comprising:
a support substrate, the support substrate comprising a porous metallic material; and
a sulfur species chemically bonded to the support substrate,
wherein the media includes at least 9 mol % iron species, and
wherein the sulfur species comprises at least 60 mol % sulfate.

### Claim 23

A sorption media, comprising:
a support substrate, the support substrate comprising a porous metallic material; and
a sulfur species chemically bonded to the support substrate,
wherein the media includes at least 9 mol % iron species, and
wherein the sorption media has a contaminant capacity of at least 340 mg-mercury/kg-media.

### Claim 24 (depends on 23)

The sorption media of claim 23, wherein the sorption media has a contaminant capacity of at least 1000 mg-mercury/kg-media.

### Claim 25 (depends on 24)

The sorption media of claim 24, wherein the sorption media has a contaminant capacity of at least 3500 mg-mercury/kg-media.

### Claim 26 (depends on 25)

The sorption media of claim 25, wherein the sorption media has a contaminant capacity of at least 12,000 mg-mercury/kg-media.

### Claim 27

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material, the support substrate further comprising iron;
providing a doping mixture comprising a first sulfur species dissolved in a solvent;
contacting the selected support substrate with the doping mixture at a first temperature for a first duration to form a doped substrate; and
reacting the doped substrate at a second temperature in a selected atmospheric environment for a second duration to form the sorption media,
wherein the sorption media comprises a second sulfur species chemically bonded to the support substrate.

### Claim 28 (depends on 27)

The method of claim 27, wherein the doping mixture includes at least one of ferric sulfate, ammonium sulfate, copper sulfate, and copper chloride.

### Claim 29 (depends on 27)

The method of claim 27, wherein the first temperature is between about 20° C. and about 60° C.

### Claim 30 (depends on 27)

The method of claim 27, wherein the first duration is between about 20 minutes and about 45 minutes.

### Claim 31 (depends on 27)

The method of claim 27, wherein the second temperature is between about 150° C. and about 400° C.

### Claim 32 (depends on 27)

The method of claim 27, wherein the second duration is between about 0.5 hours and about 6 hours.

### Claim 33 (depends on 27)

The method of claim 27, wherein the atmospheric environment comprises about 3 vol % to about 10 vol % hydrogen.

### Claim 34 (depends on 27)

The method of claim 27, wherein the atmospheric environment comprises about 50 vol % to about 95 vol % nitrogen.

### Claim 35 (depends on 27)

The method of claim 27, wherein the doping mixture further comprises copper.

### Claim 36 (depends on 27)

The method of claim 27, the support substrate further comprising a copper species.

### Claim 37 (depends on 27)

The method of claim 27, wherein the second sulfur species is chemically bonded to the support substrate by at least one of an ionic bond and a covalent bond.

### Claim 38

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material, the support substrate further comprising alumina;
providing a doping mixture comprising a first sulfur species dissolved in a solvent;
contacting the selected support substrate with the doping mixture at a first temperature for a first duration to form a doped substrate; and
reacting the doped substrate at a second temperature in a selected atmospheric environment for a second duration to form the sorption media,
wherein the sorption media comprises a second sulfur species chemically bonded to the support substrate.

### Claim 39

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material;
providing a do in mixture comprising a first sulfur species dissolved in a solvent;
contacting the selected support substrate with the doping mixture at a first temperature for a first duration to form a doped substrate; and
reacting the doped substrate at a second temperature in a selected atmospheric environment for a second duration to form the sorption media, wherein the atmospheric environment comprises about 2 vol % to about 5 vol % hydrogen sulfide,
wherein the sorption media comprises a second sulfur species chemically bonded to the support substrate.

### Claim 40

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material;
providing a doping mixture comprising a first sulfur species dissolved in a solvent;
contacting the selected support substrate with the doping mixture at a first temperature for a first duration to form a doped substrate; and
reacting the doped substrate at a second temperature in a selected atmospheric environment for a second duration to form the sorption media, wherein the atmospheric environment comprises less than about 35 vol % air,
wherein the sorption media comprises a second sulfur species chemically bonded to the support substrate.

### Claim 41

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material, the support substrate further comprising alumina;
selecting an atmospheric environment comprising at least hydrogen sulfide; and
reacting the support substrate at a first temperature in the selected atmospheric environment for a first duration to form the sorption media,
wherein the selected sorption media comprises a sulfur species chemically bonded to the support substrate.

### Claim 42 (depends on 41)

The method of claim 41, wherein the first temperature is between about 120° C. and about 400° C.

### Claim 43 (depends on 41)

The method of claim 41, wherein the first duration is between about 1 hours and about 6 hours.

### Claim 44 (depends on 41)

The method of claim 41, wherein the atmospheric environment comprises about 2 vol % to about 5 vol % hydrogen sulfide.

### Claim 45 (depends on 41)

The method of claim 41, the support substrate further comprising iron and a copper species.

### Claim 46 (depends on 41)

The method of claim 41, wherein the sulfur species is chemically bonded to the support substrate by at least one of an ionic bond and a covalent bond.

### Claim 47

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material;
selecting an atmospheric environment comprising at least hydrogen sulfide and further comprising about 3 vol % to about 10 vol % hydrogen; and
reacting the support substrate at a first temperature in the selected atmospheric environment for a first duration to form the sorption media,
wherein the selected sorption media comprises a sulfur species chemically bonded to the support substrate.

### Claim 48

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material;
selecting an atmospheric environment comprising at least hydrogen sulfide and further comprising about 50 vol % to about 95 vol % nitrogen; and
reacting the support substrate at a first temperature in the selected atmospheric environment for a first duration to form the sorption media,
wherein the selected sorption media comprises a sulfur species chemically bonded to the support substrate.

### Claim 49

A method of manufacturing a sorption media, comprising:
selecting a support substrate comprising a porous metallic material;
selecting an atmospheric environment comprising at least hydrogen sulfide and further comprising less than about 35 vol % air; and
reacting the support substrate at a first temperature in the selected atmospheric environment for a first duration to form the sorption media,
wherein the selected sorption media comprises a sulfur species chemically bonded to the support substrate.

### Claim 50

A method manufacturing a
sorption media, comprising:
selecting a support substrate comprising a porous metallic material;
selecting an atmospheric environment comprising at least hydrogen sulfide;
mixing elemental sulfur with the selected substrate; and
reacting the support substrate at a first temperature in the selected atmospheric environment for a first duration to form the sorption media, wherein the mixing elemental sulfur with the selected substrate occurs before reacting the support substrate in the selected atmospheric environment,
wherein the selected sorption media comprises a sulfur species chemically bonded to the support substrate.

### Claim 51 (depends on 50)

The method of claim 50, wherein an amount of the elemental sulfur mixed with the selected substrate is between about 10 wt % and about 35 wt % of a total weight of the elemental sulfur and selected substrate combined.

### Claim 52 (depends on 50)

The method of claim 50, wherein the first temperature is between about 130° C. and about 300° C.

### Claim 53 (depends on 50)

The method of claim 50, wherein the first duration is between about 0.5 hours and about 6 hours.

### Claim 54 (depends on 50)

The method of claim 50, wherein the atmospheric environment comprises about 85 vol % to about 95 vol % nitrogen.

### Claim 55 (depends on 50)

The method of claim 50, wherein the atmospheric environment comprises substantially no air.
