Method for obtaining ammonia from waste water containing NH3 and acid gases

• US 6,558,452 B1
• Filed: 05/30/2001
• Issued: 05/06/2003
• Est. Priority Date: 10/21/1998
• Status: Expired due to Fees

• Current Assignee: Lurgi Clean Coal Technology (PTY) Ltd.
• Original Assignee: MG Technologies AG (GEA Group AG)
• Inventors: Stönner, Hans-Martin, Ungar, Gert, Linicus, Matthias
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US09/830,220
• Time in Patent Office: 706 Days
• Field of Search: 952/43, 952/45, 952/51, 952/63, 962/02, 962/18, 962/67, 962/99, 963/00, 210/180, 210/182, 210/188, 210/195.1, 210/903, 210/774, 210/805, 210/806, 202/154, 202/158, 203/71, 203/80, 423/237, 423/352, 423/357
• US Class Current: 95/245
• CPC Class Codes: B01D 19/0015 in contact columns containing plates, grids or other filling elements
• CPC Class Codes: C01C 1/10 Separation of ammonia from ammonia liquors, e.g. gas liquors as part of the ammonia synthesis process C01C1/04
• CPC Class Codes: C02F 1/20 by degassing, i.e. liberation of dissolved gases degasification of liquids in general B01D19/00; arrangement of degassing apparatus in boiler feed supply F22D
• CPC Class Codes: C02F 1/586 by removing ammoniacal nitrogen for biological methods C02F3/00
• CPC Class Codes: C02F 2101/16 Nitrogen compounds, e.g. ammonia
• CPC Class Codes: Y10S 210/903 Nitrogenous

Abstract

Ammonia is recovered from waste water containing NH₃, at least one acid gas (CO₂, H₂S) and inert gases. Firstly, the waste water is passed through a pretreatment column and then, at least in part, into a total stripping column. The top product from the total stripping column is cooled in a condenser, and an aqueous NH₃-containing condensate coming from the condenser is fed to an NH₃ stripping column. The top product from the NH₃ stripping column is brought into direct contact with circulating aqueous NH₃-containing condensate in a wash column, and NH₃ is recovered from the top product from the wash column. Some of the bottom product from the wash column is fed back into the NH₃ stripping column. The temperature in the bottom region of the pretreatment column is set to from less than 30 to 200° C., a sub-stream of the waste water is introduced into the upper region of the pretreatment column, and a second sub-stream of the waste water is fed into the pretreatment column below the first sub-stream. At least 80% of the NH₃ introduced from the total stripping column is condensed in the condenser. A waste-water stream is taken off from the total stripping column, at least part thereof is cooled to temperatures of from 10 to 60° C., and the cooled waste-water stream is passed into the top region of the pretreatment column.

Claims

1. A process for the recovery of NH₃ from a waste water containing NH₃, at least one acid gas selected from the group consisting of CO₂ and H₂S, and an inert gas, which comprises the steps of:

(a) dividing the waste water containing NH₃, at least one acid gas selected from the group consisting of CO₂ and H₂S, and an inert gas into a first waste water sub-stream and a second waste water sub-stream;

(b) providing a pretreatment column with a heating means at the bottom to heat the bottom to a temperature of 130 to 200°

C., introducing the first waste water sub-stream into an upper region of the pretreatment column, and the second waste water sub-stream into the pretreatment column at a location below the upper region of the pretreatment column where the first waste water sub-stream was introduced, to pretreat both the first and the second waste water sub-streams to remove the at least one acid gas from the waste water thereby providing a waste water stream at the bottom of said pretreatment column having undergone removal of said at least one acid gas;

(c) cooling the waste water stream at the bottom of said pretreatment column and channeling in part the waste water stream from the bottom of said pretreatment column to a total stripping column to obtain a top product comprising NH₃ and at least one acid gas, and a bottom product comprising a waste-water stream, cooling the top product, and condensing at least 80% of the NH₃ present in the top product in a condenser in which the top product is scrubbed with circulated and cooled condensate to obtain a waste gas comprising the inert gas and an aqueous NH₃-containing condensate while channeling 1 to 40% of the waste water having undergone removal of the at least one acid gas according to step (b) directly from the bottom of said pretreatment column to the condenser thereby avoiding the total stripping column to obtain additional waste gas comprising the inert gas and additional aqueous NH₃-containing condensate;

(d) cooling the waste-water stream obtained as a bottom product from the total stripping column according to step (c) to a temperature of 10 to 60°

C. and passing the cooled waste-water stream to the top region of the pretreatment column according to step (b);

(e) splitting the NH₃-containing condensate obtained from the condenser during step (c) into two portions, recirculating a first portion of the NH₃-containing condensate back to the condenser in step (c) to condense additional quantities of NH₃ present in the top product, and from a second portion of the NH₃-containing condensate stripping NH₃ in an NH₃-stripping column to obtain NH₃ vapor at the top and a waste stream at the bottom; and

(f) washing the NH₃ vapor with circulating NH₃-containing condensate in a wash column and recovering NH₃ as a top product from the wash column, said NH₃ free of said acid gas and said inert gas, while obtaining a bottom product from the wash column, said bottom product recirculated to the NH₃-stripping column in step (e).

2. The process defined in claim 1 wherein according to step (b) the pressure in the pretreatment column according to step (b) is from 1 to 20 bar.

3. The process defined in claim 1 wherein according to step (b) a second waste water stream is taken off from the pretreatment column, said second waste water stream taken off from the top of said column and comprising hydrocarbons or solvents.

4. The process defined in claim 1 wherein according to step (e) a substream of the waste water from the bottom of the NH₃-stripping column is fed into the pretreatment column of step (b).

5. A process for the recovery of NH₃ from a waste water containing NH₃, at least one acid gas selected from the group consisting of CO₂ and H₂S, and an inert gas, which comprises the steps of:

(a) dividing the waste water containing NH₃, at least one acid gas selected from the group consisting of CO₂ and H₂S, and an inert gas into a first waste water sub-stream and a second waste water sub-stream;

(b) providing a pretreatment column with a heating means at the bottom to heat the bottom to a temperature of 130 to 200°

C., introducing the first waste water sub-stream into an upper region of the pretreatment column, and the second waste water sub-stream into the pretreatment column at a location below the upper region of the pretreatment column where the first waste water sub-stream was introduced, to pretreat both the first and the second waste water sub-streams to remove the at least one acid gas from the waste water thereby providing a waste water stream at the bottom of said pretreatment column having undergone removal of said at least one acid gas;

(c) cooling the waste water stream at the bottom of said pretreatment column and channeling in part the waste water stream from the bottom of said pretreatment column to a total stripping column to obtain a top product comprising NH₃ and at least one acid gas, and a bottom product comprising a waste-water stream, cooling the top product, and condensing at least 80% of the NH₃ present in the top product in a condenser in which the top product is scrubbed with circulated and cooled condensate to obtain a waste gas comprising the inert gas and an aqueous NH₃-containing condensate;

(d) cooling the waste-water stream obtained as a bottom product from the total stripping column according to step (c) to a temperature of 10 to 60°

C. and passing the cooled waste-water stream to the top region of the pretreatment column according to step (b);

(e) splitting the NH₃-containing condensate obtained from the condenser during step (c) into two portions, recirculating a first portion of the NH₃-containing condensate back to the condenser in step (c) to condense additional quantities of NH₃ present in the top product, and from a second portion of the NH₃-containing condensate stripping NH₃ in an NH₃-stripping column to obtain NH₃ vapor at the top and a waste stream at the bottom; and

(f) washing the NH₃ vapor with circulating NH₃-containing condensate in a wash column and recovering NH₃ as a top product from the wash column, said NH₃ free of said acid gas and said inert gas, while obtaining a bottom product from the wash column, said bottom product recirculated to the NH₃-stripping column in step (e).