IP Library Granted Patent US 9,708,188
Granted Patent B1
US 9,708,188 · App. 15/049,704 · Granted Jul 18, 2017

Method for argon production via cold pressure swing adsorption

Inventors: Shubhra Jyoti Bhadra (Macungie, PA); Roger Dean Whitley (Allentown, PA); Garret Chi-Ho Lau (Emmaus, PA); David Ross Graham (Harleysville, PA); Donn Michael Herron (Fogelsville, PA); Qiao Zhao (Macungie, PA); Erin Marie Sorensen (Allentown, PA)
Assignee: Air Products and Chemicals, Inc.
C01B23/0068B01D53/047B01D2256/00B01D2256/18B01D2257/102B01D2257/104B01D2259/401B01D2259/40086
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Quick Facts
Patent No.
US 9,708,188
App. No.
15/049,704
Granted
Jul 18, 2017
Kind
B1
Abstract

Methods and systems for purifying argon from a crude argon stream are disclosed, employing pressure swing adsorption at cold temperatures from −186° C. to −20° C.; more preferably from −150° C. to −50° C.; and most preferably from −130° C. to −80° C. with oxygen-selective zeolite adsorbent. In some embodiments, the oxygen-selective zeolite adsorbent is a 4A zeolite, a chabazite, or a combination thereof.

Claims (36)

1. A method for producing a purified argon product, the method comprising:

providing a pressurized crude argon vapor stream at a temperature from −186° C. to −20° C.;

introducing the pressurized crude argon vapor stream into a pressure swing adsorption apparatus containing an oxygen-selective zeolite adsorbent and operating the pressure swing adsorption apparatus at a temperature from −186° C. to −20° C.;

withdrawing an argon enriched product from the pressure swing adsorption apparatus; and

regenerating the oxygen-selective zeolite at a pressure greater than prevailing ambient pressure; wherein the operating temperature of the pressure swing adsorption apparatus during operation is not increased except as a function of pressure change or adsorption/desorption.

2. The method of claim 1 , wherein the pressurized crude argon vapor stream comes from an air distillation process produced from the top or near top of a crude argon column, having a composition comprising oxygen, nitrogen, and 50 mole % to 99.5 mole % argon.

3. The method of claim 1 , wherein the pressurized crude argon vapor stream comprises oxygen, about 70 mole % to about 97 mole % argon, and about 0.5 mole % nitrogen.

4. The method of claim 1 , wherein the pressurized crude argon vapor stream is introduced into the pressure swing adsorption apparatus at a temperature from −150° C. to −50° C., and operating the pressure swing adsorption apparatus at a temperature from −150° C. to −50° C.

5. The method of claim 1 , wherein the pressurized crude argon vapor stream is introduced into the pressure swing adsorption apparatus at a temperature from −130° C. to −80° C., and operating the pressure swing adsorption apparatus at a temperature from −130° C. to −80° C.

6. The method of claim 1 , wherein the pressurized crude argon vapor stream is introduced into the pressure swing adsorption apparatus at a feed pressure from 2 bara to 20 bara.

7. The method of claim 1 , wherein the pressurized crude argon vapor stream is introduced into the pressure swing adsorption apparatus at a feed pressure from 2 bara to 8 bara.

8. The method of claim 1 , wherein the oxygen-selective zeolite adsorbent is selected from the 4A type zeolites and sodium exchanged chabazite zeolites.

9. The method of claim 1 , wherein the oxygen-selective zeolite adsorbent is a sodium exchanged chabazite zeolite having a Si/Al ratio from 1.3 to 1.8.

10. The method of claim 9 , wherein the sodium exchanged chabazite zeolite has a Si/Al ratio of about 1.6.

11. The method of claim 1 , wherein the pressure swing adsorption apparatus also comprises one or more equilibrium based zeolites for removing nitrogen.

12. The method of claim 11 , wherein the equilibrium based zeolites for removing nitrogen are selected from sodium X-type zeolite, calcium X-type zeolite, calcium exchanged A zeolite (CaA or 5A), or combinations thereof.

13. The method of claim 1 , wherein prior to introducing the pressurized crude argon vapor stream into the pressure swing adsorption apparatus, at least a portion of the pressurized crude argon vapor stream is increased in pressure to form a compressed argon-containing stream to be fed to the pressure swing adsorption apparatus.

14. The method of claim 1 , wherein the pressurized crude argon vapor stream is created by withdrawing crude argon from an air distillation process as a low pressure vapor, warming the low pressure crude argon vapor and compressing the warmed low pressure crude argon vapor from 2 bara to 8 bara to form the pressurized crude argon vapor.

15. The method of claim 14 , further comprising cooling the pressurized crude argon vapor to from −186° C. to −20° C.

16. The method of claim 1 , wherein the pressurized crude argon vapor stream is created by withdrawing crude argon from an air distillation process as a low pressure vapor and directly compressing the low pressure crude argon vapor to from 2 bara to 8 bara to form the pressurized crude argon vapor.

17. The method of claim 16 , further comprising, adjusting the temperature of the pressurized crude argon vapor to from −186° C. to −20° C.

18. The method of claim 1 , wherein the pressurized crude argon vapor stream is created by withdrawing crude argon from an air distillation process as a low pressure liquid, increasing the pressure of the low pressure crude argon liquid to from 2 bara to 8 bara, and vaporizing the pressurized crude argon liquid to form the pressurized crude argon vapor stream.

19. The method of claim 18 , further comprising adjusting the temperature of the pressurized crude argon vapor stream to from −186° C. to −20° C.

20. The method of claim 1 , wherein regenerating the oxygen-selective zeolite adsorbent is conducted at a pressure from 0.1 bar to 0.5 bar above prevailing ambient pressure.

21. The method of claim 1 , wherein regenerating the oxygen-selective zeolite adsorbent comprises withdrawing an oxygen-enriched gas from the pressure swing adsorption apparatus and recycling it back into a cryogenic distillation column.

22. The method of claim 1 , further comprising feeding the argon enriched product into a distillation column to remove nitrogen.

23. A method for producing a purified argon product, the method comprising:

providing a pressurized crude argon stream from a first cryogenic distillation column;

vaporizing the pressurized crude argon stream;

introducing the vaporized crude argon stream at a temperature from −186° C. to −20° C. and a feed pressure from 2 bara to 8 bara into a pressure swing adsorption (PSA) apparatus containing an oxygen-selective zeolite adsorbent;

operating the PSA apparatus at a temperature from −186° C. to −20° C.;

withdrawing an argon enriched product from the PSA apparatus; and

regenerating the oxygen-selective zeolite at a pressure greater than prevailing ambient pressure; wherein the operating temperature of the PSA apparatus during operation is not increased except as a function of pressure change or adsorption/desorption.

24. The method of claim 23 , wherein the vaporized crude argon stream is introduced to the PSA apparatus at a temperature from −150° C. to −50° C., and operating the PSA apparatus at a temperature from −150° C. to −50° C.

25. The method of claim 23 , wherein the vaporized crude argon stream is introduced to the PSA apparatus at a temperature from −130° C. to −80° C., and operating the PSA apparatus at a temperature from −130° C. to −80° C.

26. The method of claim 23 , wherein the oxygen-selective zeolite adsorbent is selected from 4A zeolites, sodium exchanged chabazites, or combinations thereof.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: BHADRA, SHUBHRA JYOTI; WHITLEY, ROGER DEAN; LAU, GARRET CH-HO; GRAHAM, DAVID ROSS; HERRON, DONN MICHAEL; ZHAO, QIAO; SORENSEN, ERIN MARIE
To: AIR PRODUCTS AND CHEMICALS, INC.
Reel/Frame 038382/0302 →