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Aqueous phase removal of nitrogen from nitrogen compounds

Assignee: Battelle Memorial Institute Inc
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Filing: 1991-04-12
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Granted: 1993-06-22
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Expires: 2011-04-12
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Abstract

Abstract A method is disclosed for denitrification of compounds containing nitrogen present in aqueous waste streams. The method comprises the steps of (1) identifying the types of nitrogen compounds present in a waste stream, (2) determining the concentrations of nitrogen compounds, (3) balancing oxidized and reduced form of nitrogen by adding a reactant, and (4) heating the mixture to a predetermined reaction temperature from about 300° C. to about 600° C., thereby resulting in less harmful nitrogen and oxygen gas, hydroxides, alcohols, and hydrocarbons.

Inventors

  • 👤 Alex G. Fassbender

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 18:11
CPC Classifications
C; C02; C02F; C02F1/00; C02F1/02; C02F1/025; C02F2101/00; C02F2101/10; C02F2101/16; C02F2303/00; C02F2303/08; Y; Y10; Y10S; Y10S210/00; Y10S210/902; Y10S210/903; Y10S210/908

Claims Analysis

Total Claims: 56
Claim 1
Independent Claim 72 words
A method of denitrification of at least one compound containing nitrogen in an aqueous stream, comprising the steps of: (a) heating said aqueous stream in the absence of a denitrification catalyst to a predetermined reaction temperature from about 300° C. to 600° C. under sufficient pressure to maintain the aqueous stream in an aqueous or supercritical phase, and (b) releasing nitrogen in the form of nitrogen gas while leaving an aqueous product.
Claim 2
Independent Claim 72 words
A method of denitrification of at least one compound containing nitrogen in an aqueous stream, comprising the steps of: (a) heating said aqueous stream in the absence of a denitrification catalyst to a predetermined reaction temperature from about 300° C. to 600° C. under sufficient pressure to maintain the aqueous stream in an aqueous or supercritical phase, and (b) releasing nitrogen in the form of nitrogen gas while leaving an aqueous product.
Claim 3
Dependent Claim 23 words
The method as recited in claim 1, further comprising the step of: mixing carbon dioxide with said aqueous product to form a carbonate.
Claim 4
Dependent Claim 15 words
The method as recited in claim 1, wherein said compound containing nitrogen is ammonium nitrate.
Claim 5
Dependent Claim 39 words
The method as recited in claim 1, wherein the compound containing nitrogen is selected from the group consisting of ammonium ion, amide ion, amides, amines, amino acids, ammonia, nitro derivatives, azo compounds, glycine, pyridine, nitric acid, nitrites, and nitrates.
Claim 6
Independent Claim 104 words
A method for denitrification of at least one compound containing nitrogen in an aqueous stream, comprising the steps of: (a) identifying at least one compound containing nitrogen in an aqueous phase waste stream, (b) determining the concentration(s) of said nitrogen compound(s), (c) balancing oxidized and reduced form(s) of nitrogen, and (d) heating the balanced mixture of step (c) in the absence of a denitrification catalyst to a predetermined reaction temperature between from about 300° C. to about 600° C. under pressure sufficient to maintain the aqueous stream in a liquid or supercritical phase, thereby forming and releasing nitrogen gas while leaving an aqueous product.
Claim 7
Independent Claim 104 words
A method for denitrification of at least one compound containing nitrogen in an aqueous stream, comprising the steps of: (a) identifying at least one compound containing nitrogen in an aqueous phase waste stream, (b) determining the concentration(s) of said nitrogen compound(s), (c) balancing oxidized and reduced form(s) of nitrogen, and (d) heating the balanced mixture of step (c) in the absence of a denitrification catalyst to a predetermined reaction temperature between from about 300° C. to about 600° C. under pressure sufficient to maintain the aqueous stream in a liquid or supercritical phase, thereby forming and releasing nitrogen gas while leaving an aqueous product.
Claim 8
Dependent Claim 80 words
The method as recited in claim 5, wherein balancing oxidized and reduced forms of nitrogen in step (c) comprises: (a) adding a compound selected from the group consisting of hydrogen, hydrogen sulfide, hydrogen peroxide, and potassium permangenate, in an amount substantially equivalent to a half mole fraction of the compound containing nitrogen, and (b) heating to a predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain an aqueous liquid or supercritical phase.
Claim 9
Dependent Claim 80 words
The method as recited in claim 5, wherein balancing oxidized and reduced forms of nitrogen in step (c) comprises: (a) heating to a predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain an aqueous liquid or supercritical phase, and (b) adding a compound selected from the group consisting of hydrogen, hydrogen sulfide, hydrogen peroxide, and potassium permangenate, in an amount substantially equivalent to a half mole fraction of the compound containing nitrogen.
Claim 10
Dependent Claim 49 words
The method as recited in claim 5, wherein balancing oxidized and reduced forms of nitrogen in step (c) comprises adding a compound selected from the group consisting of nitrates, nitrites, nitric acid amides, amides, nitro derivatives, azo compounds, glycine, pyridine ammonium ion, amide ion, amides, amines, and amino acids.
Claim 11
Dependent Claim 26 words
The method as recited in claim 5, further comprising the step of: mixing carbon dioxide with said aqueous product in step (d) to form a carbonate.
Claim 12
Dependent Claim 14 words
The method as recited in claim 5, further comprising the step of: lowering pH.
Claim 13
Dependent Claim 26 words
The method as recited in claim 10, wherein lowering pH comprises: adding a compound from the group consisting of mineral acids, carbon dioxide, and organic acids.
Claim 14
Independent Claim 114 words
A method for denitrification of at least one compound containing nitrogen in an aqueous stream, comprising the steps of: (a) identifying at least one compound containing nitrogen in an aqueous stream, (b) determining the concentration(s) of said nitrogen compound(s), (c) determining oxidized and reduced state(s) of said nitrogen compound(s), (d) heating the aqueous stream in the absence of a denitrification catalyst to a predetermined reaction temperature between from about 300° C. to about 600° C. under pressure sufficient to maintain the aqueous stream in a liquid or supercritical phase, and (e) balancing oxidized and reduced form(s) of nitrogen, thereby forming and releasing nitrogen in the form of nitrogen gas while leaving an aqueous product.
Claim 15
Independent Claim 114 words
A method for denitrification of at least one compound containing nitrogen in an aqueous stream, comprising the steps of: (a) identifying at least one compound containing nitrogen in an aqueous stream, (b) determining the concentration(s) of said nitrogen compound(s), (c) determining oxidized and reduced state(s) of said nitrogen compound(s), (d) heating the aqueous stream in the absence of a denitrification catalyst to a predetermined reaction temperature between from about 300° C. to about 600° C. under pressure sufficient to maintain the aqueous stream in a liquid or supercritical phase, and (e) balancing oxidized and reduced form(s) of nitrogen, thereby forming and releasing nitrogen in the form of nitrogen gas while leaving an aqueous product.
Claim 16
Dependent Claim 80 words
The method as recited in claim 12, wherein balancing oxidized and reduced forms of nitrogen in step (c) comprises: (a) heating to a predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain an aqueous liquid or supercritical phase, and (b) adding a compound selected from the group consisting of hydrogen, hydrogen sulfide, hydrogen peroxide, and potassium permangenate, in an amount substantially equivalent to a half mole fraction of the compound containing nitrogen.
Claim 17
Dependent Claim 49 words
The method as recited in claim 12, wherein balancing oxidized and reduced forms of nitrogen in step (c) comprises adding a compound selected from the group consisting of nitrates, nitrites, nitric acid, amides, amines, nitro derivatives, azo compounds, glycine, pyridine ammonium ion, amide ion, amides, amines, and amino acids.
Claim 18
Dependent Claim 26 words
The method as recited in claim 12, further comprising the step of: mixing carbon dioxide with said aqueous product in step (d) to form a carbonate.
Claim 19
Dependent Claim 14 words
The method as recited in claim 12, further comprising the step of: lowering pH.
Claim 20
Dependent Claim 26 words
The method as recited in claim 16, wherein lowering pH comprises: adding a compound from the group consisting of mineral acids, carbon dioxide, and organic acids.
Claim 21
Independent Claim 134 words
A method for denitrification of at least one first compound containing nitrogen in an aqueous stream, comprising the steps of: (a) mixing at least one other second compound containing nitrogen having an oxidized or reduced state opposite that of said compound(s) containing nitrogen in the aqueous stream in an amount substantially equivalent to a mole fraction of the compound(s) containing nitrogen in the aqueous stream, wherein said mole fraction is from about TKN detection limits up to a saturated solution, (b) heating said mixture in the absence of a denitrification catalyst to a predetermined reaction temperature from about 300° C. to about 370° C. at a pressure sufficient to maintain the aqueous stream in a liquid phase for a period of time from about one minute to about two hours, thereby releasing nitrogen gas.
Claim 22
Independent Claim 134 words
A method for denitrification of at least one first compound containing nitrogen in an aqueous stream, comprising the steps of: (a) mixing at least one other second compound containing nitrogen having an oxidized or reduced state opposite that of said compound(s) containing nitrogen in the aqueous stream in an amount substantially equivalent to a mole fraction of the compound(s) containing nitrogen in the aqueous stream, wherein said mole fraction is from about TKN detection limits up to a saturated solution, (b) heating said mixture in the absence of a denitrification catalyst to a predetermined reaction temperature from about 300° C. to about 370° C. at a pressure sufficient to maintain the aqueous stream in a liquid phase for a period of time from about one minute to about two hours, thereby releasing nitrogen gas.
Claim 23
Dependent Claim 14 words
The method as recited in claim 18, further comprising the step of: lowering pH.
Claim 24
Dependent Claim 26 words
The method as recited in claim 19, wherein lowering pH comprises: adding a compound from the group consisting of mineral acids, carbon dioxide, and organic acids.
Claim 25
Dependent Claim 26 words
The method as recited in claim 18, wherein said first compound containing nitrogen is glycine, and said other second compound in step (a) is nitric acid.
Claim 26
Dependent Claim 26 words
The method as recited in claim 18, wherein said first compound containing nitrogen is pyridine, and said other second compound in step (a) is nitric acid.
Claim 27
Dependent Claim 26 words
The method as recited in claim 18, wherein said first compound containing nitrogen is nitric acid, and said other second compound in step (a) is glycine.
Claim 28
Dependent Claim 26 words
The method as recited in claim 18, wherein said first compound containing nitrogen is nitric acid, and said other second compound in step (a) is pyridine.
Claim 29
Dependent Claim 54 words
The method as recited in claim 18, wherein said first compound containing nitrogen is selected from the group consisting of ammonium ion, amide ion, amides, amines, amino acids, ammonia, azo compounds, glycine, and pyridine and said other second compound in step (a) is selected from the group consisting of nitrites, nitrates and nitric acid.
Claim 30
Dependent Claim 54 words
The method as recited in claim 18, wherein said first compound containing nitrogen is selected from the group consisting of nitrates, nitrites and nitric acid and said other second compound in step (a) is selected from the group consisting of ammonium ion, amide ion, amides, amines, amino acids, ammonia, azo compounds, glycine, and pyridine.
Claim 31
Dependent Claim 47 words
The method as recited in claim 18, wherein said first compound containing nitrogen is selected from the group consisting of R-NO and nitro derivatives, and said other second compound in step (a) is selected from the group consisting of ammonia, amide ion, amines, amides, and ammonium ion.
Claim 32
Dependent Claim 47 words
The method as recited in claim 18, wherein said first compound containing nitrogen is selected from the group consisting of ammonia, amide ion, amines, amides, and ammonium ion, and said other second compound in step (a) is selected from the group consisting of R-NO and nitro derivatives.
Claim 33
Independent Claim 138 words
A method for denitrification of at least one first compound containing nitrogen in an aqueous stream, comprising the steps of: (a) heating the aqueous stream in the absence of a denitrification catalyst to a predetermined reaction temperature from about 300° C. to about 350° C. at a pressure sufficient to maintain the aqueous stream in a liquid or supercritical phase for a period of time from about one minute to about two hours, and (b) mixing at least one other second compound containing nitrogen having an oxidized or reduced state opposite that of said compound(s) containing nitrogen in the aqueous stream in an amount substantially equivalent to a mole fraction of the compound(s) containing nitrogen in the aqueous stream, wherein said mole fraction is from about TKN detection limits up to a saturated solution, thereby releasing nitrogen gas.
Claim 34
Independent Claim 138 words
A method for denitrification of at least one first compound containing nitrogen in an aqueous stream, comprising the steps of: (a) heating the aqueous stream in the absence of a denitrification catalyst to a predetermined reaction temperature from about 300° C. to about 350° C. at a pressure sufficient to maintain the aqueous stream in a liquid or supercritical phase for a period of time from about one minute to about two hours, and (b) mixing at least one other second compound containing nitrogen having an oxidized or reduced state opposite that of said compound(s) containing nitrogen in the aqueous stream in an amount substantially equivalent to a mole fraction of the compound(s) containing nitrogen in the aqueous stream, wherein said mole fraction is from about TKN detection limits up to a saturated solution, thereby releasing nitrogen gas.
Claim 35
Dependent Claim 14 words
The method as recited in claim 29, further comprising the step of: lowering pH.
Claim 36
Dependent Claim 26 words
The method as recited in claim 30, wherein lowering pH comprises: adding a compound from the group consisting of mineral acids, carbon dioxide, and organic acids.
Claim 37
Dependent Claim 26 words
The method as recited in claim 29, wherein said first compound containing nitrogen is glycine, and said other second compound in step (a) is nitric acid.
Claim 38
Dependent Claim 26 words
The method as recited in claim 29, wherein said first compound containing nitrogen is pyridine, and said other second compound in step (a) is nitric acid.
Claim 39
Dependent Claim 26 words
The method as recited in claim 29, wherein said first compound containing nitrogen is nitric acid, and said other second compound in step (a) is glycine.
Claim 40
Dependent Claim 26 words
The method as recited in claim 29, wherein said first compound containing nitrogen is nitric acid, and said other second compound in step (a) is pyridine.
Claim 41
Dependent Claim 54 words
The method as recited in claim 29, wherein said first compound containing nitrogen is selected from the group consisting of ammonium ion, amide ion, amides, amines, amino acids, ammonia, azo compounds, glycine, and pyridine and said other second compound in step (a) is selected from the group consisting of nitrites, nitrates and nitric acid.
Claim 42
Dependent Claim 54 words
The method as recited in claim 29, wherein said first compound containing nitrogen is selected from the group consisting of nitrates, nitrites and nitric acid and said other second compound in step (a) is selected from the group consisting of ammonium ion, amide ion, amides, amines, amino acids, ammonia, azo compounds, glycine, and pyridine.
Claim 43
Dependent Claim 47 words
The method as recited in claim 29, wherein said first compound containing nitrogen is selected from the group consisting of R-NO and nitro derivatives, and said other second compound in step (a) is selected from the group consisting of ammonia, amide ion, amines, amides, and ammonium ion.
Claim 44
Dependent Claim 47 words
The method as recited in claim 29, wherein said first compound containing nitrogen is selected from the group consisting of ammonia, amide ion, amines, amides, and ammonium ion, and said other second compound in step (a) is selected from the group consisting of R-NO and nitro derivatives.
Claim 45
Independent Claim 199 words
A method for denitrification of at least one compound containing nitrogen in an aqueous waste stream, comprising the steps of: (a) splitting an aqueous waste stream into a first stream and a second stream, (b) adding an oxidant compound in an amount substantially equivalent to a mole fraction of said compound(s) containing nitrogen in said first stream wherein said mole fraction is from about TKN detection limits up to a saturated solution, (c) heating the first stream to a first predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain said first stream in an aqueous liquid phase, thereby oxidizing said compound(s) containing nitrogen to a different and distinct compound (s) containing nitrogen, (d) combining the first stream with the second stream, and (e) heating the combine stream to a second predetermined reaction temperature from about 300° C. to about 370° C. at a pressure sufficient to maintain a liquid phase for a period of time from about one minute to about two hours, and reacting compound(s) containing nitrogen from the second stream with the oxidized compound(s) containing nitrogen from the first stream and releasing nitrogen gas and leaving an aqueous product.
Claim 46
Independent Claim 199 words
A method for denitrification of at least one compound containing nitrogen in an aqueous waste stream, comprising the steps of: (a) splitting an aqueous waste stream into a first stream and a second stream, (b) adding an oxidant compound in an amount substantially equivalent to a mole fraction of said compound(s) containing nitrogen in said first stream wherein said mole fraction is from about TKN detection limits up to a saturated solution, (c) heating the first stream to a first predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain said first stream in an aqueous liquid phase, thereby oxidizing said compound(s) containing nitrogen to a different and distinct compound (s) containing nitrogen, (d) combining the first stream with the second stream, and (e) heating the combine stream to a second predetermined reaction temperature from about 300° C. to about 370° C. at a pressure sufficient to maintain a liquid phase for a period of time from about one minute to about two hours, and reacting compound(s) containing nitrogen from the second stream with the oxidized compound(s) containing nitrogen from the first stream and releasing nitrogen gas and leaving an aqueous product.
Claim 47
Dependent Claim 11 words
The method as recited in claim 40, further comprising: lowering pH.
Claim 48
Dependent Claim 26 words
The method as recited in claim 41, wherein lowering pH comprises: adding a compound from the group consisting of mineral acids, carbon dioxide, and organic acids.
Claim 49
Dependent Claim 27 words
The method as recited in claim 40, wherein said compound containing nitrogen is selected from the group consisting of ammonia, amide ion, amines, amides, and ammonium ion.
Claim 50
Dependent Claim 25 words
The method as recited in claim 40, wherein said oxidant compound is selected from the group consisting of, hydrogen peroxide, hydrogen sulfide, and potassium permanganate.
Claim 51
Independent Claim 198 words
A method for denitrification of at least one compound containing nitrogen in an aqueous waste stream, comprising the steps of: (a) splitting an aqueous waste stream into a first stream and a second stream, (b) heating the first stream to a first predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain said first stream in an aqueous liquid phase, (c) adding an oxidant compound in an amount substantially equivalent to a mole fraction of said compound(s) containing nitrogen in said first stream wherein said mole fraction is from about TKN detection limits up to a saturated solution, thereby oxidizing said compound(s) containing nitrogen to a different and distinct compound(s) containing nitrogen, (d) combining the first stream with the second stream, and (e) heating the combine stream to a second predetermined reaction temperature from about 300° C. to about 370° C. at a pressure sufficient to maintain a liquid phase for a period of time from about one minute to about two hours, and reacting compound(s) containing nitrogen from the second stream with the oxidized compound(s) containing nitrogen from the first stream and releasing nitrogen gas and leaving an aqueous product.
Claim 52
Independent Claim 198 words
A method for denitrification of at least one compound containing nitrogen in an aqueous waste stream, comprising the steps of: (a) splitting an aqueous waste stream into a first stream and a second stream, (b) heating the first stream to a first predetermined reaction temperature from about 90° C. to about 150° C. at a pressure sufficient to maintain said first stream in an aqueous liquid phase, (c) adding an oxidant compound in an amount substantially equivalent to a mole fraction of said compound(s) containing nitrogen in said first stream wherein said mole fraction is from about TKN detection limits up to a saturated solution, thereby oxidizing said compound(s) containing nitrogen to a different and distinct compound(s) containing nitrogen, (d) combining the first stream with the second stream, and (e) heating the combine stream to a second predetermined reaction temperature from about 300° C. to about 370° C. at a pressure sufficient to maintain a liquid phase for a period of time from about one minute to about two hours, and reacting compound(s) containing nitrogen from the second stream with the oxidized compound(s) containing nitrogen from the first stream and releasing nitrogen gas and leaving an aqueous product.
Claim 53
Dependent Claim 11 words
The method as recited in claim 45, further comprising: lowering pH
Claim 54
Dependent Claim 26 words
The method as recited in claim 46, wherein lowering pH comprises; adding a compound from the group consisting of mineral acids, carbon dioxide, and organic acids.
Claim 55
Dependent Claim 27 words
The method as recited in claim 45, wherein said compound containing nitrogen is selected from the group consisting of ammonia, amide ion, amines, amides, and ammonium ion.
Claim 56
Dependent Claim 25 words
The method as recited in claim 45, wherein said oxidant compound is selected from the group consisting of, hydrogen peroxide, hydrogen sulfide, and potassium permanganate.

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