TWI763175B - 自液氧回收氪與氙的方法 - Google Patents

自液氧回收氪與氙的方法 Download PDF

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TWI763175B
TWI763175B TW109144016A TW109144016A TWI763175B TW I763175 B TWI763175 B TW I763175B TW 109144016 A TW109144016 A TW 109144016A TW 109144016 A TW109144016 A TW 109144016A TW I763175 B TWI763175 B TW I763175B
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liquid oxygen
xenon
liquid
krypton
pressure
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TW202124264A (zh
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學昆 羅
艾倫Ｄ 伯格
唐麥克 赫朗
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美商氣體產品及化學品股份公司
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Abstract

於一製程中自一含有氧與氙與/或氪之一液氧流分離氙與/或氪，該製程包含：將該液氧流之至少一部分做為一迴流液提供至一稀有氣體回收塔之頂部，該塔之作業壓力係介於5至25巴絕對壓力之間，於該稀有氣體回收塔之一再沸區中蒸發一再沸器液體，以產生一上升蒸氣與富含氙與/或氪之液流的混合物；以及於該塔之至少一蒸餾區中使該上升蒸氣與迴流液接觸，以使氙以及/或氪自上升蒸氣中經提取至迴流液中。該製程提供高於90%之一氙回收率以及介於15%至90%之一氪回收率。

Description

自液氧回收氪與氙的方法
本發明係整體上關於空氣分離領域，更詳而言之，係關於自液氧中粗回收稀有氣體，其係選自氪與氙所組成群組中之至少一者。
自液氧流中回收氪與氙之傳統方法係廣為人知。此等傳統方法及裝置中係存在問題，例如：較低之氪與/或氙之回收量、較高耗能、操作壓力受到限制或約束，並且難以將回收製程整合至主要之空氣分離設備中。其方法及裝置有改善之需求。
氪與氙係以極低濃度存在空氣中，一般約分別為1.14百萬分率(ppm)與約0.087ppm。其兩者皆為珍貴之氣體，因此，盡可能將其等自空氣分離程序中之回收量提升確有其經濟誘因。此外，氙又較氪具有顯著較高之價值，因此具有高氙回收率並可調控氪回收率之作業製程係有其效益。
於一般用於回收氧之低溫空氣蒸餾製程中，氪與氙會集中於自低壓(LP)蒸餾塔底部所取得之液氧(LOX)之中，因為其等之揮發性遠低於氧。因此，液氧的流動性愈低，則產物中之氪與氙濃度愈高。
在大部分氧產物以氣態自低壓塔中取出的低溫空氣蒸餾製程中，係可能透過減少低壓塔底部上方的一個或數個蒸餾階段來確保氣態氧(GOX)中只流失極少量的氪與氙。此等底部保護階段主要係用以預防實質上較氙更容易揮發的氪大量流失。當產物氧以蒸氣形態自低壓塔抽出時，幾乎所有進入空氣分離設備的氪與氙都能自液氧產物中回收，其只占整體氧流的極小部分。此液氧產物係可隨後經加工以製成純化之稀有氣體產物。若主要係欲取得氙產物，則可省去大部分或所有底部保護階段，且仍可自液氧產物中回收少部分之氪以及幾乎所有進入設備中之氙。
現今大多數用於氧氣回收之低溫空氣蒸餾法不再將主要氧產物以蒸氣形態抽出。而是將所有回收之氧以液氧形態自低壓塔底部抽出，抽取至所需之壓力並於主要熱交換器中蒸發。於此情況下將流失所有的氪與氙。即使將液氧產物自低壓塔底部上方之數個階段取出，並自底部抽出少量含有氪與氙之洗清液，回收率仍受到嚴重限制。關於抽取液氧製程之概述係可見於AOAC國際期刊78：1010-1018。空氣液化：蒸餾。R.Agrawal及D.M.Herron。
有限的回收率係可解釋如下。基本上所有進入空氣分離裝置的氪與氙都會以液體形態流向低壓塔之底部。自底部上方位置抽出之任何液體都 將含有與以液氧產物形態抽出之總液體量成比例的氪與氙。此通常會導致這些珍貴產物損失約30%。
因此，期望可增加自空氣分離裝置中回收之氪與氙，其中至少部分氧產物係以液氧形態自塔中抽出。
當現有設備以液體形態抽取主要的氧產物時，例如經抽取之液氧循環設備，通常不會有包含濃縮稀有氣體成分之小液流。因此，由於氪與氙極為珍貴，因此亦期望可使現有設備加裝稀有氣體回收系統。
此外，期望提供一種氙與/或氪之回收設備，其可加工來自外部來源之富含稀有氣體之注入流，例如來自儲存槽之液氧。
美國專利號3,779,028揭露一種自空氣分離塔中回收氪與氙之方法。
EP-0218740-B1揭露一種用於自空氣分離設備回收三種產物流之方法。氣態氧與液氧產物缺乏稀有氣體，且第三種產品係維富含氪與氙之稀有氣體濃縮液，其係透過將取自低壓塔集液槽或儲藏罐之液氧加工製成。
美國專利號6,301,929揭露一種空氣分離製程，其中係可形成稀有氣體貧乏之液氧流以及富有稀有氣體之液氧流。
DE-A-19855485揭露一種空氣分離製程，其中係可於低壓塔中形成稀有氣體貧乏之液氧以及富有稀有氣體之液氧。
美國專利號6,694,775揭露透過至少部分蒸發至少一部分加壓液氧並將所得蒸氣送至一稀有氣體回收系統，以自加壓液氧回收含有稀有氣體的液體流之方法。
提供一種可將氧加工並產生相對高濃度之氪與氙流之分離方法及裝置仍係必要目標。可促成氙之高回收率以及可調控之氪回收率的該方法及裝置，係具有高熱力學效率以及不受其他製程約束之作業壓力。本發明另一目的係提供一種分離方法及裝置，其等係可輕易整合至主要的空氣分離設備中，或可做為獨立或改裝的部件。如下所詳細地闡述之內容，發明人已發現經揭露與主張之製程係可實現此等所有目標。
於一實施例中，提供一種自包含氧與氙以及/或氪之液氧流中回收氙與/或氪之方法，該方法包括：提供一種稀有氣體回收系統，其包含一稀有氣體回收塔，該稀有氣體回收塔具有一頂部、一底部、至少一蒸餾區，以及具有一再沸器之一再沸區；提供至少含有氧與氙以及/或氪之液氧進料；提供至少一部分液氧進料至該稀有氣體回收塔之頂部以形成迴流液； 於再沸區中蒸發一再沸器液體以產生一上升蒸氣與富含氙以及/或氪之液體流的混合物；於至少一蒸餾區中使該上升蒸氣與迴流液接觸，以使氙以及/或氪自上升蒸氣中經提取至迴流液中，以產生該再沸器液體；自該稀有氣體回收塔之頂部移出該上升蒸氣，形成氙以及/或氪匱乏之氣態氧流；自該稀有氣體回收塔之底部移出富有氙以及/或氪之液流；使氙以及/或氪貧乏之氣態氧蒸氣通過可形成一冷壓縮氧流之冷壓縮器；使冷壓縮氧流通過該再沸器，該再沸器係可藉由與該再沸區中之再沸器液體間接熱交換而產生冷凝液氧；以及將等同於氙以及/或氪貧乏液氧之冷凝液氧自該稀有氣體回收系統移出。
發明人已了解可在沒有顯著功率負擔之情況下自液氧進料中獲得氙的高回收率以及可變的氪回收率。氙的高回收率定義為大於90%，較佳者係大於95%。可變的氪回收率定義為15%至90%，可根據製程運行之條件進行調整。
發明人並了解，不需在低壓塔壓力或氧產物壓力下操作，該稀有氣體塔之操作壓力係可經調控以滿足特定性能目標，並且仍具有經濟與能源效益。
本發明提供此種氙與/或氪之回收方法。於本文所提供之發明描述中，本發明之此等及其他優點將顯而易見。
100:稀有氣體回收系統
115:流
121:控制閥
118:第一部分
124:迴流液
127:塔
130:第二部分
133:控制閥
136:流
139:流
142:冷壓縮器
145:流(冷壓縮氧流)
148:再沸器
151:流
154:冷凝液氧
191:頂部
192:蒸餾區
193:再沸區
200:流
203:泵
209:流
212:去過冷器
257:流(過冷的氙與/或氪貧乏液氧流)
260:閥
263:流
266:相分離器
269:流(驟沸蒸氣流)
272:流(低壓迴流液流)
300:流
303:閥
375:泵
378:迴流液
〔圖1〕係本發明製程實施例示意圖。
〔圖2〕係本發明另一實施例示意圖，其中該液氧進料源係衍生自一低壓液氧源。
〔圖3〕係本發明另一實施例示意圖，其中該液氧進料源係衍生自一高壓液氧源。
本發明製程將參照圖式進行詳細說明。
參照圖1，提供一種稀有氣體回收系統100，並提供一液氧進料流115。流115於較稀有氣體回收塔127更高之任何壓力之下係可為一過冷或飽和液體。流115係可分離為一第一部分118與一第二部分130。至少該第一部分 118係通過控制閥121並做為迴流液124經引入塔127之頂部191。可選地，第二部分130係通過控制閥133並做為進料流136經引入塔127，成為第二進料。進料流136係可於頂部191與靠近塔底部之再沸區193之間任何位置經引入塔127，但較佳位置係接近塔之底部。
在稀有氣體回收塔127中，液體通過蒸餾區192下降至再沸區193中。再沸區193包含再沸器148，其係為一間接熱交換器，可將進入再沸區193之液體轉化為上升蒸氣與富含氙以及/或氪之液流151。進入再沸區193之液體系實質上受到氣化，藉此將氪與氙等揮發性較小之成分濃縮。一般而言，至少99%之液體被蒸發。上升蒸氣會流入蒸餾區192。
在蒸餾區192內，上升蒸氣會接觸下降之液體。上升蒸氣中所含之氪與/或氙係實質上受下降液體捕捉。上升蒸氣隨後以流139通過頂部離開塔127。
蒸氣流139，通常占塔流量的99%以上，被抽入冷壓縮機142中並以較高之壓力以流145排出。流145被抽入再沸器148中，並於其中冷凝以形成冷凝液氧154。經過該使冷壓縮機142之壓力增加是需要的，以增加冷壓縮氧流145之冷凝溫度。需要更高的冷凝溫度，使熱量得以自冷凝側傳遞至沸騰側。為冷凝作用所排除之熱量可透過再沸器148提供輸入至再沸區193之熱量。
操作冷壓縮機142的功率取決於需要提升壓力的大小。因此，需要導入以將壓力之上升減至最小。由於沸騰流體與冷凝流體實際上係為相同的整體組成，所以若再沸器溫度差趨近於零，並且使進出冷壓縮機142管道中之 壓降減至最小，理論上只需要花費少量的工作。另一方面，若循環流量高，而且管道壓降大，則操作該製成的功率可能極大。
因此，加入冷壓縮機是該製程作業的關鍵特徵。於傳統低溫製程中並不期望使用冷壓縮，因為壓縮的熱量必須被冷卻排除，對製程造成冷卻負擔並降低功率效率。然而，令人驚訝地，相對於熱壓縮，於此製程中使用冷壓縮可提高功率效率。此係透過消除與下列因素相關之寄生壓降功率損失所達成：1)於熱交換器及相關聯管道中將來自冷作業之流體加熱至周圍溫度；2)冷卻壓縮氣體以消除熱交換器與相關聯管道中之壓縮熱量；以及3)於熱交換器與相關聯管道中將流體從自環境溫度冷卻至冷作業溫度。
原則上，稀有氣體回收塔之操作壓力幾乎並無限制。唯一例外者係為塔壓力需低於氧之臨界壓力(約50巴絕對壓力(bara))。
基於至少三個原因，於高壓下作業係符合期望：1)由於氣體密度高故壓降較低；2)由於壓力高故壓降本身之重要性降低，因此相對壓降較低；以及3)微量成分之固溶度增加，因此可減少富含氙與/或氪之液流151(亦稱為洗清液)的流動，藉此增加所需之氪與氙的濃度。前兩項效益可降低功率，第三項效益可降低洗清液之下游淨化成本。
另一方面，基於至少兩個原因，於低壓下操作係符合期望：1)由於分離作業更有效，使氪與氙進入離開塔127之蒸氣(流139)所導致的損失降至最小；以及2)由於設計壓力較低，可降低設備成本。
藉由減少迴流液124相對於液體進料流136(下部液體進料)之流量，可減少在任何塔壓力下的氪與氙回收損失。增加迴流液124流量之潛在缺點在於，例如甲烷等輕質烴將被阻止排入流139中，因此於富含氙與/或氪之液流151中積聚至較高濃度。由於在洗清液流上一般具有烴濃度限制，因此會由於洗清液流量的增加而提升製程成本。
發明人已發現，較佳之塔作業壓力範圍為5至25巴絕對壓力，更佳者係為10至20巴絕對壓力。迴流液124之相對流量係可介於液氧進料115的10%至50%之間，且較佳者係為液氧進料115之10%至30%之間。
圖2示出液氧進料源來自一低壓來源的製程。一低壓液氧源係經提供作為料流200。料流200係可為在大於大氣壓力但小於稀有氣體回收塔127壓力之任何壓力下的過冷或飽和液體。料流200在泵203中被壓縮至高於塔127之壓力以形成壓縮液氧流209。將液氧流209於去過冷卻器212中加熱以產生液氧進料115。如圖1所述，流115係經加工以產生富含氙與/或氪之液流151與冷凝液氧154。流154係於去過冷卻器212中冷卻以形成過冷的氙與/或氪貧乏液氧流257。流257係可選擇性經減少閥260上之壓力以形成流263，其係經引入相分離器266。閥260上之壓降可能導致形成一些驟沸蒸氣，將其作為流269自分離器266中除去。驟沸後之剩餘液體係做為低壓迴流液流272自分離器中移出。儘管非必然，但流272之壓力通常係介於低壓液氧源與稀有氣體回收塔的壓力之間。可選擇性將驟沸蒸氣流269引導至任何合適來源或目的地以回收氧分子。
低壓液氧源之範例係可包括低溫雙塔空氣分離單元之低壓塔的集水槽、自低壓塔至液氧儲存槽之管線，或液氧儲存槽。
液氧進料之來源亦可源自如圖3所示之高壓來源。一高壓液氧源係經提供做為料流300。料流300係可為在任何大於稀有氣體回收塔127之壓力之一過冷卻液體。料流300係經減少閥303上之壓力至表面上大於蒸餾塔127之壓力，以形成流209。流209於去過冷卻器212中經過加熱以產生液氧進料115。如圖1所述，流115係經加工以產生富含氙與/或氪之液流151以及冷凝液氧154。液氧流154於去過冷卻器212中冷卻以形成流257。流257係可選擇性經減少閥260上之壓力以形成流263，其係經引入相分離器266。閥260上之壓降可能導致形成一些驟沸蒸氣，其係以驟沸蒸氣流269自分離器266中移出。驟沸後殘留之液體係做為低壓迴流液流272自分離器中移出。儘管非必然，但流272之壓力介於1.0至3.0巴絕對壓力之間。通過泵375使流272之壓力增加，以產生高壓迴流液378。驟沸蒸氣流269可選擇性地經引導至任何合適來源以回收氧分子。
一高壓液氧源範例係來自習知泵送液氧循環之泵排量。一般而言，此來源之壓力大於30巴絕對壓力，且經常超過60巴絕對壓力。於接近30巴絕對壓力之壓力下，難以對含氧流體進行蒸餾，而在大於氧氣臨界壓力(約50巴絕對壓力)之任何壓力下，都無法進行蒸餾。當使用高壓源時，高壓迴流液之壓力通常係對應於來源之壓力。
範例
作為本發明之範例，已對圖1所示之製程進行模擬。模擬結果如表1所示。
Figure 109144016-A0305-02-0014-1
結果顯示，在將洗清液流量減少至液氧進料的0.3%時，可使氙回收率大於97.0%。驅動冷壓縮機的功率適中，僅161kW。此係由於大約1.1的低壓縮比所致。與再沸器148相關聯的溫度差係為1.0℃，其對於此目的係為合理，並且已透過計算驗證。
一般而言，並且基於現有技術之教示，本領域具有通常技藝者會認為較佳之作法為在環境溫度下壓縮流139，即來自稀有氣體回收塔的蒸 氣。然而，發明人已發現，此種方法對於該製程之效率將顯著降低。於環境溫度下壓縮需要以下步驟：1)於熱交換器中將流139加熱至環境溫度；2)壓縮經加熱之氣體；3)於壓縮機後冷卻器中將經壓縮之熱氣體冷卻至接近環境溫度；4)冷卻環境氣體中流145的溫度。
如範例1所揭露，塔中的流139之壓力為15巴絕對壓力；再沸器148入口處之壓力為16.6巴絕對壓力。假設在塔與壓縮機之間沒有管道壓降，且壓縮機與再沸器148之間沒有管道壓降，則壓縮比(CR)將為1.107(16.6/15.0)。然而，對於商業規模之設備而言，自塔至冷壓縮機抽吸以及自冷壓縮機排放至再沸器148之管道壓降(dP)將分別為約0.05巴絕對壓力。壓縮機抽吸處之吸入壓力為14.95巴絕對壓力，而於壓縮機排放處則為16.65巴絕對壓力。所得壓縮比(CR)為1.113(16.65/14.95)。考慮到在環境溫度條件下壓縮之過程，壓縮機上游的壓降將為0.25巴絕對壓力(通過管道為0.1，加上熱交換器中的0.15巴絕對壓力)；壓縮機之下游壓降將為0.35巴絕對壓力(通過管道為0.1，加上壓縮機後冷卻器的0.1+熱交換器的0.15巴絕對壓力)。於此暖壓縮機上的合成壓縮比將為1.142(16.85/14.75)。
壓縮功率與F*T*ln(CR)成比例，其中F為流量、T為壓縮的平均絕對溫度(K)、CR為壓縮比。上述三者之比較係列於表2，所有情況下的循環流量(F)皆相同。
Figure 109144016-A0305-02-0016-2
「相對的」一詞係指術語：T*ln(CR)之比率
表2所示之結果說明，將情況2與情況3進行比較，壓降差會導致25%的功率差。冷壓縮和熱壓縮之間的較大差異係由壓縮溫度所導致。通常，基於需要冷卻作用以去除冷壓縮之熱量，因此冷壓縮之顯著效益常受到忽略。相反地，熱壓縮之熱量係被排放至周圍的後冷卻器中。
冷壓縮機上之溫度僅上升4.6℃。因此，必須透過在大約-146℃溫度下之外部冷卻作用來提供4.6℃的氣體冷卻。相反，為進行熱壓縮，必須使用預熱/冷卻之熱交換器將氣體自-146℃加熱至表面上25℃，並將氣體自表面上30℃冷卻至較冷之溫度，透過能量平衡之方式，冷卻至-141℃。因此，為使熱交換器之操作可行，將需要在約-146℃具有5℃之溫度差，此係代表冷卻損失。結果係為，對於一第一近似值，為補償冷壓縮熱量所需之冷卻需求，係等於讓實施熱壓縮作業所需要之熱交換器作業可行所需之冷卻需求。因此，消除對周圍環境的循環與壓縮熱能，係出乎意料地使使功率實質降低66%(如表1所示)。
本文引用的所有參考文獻，包括出版物、專利申請及專利，均以引用方式併入本文，其程度如同各參考文獻係單獨且經具體指示以引用方式併入本文，並於本全文內闡述。
在描述本發明之上下文中(尤其係於所附申請專利範圍之上下文中)術語「一」和「一種」與類似指稱之使用應解釋為涵蓋單數形式與複數形式，本文另有說明或與上下文明顯矛盾者除外。除非在此另外指出，否則本文中數值範圍之列舉僅用於分別指稱落入該範圍內之各獨立數值之簡寫方法，且各獨立數值皆被併入說明書中，如同其係於本文中單獨描述一樣。除非本文另外指出或與上下文明顯矛盾，否則本文描述之所有方法皆可以任何合適之順序執行。除非另有要求，否則本文提供之任何與所有範例或範例性語言(如「例如」)之使用僅旨在更清楚闡述本發明，且不對本發明之範圍構成限制。說明書中任何語言皆不應解釋為指示任何未經主張保護之元素對於實施本發明係為必要。
本文描述了本發明之較佳實施方式，包括發明人已知用於實施本發明之最佳方法。應當理解，本發明不限於上述參照較佳實施例描述之細節，而係可於不脫離所附申請專利範圍限定之本發明精神與範圍的情況下進行各種修改和變化。
100:稀有氣體回收系統
115:流
121:控制閥
118:第一部分
124:迴流液
127:塔
130:第二部分
133:控制閥
136:流
139:流
142:冷壓縮器
145:流(冷壓縮氧流)
154:冷凝液氧
191:頂部
192:蒸餾區
193:再沸區

Claims (13)

  1. 一種自含有氧與氙與/或氪之一液氧流回收氙與/或氪之方法，該方法包含：提供一稀有氣體回收系統，其包含一稀有氣體回收塔，其具有一頂部，一底部，至少一蒸餾區，以及包含一再沸器之一再沸區；提供至少一液氧進料，其包含氧與氙與/或氪；提供該液氧進料之至少一部分至該稀有氣體回收塔之頂部，以形成一迴流液；於該再沸區蒸發一再沸器液體，以形成一上升蒸氣與富含氙與/或氪之液流的混合物；於至少一蒸餾區中使該上升蒸氣與迴流液接觸，以使氙以及/或氪自上升蒸氣中經提取至迴流液中，以產生該再沸器液體；自該稀有氣體回收塔之頂部移出該上升蒸氣，形成氙以及/或氪匱乏之氣態氧流；自該稀有氣體回收塔之底部移出該富有氙以及/或氪之液流；使該氙以及/或氪貧乏之氣態氧流通過可形成一冷壓縮氧流之冷壓縮器；使該冷壓縮氧流通過該再沸器，該再沸器係可藉由與該再沸區中之再沸器液體間接熱交換而產生冷凝液氧；以及 將該冷凝液氧做為氙以及/或氪貧乏液氧自該稀有氣體回收系統移出。
  2. 如請求項1所述之方法，進一步包括將該液氧進料分為一第一部分以及一第二部分，並於至少一蒸餾區與該再沸區間之一位置將該液氧進料之第二部分提供至該稀有氣體回收塔。
  3. 如請求項1所述之方法，其中該稀有氣體回收塔係於5至25巴絕對氣壓之一壓力中進行操作。
  4. 如請求項1所述之方法，其中該稀有氣體回收塔係於10至20巴絕對氣壓之一壓力中進行操作。
  5. 如請求項3所述之方法，進一步包含提供一低壓液氧流，該低壓為大於大氣壓力但小於該稀有氣體回收塔之壓力之任何壓力，將該低壓液氧流於一泵內壓縮至一大於該稀有氣體回收塔的作業壓力的壓力而形成一壓縮液氧流，於一去過冷卻器內透過間接熱交換加熱該壓縮液氧流以形成該液氧進料；以及將該冷凝液氧傳送至該去過冷卻器，並透過與該壓縮液氧流之間接熱交換冷卻，以產生一過冷卻氙與/或氪貧乏液氧。
  6. 如請求項5所述之方法，進一步包含於一閥中降低該過冷卻氙與/或氪貧乏液氧之壓力，並將該過冷卻氙與/或氪貧乏液氧傳送至可形成一低壓迴流液之一相分離器。
  7. 如請求項3所述之方法，進一步包含提供一高壓液氧流，於一閥中將該高壓液氧流之壓力降低至一大於該稀有氣體回收塔之作業壓力的壓力而形成一壓縮液氧流，於一去過冷卻器中透過間接熱交換加熱該壓縮液氧流，以形成該液氧進料；以及將該冷凝液氧傳送至該去過冷卻器，並透過與該壓縮液氧流之間接熱交換冷卻，以產生一過冷卻氙與/或氪貧乏液氧。
  8. 如請求項7所述之方法，進一步包含於一閥中降低該過冷卻氙與/或氪貧乏液氧之壓力，並將該過冷卻氙與/或氪貧乏液氧傳送至可形成一低壓迴流液之一相分離器；以及於一泵中壓縮該低壓迴流液，以形成一高壓迴流液。
  9. 如請求項8所述之方法，其中該高壓迴流液之壓力係對應於該高壓液氧流之壓力。
  10. 如請求項1所述之方法，其中根據該液氧進料中之氙濃度，係達成90%或以上之一氙回收率。
  11. 如請求項1所述之方法，其中根據該液氧進料中之氙濃度，係達成95%或以上之一氙回收率。
  12. 如請求項1所述之方法，其中該液氧進料之該至少一部分係介於該液氧進料之10至50%。
  13. 如請求項1所述之方法，其中根據該液氧進料中之氪濃度，係達成15至90%或以上之一氪回收率。
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