Method and apparatus for removing residual hydrogen from a purified gas

• US 5,238,469 A
• Filed: 04/02/1992
• Issued: 08/24/1993
• Est. Priority Date: 04/02/1992
• Status: Expired

• Current Assignee: SAES Pure Gas Incorporated (Entegris Incorporated)
• Original Assignee: SAES Pure Gas Incorporated (Entegris Incorporated)
• Inventors: Briesacher, Jeffrey L., Applegarth, Charles H., Lorimer, D'Arcy H.
• Primary Examiner(s): SPITZER, ROBERT H
• Application Number:
  US07/862,399
• Time in Patent Office: 509 Days
• Field of Search: 55/27, 55/28, 55/66, 55/68, 55/74, 55/76, 55/208, 55/267-269, 55/387, 165/171
• US Class Current: 95/115
• CPC Class Codes: B01D 2256/10 Nitrogen
• CPC Class Codes: B01D 2256/18 Noble gases
• CPC Class Codes: B01D 2257/102 Nitrogen
• CPC Class Codes: B01D 2257/108 Hydrogen
• CPC Class Codes: B01D 2257/11 Noble gases
• CPC Class Codes: B01D 2258/0216 from CVD treatment or semi-conductor manufacturing
• CPC Class Codes: B01D 2259/402 using two beds
• CPC Class Codes: B01D 2259/41 using plural beds of the same adsorbent in series
• CPC Class Codes: B01D 53/04 with stationary adsorbents B01D53/025 takes precedence
• CPC Class Codes: B01D 53/0407 Constructional details of adsorbing systems

Abstract

The invention relates generally to a gas purification system for the purification of noble gasses and nitrogen. An improved method of purification generally includes the following steps: (a) heating an impure gas; (b) contacting the impure gas with an impurity sorbing material to produce a purified gas; (c) cooling the purified gas to a temperature less than about 100° C.; and (d) contacting the purified gas with a hydrogen sorbing gas to remove residual hydrogen. The system includes an improved heat exchange apparatus for cooling the purified gas and a low temperature hydrogen sorption apparatus.

Claims

1. A method for removing residual hydrogen from a purified gas comprising the steps of:

(a) heating an impure gas;

(b) contacting the heated impure gas with an impurity sorbing material to produce a purified gas having trace amounts of residual hydrogen;

(c) cooling the purified gas to a temperature less than about 100°

C.; and

(d) contacting the cooled purified gas with a hydrogen sorbing material to at least partially remove said residual hydrogen.

2. A method as recited in claim 1 wherein the impure gas is heated to more than about 200°

C.

3. A method as recited in claim 2 wherein the purified gas is cooled to less than about 60°

C.

4. A method as recited in claim 3 wherein the purified gas is cooled to less than about 40°

C.

5. A method as recited in claim 1 wherein said impure gas includes at least a component which is selected from the group consisting essentially of nitrogen, helium, neon, argon, krypton, xenon, and radon.

6. A method as recited in claim 1 wherein said impurity sorbing material includes a non-evaporative getter material selected from the group consisting essentially of zirconium-vanadium-iron alloys and zirconium-iron alloys.

7. A method as recited in claim 1 wherein said hydrogen sorbing material includes a material selected from the group consisting essentially of zirconium, palladium, platinum, rhodium, ruthenium, nickel, titanium, and alloys thereof.

8. A method as recited in claim 7 wherein said hydrogen sorbing material includes a non-evaporative getter material selected from the group consisting essentially of zirconium-vanadium-iron alloys and zirconium-iron alloys.

9. A method as recited in claim 1 wherein said step of cooling said purified gas comprises flowing said purified gas through at least one conduit, wherein said conduit has a substantially constant wall temperature which is less than about 100°

C.

10. A gas purification system comprising:

(a) gas inlet means for impure gas;

(b) heating means coupled to said gas inlet means for heating said impure gas to a temperature greater than about 200°

C.;

(c) purifier means coupled to said heating means, said purifier means including a getter material capable of removing impurities from said impure gas to produce a purified gas;

(d) cooling means coupled to said purifier means for cooling said purified gas to a temperature less than about 100°

C.;

(e) hydrogen sorbing means coupled to said cooling means which includes a hydrogen sorbing material to remove residual hydrogen from said purified gas; and

(f) a gas outlet for said purified gas.

11. A gas purification system as recited in claim 10 wherein said impure gas is heated to about 300°

-450°

C. by said heating means and said purified gas is cooled to less than about 60°

C. by said cooling means.

12. A gas purification system as recited in claim 10 wherein said getter material comprises a non-evaporative getter alloy selected from the group consisting essentially of zirconium-vanadium-iron alloys and zirconium-iron alloys.

13. A gas purification system as recited in claim 10 wherein said hydrogen sorbing material is selected from the group consisting essentially of zirconium, palladium, platinum, rhodium, ruthenium, nickel, titanium, and alloys thereof.

14. A gas purification system as recited in claim 10 wherein said hydrogen sorbing material comprises a non-evaporative getter alloy selected from the group consisting essentially of zirconium-vanadium-iron alloys and zirconium-iron alloys.

15. A gas purification system as recited in claim 10 wherein said cooling means comprises:

(a) a first manifold, including a first plurality of integral connector nipples;

(b) a second manifold, including a second plurality of integral connector nipples aligned with said connector nipples of said first manifold;

(c) a plurality of straight tubes, each tube extending between a first connector nipple on said first manifold and a second connector nipple on said second manifold, each of said straight tubes being welded in place at the first manifold and at the second manifold.

16. A gas purification system as recited in claim 15 wherein said cooling means further comprises heat sink means contacting said plurality of straight tubes to maintain the temperature of said tubes at a substantially constant temperature along their lengths.

17. A gas purification system as recited in claim 16 wherein said heat sink means comprises a first plate contacting said plurality of tubes on a first side thereof and a second plate contacting said plurality of tubes on a second side thereof.

18. A gas purification system as recited in claim 16 further comprising means for removing heat energy from said heat sink means.

19. A heat exchange apparatus comprising:

(a) a first monoblock manifold formed from a single piece of material and including a first plurality of integral connector nipples such that interior surfaces of said first plurality of connector nipples do not include a joint between a plurality of pieces;

(b) a second monoblock manifold formed from a single piece of material and including a second plurality of integral connector nipples aligned with said connector nipples of said first manifold such that interior surfaces of said second plurality of connector nipples do not include a joint between a plurality of pieces;

(c) a plurality of straight tubes, each tube extending between a first connector nipple on said first manifold and a second connector nipple on said second manifold, each of said straight tubes being welded in place at the first manifold and at the second manifold.

20. A heat exchange apparatus as recited in claim 19 further comprising heat sink means contacting said plurality of straight tubes to maintain the temperature of said tubes at a substantially constant temperature along their lengths.

21. A gas purification system as recited in claim 20 wherein said heat sink means comprises a first plate contacting said plurality of tubes on a first side thereof and a second plate contacting said plurality of tubes on a second side thereof.

22. A gas purification system as recited in claim 21 further comprising means for removing heat energy at least one of said first plate and said second plate.