US4689062A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Argon recovery from ammonia plant purge gas utilizing a combination of cryogenic and non-cryogenic separating means
Assignee: Messer LLC
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Filing: 1986-02-24
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Granted: 1987-08-25
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Expires: 2006-02-24
Abstract
Abstract An improved process is disclosed for argon recovery from an ammonia synthesis plant purge gas comprising hydrogen, nitrogen, argon, ammonia, and methane. In one embodiment of the present invention, this purge gas is subjected to the following steps: (i) Separation of ammonia at high pressure by adsorption using zeolite molecular sieve material, which is subsequently regenerated by hot purge combined with pressure reduction; (ii) Separation of methane and most of the nitrogen by pressure swing adsorption using a molecular sieve or an activated carbon material having greater selectivity for methane than argon; (iii) Separation of hydrogen for recycle to the ammonia synthesis plant using a high pressure cryogenic distillation column of a membrane separator; and (iv) Separation of the nitrogen by cryogenic distillation means to obtain essentially pure liquid argon product.
Inventors
- 👤 Donald L. MacLean
- 👤 Ramachandran Krishnamurthy
- 👤 Steven L. Lerner
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 11:40
CPC Classifications
F; F25; F25J; F25J3/00; F25J3/02; F25J3/0204; F25J3/0219; B; B01; B01D; B01D53/00; B01D53/02; B01D53/04; C; C01; C01B; C01B23/00; C01C; C01C1/00; C01C1/02; C01C1/04; C01C1/0405; C01C1/0476; F25J3/0228; F25J3/0252; F25J3/028; F25J3/0285; B01D2253/00; B01D2253/10; B01D2253/102; B01D2253/106; B01D2253/108; B01D2256/00; B01D2256/18; B01D2257/00; B01D2257/10; B01D2257/102; B01D2257/108; B01D2257/40; B01D2257/406; B01D2257/70; B01D2257/702; B01D2259/00; B01D2259/40; B01D2259/402; B01D2259/404; F25J2205/00; F25J2205/40; F25J2205/60; F25J2205/80; F25J2210/00; F25J2210/20; Y; Y02; Y02P; Y02P20/00; Y02P20/10; Y02P20/129; Y02P20/50; Y02P20/52; Y10; Y10S; Y10S62/00; Y10S62/902; Y10S62/908
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
118 words
A process for the recovery of argon from a gas mixture comprising hydrogen, nitrogen, methane, argon, and ammonia, the steps comprising: (i) passing said gas mixture to a means for removing ammonia to produce an ammonia depleted gas mixture; (ii) passing said ammonia depleted gas mixture to a pressure swing adsorption means for removing essentially all of the methane and most of the nitrogen to produce a methane depleted gas mixture; (iii) passing said methane depleted gas mixture to a means for removing most of the hydrogen to produce a hydrogen depleted mixture; and (iv) passing said hydrogen depleted stream to a cryogenic distillation column for the separation of an argon product from remaining nitrogen and residual hydrogen.
Claim 2
Dependent Claim
118 words
A process for the recovery of argon from a gas mixture comprising hydrogen, nitrogen, methane, argon, and ammonia, the steps comprising: (i) passing said gas mixture to a means for removing ammonia to produce an ammonia depleted gas mixture; (ii) passing said ammonia depleted gas mixture to a pressure swing adsorption means for removing essentially all of the methane and most of the nitrogen to produce a methane depleted gas mixture; (iii) passing said methane depleted gas mixture to a means for removing most of the hydrogen to produce a hydrogen depleted mixture; and (iv) passing said hydrogen depleted stream to a cryogenic distillation column for the separation of an argon product from remaining nitrogen and residual hydrogen.
Claim 3
Dependent Claim
16 words
The process of claim 1, wherein said means for removing ammonia comprises a zeolite adsorption bed.
Claim 4
Dependent Claim
22 words
The process of claim 2, wherein said zeolite adsorption bed operates at a pressure in the range of 400 to 1900 psig.
Claim 5
Dependent Claim
35 words
The process of claim 2, wherein regeneration of said zeolite adsorption bed is carried out by passing a hot mixture of nitrogen and hydrogen gas through said adsorption bed at the same or reduced pressure.
Claim 6
Dependent Claim
42 words
The process of claim 1, wherein said pressure swing adsorption means for removing essentially all of the methane and most of the nitrogen comprises at least one adsorption bed containing an adsorbent material which exhibits a greater selectivity for methane than argon.
Claim 7
Dependent Claim
20 words
The process of claim 5, wherein said adsorption bed operates at a pressure in the range 400 to 1100 psig.
Claim 8
Dependent Claim
13 words
The process of claim 5, wherein said adsorbent material is a molecular sieve.
Claim 9
Dependent Claim
13 words
The process of claim 7, wherein said molecular sieve is an aluminosilicate zeolite.
Claim 10
Dependent Claim
20 words
The process of claim 8, wherein said aluminosilicate is selected from the group consisting of 5A, 10X, 13X or mordenites.
Claim 11
Dependent Claim
18 words
The process of claim 9, wherein said aluminosilicate zeolite is 5A medical grade sieve or 5A HC sieve.
Claim 12
Dependent Claim
26 words
The process of claim 7, wherein periodically said adsorption bed containing molecular sieve adsorbent material is regenerated by applying vacuum or by the use of purge.
Claim 13
Dependent Claim
13 words
The process of claim 5, wherein said adsorbent material is an activated carbon.
Claim 14
Dependent Claim
15 words
The process of claim 1, wherein said means for removing hydrogen is a membrane separator.
Claim 15
Dependent Claim
18 words
The process of claim 1, wherein said means for removing hydrogen is a high pressure cryogenic distillation column.
Claim 16
Dependent Claim
21 words
The process of claim 1, wherein the methane concentration in said argon product is equal to or less than 20 ppm.
Claim 17
Dependent Claim
21 words
The process of claim 1, wherein the methane concentration in said argon product is equal to or less than 1 ppm.
Claim 18
Dependent Claim
12 words
The process of claim 1, wherein said argon product is a liquid.
Claim 19
Independent Claim
76 words
An apparatus for the recovery of argon from a gas mixture comprising hydrogen, nitrogen, methane, argon, and ammonia, comprising in sequence: (i) a means for removing ammonia from said gas mixture; (ii) a pressure swing adsorption means for removing essentially all of the methane and most of the nitrogen; (iii) a means for removing most of the hydrogen; and (iv) a cryogenic distillation column for the separation of argon product from remaining nitrogen and residual hydrogen.
Claim 20
Independent Claim
76 words
An apparatus for the recovery of argon from a gas mixture comprising hydrogen, nitrogen, methane, argon, and ammonia, comprising in sequence: (i) a means for removing ammonia from said gas mixture; (ii) a pressure swing adsorption means for removing essentially all of the methane and most of the nitrogen; (iii) a means for removing most of the hydrogen; and (iv) a cryogenic distillation column for the separation of argon product from remaining nitrogen and residual hydrogen.
Claim 21
Dependent Claim
16 words
The apparatus of claim 18, wherein said means for removing ammonia comprises a zeolite adsorption bed.
Claim 22
Dependent Claim
20 words
The apparatus of claim 18, wherein said means for removing ammonia comprises a water scrubber and a plurality of dehydrators.
Claim 23
Dependent Claim
36 words
The apparatus of claim 18, wherein said pressure swing adsorption means for removing essentially all of the methane and most of the nitrogen comprises an adsorbent material which exhibits a greater selectivity for methane than argon.
Claim 24
Dependent Claim
13 words
The apparatus of claim 21, wherein said adsorbent material is a molecular sieve.
Claim 25
Dependent Claim
13 words
The apparatus of claim 22, wherein said molecular sieve comprises an aluminosilicate zeolite.
Claim 26
Dependent Claim
21 words
The apparatus of claim 23, wherein said aluminosilicate zeolite is selected from the group consisting of 5A, 10X, 13X or mordenites.
Claim 27
Dependent Claim
17 words
The apparatus of claim 24, wherein said aluminosilicate zeolite is 5A medical grade or 5A HC sieve.
Claim 28
Dependent Claim
14 words
The apparatus of claim 21, wherein said adsorbent material comprises an activated carbon material.
Claim 29
Dependent Claim
15 words
The apparatus of claim 18, wherein said means for removing hydrogen is a membrane separator.
Claim 30
Dependent Claim
17 words
The apparatus of claim 18, wherein said means for removing hydrogen is high pressure cryogenic distillation column.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-08-24 | 1991-02-23 | 1991-08-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-08-24 | 1995-02-23 | 1995-08-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-08-24 | 1999-02-23 | 1999-08-25 | $7700.00 | Window Closed / Lapsed |