Helium recovery

• US 5,542,966 A
• Filed: 10/21/1994
• Issued: 08/06/1996
• Est. Priority Date: 10/21/1994
• Status: Expired due to Term

• Current Assignee: IACX Energy, LLC
• Original Assignee: Nitrotec Corporation
• Inventors: Reinhold, Herbert E. III, Knaebel, Kent S., D'Amico, Joseph S.
• Primary Examiner(s): SPITZER, ROBERT H
• Application Number:
  US08/326,917
• Time in Patent Office: 655 Days
• Field of Search: 95/98, 95/100-105, 95/143-148
• US Class Current: 95/101
• CPC Class Codes: B01D 2253/102 Carbon
• CPC Class Codes: B01D 2253/104 Alumina
• CPC Class Codes: B01D 2253/106 Silica or silicates
• CPC Class Codes: B01D 2253/304 Linear dimensions, e.g. particle shape, diameter
• CPC Class Codes: B01D 2256/18 Noble gases
• CPC Class Codes: B01D 2257/11 Noble gases
• CPC Class Codes: B01D 2259/404 using four beds
• CPC Class Codes: B01D 2259/406 using more than four beds
• CPC Class Codes: B01D 2259/41 using plural beds of the same adsorbent in series
• CPC Class Codes: B01D 53/04 with stationary adsorbents B01D53/025 takes precedence
• CPC Class Codes: B01D 53/047 Pressure swing adsorption
• CPC Class Codes: B01D 53/229 Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
• CPC Class Codes: C01B 2210/001 by making use of membranes
• CPC Class Codes: C01B 2210/0014 by adsorption in solids
• CPC Class Codes: C01B 2210/0031 Helium
• CPC Class Codes: C01B 2210/0068 Organic compounds
• CPC Class Codes: C01B 2210/007 Hydrocarbons
• CPC Class Codes: C01B 23/0052 by adsorption in solids
• CPC Class Codes: C01B 23/0094 Combined chemical and physical processing

Abstract

The disclosed pressure swing adsorption processes can recover helium from source streams of less than about 10 percent by volume helium and concentrate the helium to a concentration of greater than about 98 percent by volume. Two stages of pressure swing adsorption are used in series. The source of the helium gas will be natural gas wells. The source gas will contain hydrocarbons but in most instances the primary gas other than helium will be nitrogen. Each stage of pressure swing adsorption will contain a plurality of adsorbent beds, and preferably about four. In each stage the adsorbent beds will be cycled through multiple phases. In the first stage the adsorbent beds will sequentially undergo the phases of adsorption, recycle, depressurization, evacuation, helium pressurization and recycle feed pressurization. The product gas from the first stage is flowed to the second stage and in the second stage sequentially will undergo the phases of adsorption, depressurization, evacuation, purge, and helium pressurization. The offgas from evacuation and purge in the second stage is flowed to input to the first stage. The processes using an adsorbent that adsorbs the gases other than helium produces a product stream in a high volume with a helium content of more than 98 percent by volume.

Claims

1. A method for the separation of helium from an input gas stream containing helium and other gases by selectively adsorbing said other gases comprising feeding said input gas stream at a pressure to an input to a first stage of a first stage and a second stage of pressure swing adsorption, each stage containing a plurality of interconnected adsorbent beds containing at least one adsorbent, the first stage of pressure swing adsorption concentrating the helium in said gas stream to greater than about 75 percent helium by volume and in said second stage of pressure swing adsorption concentrating said gas stream to greater than about 95 percent helium by volume, feeding a depressurization gas from a depressurization of an adsorbent bed in said first stage to an adsorbent bed of said first stage through which the flow of input gas has ceased and recovering a recycle feed gas therefrom, and flowing said recycle feed gas to an adsorbent bed of said first stage that is to be fed said input gas to at least partially repressurize said adsorbent bed.

2. A method for the separation of helium as in claim 1 wherein in said first stage of pressure swing adsorption there are six phases, each interconnected adsorbent bed undergoing said six phases for each complete cycle, said six phases comprising in sequence an adsorption phase, a recycle phase, a depressurization phase, an evacuation phase, a helium pressurization phase and a recycle feed pressurization phase, a portion of an effluent gas from an adsorbent bed on said depressurization phase being pressurized to about the pressure of said input gas to said adsorption phase and being flowed to an adsorbent bed on said recycle phase with an effluent first stage recycle feed gas enriched in helium flowing therefrom, said effluent first stage recycle feed gas being flowed to an adsorbent bed that is to enter said adsorption phase to pressurize said adsorbent bed to about the input gas pressure of the first stage of pressure swing adsorption.

3. A method for the separation of helium as in claim 2 wherein there are at least four adsorbent beds, feeding said input gas stream to the input end of a first adsorbent bed of said first stage entering on said adsorption phase and selectively adsorbing said other gases, collecting a gas enriched in helium flowing from said first adsorbent bed of said first stage and flowing a portion thereof to said second stage pressure swing adsorption and a portion thereof to a second adsorbent bed of said first stage that has completed said evacuation phase and that has entered said helium pressurization phase, concurrently depressurizing a fourth adsorbent bed of said first stage and collecting said effluent first stage recycle gas, pressurizing said effluent first stage recycle gas to about the pressure of said input gas stream and flowing a pressurized effluent first stage recycle gas to said first adsorbent bed of said first stage upon the completion of said adsorption phase and the initiation of said recycle phase, flowing the effluent from said first adsorbent bed of said first stage during said recycle phase to said second adsorbent bed of said first stage upon the completion of said helium pressurization phase and that is to enter said adsorption phase to pressurize said second adsorbent bed of said first stage to about the input gas stream pressure, and concurrently evacuating a third adsorbent bed of said first stage that has completed said depressurization phase to remove said other gases therefrom.

4. A method for the separation of helium as in claim 3 wherein said second adsorbent bed of said first stage is further pressurized with input gas prior to entering said adsorption phase.

5. A method for the separation of helium as in claim 2 wherein the adsorbent within each of said adsorbent beds is an activated carbon.

6. A method for the separation of helium as in claim 1 wherein in said second stage of pressure swing adsorption there are five phases, each interconnected adsorbent bed undergoing said five phases for each complete cycle said five phases comprising in sequence an adsorption phase, a depressurization phase, an evacuation phase, a purge phase and a helium pressurization phase, flowing a feed gas enriched in helium from said first stage to an adsorbent bed in said second stage undergoing said adsorption phase with a further enriched helium gas effluent flowing therefrom, flowing a first portion of said further enriched helium gas to purge at least some other gases from an other adsorbent bed in said purge phase, flowing a second portion of said enriched helium gas to a further adsorbent bed that has completed said purge phase and which is to enter said adsorption phase to pressurize this adsorbent bed, and flowing a third portion of said further enriched helium to product.

7. A method for the separation of helium as in claim 6 wherein there are at least four adsorbent beds, feeding said gas from said first stage as said feed gas to a first adsorbent bed in said second stage and collecting three portions of a further enriched helium gas therefrom, concurrently depressurizing a fourth adsorbent bed of said second stage which has completed the production of said further enriched helium and which contains substantial amounts of said other gases, recovering an effluent second stage recycle gas from said fourth adsorbent bed of said second stage and pressurizing said second stage recycle gas to about the pressure of said feed gas to said second stage and flowing said second stage recycle gas to said first adsorbent bed of said second stage, concurrently reducing the pressure in a third adsorbent bed of said second stage to less than about ambient pressure in said evacuation phase and removing a portion of said other gases therefrom, concurrently flowing a first portion of further enriched helium from said first adsorbent bed of said second stage to said third adsorbent bed of said second stage which has completed said evacuation phase as purge gas and further removing said other gases therefrom, and concurrently flowing a second portion of said further enriched helium to a second adsorbent bed of said second stage to increase the pressure within said second adsorbent bed of said second stage.

8. A method for the separation of helium as in claim 6 wherein the adsorbent within each of said adsorbent beds is an activated carbon.

9. A method for the separation of helium from an input gas containing helium and other gases by selectively adsorbing said other gases comprising feeding said input gas to a plurality of interconnected adsorbent beds in a pressure swing adsorption system with each adsorbent bed containing at least one adsorbent, each interconnected adsorbent bed undergoing six phases for each complete cycle, said six phases comprising in sequence an adsorption phase, a recycle phase, a depressurization phase, an evacuation phase, a helium pressurization phase and a recycle feed pressurization phase wherein a portion of an effluent gas from an adsorbent bed being reduced in pressure in said depressurization phase is pressurized to about the pressure of said input gas to said adsorbent bed on said adsorption phase and is flowed to an adsorbent bed on said recycle phase with an effluent recycle feed gas enriched in helium flowing therefrom, said effluent recycle feed gas being flowed to an adsorbent bed that is to enter said adsorption phase to pressurize said adsorbent bed to about the pressure of the input gas to said adsorption phase.

10. A method for the separation of helium as in claim 9 comprising feeding said input gas to a first adsorbent bed with an enriched helium gas stream flowing therefrom, flowing a portion of said enriched helium gas stream as a pressurization gas to a second adsorbent bed to increase the pressure in said second adsorbent bed, concurrently depressurizing a fourth adsorbent bed from an elevated pressure and recovering a first gas as a depressurization gas and a second gas, increasing the pressure of said depressurization gas and flowing said depressurization gas to said first adsorbent bed upon the completion of feeding said input gas stream thereto to produce said effluent recycle feed gas, flowing said effluent recycle feed gas to said second adsorbent bed after the flow of helium enriched gas from said first adsorbent bed to pressurize said second adsorbent bed to further increase the pressure in said second adsorbent bed, and concurrently reducing the pressure in a third adsorbent bed to less than ambient to remove said adsorbed other gases therefrom.

11. A method for the separation of helium as in claim 10 wherein said third and fourth adsorbent beds are depressurized countercurrently with said first gas flowed cocurrently into said first adsorbent bed.

12. A method for the separation of helium as in claim 10 wherein said second adsorbent bed is further pressurized with said input gas prior to entering said adsorption phase.

13. A method for the separation of helium as in claim 10 wherein each adsorbent bed contains an activated carbon adsorbent.

14. A method for the separation of helium from a feed gas containing helium and other gases by selectively adsorbing said other gases comprising flowing said feed gas sequentially to a plurality of interconnected adsorbent beds containing at least one adsorbent in a pressure swing adsorption system, each interconnected adsorbent bed undergoing five phases for each complete cycle, said five phases comprising in sequence an adsorption phase, a depressurization phase, an evacuation phase, a purge phase and a helium pressurization phase, flowing said feed gas along with an effluent recycle gas from the depressurization of an adsorbent bed on said depressurization phase to an adsorbent bed undergoing an adsorption phase with an enriched helium gas effluent flowing therefrom, flowing a first portion of said enriched helium gas to purge other gases from an adsorbent bed that has completed said evacuation phase and that is in said purge phase, flowing a second portion of said enriched helium gas to an adsorbent bed that has completed said purge phase and which is to enter said absorbent phase, and flowing a third portion of said enriched helium to product.

15. A method for the separation of helium as in claim 14 comprising feeding said feed gas to the inlet of a first adsorbent bed with said enriched helium gas flowing therefrom, flowing said first portion of said enriched helium gas to a third adsorbent bed to purge said other gases from said third adsorbent bed when said third adsorbent bed is at a pressure less than about ambient, flowing said second portion of said enriched helium gas to a second adsorbent bed to pressurize said second adsorbent bed, concurrently depressurizing a fourth adsorbent bed and flowing said effluent recycle gas therefrom to said first adsorbent bed as additional feed gas, and concurrently decreasing the pressure in said third adsorbent bed to less than about ambient and flowing a gas enriched in other gases therefrom.

16. A method for the separation of helium as in claim 15 wherein the flow of gas from said fourth adsorbent bed and said third adsorbent bed is countercurrent.

17. A method for the separation of helium as in claim 15 wherein said second adsorbent bed is further pressurized with said feed gas.

18. A method for the separation of helium as in claim 14 wherein the adsorbent in each of said adsorbent beds is an activated carbon adsorbent.

19. A method for the separation of helium from an input gas stream containing helium and other gases by selectively adsorbing said other gases in a first stage of pressure swing adsorption, said first stage consisting of at least four interconnected adsorbent beds, each adsorbent bed containing at least one adsorbent and undergoing six phases for each complete cycle of pressure swing adsorption, said six phases comprising in sequence an adsorption phase, a recycle phase, a depressurization phase, an evacuation phase, a helium pressurization phase and a recycle feed pressurization phase, feeding said input gas stream at a pressure to the input end of a first adsorbent bed of said first stage entering on said adsorption phase and selectively adsorbing said other gases, collecting a gas enriched in helium flowing from said first adsorbent bed of said first stage and flowing a portion thereof to a second adsorbent bed of said first stage that has completed said evacuation phase and that has entered said helium pressurization phase, concurrently depressurizing a fourth adsorbent bed of said first stage and collecting an effluent first stage recycle gas, pressurizing said effluent first stage recycle gas to about the pressure of said input gas stream and flowing a pressurized effluent first stage recycle gas to said first adsorbent bed of said first stage upon the completion of said adsorption phase and the initiation of said recycle phase, flowing the effluent from said first adsorbent bed of said first stage during said recycle phase to said second adsorbent bed of said first stage upon the completion of said helium pressurization phase and that is to enter said adsorption phase to pressurize said second adsorbent bed of said first stage to about the pressure of said input gas, concurrently evacuating a third adsorbent bed of said first stage that has completed said depressurization phase to remove said other gases therefrom, flowing another portion of said gas enriched in helium to a second stage of pressure swing adsorption which consists of at least four interconnected adsorbent beds containing at least one adsorbent, each such adsorbent bed undergoing five phases for each complete cycle of pressure swing adsorption, said five phases comprising in sequence an adsorption phase, a depressurization phase, an evacuation phase, a purge phase and a helium pressurization phase, feeding said enriched helium gas from said first stage at a pressure as a feed gas to a first adsorbent bed in said second stage and collecting three portions of a further enriched helium gas therefrom, concurrently depressurizing a fourth adsorbent bed of said second stage which has completed the production of said further enriched helium gas and which contains substantial amounts of said other gases, recovering an effluent second stage recycle gas from said fourth adsorbent bed of said second stage and pressurizing said effluent second stage recycle gas to about the pressure of said feed gas to said second stage and flowing said effluent second stage recycle gas to said first adsorbent bed of said second stage, concurrently reducing the pressure in a third adsorbent bed of said second stage to less than about ambient pressure and removing a portion of said other gases therefrom, concurrently flowing a first portion of further enriched helium from said first adsorbent bed of said second stage to said third adsorbent bed of said second stage which has completed said evacuation phase as a purge gas and further removing said other gases therefrom, concurrently flowing a second portion of said further enriched helium to a second adsorbent bed of said second stage to increase the pressure within such adsorbent bed, and flowing said other gases from said third adsorbent bed of said second stage to said first adsorbent bed in said first stage.

20. A method for the separation of helium as in claim 19 wherein the adsorbent in each adsorbent bed is an activated carbon adsorbent.