IP Library Granted Patent US 7,446,078
Granted Patent B2
US 7,446,078 · App. 10/191,719 · Granted Nov 4, 2008

Adsorbent for water removal from ammonia

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Quick Facts
Patent No.
US 7,446,078
App. No.
10/191,719
Granted
Nov 4, 2008
Kind
B2
Abstract

The present invention provides an adsorbent for removing water and/or other oxygen-containing impurities from a fluid comprising ammonia to the ppb level and methods for making and using same. The adsorbent preferably comprises a substrate having a plurality of pores and a surface area that ranges from about 100 to about 2,500 m 2 /g and a compound disposed within a least a portion of the substrate. In certain preferred embodiments, the compound comprises at least one cation from the group consisting of ammonium (I), lithium (I), sodium (I), potassium (I), cesium (I); magnesium (II), calcium (II), strontium (II), barium (II), manganese (II), nickel (II), iron (II), zinc (II); aluminum (III), indium (III), iron (III), and zirconium (IV) or combinations thereof that is ionically associated with an anion from the group consisting of halide, sulfide, sulfite, or sulfate.

Claims (32)

1. An adsorbent for removing water from a fluid comprising ammonia, the absorbent comprising:

a substrate having a plurality of pores and a surface area that ranges from about 100 to about 2,500 m 2 /g; and

a compound disposed within at least a portion of the substrate, the compound comprising at least one cation selected from the group consisting of ammonium (I), lithium (I), potassium (I), cesium (I); magnesium (II), calcium (II), strontium (II), barium (II), manganese (II), zinc (II); aluminum (Ill), indium (Ill), and zirconium (IV) or combinations thereof that is ionically associated with an anion from the group consisting of sulfide, sulfite and sulfate.

2. The adsorbent of claim 1 wherein the surface area ranges from about 100 to about 1,500 m 2 /g.

3. The adsorbent of claim 2 wherein the surface area ranges from about 100 to about 1,200 m 2 /g.

4. The adsorbent of claim 1 wherein the average pore size within the substrate ranges from about 8 to about 500 Angstroms.

5. The adsorbent of claim 1 wherein the weight percentage of compound disposed within the substrate ranges from about 1 to about 80%.

6. The adsorbent of claim 5 wherein the weight percentage of compound disposed within the substrate ranges from about 2 to about 50%.

7. The adsorbent of claim 1 wherein the cation comprises ammonium.

8. The adsorbent of claim 7 wherein the anion comprises sulfate.

9. The adsorbent of claim 1 wherein the substrate is selected from the group consisting of alumina, activated carbon, or zeolite.

10. A method for preparing an adsorbent for removing water from ammonia, the method comprising:

providing a mixture comprising at least one cation selected from the group consisting of ammonium (I), lithium (I), potassium (I), cesium (I); magnesium (II), calcium (II), strontium (II), barium (II), manganese (II), zinc (II); aluminum (Ill), indium (Ill), and zirconium (IV) or combinations thereof that is ionically associated with an anion from the group consisting of sulfide, sulfite, and sulfate;

impregnating a porous substrate with the mixture to form an adsorbent precursor; and

heating the adsorbent precursor to a temperature of at least about 100° C.or greater to form the adsorbent.

11. The method of claim 10 wherein the mixture further comprises a solvent.

12. The method of claim 11 wherein the method further comprises the step of removing the solvent from the adsorbent precursor.

13. The method of claim 12 wherein the removing and heating are conducted simultaneously.

14. The method of claim 10 wherein the heating is conducted under vacuum conditions.

15. The method of claim 10 wherein the heating is conducted in a nitrogen atmosphere.

16. The method of claim 10 wherein the heating is conducted in an inert atmosphere.

17. The method of claim 10 wherein the substrate is selected from the group consisting of alumina, activated carbon, or zeolite.

18. A method for preparing an adsorbent comprising at least one cation ionically associated with at least one anion, the method comprising:

providing a compound precursor having at least one cation is selected from the group consisting of ammonium (I), lithium (I), sodium (I), potassium (I), cesium (I); magnesium (II), calcium (II), strontium (II), barium (II), manganese (II), zinc (II); aluminum (Ill), indium (Ill), and zirconium (IV) or combinations thereof;

depositing the compound precursor on at least a portion of a porous substrate to form an adsorbent precursor;

heating the adsorbent precursor to a temperature of at least about 100° C. or greater in a gaseous atmosphere to provide an anion from the group consisting of halide, sulfide, sulfite, or sulfate, wherein the gaseous atmosphere comprises a halide gas, a sulfur-containing gas, and combinations thereof; and

reacting the at least one cation and an anion under temperature conditions sufficient to form the adsorbent.

19. The method of claim 18 wherein the substrate is selected from the group consisting of alumina, activated carbon, or zeolite.

20. An adsorbent for removing water from a fluid comprising ammonia comprising:

a substrate comprising an inorganic material, a plurality of pores with an average pore size ranging from about 8 to about 500 Angstroms, and a surface area ranging from about 100 to about 2,500 m 2 /g; and

from 1 to 80% by weight of a compound disposed within at least a portion of the substrate, the compound comprising at least one cation selected from the group consisting of ammonium (I), lithium (I), potassium (I), cesium (I); magnesium (II), calcium (II), strontium (II), barium (II), manganese (II), zinc (II); aluminum (Ill), indium (Ill), and zirconium (IV) or combinations thereof that is ionically associated with an anion from the group consisting of sulfide, sulfite and sulfate.

21. The method of claim 18 wherein the gaseous atmosphere comprises a halide gas, a sulfur-containing gas, or combinations thereof.

Assignments (4)
RELEASE OF SECURITY INTEREST Recorded Oct 7, 2019
From: CITIBANK, N.A., AS AGENT
To: VERSUM MATERIALS US, LLC
Reel/Frame 050647/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 20, 2017
From: AIR PRODUCTS AND CHEMICALS, INC.
To: VERSUM MATERIALS US, LLC
Reel/Frame 041772/0733 →
PATENT SECURITY AGREEMENT Recorded Oct 27, 2016
From: VERSUM MATERIALS US, LLC
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 040503/0442 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 19, 2002
From: DONG, CHUN CHRISTINE; RAO, MADHUKAR BHASKARA; WU, DINGJUN
To: AIR PRODUCTS AND CHEMICALS, INC.
Reel/Frame 013210/0818 →