TWI581855B - Method and apparatus for making a high purity gas - Google Patents

Method and apparatus for making a high purity gas Download PDF

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TWI581855B
TWI581855B TW100115796A TW100115796A TWI581855B TW I581855 B TWI581855 B TW I581855B TW 100115796 A TW100115796 A TW 100115796A TW 100115796 A TW100115796 A TW 100115796A TW I581855 B TWI581855 B TW I581855B
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valve
container
gas
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TW201206551A (en
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華特Ｈ 惠洛克
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林德股份公司
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    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Gases By Adsorption (AREA)

Description

製造高純度氣體的方法及裝置Method and device for manufacturing high purity gas

本發明係關於製造高純度氣體之方法及裝置。特定言之，本發明係關於製造具有大於99.999%(5個9)純度之氦氣或氫氣之方法及裝置。The present invention relates to a method and apparatus for producing high purity gases. In particular, the present invention relates to a method and apparatus for producing helium or hydrogen having a purity greater than 99.999% (5 9).

氣體純化常係藉由使用變壓吸附(PSA)法實施。PSA技術可基於氣體種類對吸附劑物質之分子特性及親和性在壓力下自氣體混合物中分離出一種氣體。PSA一般係於近周溫下操作及使用特定吸附物質(例如，沸石)以於高壓下優先吸附標的氣體。該方法隨後變為低壓以使標的氣體自吸附物質解吸附。PSA製程依賴於在壓力下氣體趨於吸引或吸附至固體表面上之事實，其中壓力越高，所吸附之氣體越多。當壓力降低時，所吸附之氣體會釋放或解吸附。Gas purification is often carried out by using a pressure swing adsorption (PSA) process. The PSA technology separates a gas from a gas mixture under pressure based on the molecular characteristics and affinity of the adsorbent species. PSA is typically operated at near ambient temperatures and uses a specific adsorbent species (eg, zeolite) to preferentially adsorb the target gas at elevated pressures. The process then becomes a low pressure to desorb the target gas from the adsorbed species. The PSA process relies on the fact that the gas tends to attract or adsorb on the solid surface under pressure, where the higher the pressure, the more gas is adsorbed. When the pressure is lowered, the adsorbed gas is released or desorbed.

PSA製程係用於將標的氣體自氣體混合物分離，係因不同氣體趨於以不同程度吸引至不同固體表面。例如，若包含空氣之氣體混合物於壓力下通過包含對氮氣的吸附性較對氧氣強的吸附劑床之容器時，一部份或全部氮氣將留於該床中，且該吸附容器排出之氣體將富含氧氣。一旦該吸附劑床飽和含有氮氣(達到其吸附氮氣之容量)，則可藉由降低壓力且進而釋放所吸附的氮氣而使該床再生。該吸附床隨後可用於製造富氧空氣之另一偱環。The PSA process is used to separate the target gas from the gas mixture as different gases tend to attract to different solid surfaces to varying degrees. For example, if a gas mixture comprising air is passed under pressure through a vessel comprising an adsorbent bed that is more adsorptive to nitrogen than oxygen, some or all of the nitrogen will remain in the bed and the gas exiting the adsorbent vessel Will be rich in oxygen. Once the adsorbent bed is saturated with nitrogen (to achieve its capacity to adsorb nitrogen), the bed can be regenerated by reducing the pressure and thereby releasing the adsorbed nitrogen. The adsorbent bed can then be used to make another loop of oxygen-enriched air.

藉由使用兩吸附劑容器，可提供標的氣體之連續製造。特定言之，當一容器係呈吸附模式時，另一容器再生。此外，兩容器系統可使壓力平衡，其中離開再生容器之氣體係用於對第二容器進行部份加壓。此明顯地節能且於工業實踐中所常見。By using two adsorbent vessels, continuous manufacture of the target gas can be provided. In particular, when one container is in the adsorption mode, another container is regenerated. In addition, the two vessel system can balance the pressure, wherein the gas system exiting the regeneration vessel is used to partially pressurize the second vessel. This is clearly energy efficient and common in industrial practice.

PSA製程可用於製造具有約99.9%純度級之純氣體，如氫氣及氦氣。然而，PSA技術一般需額外的純化製程(例如，熱回轉吸附法)才能製造出具有99.999%或更高純度之高純度氣體。The PSA process can be used to produce pure gases having a purity level of about 99.9%, such as hydrogen and helium. However, PSA technology generally requires an additional purification process (eg, hot swing adsorption) to produce a high purity gas with a purity of 99.999% or higher.

PSA製程之平衡過程一般係於相對低壓下實施以避免床體升高。床體升高可因常見PSA裝置使氣體自高壓容器出口導向低壓容器出口而發生。The equilibrium process of the PSA process is generally carried out at a relatively low pressure to avoid bed rise. The rise in bed can occur as a result of the common PSA unit directing gas from the outlet of the high pressure vessel to the outlet of the low pressure vessel.

本技藝需改良PSA製程，特定言之用於製造具有高於99.9%之純度之氣體。The art requires an improved PSA process, specifically for the manufacture of gases having a purity greater than 99.9%.

本發明克服與先前技藝PSA製程有關之問題並提供製造高純度氣體之方法及裝置。特定言之，本發明提供用於製造具有99.999%純度或更高之氣體而無需二次純化製程之方法及裝置。The present invention overcomes the problems associated with prior art PSA processes and provides methods and apparatus for making high purity gases. In particular, the present invention provides methods and apparatus for making a gas having a purity of 99.999% or higher without the need for a secondary purification process.

本發明提供使用PSA製程製造高純度(例如，具有99.999%或更高純度)之氣體而無需任何二次純化製程之方法及裝置。本發明之方法及裝置將參照顯示本發明各純化操作階段之圖1至6詳細描述。The present invention provides methods and apparatus for producing high purity (e.g., having a purity of 99.999% or higher) using a PSA process without any secondary purification process. The method and apparatus of the present invention will be described in detail with reference to Figures 1 through 6 showing the various stages of purification of the present invention.

圖1顯示本發明純化操作之一階段，其中一第一吸附床10係處於運作中及一第二吸附床20係處於備用狀態。床10之操作壓力為約160 psig，而床20之壓力係低壓，例如，0 psig或真空。待純化之進料氣體係由進料氣體源30提供並經由閥門V1A進入床10。進料氣體中之雜質被吸附於床10中且純化產物自床10排出及經由止回閥CV1A通向系統出口以立即使用或至視需要之存儲容器40。Figure 1 shows a stage of the purification operation of the present invention in which a first adsorbent bed 10 is in operation and a second adsorbent bed 20 is in standby. The operating pressure of bed 10 is about 160 psig, while the pressure of bed 20 is low pressure, for example, 0 psig or vacuum. The feed gas system to be purified is supplied from feed gas source 30 and enters bed 10 via valve V1A. Impurities in the feed gas are adsorbed in bed 10 and the purified product is withdrawn from bed 10 and passed through check valve CV1A to the system outlet for immediate use or to desired storage vessel 40.

當床10中之吸附劑經雜質飽和時，需對床10進行再生。當床10進行再生時，床20係以吸附模式操作。自床10至床20之切換操作之第一步驟包含床10與床20間之壓力平衡。圖2顯示平衡製程開始時之操作階段。閥門V3A開啟且閥門V2B開啟或自先前操作時就維持開啟。止回閥CV1A亦可關閉，或將自動阻止一旦閥門V3A開啟時氣體自床10進一步排出。由於床10係處於較床20高之壓力下，故壓力平衡將係藉由使床10與床20經由閥門V3A及閥門V2B連接來實施。氣體將自床10之底端出口流出並經由閥門V3A及閥門V2B流向床20之頂端入口。藉由使氣流自床10之出口流向床20之入口，可避免床體升高，係因氣流總是沿向下方向通過吸附床。此容許使用較高氣體速度及較快速平衡而不存在床體升高及中斷之風險。如PSA操作中所常見，平衡結束時，一些雜質將自床10之出口排出並進入床20。於習知PSA操作中，平衡流係自第一床之出口至第二床之出口，此可導致雜質累積於第二床之出口及導致當將第二床置於吸附模式時，自第二床排出之產物受污染。本發明亦提供此點優勢。特定言之，藉由使流自床10之出口流向床20之入口，可避免雜質累積於床20之出口及因此減小床20所排出產物之污染。此獲得較標準PSA製程所能達到的純度更高之產物純度。特定言之，本發明可獲得5個9(99.999%)的純度級。When the adsorbent in the bed 10 is saturated with impurities, the bed 10 needs to be regenerated. When the bed 10 is being regenerated, the bed 20 is operated in an adsorption mode. The first step of the switching operation from bed 10 to bed 20 involves a pressure balance between bed 10 and bed 20. Figure 2 shows the operational phase at the beginning of the balancing process. Valve V3A is open and valve V2B is open or remains open from previous operations. The check valve CV1A can also be closed, or will automatically prevent further gas from being discharged from the bed 10 once the valve V3A is opened. Since bed 10 is at a higher pressure than bed 20, pressure equalization will be achieved by connecting bed 10 to bed 20 via valve V3A and valve V2B. Gas will flow from the bottom end outlet of bed 10 and will flow to the top inlet of bed 20 via valve V3A and valve V2B. By flowing the gas stream from the outlet of the bed 10 to the inlet of the bed 20, the bed rise can be avoided because the gas flow always passes through the adsorbent bed in a downward direction. This allows for higher gas velocities and faster balancing without the risk of bed rise and break. As is common in PSA operations, some impurities will exit the bed 10 and enter the bed 20 at the end of the equilibrium. In the conventional PSA operation, the equilibrium flow system is from the outlet of the first bed to the outlet of the second bed, which may cause impurities to accumulate at the outlet of the second bed and cause the second bed to be placed in the adsorption mode, since the second The product discharged from the bed is contaminated. The present invention also provides this advantage. In particular, by flowing the outlet from the bed 10 to the inlet of the bed 20, impurities can be prevented from accumulating at the outlet of the bed 20 and thus reducing the contamination of the product discharged from the bed 20. This results in a higher purity product purity than can be achieved with standard PSA processes. In particular, the present invention achieves five 9 (99.999%) purity levels.

床10與床20達到平衡時，則吸附製程自床10切換至床20。特定言之，如圖3所示，關閉閥門V1A以終止進料氣體流入床10及開啟閥門V1B以使進料氣體自進料氣體源30流入床20中。同時，關閉閥門V2B以終止再生流流向床20及開啟閥門V2A以使再生流流向床10。When bed 10 and bed 20 are in equilibrium, the adsorption process is switched from bed 10 to bed 20. Specifically, as shown in FIG. 3, valve V1A is closed to terminate the flow of feed gas into bed 10 and to open valve V1B to cause feed gas to flow from feed gas source 30 into bed 20. At the same time, valve V2B is closed to terminate the regeneration flow to bed 20 and to open valve V2A to cause regeneration flow to bed 10.

將進料氣體流自床10切換至床20後，發生以下兩事件，使床10減壓及將床20升至操作壓力。特定言之，如圖4所示，藉由使氣體自床10經由閥門V2A及閥門V5排出來減壓，並關閉閥門V3A。或者，可使床10經由閥門V3A及閥門V5排氣，同時關閉閥門V2A。以任一方式，將床10減壓至低標的壓力，例如，0 psig或真空。同時，將床20增壓至操作壓力。到達操作壓力，例如160 psig時，純化產物氣體自床20排出及經由止回閥CV1B流向系統出口以立即使用或至視需要之存儲容器40。After switching the feed gas stream from bed 10 to bed 20, the following two events occur, depressurizing bed 10 and raising bed 20 to operating pressure. Specifically, as shown in FIG. 4, the gas is depressurized by discharging the gas from the bed 10 through the valve V2A and the valve V5, and the valve V3A is closed. Alternatively, bed 10 can be vented via valve V3A and valve V5 while valve V2A is closed. In either manner, bed 10 is depressurized to a low pressure, for example, 0 psig or vacuum. At the same time, bed 20 is pressurized to operating pressure. Upon reaching an operating pressure, such as 160 psig, the purified product gas exits the bed 20 and flows through the check valve CV1B to the system outlet for immediate use or to the desired storage vessel 40.

當床20處於操作中時，藉由床10之逆流清洗使床10再生。特定言之，如圖5所示，關閉閥門V3A及開啟閥門V4A。閥門V4A之開啟容許經由止回閥CV1B排出之至少一部份氣體流經閥門V4A及隨後逆向流經床10。清洗氣體低壓下流經床10以移除殘餘雜質及隨後經由閥門V2A及閥門5自系統排出。於另一方案中，不將自止回閥CV1B排出之高純度產物氣體用作清洗氣體，而係可提供獨立的高純度清洗氣體源。When the bed 20 is in operation, the bed 10 is regenerated by countercurrent cleaning of the bed 10. Specifically, as shown in FIG. 5, the valve V3A is closed and the valve V4A is opened. Opening of valve V4A allows at least a portion of the gas exiting via check valve CV1B to flow through valve V4A and subsequently reverse through bed 10. The purge gas flows through the bed 10 at low pressure to remove residual impurities and is subsequently discharged from the system via valve V2A and valve 5. In another embodiment, the high purity product gas discharged from the check valve CV1B is not used as the purge gas, and a separate high purity purge gas source can be provided.

當床10完全再生時，如圖6所示，關閉閥門V4A及閥門5。隨後使床10維持於備用狀態及床20繼續以吸附模式操作，高純度氣體經由止回閥CV1B自系統排出。當床10經雜質飽和時，PSA系統之操作切換回床10，如將於下文參照圖7至12所論述。When the bed 10 is fully regenerated, as shown in Fig. 6, the valve V4A and the valve 5 are closed. The bed 10 is then maintained in a standby state and the bed 20 continues to operate in the adsorption mode, and high purity gas is discharged from the system via the check valve CV1B. When bed 10 is saturated with impurities, the operation of the PSA system is switched back to bed 10 as will be discussed below with reference to Figures 7-12.

如圖所示，圖6顯示純化操作之一階段，其中第二吸附床20係處於運作狀態，且第一吸附床10已再生且處於備用狀態。床20之操作壓力為約160 psig，而床10之壓力為低壓，例如，0 psig或真空。待純化之進料氣體係由進料氣體源30提供及經由閥門V1B進入床20。進料氣體中之雜質吸附於床20中且純化產物自床20排出並經由止回閥CV1B通向系統出口以立即使用或至視需要之存儲容器40。As shown, Figure 6 shows one stage of the purification operation in which the second adsorbent bed 20 is in operation and the first adsorbent bed 10 has been regenerated and in a standby state. The operating pressure of bed 20 is about 160 psig, while the pressure of bed 10 is low pressure, for example, 0 psig or vacuum. The feed gas system to be purified is supplied from feed gas source 30 and enters bed 20 via valve V1B. Impurities in the feed gas are adsorbed in the bed 20 and the purified product is withdrawn from the bed 20 and passed through the check valve CV1B to the system outlet for immediate use or to the desired storage vessel 40.

當床20中之吸附劑經雜質飽和時，則實施床20之再生。當床20再生時，床10係以吸附模式操作。自床20至床10之切換操作之第一步驟包含床20與床10間之壓力平衡。圖7顯示平衡製程開始時之操作階段。閥門V3B開啟且閥門V2A開啟或自先前階段時就維持開啟。止回閥CV1B亦可關閉，或一旦閥門V3B開啟時將自動阻止氣體自床20進一步排出。由於床20係處於較床10高之壓力下，故將藉由使床20與床10經由閥門V3B及閥門V2A連接而發生壓力平衡。氣體將自床20之底端出口流出並經由閥門V3B及閥門V2A流向床20之頂端入口。藉由使氣流自床20之出口流向床10之入口，亦可認識到本發明之優點。特定言之，由於氣流總是沿向下方向通過吸附床，故可避免床體升高。此容許使用較高氣體速度及平衡較快，而不存在床體升高及中斷之風險。且，避免雜質於床10之出口之累積，導致自床10排出之產物所受污染減少及可獲得五個9(99.999%)的純度級。When the adsorbent in bed 20 is saturated with impurities, regeneration of bed 20 is performed. When the bed 20 is regenerated, the bed 10 is operated in an adsorption mode. The first step of the switching operation from bed 20 to bed 10 comprises a pressure balance between bed 20 and bed 10. Figure 7 shows the operational phase at the beginning of the balancing process. Valve V3B is open and valve V2A is open or remains open from the previous stage. The check valve CV1B can also be closed, or will automatically prevent gas from being further discharged from the bed 20 once the valve V3B is opened. Since bed 20 is at a higher pressure than bed 10, pressure equalization will occur by connecting bed 20 to bed 10 via valve V3B and valve V2A. Gas will flow from the bottom end outlet of bed 20 and will flow to the top inlet of bed 20 via valve V3B and valve V2A. The advantages of the present invention are also recognized by flowing a gas stream from the outlet of the bed 20 to the inlet of the bed 10. In particular, since the airflow always passes through the adsorbent bed in the downward direction, the bed can be prevented from rising. This allows for higher gas velocities and faster balancing without the risk of bed rise and interruption. Moreover, accumulation of impurities at the outlet of the bed 10 is avoided, resulting in reduced contamination of the product discharged from the bed 10 and a purity level of five 9 (99.999%).

床20與床10達到平衡時，則使吸附製程自床20切換至床10。特定言之，如圖8所示，關閉閥門V1B以終止進料氣體流入床20及開啟閥門V1A以使進料氣體自進料氣體源30流入床10中。同時關閉閥門V2A以終止再生流流向床10及開啟閥門V2B以使再生流流向床20。When the bed 20 and the bed 10 are in equilibrium, the adsorption process is switched from the bed 20 to the bed 10. Specifically, as shown in FIG. 8, valve V1B is closed to terminate the flow of feed gas into bed 20 and to open valve V1A to cause feed gas to flow from feed gas source 30 into bed 10. At the same time, valve V2A is closed to terminate the regeneration flow to bed 10 and to open valve V2B to cause regeneration flow to bed 20.

將進料氣流自床20切換至床10之後，發生以下兩事件，使床20減壓及使床10升高至操作壓力。特定言之，如圖9所示，藉由使氣體經由閥門V2B及閥門V5自床20排出使床20減壓，並關閉閥門V3B。或者，可使床20經由閥門V3B及閥門V5排氣，同時關閉閥門V2B。以任一方式，使床20減壓至低標的壓力，例如，0 psig或真空。同時，使床10加壓至操作壓力。達到操作壓力，例如，160 psig時，純化產物氣體自床10排出並經由止回閥CV1A流向系統出口以立即使用或至視需要之存儲容器40。After switching the feed gas stream from bed 20 to bed 10, the following two events occur, depressurizing bed 20 and raising bed 10 to operating pressure. Specifically, as shown in Fig. 9, the bed 20 is decompressed by discharging the gas from the bed 20 via the valve V2B and the valve V5, and the valve V3B is closed. Alternatively, bed 20 can be vented via valve V3B and valve V5 while valve V2B is closed. In either manner, bed 20 is depressurized to a low pressure, for example, 0 psig or vacuum. At the same time, the bed 10 is pressurized to the operating pressure. Upon reaching the operating pressure, for example, at 160 psig, the purified product gas exits the bed 10 and flows through the check valve CV1A to the system outlet for immediate use or to the desired storage vessel 40.

當床10處於操作中時，床20係藉由床20之逆流清洗再生。特定言之，如圖10所示，關閉閥門V3B及開啟閥門V4B。閥門V4B之開啟容許經由止回閥CV1A排出之至少一部份氣體流經閥門V4B及隨後逆向流經床20。清洗氣體低壓下流經床20以移除餘下雜質及隨後經由閥門V2B及閥門5自系統排出。於另一方案中，不將自止回閥CV1A排出之高純度產物氣體用作清洗氣體，而提供單獨高純度清洗氣體源。When the bed 10 is in operation, the bed 20 is regenerated by countercurrent cleaning of the bed 20. Specifically, as shown in FIG. 10, the valve V3B is closed and the valve V4B is opened. Opening of valve V4B allows at least a portion of the gas exiting via check valve CV1A to flow through valve V4B and subsequently flow back through bed 20. The purge gas flows through the bed 20 at a low pressure to remove the remaining impurities and is subsequently discharged from the system via valve V2B and valve 5. In another aspect, the high purity product gas discharged from the check valve CV1A is not used as the purge gas, and a separate high purity purge gas source is provided.

床20完全再生時，則關閉閥門V4B及閥門5。隨後使床20維持於備用狀態及床10繼續以吸附模式操作，高純度氣體經由止回閥CV1A自系統排出，如圖6所示。此操作順序表示本發明之PSA系統之一完整偱環。床10經雜質飽和時，如上所述般將PSA系統之操作再切換回床20。When the bed 20 is fully regenerated, the valve V4B and the valve 5 are closed. The bed 20 is then maintained in the standby state and the bed 10 continues to operate in the adsorption mode, and the high purity gas is discharged from the system via the check valve CV1A, as shown in FIG. This sequence of operations represents a complete loop of one of the PSA systems of the present invention. When the bed 10 is saturated with impurities, the operation of the PSA system is switched back to the bed 20 as described above.

下表1中描述閥門位置及上述操作各階段之流動情況的概述。An overview of the valve position and the flow conditions at each stage of the above operation is described in Table 1 below.

如上所述，本發明提供優於先前技藝中已知之標準PSA製程之數個優點。藉由使用將各吸附床之出口連接至另一吸附床之入口之本發明裝置及方法，可獲得極高純度之產物氣體而無需使用二次純化製程。特定言之，本發明之裝置及方法可僅利用本發明之PSA製程獲得99.999%或更高純度。此外，於本發明中利用總是沿向下方向流經吸附床之氣體實施平衡來避免床體升高。此容許使用較高氣體速度及因此平衡較快，而不存在床體升高及中斷之風險。As described above, the present invention provides several advantages over the standard PSA process known in the prior art. By using the apparatus and method of the present invention that connects the outlet of each adsorbent bed to the inlet of another adsorbent bed, a very high purity product gas can be obtained without the need for a secondary purification process. In particular, the apparatus and method of the present invention can achieve a purity of 99.999% or higher using only the PSA process of the present invention. Further, in the present invention, the balance is maintained by using a gas which always flows in the downward direction through the adsorption bed to avoid bed rise. This allows for higher gas velocities and therefore faster balancing without the risk of bed rise and interruption.

本發明可藉由選擇適宜吸附劑物質來純化任何氣體。特定言之，本發明係用於製造極高純度氫氣及氦氣。The present invention can purify any gas by selecting a suitable adsorbent material. In particular, the invention is used to produce very high purity hydrogen and helium.

將瞭解本文所述之實施例僅係示例性且熟習此項技術者可於不脫離本發明精神及範圍下實施變化及修改。所有此等變化及修改將包含於如上所述之本發明範圍內。且，所揭示之所有實施例不必彼此替代，係因本發明之各實施例可組合以提供所需結果。It will be appreciated that the embodiments described herein are merely exemplary and that modifications and variations can be made without departing from the spirit and scope of the invention. All such changes and modifications are intended to be included within the scope of the invention as described above. Moreover, all of the disclosed embodiments are not necessarily substituted for each other, as various embodiments of the invention may be combined to provide the desired results.

10．．．第一吸附床10. . . First adsorption bed

20．．．第二吸附床20. . . Second adsorption bed

30．．．進料氣體源30. . . Feed gas source

40．．．存儲容器40. . . Storage container

CV1A．．．止回閥CV1A. . . Check valve

CV1B．．．止回閥CV1B. . . Check valve

V1A．．．閥門V1A. . . valve

V1B．．．閥門V1B. . . valve

V2A．．．閥門V2A. . . valve

V2B．．．閥門V2B. . . valve

V3A．．．閥門V3A. . . valve

V3B．．．閥門V3B. . . valve

V4A．．．閥門V4A. . . valve

V4B．．．閥門V4B. . . valve

V5．．．閥門V5. . . valve

圖1係顯示本發明之一階段操作之裝置之示意圖；Figure 1 is a schematic view showing the apparatus operated at one stage of the present invention;

圖2係顯示本發明之另一階段操作之裝置之示意圖；Figure 2 is a schematic view showing the apparatus for operating at another stage of the present invention;

圖3係顯示本發明之又一階段操作之裝置之示意圖；Figure 3 is a schematic view showing the apparatus for performing another stage of the present invention;

圖4係顯示本發明之又一階段操作之裝置之示意圖；Figure 4 is a schematic view showing the apparatus for performing another stage of the present invention;

圖5係顯示本發明之另一階段操作之裝置之示意圖；Figure 5 is a schematic view showing the apparatus for operating at another stage of the present invention;

圖6係顯示本發明之另一階段操作之裝置之示意圖；Figure 6 is a schematic view showing the apparatus for operating at another stage of the present invention;

圖7係顯示本發明之又一階段操作之裝置之示意圖；Figure 7 is a schematic view showing the apparatus for performing another stage of the present invention;

圖8係顯示本發明之又一階段操作之裝置之示意圖；Figure 8 is a schematic view showing the apparatus for performing another stage of the present invention;

圖9係顯示本發明之另一階段操作之裝置之示意圖；及Figure 9 is a schematic view showing the apparatus for operating at another stage of the present invention;

圖10係顯示本發明之另一階段操作之裝置之示意圖。Figure 10 is a schematic illustration of an apparatus for performing another stage of the present invention.

10．．．第一吸附床10. . . First adsorption bed

20．．．第二吸附床20. . . Second adsorption bed

30．．．進料氣體源30. . . Feed gas source

40．．．存儲容器40. . . Storage container

CV1A．．．止回閥CV1A. . . Check valve

CV1B．．．止回閥CV1B. . . Check valve

V1A．．．閥門V1A. . . valve

V1B．．．閥門V1B. . . valve

V2A．．．閥門V2A. . . valve

V2B．．．閥門V2B. . . valve

V3A．．．閥門V3A. . . valve

V3B．．．閥門V3B. . . valve

V4A．．．閥門V4A. . . valve

V4B．．．閥門V4B. . . valve

V5．．．閥門V5. . . valve

Claims (12)

一種變壓吸附系統，其包含：第一吸附床，其具有用於接收待純化氣體之入口及用於排出純化氣體之出口；及第二吸附床，其具有用於接收待純化氣體之入口及用於排出純化氣體之出口；其中該第一吸附床之出口係與該第二吸附床之入口連接。 A pressure swing adsorption system comprising: a first adsorption bed having an inlet for receiving a gas to be purified and an outlet for discharging a purified gas; and a second adsorption bed having an inlet for receiving a gas to be purified and An outlet for discharging the purified gas; wherein the outlet of the first adsorbent bed is connected to the inlet of the second adsorbent bed. 如請求項1之變壓吸附系統，其中該純化氣體係氦氣。 The pressure swing adsorption system of claim 1, wherein the purified gas system is helium. 如請求項1之變壓吸附系統，其中該純化氣體係氫氣。 The pressure swing adsorption system of claim 1, wherein the purified gas system is hydrogen. 如請求項1之變壓吸附系統，其中該純化氣體具有99.999%或更高之純度。 The pressure swing adsorption system of claim 1, wherein the purified gas has a purity of 99.999% or higher. 一種製造高純度氣體之方法，其包含：提供一變壓吸附系統，該變壓吸附系統包含第一吸附床，該第一吸附床具有用於接收待純化氣體之入口及用於排出高純度氣體之出口，及第二吸附床，該第二吸附床具有用於接收待純化氣體之入口及用於排出高純度氣體之出口，其中該第一吸附床之出口係與該第二吸附床之入口連接；將該待純化氣體提供至該變壓吸附系統；及自該變壓吸附系統收集該高純度氣體。 A method of producing a high purity gas, comprising: providing a pressure swing adsorption system comprising a first adsorption bed having an inlet for receiving a gas to be purified and for discharging a high purity gas An outlet, and a second adsorption bed, the second adsorption bed having an inlet for receiving a gas to be purified and an outlet for discharging a high purity gas, wherein an outlet of the first adsorption bed and an inlet of the second adsorption bed Connecting; supplying the gas to be purified to the pressure swing adsorption system; and collecting the high purity gas from the pressure swing adsorption system. 如請求項5之方法，其中該高純度氣體係氦氣。 The method of claim 5, wherein the high purity gas system is helium. 如請求項5之方法，其中該高純度氣體係氫氣。 The method of claim 5, wherein the high purity gas system is hydrogen. 如請求項5之方法，其中該高純度氣體具有99.999%或更 高之純度。 The method of claim 5, wherein the high purity gas has 99.999% or more High purity. 一種具有99.999%或更高純度之高純度氣體，其藉由如請求項1之變壓吸附系統製得。 A high purity gas having a purity of 99.999% or higher, which is produced by the pressure swing adsorption system of claim 1. 如請求項9之氣體，其中該氣體係氦氣。 The gas of claim 9, wherein the gas system is helium. 如請求項9之氣體，其中該氣體係氫氣。 The gas of claim 9, wherein the gas system is hydrogen. 一種操作變壓吸附系統之方法，該系統包含：第一吸附床容器，其具有入口及出口；第二吸附床容器，其具有入口及出口；待純化氣體源，其經由第一閥門與該第一容器之入口流體連通及亦經由第二閥門與該第二容器之入口流體連通；該第一容器之該出口經由第三閥門及第四閥門與該第二容器之入口流體連通；該第二容器之該出口經由第五閥門及第六閥門與該第一容器之入口流體連通；該第一容器之該出口經由第一止回閥與一單元操作或一儲藏罐流體連通；該第二容器之該出口經由第二止回閥與該單元操作或該儲藏罐流體連通；該第一容器之該出口經由該第一止回閥及第七閥門與該第二容器之該出口流體連通；該第二容器之該出口經由該第二止回閥及第八閥門與該第一容器之該出口流體連通；該第一容器之該入口經由該第六閥門及第九閥門與一 排放孔流體連通；該第二容器之該入口經由該第四閥門及該第九閥門與一排放孔流體連通；該方法包含根據以下順序操作該第一至該第九閥門及該第一及第二止回閥：在操作階段期間，當該第一容器處於純化操作中及該第二容器處於備用狀態時，開啟該第一閥門及該第一止回閥，關閉該第二閥門、該第三閥門、該第五閥門、該第六閥門、該第七閥門、該第八閥門、該第九閥門及該第二止回閥，及開啟或關閉該第四閥門；在操作階段期間，當平衡該第一容器與該第二容器間之壓力時，開啟該第一閥門、該第三閥門及該第四閥門，並關閉該第二閥門、該第五閥門、該第六閥門、該第七閥門、該第八閥門、該第九閥門、該第一止回閥及該第二止回閥；在操作階段期間，當氣體純化自該第一容器切換至該第二容器時，開啟該第二閥門及該第六閥門，並關閉該第一閥門、該第三閥門、該第四閥門、該第五閥門、該第七閥門、該第八閥門、該第九閥門、該第一止回閥及該第二止回閥；在操作階段期間，當使該第一容器減壓及使該第二容器加壓時，開啟該第二閥門、該第六閥門、該第九閥門及該第二止回閥，並關閉該第一閥門、該第三閥門、該第四閥門、該第五閥門、該第七閥門、該第八閥門及該 第一止回閥，或開啟該第二閥門、該第三閥門、該第九閥門及該第二止回閥，並關閉該第一閥門、該第四閥門、該第五閥門、該第六閥門、該第七閥門、該第八閥門及該第一止回閥；在操作階段期間，當清洗該第一容器及該第二容器處於純化操作中時，開啟該第二閥門、該第六閥門、該第八閥門、該第九閥門及該第二止回閥，並關閉該第一閥門、該第三閥門、該第四閥門、該第五閥門、該第七閥門及該第一止回閥；在操作階段期間，當該第二容器處於純化操作中及該第一容器處於備用狀態時，開啟該第二閥門及該第二止回閥，關閉該第一閥門、該第三閥門、該第四閥門、該第五閥門、該第七閥門、該第八閥門、該第九閥門及該第一止回閥，及開啟或關閉該第六閥門；在操作階段期間，當平衡該第二容器與該第一容器間之壓力時，開啟該第二閥門、該第五閥門及該第六閥門，並關閉該第一閥門、該第三閥門、該第四閥門、該第七閥門、該第八閥門、該第九閥門、該第一止回閥及該第二止回閥；在操作階段期間，當氣體純化自該第二容器切換至該第一容器時，開啟該第一閥門及該第四閥門，並關閉該第二閥門、該第三閥門、該第五閥門、該第六閥門、該第七閥門、該第八閥門、該第九閥門、該第一止回閥及該第二止回閥； 在操作階段期間，當使該第二容器減壓及使該第一容器加壓時，開啟該第一閥門、該第四閥門、該第九閥門及該第一止回閥，並關閉該第二閥門、該第三閥門、該第五閥門、該第六閥門、該第七閥門、該第八閥門及該第二止回閥，或開啟該第一閥門、該第五閥門、該第九閥門及該第一止回閥，並關閉該第二閥門、該第三閥門、該第四閥門、該第六閥門、該第七閥門、該第八閥門及該第二止回閥；在操作階段期間，當清洗該第二容器及該第一容器係處於純化操作中時，開啟該第一閥門、該第四閥門、該第七閥門、該第九閥門及該第一止回閥，並關閉該第二閥門、該第三閥門、該第五閥門、該第六閥門、該第八閥門及該第二止回閥；及以連續方式重複以上操作階段。A method of operating a pressure swing adsorption system, the system comprising: a first adsorbent bed vessel having an inlet and an outlet; a second adsorbent bed vessel having an inlet and an outlet; a source of gas to be purified, via the first valve and the first An inlet of a container is in fluid communication and is also in fluid communication with an inlet of the second container via a second valve; the outlet of the first container is in fluid communication with an inlet of the second container via a third valve and a fourth valve; the second The outlet of the container is in fluid communication with the inlet of the first container via a fifth valve and a sixth valve; the outlet of the first container is in fluid communication with a unit operation or a storage tank via a first check valve; the second container The outlet is in fluid communication with the unit operation or the storage tank via a second check valve; the outlet of the first container is in fluid communication with the outlet of the second container via the first check valve and the seventh valve; The outlet of the second container is in fluid communication with the outlet of the first container via the second check valve and the eighth valve; the inlet of the first container is connected to the ninth valve and the ninth valve The discharge port is in fluid communication; the inlet of the second container is in fluid communication with a discharge port via the fourth valve and the ninth valve; the method comprising operating the first to the ninth valve and the first and the first according to the following sequence a second check valve: during the operation phase, when the first container is in the purification operation and the second container is in the standby state, the first valve and the first check valve are opened, and the second valve is closed a third valve, the fifth valve, the sixth valve, the seventh valve, the eighth valve, the ninth valve and the second check valve, and opening or closing the fourth valve; during the operation phase, when When balancing the pressure between the first container and the second container, opening the first valve, the third valve and the fourth valve, and closing the second valve, the fifth valve, the sixth valve, the first a seven valve, the eighth valve, the ninth valve, the first check valve, and the second check valve; opening the gas when the gas is purified from the first container to the second container during an operation phase Second valve and the sixth valve are closed a first valve, the third valve, the fourth valve, the fifth valve, the seventh valve, the eighth valve, the ninth valve, the first check valve, and the second check valve; During the phase, when the first container is depressurized and the second container is pressurized, the second valve, the sixth valve, the ninth valve and the second check valve are opened, and the first valve is closed The third valve, the fourth valve, the fifth valve, the seventh valve, the eighth valve, and the a first check valve, or opening the second valve, the third valve, the ninth valve and the second check valve, and closing the first valve, the fourth valve, the fifth valve, the sixth a valve, the seventh valve, the eighth valve, and the first check valve; during the operating phase, when the first container is cleaned and the second container is in a purification operation, the second valve is opened, the sixth a valve, the eighth valve, the ninth valve and the second check valve, and closing the first valve, the third valve, the fourth valve, the fifth valve, the seventh valve, and the first stop Returning valve; during the operation phase, when the second container is in the purging operation and the first container is in the standby state, the second valve and the second check valve are opened, and the first valve and the third valve are closed The fourth valve, the fifth valve, the seventh valve, the eighth valve, the ninth valve and the first check valve, and opening or closing the sixth valve; during the operation phase, when balancing Opening the second valve when the pressure between the second container and the first container is a fifth valve and the sixth valve, and closing the first valve, the third valve, the fourth valve, the seventh valve, the eighth valve, the ninth valve, the first check valve, and the first a second check valve; during the operation phase, when the gas purification is switched from the second container to the first container, the first valve and the fourth valve are opened, and the second valve, the third valve, the a fifth valve, the sixth valve, the seventh valve, the eighth valve, the ninth valve, the first check valve, and the second check valve; During the operation phase, when the second container is depressurized and the first container is pressurized, the first valve, the fourth valve, the ninth valve, and the first check valve are opened, and the first valve is closed a second valve, the third valve, the fifth valve, the sixth valve, the seventh valve, the eighth valve and the second check valve, or the first valve, the fifth valve, the ninth a valve and the first check valve, and closing the second valve, the third valve, the fourth valve, the sixth valve, the seventh valve, the eighth valve, and the second check valve; During the phase, when the second container is cleaned and the first container is in a purification operation, the first valve, the fourth valve, the seventh valve, the ninth valve, and the first check valve are opened, and Closing the second valve, the third valve, the fifth valve, the sixth valve, the eighth valve, and the second check valve; and repeating the above operational stages in a continuous manner.
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