US4283379A
Expired / Lapsed
US
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Method for removing hydrogen sulfide from gas streams
Assignee: Honeywell UOP LLC
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Filing: 1979-06-20
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Granted: 1981-08-11
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Expires: 1999-06-20
Abstract
Abstract A hydrogen sulfide removal and conversion method in which a hydrogen sulfide-containing gas stream is contacted with a substantially quinone-free aqueous washing solution containing, inter alia, solubilized vanadium, thiocyanate ions, and one or more water-soluble nonquinone aromatic compounds capable of solubilizing tetravalent vanadium. The absorbed hydrogen sulfide is converted to elemental sulfur which, after oxidative regeneration of the washing solution, is separated from the regenerated solution.
Inventors
- 👤 Donald M. Fenton
- 👤 Hugh W. Gowdy
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 16:32
CPC Classifications
C; C01; C01B; C01B17/00; C01B17/02; C01B17/04; C01B17/05; B; B01; B01D; B01D53/00; B01D53/34; B01D53/46; B01D53/48; B01D53/52
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
150 words
A method for removing hydrogen sulfide from a hydrogen sulfide-containing gas stream and converting said hydrogen sulfide to elemental sulfur, which comprises: (a) contacting said gas stream with a regenerable washing solution so as to absorb said hydrogen sulfide into said washing solution, the washing solution introduced into contact with said gas stream comprising a substantially quinone-free aqueous solution having a pH between about 5 and about 10 and containing (1) solubilized vanadium, (2) one or more water-soluble nonquinone aromatic compounds capable of solubilizing tetravalent vanadium, (3) thiocyanate ions and (4) a water-soluble carboxylate complexing agent; (b) allowing the absorbed hydrogen sulfide to react with constituents of said washing solution so as to convert said absorbed hydrogen sulfide substantially exclusively to elemental sulfur; (c) oxidatively regenerating the washing solution from step (b) so as to form a regenerated washing solution; and (d) separating said elemental sulfur from said washing solution.
Claim 2
Independent Claim
150 words
A method for removing hydrogen sulfide from a hydrogen sulfide-containing gas stream and converting said hydrogen sulfide to elemental sulfur, which comprises: (a) contacting said gas stream with a regenerable washing solution so as to absorb said hydrogen sulfide into said washing solution, the washing solution introduced into contact with said gas stream comprising a substantially quinone-free aqueous solution having a pH between about 5 and about 10 and containing (1) solubilized vanadium, (2) one or more water-soluble nonquinone aromatic compounds capable of solubilizing tetravalent vanadium, (3) thiocyanate ions and (4) a water-soluble carboxylate complexing agent; (b) allowing the absorbed hydrogen sulfide to react with constituents of said washing solution so as to convert said absorbed hydrogen sulfide substantially exclusively to elemental sulfur; (c) oxidatively regenerating the washing solution from step (b) so as to form a regenerated washing solution; and (d) separating said elemental sulfur from said washing solution.
Claim 3
Dependent Claim
48 words
The method defined in claim 1 wherein said washing solution contains between 5 and about 400 grams of thiocyanate ions per liter, between about 0.006 and about 0.4 gram-moles of vanadium per liter, and between about 0.01 and about 0.25 gram-moles of said nonquinone aromatic compounds per liter.
Claim 4
Dependent Claim
49 words
The method defined in claim 1 wherein said washing solution contains between about 30 and about 150 grams of thiocyanate ions per liter, between about 0.01 and about 0.2 gram-moles of vanadium per liter and between about 0.02 and about 0.15 gram-moles of said nonquinone aromatic compounds per liter.
Claim 5
Dependent Claim
49 words
The method defined in claim 1 wherein said washing solution contains between about 50 and about 75 grams of thiocyanate ions per liter, between about 0.04 and about 0.16 gram-moles of vanadium per liter, and between about 0.05 and about 0.12 gram-moles of said nonquinone aromatic compounds per liter.
Claim 6
Dependent Claim
28 words
The method defined in claim 1 wherein said washing solution has a molar ratio of said vanadium to said nonquinone aromatic compounds between about 0.5 and about 2.
Claim 7
Dependent Claim
19 words
The method defined in claim 1 wherein said washing solution has a pH between about 7 and about 9.5.
Claim 8
Dependent Claim
61 words
The method defined in claim 1 wherein said carboxylate complexing agent is an alkali metal or ammonium salt of a hydroxycarboxylic acid, and wherein said washing solution further contains a buffering agent selected from group consisting of the alkali metal and ammonium carbonates, the alkali metal and ammonium bicarbonates, the alkali metal and ammonium salts of carboxylic acids and mixtures thereof.
Claim 9
Dependent Claim
21 words
The method defined in claim 1 wherein said carboxylate complexing agent is an alkali metal or ammonium salt of citric acid.
Claim 10
Dependent Claim
233 words
The method defined in claim 1 wherein said non-quinone aromatic compounds are alkali metal or ammonium salts or acids of one or more compounds selected from the group consisting of the 1-hydroxybenzene-x-sulfonates (wherein x=2, 3 or 4), the 1-hydroxybenzene-x,y-disulfonates (wherein x=2 or 3, y=3, 4, 5 or 6 and x≠y), the 1,x-dihydroxybenzene-y-sulfonates (wherein x=2, 3 or 4, y=2, 3, 4 or 5 and x≠y), the 1,x-dihydroxybenzene-y,z-disulfonates (wherein x=2, 3 or 4, y=2, 3 or 4, z=3, 4, 5 or 6 and x≠y≠z), 1-methoxybenzene-4-sulfonate, 1-methylbenzene-4-sulfonate, 1-acetylbenzene-4-sulfonate, the 1-aminobenzene-x-sulfonates (wherein x=2, 3 or 4), benzene sulfonate, benzene disulfonate, 1-nitrobenzene-3-sulfonate, 1,3,5-trinitrobenzene-2-sulfonate, 1,4-diaminobenzene-2-sulfonate, 1,3,5-trimethylbenzene-2-sulfonate, 1,3-dicarboxylbenzene-5-sulfonate, the 1-hydroxynaphthalene-x-sulfonates (wherein x=2, 3, 4, 5, 6, 7 or 8), the 1-hydroxynaphthalene-x,y-disulfonates (wherein x=2, 3 or 4 and y=5, 6, 7 or 8), the 2-hydroxynaphthalene-x,y-disulfonates (wherein x=3, 4, 5 or 6, y=5, 6, 7 or 8 and x≠y), 4,5-dihydroxynaphthalene-2,7-disulfonate, the 2,x-dihydroxynaphthalene-3,y-disulfonates (wherein x=6 or 7, y=6 or 7 and x≠y), naphthalene sulfonate, the naphthalene-x,y-disulfonates (wherein x=1 or 2 and y=5, 6, 7 or 8), the x-aminonaphthalene-1-sulfonates (wherein x=4 or 5), 2-aminonaphthalene-1,5-disulfonate, calmagite, erichrome black T, Ponceau 3R, indigo carmine, the N-ethyl-5-phenylisoxazolium-x-sulfonates (wherein x=3' or 4'), 5-formylfuran-2-sulfonate, 3-hydroxy-4-(2-hydroxy-4-sulfo-1-naphthylazo)naphthalene-2-carboxylate, o-(2-[α-(2-hydroxy-5-sulfophenylazo)benzylidenehydrazino])benzoate, 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine-p,p-disulfonate, 2,3-dioxoindoline-5-sulfonate, the pyridine-x-sulfonates (x=2, 3 or 4), 5-carboxypyridine-3-sulfonate, 8-hydroxyquinoline-5-sulfonate, 2-methykl-8-hydroxyquinoline-5-sulfonate, 2-hydroxy-4-methoxybenzophenone-5-sulfonate, the benzophenone-x,y-disulfonates (wherein x=3 or 4 and y=3' or 4'), diphenylether-4,4'-disulfonate, diphenylamine-4,4'-disulfonate, the diphenylsulfone-x,y-disulfonates (wherein x=3 or 4 and y=3' or 4'), methylphenylsulfone, the water-soluble nonquinone derivatives thereof and mixtures thereof.
Claim 11
Dependent Claim
45 words
The method defined in claim 1 wherein said non-quinone aromatic compounds are alkali metal or ammonium salts or acids of one or more aromatic sulfonates selected from the group consisting of 1-hydroxybenzene-4-sulfonate, 1,4-dihydroxybenzene-2-sulfonate, the 1,4-dihydroxybenzene-2,x-disulfonates (wherein x=5 or 6), 4,5-dihydroxynaphthalene-2,7-disulfonate, pyridine-3-sulfonate, 8-hydroxyquinoline-5-sulfonate, and mixtures thereof.
Claim 12
Independent Claim
198 words
A method for removing hydrogen sulfide from a hydrogen sulfide-containing gas stream and converting said hydrogen sulfide to elemental sulfur, which comprises: (a) contacting said gas stream with a regenerable washing solution so as to absorb said hydrogen sulfide into said washing solution, the washing solution introduced into contact with said gas stream comprising a substantially quinone-free aqueous alkaline solution having a pH between about 7 and about 9.5 and containing (1) between about 0.006 and about 0.4 gram-moles of solubilized vanadium per liter, (2) between about 0.01 and about 0.25 gram-moles of one or more water-soluble alkali metal salts of nonquinone hydroxyaromatic sulfonates per liter, (3) between about 30 and about 150 grams of thiocyanate ions per liter, and (4) a water-soluble carboxylate complexing agent; (b) allowing the absorbed hydrogen sulfide to react with constituents of said washing solution so as to convert said hydrogen sulfide substantially exclusively to elemental sulfur; (c) oxidatively regenerating the washing solution from step (b) so as to form a regenerated washing solution; (d) separating said elemental sulfur from said regenerated washing solution; and (e) recycling the regenerated washing solution from step (d) into contact with said gas stream in step (a).
Claim 13
Independent Claim
198 words
A method for removing hydrogen sulfide from a hydrogen sulfide-containing gas stream and converting said hydrogen sulfide to elemental sulfur, which comprises: (a) contacting said gas stream with a regenerable washing solution so as to absorb said hydrogen sulfide into said washing solution, the washing solution introduced into contact with said gas stream comprising a substantially quinone-free aqueous alkaline solution having a pH between about 7 and about 9.5 and containing (1) between about 0.006 and about 0.4 gram-moles of solubilized vanadium per liter, (2) between about 0.01 and about 0.25 gram-moles of one or more water-soluble alkali metal salts of nonquinone hydroxyaromatic sulfonates per liter, (3) between about 30 and about 150 grams of thiocyanate ions per liter, and (4) a water-soluble carboxylate complexing agent; (b) allowing the absorbed hydrogen sulfide to react with constituents of said washing solution so as to convert said hydrogen sulfide substantially exclusively to elemental sulfur; (c) oxidatively regenerating the washing solution from step (b) so as to form a regenerated washing solution; (d) separating said elemental sulfur from said regenerated washing solution; and (e) recycling the regenerated washing solution from step (d) into contact with said gas stream in step (a).
Claim 14
Dependent Claim
49 words
The method defined in claim 11 wherein said washing solution contains between about 50 and about 75 grams of thiocyanate ions per liter, between about 0.01 and about 0.2 gram-moles of vanadium per liter, and between about 0.02 and about 0.15 gram-moles of said nonquinone hydroxyaromatic sulfonates per liter.
Claim 15
Dependent Claim
47 words
The method defined in claim 11 wherein said carboxylate complexing agent is an alkali metal salt of a hydroxycarboxylic acid, and wherein said washing solution also contains a buffering agent selected from the group consisting of the alkali metal carbonates, the alkali metal bicarbonates and mixtures thereof.
Claim 16
Dependent Claim
19 words
The method defined in claim 11 wherein said carboxylate complexing agent is an alkali metal salt of citric acid.
Claim 17
Dependent Claim
34 words
The metod defined in claim 11 wherein said one or more nonquinone hydroxyaromatic sulfonates is selected from the group consisting of 1-hydroxybenzene-4-sulfonate, 1,4-dihydroxybenzene-2-sulfonate, the 1,4-dihydroxybenzene-2,x-disulfonates (wherein x=5 or 6), 4,5-dihydroxynaphthalene-2,7-disulfonate, 8-hydroxyquinoline-5-sulfonate, and mixtures thereof.
Claim 18
Dependent Claim
16 words
The method defined in claim 11 wherein said one or more nonquinone hydroxyaromatic sulfonates is 8-hydroxyquinoline-5-sulfonate.
Claim 19
Dependent Claim
16 words
The method defined in claim 11 wherein said one or more nonquinone hydroxyaromatic sulfonates is 1-hydroxybenzene-4-sulfonate.
Claim 20
Dependent Claim
28 words
The method defined in claim 11 wherein said washing solution has a molar ratio of said vanadium to said nonquinone hydroxyaromatic sulfonates between about 0.5 and about 2.
Claim 21
Independent Claim
200 words
A method for removing hydrogen sulfide from a hydrogen sulfide-containing gas stream and converting said hydrogen sulfide to elemental sulfur, which comprises: (a) contacting said gas stream with a regenerable washing solution so as to absorb said hydrogen sulfide into said washing solution, the washing solution introduced into contact with said gas stream comprising a quinone-free aqueous alkaline solution having a pH between about 8 and about 9 and containing (1) between about 0.01 and about 0.2 gram-moles of solubilized vanadium per liter, (2) between about 0.02 and about 0.15 gram-moles of an alkali metal 1-hydroxybenzene-4-sulfonate per liter, (3) between about 30 and about 150 grams of thiocyanate ions per liter, (4) an alkali metal citrate, and (5) a mixture of alkali metal carbonates and alkali metal bicarbonates; (b) allowing the absorbed hydrogen sulfide to react with constituents of said washing solution so as to convert said hydrogen sulfide substantially exclusively to elemental sulfur; (c) oxidatively regenerating the washing solution from step (b) so as to form a regenerated washing solution; (d) separating said elemental sulfur from said regenerated washing solution; and (e) recycling the regenerated washing solution from step (d) into contact with said gas stream in step (a).
Claim 22
Independent Claim
200 words
A method for removing hydrogen sulfide from a hydrogen sulfide-containing gas stream and converting said hydrogen sulfide to elemental sulfur, which comprises: (a) contacting said gas stream with a regenerable washing solution so as to absorb said hydrogen sulfide into said washing solution, the washing solution introduced into contact with said gas stream comprising a quinone-free aqueous alkaline solution having a pH between about 8 and about 9 and containing (1) between about 0.01 and about 0.2 gram-moles of solubilized vanadium per liter, (2) between about 0.02 and about 0.15 gram-moles of an alkali metal 1-hydroxybenzene-4-sulfonate per liter, (3) between about 30 and about 150 grams of thiocyanate ions per liter, (4) an alkali metal citrate, and (5) a mixture of alkali metal carbonates and alkali metal bicarbonates; (b) allowing the absorbed hydrogen sulfide to react with constituents of said washing solution so as to convert said hydrogen sulfide substantially exclusively to elemental sulfur; (c) oxidatively regenerating the washing solution from step (b) so as to form a regenerated washing solution; (d) separating said elemental sulfur from said regenerated washing solution; and (e) recycling the regenerated washing solution from step (d) into contact with said gas stream in step (a).
Claim 23
Dependent Claim
48 words
The method defined in claim 19 wherein said washing solution contains between about 5 and about 10 grams of sodium carbonate per liter, between about 25 and about 30 grams of sodium bicarbonate per liter, and between about 10 and about 20 grams of sodium citrate per liter.
Claim 24
Dependent Claim
16 words
The method defined in claim 19 wherein said gas stream is hydrogenated Claus process tail gas.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-08-10 | 1985-02-09 | 1985-08-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-08-10 | 1989-02-09 | 1989-08-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-08-10 | 1993-02-09 | 1993-08-11 | $7700.00 | Window Closed / Lapsed |