TW587151B - Process and apparatus for producing krypton and/or xenon by low-temperature fractionation of air - Google Patents

Process and apparatus for producing krypton and/or xenon by low-temperature fractionation of air Download PDF

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Publication number
TW587151B
TW587151B TW091124677A TW91124677A TW587151B TW 587151 B TW587151 B TW 587151B TW 091124677 A TW091124677 A TW 091124677A TW 91124677 A TW91124677 A TW 91124677A TW 587151 B TW587151 B TW 587151B
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Taiwan
Prior art keywords
krypton
xenon
column
condenser
evaporator
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TW091124677A
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English (en)
Inventor
Dirk Dr Schwenk
Original Assignee
Linde Ag
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Publication of TW587151B publication Critical patent/TW587151B/zh

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same column
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
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    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J3/04642—Recovering noble gases from air
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    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04703—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser being arranged in more than one vessel
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
    • F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
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    • F25J3/04745—Krypton and/or Xenon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10S62/00—Refrigeration
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Description

587151 玖、發明說萌 (發明說明應敘明：發明所屬之技術領域、先前技術、內容、實施方式及圖式簡單說明） (一） 發明所屬之技術領域 本發明係關於依照申請專利範圍第1項之序言之方法， 使用此方法經由低溫分餾空氣而產生氪及/或氙。 (二） 先前技術 就大體而論，低溫分餾空氣的基本原理及用於氮-氧分 離之精餾系統之構造將記述於HauSen/Linde(l 9 8 5年第五 版）專論 ’’TieftemperaturtechnikM (超低溫工程）及 Latimer 在化學工程發展（第63卷，1 9 6 7，第2號，p.35)中之論 ® 文。將高壓柱在較低壓柱較高之壓力下操作；兩柱宜相互 呈熱交換關係，舉例而言，經由主冷凝器，其中將來自高 壓柱之頂部氣體液化對照將來自低壓柱之底部液體蒸發。 可將本發明的精餾系統設計成爲習用之雙柱系統，但是亦 可設計成爲三柱或多柱系統。除去氮-氧分離之柱以外， 亦可能有用以製造其他空氣組份，尤其是稀有氣體之另外 裝置，舉例而言氬製造裝置。 # 經由低溫分餾空氣來產生氪及/或氙之方法及相對應之 裝置自德國專利1 〇 〇 〇 〇 〇 1 7 A 1得知。此方法中，將來自氮 -氧分離之雙柱的高壓柱之含氪和氙之餾份，特別是底部 液體，不須改變濃度之任何措施而通入使用以產生氪/氙 之另外柱中。 德國專利2 6 0 5 3 0 5 A中顯示：經由引言中所述之該型的 低溫分餾空氣來產生氪及/或氙之方法和裝置。此文獻中 587151 ，第一冷凝器-蒸發器經由冷凝來自粗氬柱之頂部氣體予 以加熱，而在同時，形成氪-氙增濃柱之底部加熱。氪-氙 增濃柱中上升之所有蒸氣係在第一冷凝器-蒸發器中產生 〇 (三）發明內容 本發明係基於更進一步改良產生氪和氙之目的，且尤其 ，以特別經濟方式進行此項生產。 此目的經由該項事實而達到，就是：將來自氪-氙增濃 柱的低部區域之液體引入第二冷凝器-蒸發器中（此第二冷 凝器-蒸發器與第一冷凝器·蒸發器分離）。 因此，本發明中，有一個分離之熱交換器，”第二冷凝 器-蒸發器”，其中與第一冷凝器-蒸發器無關，產生氪/氙 增濃柱之上昇蒸氣而以此方式，更進一步濃縮相對低揮發 性組份。宜將該第二冷凝器-蒸發器設計成爲底部加熱氪/ 氙增濃柱。可將它安排在此柱內部或在分開容器中。 該第二冷凝器-蒸發器導致較小高氧濃度建立在第一冷 凝器-蒸發器中，以致，因爲相對應地減小溫差，可減少 第一冷凝器-蒸發器的總尺寸。而且，在第一冷凝器-蒸發 器中有較少相對濃度的相對低揮發性組份，爲了操作上原 因，在此位置，此現象是所不欲的。本發明之上下文中， 視需要可選擇第二冷凝器-蒸發器之加熱設備。原則上， 可使用任何適當處理餾份，舉例而言，也許來自高壓柱之 氮，來自高壓柱之任何其他餾份，進料空氣之分流或來自 587151 粗氬柱（將其連接至低壓柱）之餾份，尤其，來自此型的粗 氬柱頂部之粗氬。 第一冷凝器-蒸發器的”沖洗液體’’充作氪-氙增濃柱之進 料餾份。本發明之上下文中，術語”氪-氙增濃柱”應了解 係指：逆流質量傳送柱其中產生一種餾份其具有較此柱的 每一種進料餾份，較高濃度之氪及/或氙。經由實例，該 氪-氙濃縮物具有較經餵供至氪-氙增濃柱中之”沖洗液體’’ ，較高莫耳含量的氪及/或氙。舉例而言，可設計此柱成 爲傳送柱，如德國專利1 0 0 0 0 17 A1中所述，及/或可同時 使用來驅出甲烷。 最好將沖洗液體引入較低區域中，舉例而言直接在底部 上方。在此情況中，爲了強制存在於上昇蒸氣中之氪向下 及強制甲烷向上，將液體加至氪-氙增濃柱之頂部。舉例 而言，可將此液體自高壓柱移出，例如自此柱之底部或高 於它之少數板。一個可能之另外或附加來源是純氬柱之頂 冷凝器的蒸發空間。在氪-氙增濃柱之底部中，可將向下 流動之液體藉底部蒸發器沸騰。此操作容許氪-氙濃縮物 的氪和氙含量進一步增加。可將底部蒸發器舉例而言使用 壓縮空氣或使用來自高壓柱頂部之壓縮之氮而操作。 本發明中，一個中間步驟（其形式是在第一冷凝器-蒸發 器中之部份蒸發）可在萃取來自高壓柱之含有氪/氙之餾份 與餵供此餾份入氪-氙增濃柱間進行。使用此步驟來濃縮 氪及/或氙，甚至在到達氪-氙增濃柱前。作爲一種另外效 -10- 587151 果，將具有較氧較低揮發性之所有其他組份，在部份蒸發 外，使用沖洗液體導引入氪-氙增濃柱中而以此方式，保 持遠離裝置的其他部份，尤其低壓柱。 氪-氙增濃柱中所產生之氪-氙濃縮物具有舉例而言，600 至5 0 0 0ppm之氪含量（宜係1 2 0 0至4 0 0 0ppm);及舉例而 言，60至500ppm之氣含量（宜係120至400ppm)。在其 他情況，其主要係由氧和典型高達大約1 〇莫耳％之氮所 組成。 可將本發明特別有利地實施作爲具有氬生產之空氣分餾 設備的一部份，其中將來自低壓柱之含氬之餾份引入粗氬 精餾階段中。特別使用該粗氬精餾階段用以氬/氧分離且 可在一或數個柱中進行（舉例而言，參閱：歐洲專利3 7 7 1 1 7 B 2及歐洲專利6 2 8 7 7 7 B 1 )。 在任何情況都需要之粗氬精餾階段的冷卻，在本發明之 上下文中係受含有氪和氙之餾份，來自將要與第一冷凝器 -蒸發器中蒸發之含有氪和氙之餾份間接熱交換之粗氬精 餾之富含氬之蒸汽所影響。因此，係爲氪/氙製造的一部 份之部份蒸發在粗氬精餾階段中同時充作產生回流及/或 液體產物。 在許多情況中，有液體進料-空氣流，舉例而言，在內 部壓縮一或數種產物時，時常將經液化之空氣分配在高壓 柱與低壓柱間，舉例而言，經由予以引入被布置在高壓柱 內部之一個容器中並將部份的該液體再自此容器中移出並 -1 1 - 587151 通至低壓柱。在本發明的上下文中，便利的是，如果將一 種含氧之液體自高壓柱中萃出並引入低壓柱中，此含氧之 液體源自第二中間點（將此第二中間點布置在第一中間點 上方，液體進料空氣係在此點引入高壓柱中）。此操作保 證：存在於液體進料空氣中之氪和氙流向高壓柱之底部而 不通入低壓柱中，在此情況下，可能損失氪-氙產量。而 且，將其他低揮發性雜質保持遠離主冷凝器。根據本發明 之此觀點，液化之空氣（或具有相似組成之含氧液體）係自 高壓柱的大體上不含氪和氙之回流液體所形成。 # 可將本發明之此觀點有利應用至任何方法，其中將來自 高壓柱之餾份餵供至氪-氙產生段。其使用不限爲連同部 份蒸發含氪和氙之餾份的方法和裝置。本發明之此觀點可 應用至相對應之另外構型。 最好沒有質傳元件，即：板或塡充物配置在第一中間點 與第二中間點間。其結果是，含氧之液體具有與空氣大體 上相同組成，除了在較氧較高溫度下沸騰之所不欲組份以 φ 外。 壓力柱中，可能有障壁板，將含有氪和氙之餾份在障壁 板下面萃出而富含氧之液體自障壁板上方被移出。因此， 富含氧之液體較含有氪和氙之餾份含有顯著較少之氪和氙 且舉例而言可將它直接通入低壓柱中及/或使用來冷卻純 氬柱的頂冷凝器，其結果，並無顯著數量之氪和氙損失。 障壁板的數目，舉例而言是1至9，宜係2至6 (理論之板 -12- 587151 數目）。 除去沖洗液體以外，可將氣體流自第一冷凝器·蒸發器 的氣化空間萃出且同樣餵供至氪-氙增濃柱，例如在與沖 洗液體相同地點。其結果是，亦將仍存在於含氪和氙之餾 份的蒸發部份中之氪餵供至氪-氙生產段。 本方法中，冷凍可經由空氣的功實施之膨脹而產生-舉 例而言-在中壓渦輪機中-至大槪高壓柱的操作壓力，其正 常包括空氣的部份液化。在本發明之上下文中，可將以功 實施之方式所膨脹之此空氣餵供至相分離，並可將至少部 份的來自相分離之液體餾份餵供至氪-氙增濃柱及/或第一 冷凝器-蒸發器的蒸發空間。 作爲另外者或另外，可將空氣以功實施方式膨脹至大槪 低壓柱壓力，例如在低壓渦輪機中。如果將此空氣流餵供 至汽提塔，則可回收存在於低壓空氣流中之氪和氙並將來 自該汽提塔之底部液體餵供至氪-氙增濃柱，宜在頂部或 在一個中間點（少數板在其下面）。而且，該汽提塔亦保留 其他低揮發性組份，例如N2o，在低壓柱中N20係所不欲 之組份。 與空氣的功實施之膨脹相關聯之本發明各方面優點不限 於具有部份蒸發含氪和氙之餾份之各種方法和裝置。毋寧 是，此等方法步驟亦可使用於製造氪/氙之其他方法中。 另外，本發明係關於依照申請專利範圍第9和1 0項， 經由低溫分餾空氣來製造氪及/或氙之裝置。 -13- 587151 (四）實施方式 已經冷卻至大槪露點之淸潔空氣以氣體形式經由第1圖 中之管路1流動入氮-氧分離之精餾系統的高壓柱2中， 此系統亦包括低壓柱3和主冷凝器4，本實例中將它設計 成爲降膜或蒸發器。將來自高壓柱的頂部之氣態氮5的第 一部份6飼供至主冷凝器4的冷凝空間。將在該空間中 所形成之冷凝器7的第一部份8添加至高壓柱作爲回流。 將第二部份9在過冷卻逆流熱交換器1 0中過冷並經由管 路1 1和節流閥1 2飼供至低壓柱3之頂部。此液體的一 部份92可獲得爲液氮產物（LIN)。 將來自高壓柱2之富含氧之底部液體1 3同樣在過冷卻 逆流熱交換器1 〇中冷卻。將過冷之富含氧之液體1 4以兩 個分流向上移動。將第一分流1 5 - 1 6作爲”含氪和氙之餾 份”引入’’第一冷凝器-蒸發器’’ 1 7的蒸發空間中，其代表粗 氬精餾級1 8 / 1 9的頂冷凝器。將第二分流1 5 - 2 0餵供入純 氬柱2 2的頂冷凝器2 1的蒸發空間中。 將第一冷凝器-蒸發器1 7設計成爲強制循環蒸發器，即 :蒸發空間含有液浴其中部份浸沒一個熱交換器組。（宜 將該熱交換器組-偏離該圖式-完全浸沒入液浴中）。將液 體經由蒸發通道的較低端上之熱虹吸效應而吸入。蒸氣和 未經蒸發之液體的混合物出現在其較高終端上，未經蒸發 之液體回流入液浴中。將含有氪和氙之餾份1 6在第一冷 凝器-蒸發器1 7中部份蒸發，經由實例，將經引入之〇 . 5 -14- 587151 至1 0莫耳％ (宜係1至5莫耳％)的液體1 6自第一冷凝器-蒸發器1 7的蒸發空間以液體形式萃取作爲沖洗液體2 6。 此部份蒸發增加液體中相對低揮發性組份之濃度，尤其氪 和氙及減少它在蒸氣中之濃度（在每一情況中，與含有氪 和氙之餾份1 6的組成比較）。將部份蒸發期間所產生之蒸 氣自第一冷凝器-蒸發器1 7的蒸發空間萃取成爲氣態流2 5 。殘餘液體自液浴中排出成爲”沖洗液體’’ 2 6並餵供至宜 接在底部上方之氪-氙增濃柱24。 該氪-氙增濃柱24具有底部蒸發器（”第二冷凝器-蒸發器”） 2 7，可將它使用任何適當餾份加熱。在例示之具體實施例 中，使用來自高壓柱2頂部之加壓氮2 8作爲加熱之工具 。（或者，可使用來自高壓柱之任何其他餾份、進料空氣 的分流，或來自第二粗氬柱1 9頂端之一部份的粗氬5 0 ) 。將在底部蒸發器27中已予以液化之氮29與來自主冷凝 器4之液體7混合。將來自純氬柱2 2的頂冷凝器2 1之蒸 發器中沖洗液體的分流2 3加至氪-氙增濃柱2 4之頂部作 爲回流液體。自底部蒸發器2 7上昇之蒸氣開始與氪·氙增 濃柱中含有較少氪和氙之液體2 3實施逆流質量傳送。其 結果是，將此等組份洗入底部中，而大部份的甲烷連同頂 氣3 0被驅出。本例示之具體實施例中，將後者在適當中 間點餵供至低壓柱3。將液體形式之氪-氙濃縮物 3 0 ( L Ο X / K r / X e )自氪-氙增濃柱2 4之底部移出，此濃縮物 ，舉例而言，具有大槪2 4 0 0 ppm之氪含量和大槪2 0 0 ppm 587151 之氙含量；在其他情況，濃縮物3 0主要係由氧並亦含有 大槪1 〇莫耳％之氮所組成。可將濃縮物3 0儲存在液體槽 中或直接餵供以便更進一步處理用以製造純氪及/或氙。 除去液氮9 2以外，將純氣態氮3 2 (在頂部）、不純之氮 3 3(同樣係氣體形式）及氧3 4(液體形式）至少自低壓柱3中 部份地萃出作爲產物。將氣態產物3 2，3 3在過冷逆流熱 交換器10中加熱，然後在主熱交換器（圖中未示）中更進 一步加熱。將液氧3 4分成總共3份。將第一份和第二份 一起經由管路3 5和泵3 6起始輸送。第一份3 7流至主冷 凝器4之蒸發空間，於此情況將它部份蒸發。所形成之蒸 氣-液體混合物3 8回流至低壓柱3之底部。將第二份經由 管路39和40萃取成爲液體產物（LOX)，如適當，在過冷 之逆流熱交換器1 〇中過冷後。 使來自低壓柱3底部之液氧3 4的第三份4 1歷經內部壓 縮係經由致使至泵4 2中之所需要的產物壓力下並經由管 路43(LOX-IC)餵供至一或數個熱交換器，在其中將它蒸 發（或在超臨界產物壓力之情況中-假蒸發）並加熱至大槪 周圍溫度。蒸發和加熱，舉例而言，可以與高壓空氣流間 接熱交換方式進行。使液化之（或超臨界）高壓空氣膨脹（ 圖中未示）並以液化之空氣44餵供至高壓柱2(在”第一中 間點”）。將含氧之液體4 5 (其數量至少相當於一部份的液 化空氣4 4 )自高壓柱（在”第二中間點"）萃出（將第二中間點 直接排列在此第一中間點上方）；液流4 5亦可能大於空氣 -16- 587151 流4 4。第一中間點與第二中間點間沒有板或其他質量傳 送元件。含氧之液體45(其組成大體上相當於空氣），在過 冷之逆流熱交換器1 〇中過冷後，經由管路4 6和節流閥4 7 餵供入低壓柱3中。 將來自低壓柱3之含氬餾份經由氬傳送管路4 8通入粗 氬精餾級中，本實例中，其以兩個串聯之粗氬柱1 8與1 9 進行。將含氬之餾份以氣體形式餵供至直接在底部上方之 第一粗氬柱18。上昇蒸氣中之氬含量增加。來自第一粗 氬柱1 8之頂氣體經由管路4 9向上流動至第二粗氬柱1 9之 底部。 將富含氬之蒸氣（粗氬）5 0在第二粗氬柱1 9的頂部產生並 大半在第一冷凝器-蒸發器17中冷凝。將所產生之液體51 加至第二粗氬柱1 9作爲回流流體。將液體5 2 (其係在第 二粗氬柱1 9底部中所產生）藉泵5 3，經由管路5 4輸送至 第一粗氬柱1 8之頂部。來自第一粗氬柱1 8之底部液體5 5 經由另外泵5 6和管路5 7流回入低壓柱3中。 將來自第一冷凝器-蒸發器17的液化空間之粗氬58(其 以氣體形式留下）在純氬柱中更進一步分解，連同移除特 別相對高揮發性組份，例如氮。純氬產物（LA R)經由管路 5 9和6 0以液體形式萃取出。另外部份6 1的底部液體在 具有連接之分離器62之純氬蒸發器63中蒸發並作爲上昇 之蒸氣，經由管路6 4回送至純氬柱2 2。純氬蒸發器6 3 經由與來自高壓柱2之至少一部份的底液體1 5間接熱交 -17- 587151 換予以加熱，將其在熱交換中過冷。如已敘述，純氬柱的 頂冷凝器2 1係使用一部份2 0的此種過冷液體予以冷卻。 將蒸氣6 6和殘餘液體2 3，6 5自頂冷凝器2 1的蒸發空間 萃取出並在適當之中間點饌供入低壓柱3中及/或（23)添 加至氪-氙增濃柱6 4。純氬柱2 2的頂氣6 7在液化空間中 部份冷凝。將該方法中所產生之回流液體6 8加至純氬柱 。將殘留蒸氣6 9排入大氣中。 在第1圖中所示之例示具體實施例中，高壓柱2中所產 生之所有富含氧之液體自底部（管路13)萃出。此方式容許 Φ 高壓柱2具有相當不複雜構造。第2圖顯示此方法之變型 ，其中更進一步改良了氪和·氣之產量。此情況中，自高壓 柱2更進一步中間取出液體2 7 0，其係經由大約四個障壁 板2 7 1與底部取出2 1 3分隔。此等板保留大多數的低揮發 性組份，尤其是氪和氙在高壓柱2之底部。其結果是，流 2 7 0具有較低液體2 1 3顯著較低氪與氙含量。將一部份2 2 0 的此流經由過冷逆流熱交換器1 〇通入純氬柱2 2之頂冷凝 φ 器2 1的蒸發空間中。其餘者2 2 3則流動至氪-氙增濃柱2 4 之頂部。此操作導致餾份2 6 5，2 6 6 (其流出頂冷凝器2 1 至低壓柱3 )兩者中及回流液體2 2 3中特別低氪和氙含量 。兩者導致氪和氙製造時特別高產量。 存在於空氣中之大比例（典型大約9 0莫耳％)的氪和氙連 同底部液體2 1 3流動經過過冷逆流熱交換器1 0和管路2 1 5 ，純氬蒸發器63，管路216及第一冷凝器-蒸發器17並 -18- 587151 向上經過管路2 2 5和2 2 6至氪-氙增濃柱2 4，於該處，其 連同氪-氙濃縮物3 0幾乎完全回收。 若須要，可將一部份的來自中間取出之液體2 7 0經由旁 通管路2 7 2與底部液體2 1 3摻合。經由實例，有2至1 4 ，宜大約5至8個理論上板在此中間取出處與第一中間點 (在此處引入來自內部壓縮之液體44)間。 雖然冷凍的產生在第1與2圖中未予舉例說明，但是第 3圖中所示之系統與第1圖中所略述者不同因爲：冷凍係 藉中壓渦輪機而獲得。該渦輪機本身並未顯示，但是毋寧 僅舉例說明部份流3 7 3 (其係來自其出口且係呈兩相混合 物形式）。將它引入分離器（相分離器）3 7 4中。如慣例，將 來自分離器374之蒸氣375連同直接空氣1餵供入高壓柱 2中。成對比，將液體3 7 6 (其具有增加含量的氪和氙）連 同一部份的來自高壓柱2之過冷底部液體1 4經由管路4 1 6 引入第一冷凝器-蒸發器17之蒸發空間中。將另外部份323 之過冷底部液體1 4加至氪-氙增濃柱2 4之頂上。當然， 亦可將第3圖中之附加特徵與第2圖中所示之變體聯合。 第4圖中，加工冷凍係藉低壓渦輪機而產生。來自此渦 輪機出口之空氣4 7 7是在大槪低壓柱3的操作壓力下，但 在此實例中，並未直接通入此柱中而毋寧是將其引入汽提 塔4 7 8中，其中，將相對低揮發性餾份洗出至底部中。然 後將底部液體4 7 9餵供至氪·氙增濃柱2 4上之適當中間點 。它形成氪-氙增濃柱2 4之部份的回流液體。僅來自汽提 -19- 587151 塔4 7 8之低氪和低氙頂氣4 8 0直接流入低壓柱3中，以此 方式旁通氪/氙製造。每一情況中，將來自高壓柱之過冷 底部液體1 4的分流4 2 3，4 9 2加至氪-氙增濃柱2 4之頂部 和汽提塔4 7 8頂部。 第5圖中，爲了簡單化，將高壓柱2、低壓柱3和主冷 凝器4舉例說明成爲雙柱。此情況中，冷凍係由來自障壁 板2 7 1上方之一個中間點之氣態中間餾份5 8 1的功實施之 膨脹而產生。此餾份可在主熱交換器5 8 2中加熱對照可將 欲予冷卻之進料空氣5 8 3經由管路5 8 4餵供至再壓縮機 585然後向上通至（586)主熱交換器582之溫端。將它在中 間溫度下經由管路5 8 7自主熱交換器5 8 2移出並餵供至功 實施之膨脹5 8 8。渦輪機5 8 8宜經由直接機械耦合來驅動 再壓縮機5 8 5。將已歷經功實施之膨脹的流最後適當管路 (5 8 9 )引入低壓柱3中。或者，如果經由虛線所舉例說明 之經由管路5 9 0之液流僅被加熱至主熱交換器5 8 2中渦輪 機5 8 8之入口溫度，然後直接餵供至此渦輪機（管路5 8 7 ) ，則可免除再壓縮和全部加熱。 氬製造及氪/氙製造未舉例說明於第5圖中彼等係以與 第1或2圖中之相同方式而進行。第5圖中，並無內部壓 縮。 (五）圖式簡單說明 本發明及本發明之另外細節參照例示之具體實施例（其 在各圖式中圖示式描述）予以更詳細解釋，圖式中： 587151 第1圖是本發明之第一例示之具體實施例， 第2圖是高壓柱中具有障壁板之變更， 第3圖是具有中壓渦輪機之另外例示之具體實施例， 第4圖顯示：具有低壓渦輪機之第四例示具體實施例， 及 第5圖顯示：具有渦輪機在高壓柱與低壓柱間之另外變 形。 主要部分之代表符號說明 1，11，13,35,39,40,43,46,49,管路 54,5 7,59,60,64,225,226,416， 5 8 4,5 8 6,5 8 7,5 8 9,5 9 0
2 3 4 5 高壓柱 低壓柱 主冷凝器 氣態氮 第一部份
冷凝液 9 10 12,47 13 14 第二部份 熱交換器 節流閥 富含氧之底部液體 過冷之富含氧之液體 15,16 第一（部）分流 -21- 587151 15-20 16 17 18,19 2 1 22 23，65 24 25,225 2 6,2 2 6 27 29 3 0,67 3 2 3 3 第二（部）分流 含氪-氙之餾份 第一冷凝器-蒸發器 粗氬精餾級 頂冷凝器 純柱 殘餘液體 氪-氙增濃柱 氣態流 β 沖洗液體 第二冷凝器-蒸發器 底部蒸發器 氮 頂氣 氣-氣濃縮物 純氣態氮 φ 不純氮 3 4 (液）氧 3 6,4 2,5 3,5 6 3 7 3 8 4 1 泵 第一份 蒸氣/液體混合物 第三份 44 液化之空氣 -22- 587151 45,270 48 5 0 5 1，5 2,2 7 0,3 7 6 5 5 5 8 62 63 66 92 213,416 223 2 5 6,2 6 6 270 27 1 272 373,423,492 3 74 477 47 8 4 8 0 5 8 2 5 8 3 含氧之液體 氬傳送管路 富含氬之蒸氣 液體 底部液體 粗氬 連接之分離器 純氬蒸發器 蒸汽 β 液氮 含氪和氙之餾份 回流液體 餾份 (液）流 障壁板 旁通管路 φ 部份流 相分離器 空氣 汽提塔 低氪與低氙頂氣 主熱交換器 進料空氣 -23- 587151 5 8 5 再壓縮機 5 8 8 渦輪機
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Claims (1)

  1. 587151 拾、申請專利範圍 第91124677號「藉由低溫分餾空氣來產生氪及/或氙的方 法及設備」專利案 (9 2年9月修正） 1. 一種藉由低溫分餾空氣來產生氪及/或氙之方法，其中 •將經壓縮且淸潔之進料空氣（1 )引入氮-氧分離之精餾
    系統中，其至少包括一個高壓柱（2)和一個低壓柱（3)， •將含有氪和氙之餾份（1 3、1 4、1 5、1 6、4 1 6)自高壓 柱（2 )中移出， •將含有氪和氙之餾份（1 3、1 4、1 5、1 6、4 1 6 )引入第 一冷凝器-蒸發器（1 7 )的蒸發空間中，於該處將它部 份蒸發， •將沖洗液體（2 6，2 2 6 )自第一冷凝器-蒸發器（1 7 )之蒸發 空間萃取出，及將其餵供至氪-氙增濃柱（24)，及 •將氪-氙濃縮物（30)自氪-氙增濃柱（24)中移出，
    其特徵爲： •將來自氪-氙增濃柱（24)之較低區域之液體引入第二冷 凝器-蒸發器（27)中，其與第一冷凝器-蒸發器（17)分開。 2. 如申請專利範圍第1項之方法，其中將來自低壓柱（3) 之含氬之餾份（48)引入粗氬精餾級（18、19)中，使來自 粗氬精餾級（1 8、1 9 )之富含氬之蒸氣（5 0 )與第一冷凝器-蒸發器（1 7 )中蒸發之含氪和氙餾份（1 6)間接熱交換。 3. 如申請專利範圍第1項之方法，其中將進料空氣的分流 -25- 587151 (4 4 )以液態在第一中間點餵供入高壓柱（2 )中，及將含氧 之液體（45)自高壓柱（2)在第二中間點萃出，而此第二中 間點經安排在此第一中間點上方並引入低壓柱（3 )中。 4. 如申請專利範圍第2項之方法，其中將進料空氣的分流 (4 4)以液態在第一中間點餵供入高壓柱（2)中，及將含氧 之液體（4 5 )自高壓柱（2 )在第二中間點萃出，而此第二中 間點經安排在此第一中間點上方並引入低壓柱（3 )中。 5. 如申請專利範圍第3項之方法，其中無質量傳送元件在 第一中間點與第二中間點間。 6. 如申請專利範圍第4項之方法，其中無質量傳送元件在 第一中間點與第二中間點間。 7. 如申請專利範圍第1至6項中任一項之方法，其中有障 壁板（2 7 1)配置在高壓柱（2)中，將含有氪和氙之餾份（213) 在障壁板（2 71)下面萃取，而富含氧之液體（2 7 0)則在障 壁板上方移出。 8. 如申請專利範圍第1至6項中任一項之方法，其中將氣 態流（2 5，2 2 5 )自第一冷凝器-蒸發器（1 7 )的蒸發空間萃出 ，並同樣餵供至氪-氙增濃柱（2 4 )。 9. 如申請專利範圍第1至6項中任一項之方法，其中將進 料空氣的分流（3 7 3 )以功實施方式膨脹至大槪高壓柱（2) 之操作壓力，然後餵供至相分離器（ 3 7 4 )，以及其中將 來自相分離器（3 7 4 )之至少部份的液體餾份（3 7 6 )餵供至 氪-氙增濃柱（2 4 )或第一冷凝器-蒸發器（1 7 )的蒸發空間 -26- 587151 1〇·如申請專利範圍第1至6項中任-項之方法，其中將進 料空氣的分流（4?7)以功實施方式膨脹至大槪低壓力柱 之操作壓力並鐵供至汽提塔（4 7 8 )，將來自汽提塔（4 7 8 ) 之底部液體（4 7 9 )餵供至氪_氙增濃柱（2 4 )。 U.〜種藉由低溫分餾空氣來產生氪及/或氙之設備，其具 有 •進料空氣管路（1)用以引入經懕縮和預先淸潔之進料空 氣至氮-氧分離之精餾系統中’此系統至少包括高壓 柱（2 )及低壓柱（3 ) ’ •具有移出管路（13、14、15、16、416)以便自高壓柱（2) 移出含有氪和氙之餾份， •將含有氪和氙之餾份之移出管路（13、14、15、I6、 4 1 6)連接至第一冷凝器-蒸發器（1 7)之蒸發空間’ •將沖洗管路（26、226)連接至冷凝器·蒸發器（17)之蒸 發空間及至氪-氙增濃柱（2 4 )上’及 •該氪-氙增濃柱（24)具有氪··氙濃縮物之生產管路（30)， 其特徵爲： •與第一冷凝器-蒸發器（17)分離之第二冷凝器-蒸發器 (2 7 )及其蒸發空間與氪-氙增濃柱（2 4 )的較低區域呈流 體連通。 12*如申請專利範圍第1 1項之設備，其中將低壓柱（3 )經 由氬轉移管路（4 8 )連接至粗氬精餾級（1 8、1 9 )’而第 -27- 587151 一冷凝器-蒸發器（1 7)的液化空間與粗氬精餾級（1 8、 1 9 )呈流體連通。
    -28-
TW091124677A 2001-10-31 2002-10-24 Process and apparatus for producing krypton and/or xenon by low-temperature fractionation of air TW587151B (en)

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