Ammonia recovery from purge gas

• US 5,114,694 A
• Filed: 04/02/1990
• Issued: 05/19/1992
• Est. Priority Date: 04/02/1990
• Status: Expired due to Fees

• Current Assignee: C.F. Braun & Co. (Halliburton Company)
• Original Assignee: C. F. Braun, Inc.
• Inventors: Grotz, Bernard J. Jr.
• Primary Examiner(s): LANGEL, WAYNE A
• Application Number:
  US07/503,266
• Time in Patent Office: 778 Days
• Field of Search: 423/359, 423/352
• US Class Current: 423/352
• CPC Class Codes: C01C 1/0476 Purge gas treatment, e.g. for removal of inert gases or recovery of H2
• CPC Class Codes: Y02P 20/52 using catalysts, e.g. selective catalysts

Abstract

A continuous process for recovering ammonia from a purge gas of an ammonia synthesis system wherein the purge gas is scrubbed by an aqueous liquid solution in counter-current flow with continuous cooling which is controlled to maintain temperature levels safely above the freezing point and to produce an aqueous solution of high ammonia concentration which is mixed with an anhydrous ammonia product of the ammonia synthesis system to form a blended ammonia product with a minimum water concentration high enough to provide corrosion protection to carbon steel storage equipment and a maximum water concentration low enough to meet a maximum design specification for the concentration of water in the blended ammonia product.

Claims

1. A process for the recovery of ammonia from a purge gas of an ammonia synthesis system, comprising the steps of absorbing ammonia contained in the purge gas in water to form an aqueous solution by means of a cooling step and an absorption step, the aqueous solution being formed by contacting the purge gas with water in counter current flow through the cooling step and the absorption step, the cooling step comprising indirect heat exchange with a coolant fluid, at least part of the aqueous solution being blended with at least part of an anhydrous ammonia product from the ammonia synthesis system to form a blended product, the flow rate of the water to the process being controlled to maintain a water concentration in the blended product between a minimum concentration required to provide corrosion protection to carbon steel storage equipment, and a maximum concentration allowed under specifications of the blended product, and the temperature of at least one point in the process being controlled at a level which avoids freezing of liquid at any point in the process.

2. A process for the recovery of ammonia from a purge gas of an ammonia synthesis system, comprising the steps of absorbing ammonia contained in the purge gas in water to form an aqueous solution, the aqueous solution being formed by contacting the purge gas with water in counter current flow, at least part of the aqueous solution being blended with at least part of an anhydrous ammonia product from the ammonia synthesis system to form a blended product, the flow rate of the water to the process being controlled to maintain a water concentration in the blended product between a minimum concentration required to provide corrosion protection to carbon steel storage equipment, and a maximum concentration allowed under specifications of the blended product, and the temperature of at least one point in the process being controlled at a level which avoids freezing of liquid at any point in the process.

3. A continuous process of recovering ammonia from a purge gas of an ammonia synthesis system, comprising the steps of:

introducing the purge gas to a vessel containing a reservoir of an aqueous solution containing ammonia to absorb ammonia from the purge gas into the aqueous solution, which is cooled to produce an aqueous solution of high ammonia concentration which is removed from the vessel and mixed with an anhydrous ammonia product of the ammonia synthesis system to form a blended ammonia product with a minimum water concentration high enough to provide corrosion protection to carbon steel storage equipment and a maximum water concentration low enough to meet a maximum concentration of water in the blended ammonia product;

passing the purge gas out of the vessel and introducing it into a counter-current absorption device;

introducing liquid scrubbing water into the counter-current absorption device;

contacting the purge gas with the liquid scrubbing water in counter-current flow to form a scrubbed gas which is passed from the counter-current absorption device and a dilute ammonia solution which is collected in the vessel to form the reservoir of the aqueous solution containing ammonia;

removing the scrubbed gas from the counter-current absorption device;

controlling the rate at which liquid scrubbing water is introduced into the counter-current absorption device in relation to the rate of purge gas introduced into the counter-current absorption device, the concentration of ammonia in the purge gas and the rate of production of the anhydrous ammonia product of the ammonia synthesis system so that the blended ammonia product will have a water concentration between the minimum and maximum water concentrations; and

controlling the temperature of at least one point in the process by operation of a cooling system to maintain temperature levels safely above the freezing point of any fluid in the counter-current absorption device at all points in the counter-current absorption device and in the vessel.

4. A process as recited in claim 3, wherein the cooling system comprises indirect heat transfer from the mixture in the vessel of purge gas and the aqueous solution containing ammonia to a refrigerant.

5. A process as recited in claim 3, wherein the temperature of the scrubbed gas removed from the counter-current absorption device is controlled to maintain temperature levels safely above the freezing point of any fluid in the counter-current absorption device at all pints in the counter-current absorption device and in the vessel.

6. A process as recited in claim 3, wherein the temperature of the purge gas passing out of the vessel is controlled to maintain temperature levels safely above the freezing point of any fluid in the counter-current absorption device at all points in the counter-current absorption device and in the vessel.

7. A process as recited in claim 3, wherein the liquid scrubbing water flow rate is adjusted automatically to control the density of the aqueous solution of high ammonia concentration such that the blended ammonia product will have a water concentration between the minimum and maximum water concentrations.

8. A process as recited in claim 3, wherein the liquid scrubbing water flow rate is adjusted automatically to control the ratio of the liquid scrubbing water flow rate to the purge gas flow rate such that the blended ammonia product will have a water concentration between the minimum and maximum water concentrations.

9. A process as recited in claim 3, wherein the concentration of ammonia in the aqueous solution of high ammonia concentration is within the range of 50 to 90 weight percent.

10. A process as recited in claim 3, wherein the concentration of ammonia in the scrubbed gas is less than 0.1 volume percent.

11. A process as recited in claim 3 wherein the minimum water concentration of water in the blended ammonia product is greater than about 0.1 weight percent and the maximum concentration of water in the blended ammonia product is less than about 1.0 weight percent.

12. A process as recited in claim 3 wherein the minimum water concentration of water in the blended ammonia product is greater than about 0.2 weight percent and the maximum concentration of water in the blended ammonia product is less than about 0.5 weight percent.

13. A continuous process for recovering ammonia from a purge gas of an ammonia synthesis system, comprising the steps of:

introducing liquid scrubbing water into a counter-current absorption device;

introducing the purge gas into the counter-current absorption device;

contacting the purge gas with the liquid scrubbing water in counter-current flow to transfer ammonia contained in the purge gas to the liquid scrubbing water to form an aqueous solution containing ammonia and a scrubbed gas;

removing the scrubbed gas from the counter-current absorption device;

removing the aqueous solution from the counter-current absorption device and mixing it with an anhydrous ammonia product of the ammonia synthesis system to form a blended ammonia product with a minimum water concentration high enough to provide corrosion protection to carbon steel storage equipment and a maximum water concentration low enough to meet a maximum concentration of water in the blended ammonia product;

controlling the rate of liquid scrubbing water introduced into the counter-current absorption device in relation to the rate of purge gas introduced into the counter-current absorption device, the concentration of ammonia in the purge gas and the rate of production of the anhydrous ammonia product of the ammonia synthesis system so that the blended ammonia product will have a water concentration between the minimum and maximum water concentrations; and

controlling the temperature of at least one point in the process by operation of a cooling system to maintain temperature levels safely above the freezing point of any fluid in the counter-current absorption device at all points in the counter-current absorption device.

14. A process as recited in claim 13, comprising the further step of passing at least part of the purge gas through an expander to extract mechanical energy, thereby lowering the temperature of the purge gas, before introducing the purge gas into the counter-current absorption device.

15. A process as recited in claim 13, comprising the further steps of collecting a portion of the aqueous solution in a vessel where it is cooled and absorbs ammonia from the purge gas to form an aqueous solution of high ammonia concentration which is used to form the blended ammonia product.

16. A process as recited in claim 15, wherein the concentration of ammonia in the aqueous solution of high ammonia concentration is within the range of 50 to 90 weight percent.

17. A process as recited in claim 13, wherein the concentration of ammonia in the aqueous solution mixed with the anhydrous ammonia product is greater than 40 weight percent.

18. A process as recited in claim 13, wherein the concentration of ammonia in the scrubbed gas is less than 0.1 volume percent.

19. A process as recited in claim 13, wherein the minimum water concentration is greater in the blended ammonia product is greater than about 0.1 weight percent.

20. A process as recited in claim 13, wherein the maximum concentration of water in the blended ammonia product is less than about 0.5 weight percent.