WO2011139894A1 - Méthode et dispositif de fabrication d'un gaz de pureté élevée - Google Patents

Méthode et dispositif de fabrication d'un gaz de pureté élevée Download PDF

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Publication number
WO2011139894A1
WO2011139894A1 PCT/US2011/034560 US2011034560W WO2011139894A1 WO 2011139894 A1 WO2011139894 A1 WO 2011139894A1 US 2011034560 W US2011034560 W US 2011034560W WO 2011139894 A1 WO2011139894 A1 WO 2011139894A1
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WIPO (PCT)
Prior art keywords
valve
vessel
gas
bed
check
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PCT/US2011/034560
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English (en)
Inventor
Walter H. Whitlock
Original Assignee
Linde Aktiengesellschaft
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Publication of WO2011139894A1 publication Critical patent/WO2011139894A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/047—Pressure swing adsorption
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof
    • C01B23/001—Purification or separation processes of noble gases
    • C01B23/0036—Physical processing only
    • C01B23/0052—Physical processing only by adsorption in solids
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/16—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/18—Noble gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40003—Methods relating to valve switching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/402—Further details for adsorption processes and devices using two beds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042—Purification by adsorption on solids
    • C01B2203/043—Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0029—Obtaining noble gases
    • C01B2210/0031—Helium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0042—Making ultrapure specific gas

Definitions

  • the present invention relates to methods and apparatus for producing high purity gas.
  • the present invention relates to method and apparatus for producing helium or hydrogen at more than 99.999% (five 9s) purity.
  • PSA pressure swing adsorption
  • PSA techniques are capable of separating one gas species from a mixture of gases under pressure based on the molecular characteristics and affinity of the gas species for an adsorbent material.
  • PSA generally operates at near-ambient temperatures and uses special adsorptive materials (e.g., zeolites) to preferentially adsorb the target gas species at high pressure. The process then swings to a low pressure in order to desorb the target gas species from the adsorbent material.
  • PSA processes rely on the fact that under pressure, gases tend to be attracted or adsorbed onto solid surfaces, wherein the higher the pressure, the more gas is adsorbed. When the pressure is reduced, the adsorbed gas is released, or desorbed.
  • PSA processes are used to separate a target gas from a mixture of gases because different gases tend to be attracted to different solid surfaces in different degrees. For example, if a gas mixture comprising air is passed under pressure through a vessel containing an adsorbent bed that attracts nitrogen more strongly than it does oxygen, then a part or all of the nitrogen will stay in the bed, and the gas exiting the adsorption vessel will be enriched in oxygen. Once the adsorbent bed is saturated with nitrogen (reaches its capacity to adsorb nitrogen), the bed can be regenerated by reducing the pressure and thereby releasing the adsorbed nitrogen. The adsorption bed is then ready for another cycle of producing oxygen enriched air.
  • PSA processes can be used for producing pure gases, such as hydrogen and helium, at purity levels of about 99.9%.
  • PSA techniques are not generally capable of producing high purity gases having purities of 99.999% or higher, without additional purification processes being required, e.g. a thermal swing adsorption process.
  • the equalization process in a PSA process is normally carried out at relatively low pressures to avoid lifting of the bed. Bed lifting can occur because typical PSA apparatus routes gas from the outlet of the high pressure vessel to the outlet of the low pressure vessel.
  • the present invention overcomes the problems associated with prior art PSA processes and provides methods and apparatus for producing high purity gas.
  • the present invention provides method and apparatus for producing gases having 99.999% purity or higher without requiring secondary purification processes.
  • Figure 1 is a schematic drawing of an apparatus showing one stage operation according to the present invention.
  • Figure 2 is a schematic drawing of an apparatus showing another stage operation according to the present invention.
  • FIG. 1 is a schematic drawing of an apparatus showing a further stage operation according to the present invention.
  • FIG. 1 is a schematic drawing of an apparatus showing a further stage operation according to the present invention.
  • FIG. 5 is a schematic drawing of an apparatus showing another stage operation according to the present invention.
  • FIG. 6 is a schematic drawing of an apparatus showing another stage operation according to the present invention.
  • FIG. 7 is a schematic drawing of an apparatus showing further stage operation according to the present invention.
  • FIG. 8 is a schematic drawing of an apparatus showing further stage operation according to the present invention.
  • Figure 9 is a schematic drawing of an apparatus showing another stage operation according to the present invention.
  • FIG. 10 is a schematic drawing of an apparatus showing another stage operation according to the present invention.
  • the present invention provides methods and apparatus for producing a high purity gas, e.g. having purity of 99.999% or higher, using a PSA process, without the need for any secondary purification process.
  • the methods and apparatus of the present invention will be described in detail with reference to drawing figures 1 through 6 that show various stages of the purification operation according to the present invention.
  • FIG. 1 shows a stage of the purification operation of the present invention, wherein a first adsorption bed 10 is in service and a second adsorption bed 20 is in standby mode.
  • Operating pressure of bed 10 is about 160 psig while the pressure for the bed 20 is at low pressure, e.g. 0 psig or vacuum.
  • Feed gas to be purified is provided from feed gas source 30 and passes into bed 10 through valve VIA.
  • Impurities in the feed gas are adsorbed in bed 10 and purified product exits bed 10 and passes through check valve CVl A to the system outlet for immediate use or to optional storage container 40.
  • FIG. 1 Upon saturation of the adsorbent in bed 10 with impurities, regeneration of bed 10 must be carried out. While bed 10 is being regenerated, bed 20 is operated in adsorption mode.
  • the first step of switching operation from bed 10 to bed 20 comprises equalization of pressure between bed 10 and bed 20.
  • Figure 2 shows a stage of operation wherein the equalization process begins. Valve V3A is opened and valve V2B is opened or remains open from earlier operation. Check valve CVl A can also be closed, or will automatically block further exit of gas from bed 10 once valve V3A is opened. Because bed 10 is at a higher pressure than bed 20, pressure equalization will occur by making the connection between bed 10 and bed 20 through valve V3A and valve V2B.
  • Gas will flow out of the bottom outlet of bed 10 and flow to the top inlet of bed 20 through valve V3A and valve V2B.
  • bed lifting is avoided because gas flow is always in a downward direction through the adsorption beds. This allows for the use of higher gas velocities and quicker equalization without the risk of bed lifting and disruption.
  • some impurities will exit the outlet of bed 10 and enter bed 20. In conventional PSA operations where equalization flow is from outlet of the first bed to outlet of the second bed this can cause buildup of impurity at the outlet of the second bed and result in contamination of the product exiting the second bed when the second bed is placed into adsorption mode.
  • the present invention provides an advantage here also.
  • by routing flow from the outlet of bed 10 to the inlet of bed 20 buildup of impurities at the outlet of bed 20 can be avoided and therefore contamination of product exiting bed 20 is reduced.
  • the present invention can achieve five 9's (99.999%) purity levels.
  • valve VIA is closed to stop flow of feed gas into bed 10 and valve VI B is open so that feed gas from feed gas source 30 now flows into bed 20.
  • valve V2B is closed to stop regeneration flow to bed 20 and valve V2A is open to begin regeneration flow to bed 10.
  • bed 10 is depressurized and bed 20 is brought up to operating pressure.
  • bed 10 is depressurized by venting gas from bed 10 though valve V2A and valve V5 and valve V3A is closed.
  • bed 10 may be vented through valve V3 A and valve V5 with valve V2A closed.
  • bed 10 is depressurized to a low target pressure, e.g. 0 psig or vacuum.
  • bed 20 is pressurizing to operation pressure.
  • operating pressure e.g. 160 psig
  • purified product gas exits bed 20 and flows through check valve CVIB to the system outlet for immediate use or to optional storage container 40.
  • bed 10 While bed 20 is in operation, bed 10 is regenerated by reverse purge of bed 10.
  • valve V3A is closed and valve V4A is opened. Opening of valve V4A allows at least some of the gas exiting through check valve CVIB to flow through valve V4A and then in reverse flow through bed 10.
  • the purge gas flows through bed 10 at low pressure to remove remaining impurities and then exits the system through valve V2A and valve 5.
  • a separate source of high purity purge gas can be provided instead of using high purity product gas exiting from check valve CVIB as the purge gas.
  • valve V4A is closed as well as valve 5.
  • Bed 10 then remains in standby mode and bed 20 continues to operate in adsorption mode with high purity gas exiting the system through check valve CVIB.
  • operation of the PSA system switches back to bed 10 as will be explained below with reference to Figures 7 through 12.
  • FIG. 6 shows a stage of the purification operation wherein the second adsorption bed 20 is in service and the first adsorption bed 10 has been regenerated and is in stand by mode.
  • Operating pressure of bed 20 is about 160 psig while the pressure for the bed 10 is at low pressure, e.g. 0 psig or vacuum.
  • Feed gas to be purified is provided from feed gas source 30 and passes into bed 20 through valve VI B. impurities in the feed gas are adsorbed in bed 20 and purified product exits bed 20 and passes through check valve CVIB to the system outlet for immediate use or to optional storage container 40.
  • FIG. 7 shows a stage of operation wherein the equalization process begins.
  • Valve V3B is opened and valve V2A is opened or remains open from an earlier stage.
  • Check valve CVIB can also be closed, or will automatically block further exit of gas from bed 20 once valve V3B is opened. Because bed 20 is at a higher pressure than bed 10, pressure equalization will occur by making the connection between bed 20 and bed 10 through valve V3B and valve V2A.
  • Gas will flow out of the bottom outlet of bed 20 and flow to the top inlet of bed 20 through valve V3B and valve V2A.
  • bed lifting is avoided because gas flow is always in a downward direction through the adsorption beds. This allows for the use of higher gas velocities and quicker equalization without the risk of bed lifting and disruption. Further, the buildup of impurities at the outlet of bed 10 is avoided resulting in reduced contamination of product exiting bed 10 and the ability to achieve five 9's (99.999%) purity levels.
  • valve VI B is closed to stop flow of feed gas into bed 20 and valve VI A is open so that feed gas from feed gas source 30 now flows into bed 10.
  • valve V2A is closed to stop regeneration flow to bed 10 and valve V2B is open to begin regeneration flow to bed 20.
  • bed 20 is depressurized and bed 10 is brought up to operating pressure.
  • bed 20 is depressurized by venting gas from bed 20 though valve V2B and valve V5 and valve V3B is closed.
  • bed 20 may be vented through valve V3B and valve V5 with valve V2B closed. In either way bed 20 is depressurized to a low target pressure, e.g. 0 psig or vacuum.
  • a low target pressure e.g. 0 psig or vacuum.
  • bed 20 is regenerated by reverse purge of bed 20.
  • valve V3B is closed and valve V4B is opened. Opening of valve V4B allows at least some of the gas exiting through check valve CV1A to flow through valve V4B and then in reverse flow through bed 20.
  • the purge gas flows through bed 20 at low pressure to remove remaining impurities and then exits the system through valve V2B and valve 5.
  • a separate source of high purity purge gas can be provided.
  • Bed 20 then remains in standby mode and bed 10 continues to operate in adsorption mode with high purity gas exiting the system through check valve CVl A as shown in Figure 6.
  • This sequence of operations represents a full cycle of the PSA system according to the present invention.
  • operation of the PSA system is again switched back to bed 20 as explained above.
  • Stage Depressurize bed 10; Pressurize bed 20 ( Figure 4)
  • Stage Reverse purge bed 10; Bed 20 in service ( Figure 5)
  • Stage Bed 20 in service; Bed 10 in stand by mode ( Figure 6)
  • VIA VIA; V3A; V4A; CV1A; Closed No V2B; V3B; V4B; V5
  • Stage Switch beds; Stop gas flow to bed 20; Start gas flow to bed 10 ( Figure 8)
  • Stage Depressurize bed 20; Pressurize bed 10 ( Figure 9)
  • Stage Reverse purge bed 20; Bed 10 in service ( Figure 10)
  • the present invention provides several advantages over standard PSA processes known in the prior art.
  • the apparatus and method of the present invention wherein the outlet of each adsorption bed is connected to the inlet of the other adsorption bed, it is possible to achieve very high purity for product gases without having to use a secondary purification process.
  • the apparatus and method of the present invention makes it possible to achieve 99.999% or higher purity using only the PSA process according to the present invention.
  • bed lifting is avoided in the present invention by performing equalization with gas always flowing down through the adsorption beds. This allows for higher gas velocities to be used and therefore quicker equalization without the risk of bed lifting and disruption.
  • the present invention can be used for purification of any gas by choosing appropriate adsorbent materials.
  • the present invention is useful for producing very high purity hydrogen and helium.

Abstract

La présente invention concerne des méthodes d'adsorption par variation de pression et un dispositif de production d'un gaz de pureté élevée. De l'hélium ou de l'hydrogène de pureté 99,999 % ou plus est obtenu par un procédé d'adsorption par variation de pression sans nécessiter de processus de purification secondaire.
PCT/US2011/034560 2010-05-05 2011-04-29 Méthode et dispositif de fabrication d'un gaz de pureté élevée WO2011139894A1 (fr)

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US61/331,491 2010-05-05

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US8906138B2 (en) 2007-11-12 2014-12-09 Exxonmobil Upstream Research Company Methods of generating and utilizing utility gas
US8921637B2 (en) 2010-11-15 2014-12-30 Exxonmobil Upstream Research Company Kinetic fractionators, and cycling processes for fractionation of gas mixtures
US9017457B2 (en) 2011-03-01 2015-04-28 Exxonmobil Upstream Research Company Apparatus and systems having a reciprocating valve head assembly and swing adsorption processes related thereto
US9034079B2 (en) 2011-03-01 2015-05-19 Exxonmobil Upstream Research Company Methods of removing contaminants from hydrocarbon stream by swing adsorption and related apparatus and systems
US9034078B2 (en) 2012-09-05 2015-05-19 Exxonmobil Upstream Research Company Apparatus and systems having an adsorbent contactor and swing adsorption processes related thereto
US9067168B2 (en) 2010-05-28 2015-06-30 Exxonmobil Upstream Research Company Integrated adsorber head and valve design and swing adsorption methods related thereto
US9120049B2 (en) 2011-03-01 2015-09-01 Exxonmobil Upstream Research Company Apparatus and systems having a rotary valve assembly and swing adsorption processes related thereto
US9126138B2 (en) 2008-04-30 2015-09-08 Exxonmobil Upstream Research Company Method and apparatus for removal of oil from utility gas stream
US9162175B2 (en) 2011-03-01 2015-10-20 Exxonmobil Upstream Research Company Apparatus and systems having compact configuration multiple swing adsorption beds and methods related thereto
US9168485B2 (en) 2011-03-01 2015-10-27 Exxonmobil Upstream Research Company Methods of removing contaminants from a hydrocarbon stream by swing adsorption and related apparatus and systems
US9352269B2 (en) 2011-03-01 2016-05-31 Exxonmobil Upstream Research Company Apparatus and systems having a rotary valve assembly and swing adsorption processes related thereto
US9358493B2 (en) 2011-03-01 2016-06-07 Exxonmobil Upstream Research Company Apparatus and systems having an encased adsorbent contactor and swing adsorption processes related thereto
US9675925B2 (en) 2014-07-25 2017-06-13 Exxonmobil Upstream Research Company Apparatus and system having a valve assembly and swing adsorption processes related thereto
US9713787B2 (en) 2014-12-10 2017-07-25 Exxonmobil Upstream Research Company Adsorbent-incorporated polymer fibers in packed bed and fabric contactors, and methods and devices using same
US9744521B2 (en) 2014-12-23 2017-08-29 Exxonmobil Upstream Research Company Structured adsorbent beds, methods of producing the same and uses thereof
US9751041B2 (en) 2015-05-15 2017-09-05 Exxonmobil Upstream Research Company Apparatus and system for swing adsorption processes related thereto
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