TW201840475A - 生產超高純度一氧化碳之純化方法 - Google Patents

生產超高純度一氧化碳之純化方法 Download PDF

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TW201840475A
TW201840475A TW106143709A TW106143709A TW201840475A TW 201840475 A TW201840475 A TW 201840475A TW 106143709 A TW106143709 A TW 106143709A TW 106143709 A TW106143709 A TW 106143709A TW 201840475 A TW201840475 A TW 201840475A
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carbon monoxide
producing ultra
purity carbon
liquefier
heat exchanger
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TWI851533B (zh
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大衛 米歐那
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德商林德股份公司
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Abstract

本發明揭示用於生產二氧化碳含量為0.1 ppm或小於0.1 ppm之超高純度一氧化碳的方法及裝置。利用一個反向熱交換器將二氧化碳凍結出產物流以從產物流中除去二氧化碳。此提供符合電子產業應用需求的超高純度一氧化碳產物。

Description

生產超高純度一氧化碳之純化方法
本發明係關於生產超高純度一氧化碳(CO)之方法及裝置。
具有低含量氮氣之CO可藉由電解法自二氧化碳(CO2 )流生產。然而，此等生產方法生產的CO在產物流中仍然殘留高達5,000 ppm的CO2 。此外，該CO產物流通常含有作為不合需要雜質之氫氣(H2 )。對於作為電子級CO使用而言，此含量之CO2 及H2 係不可接受的。電子級CO必需為超高純度(UHP)，其具有0.1 ppm或小於0.1 ppm之CO2 及H2 含量。 在本領域中仍然需要改進UHP CO之生產，特定言之以用作電子級氣體。
本發明提供用於生產CO2 含量為0.1 ppm或小於0.1 ppm之UHP CO的方法和裝置。此係藉由利用一個反向熱交換器將CO2 凍結出源流處理來自主要CO生產程序的CO(可高達99.5%CO)流來達成。 藉由本發明之方法及裝置生產的CO產物含有0.1 ppm或小於0.1 ppm之CO2 且因此用作電子級CO產物係可接受的。
相關申請案之交互參照 本申請案主張2016年12月13日申請的美國臨時申請案第62/433,274號的優先權。 本發明將參照圖式進行描述。 圖1中，待純化之CO源可由CO進料氣體鋼瓶或直接由CO產生器提供至系統。在任一情況下，供應壓力應為3至6巴。藉由在約6巴之壓力下生產產物CO，有可能有利地利用單級壓縮機填充產物鋼瓶。生產壓力之下限係最低實際液氮壓力的函數以便能夠逆著此液氮流液化產物流。 欲純化之CO輸送至系統且進入包含反向熱交換器及雪捕捉器的CO2 移除單元。CO源氣體中之CO2 內容物在反向熱交換器中凍結。任何並未黏附於熱交換器壁且以結晶或雪之形式藉由程序流運輸之CO2 隨後捕獲於雪捕捉器中。關鍵在於雪捕捉器以儘可能接近程序液化溫度操作而不使液化發生。若CO2 粒子溶解或懸浮於液體產物流中，則雪分離器中的液化可導致產物純度降低。較佳為反向熱交換器、雪捕捉器及CO液化器與H2 移除容器置於真空絕熱冷箱中。 雪捕捉器及熱交換器定期利用熱、真空及合適沖洗氣體之一些組合再生，該氣體諸如氦氣或氬氣，由於其後續應用，不被視為程序氣體中的雜質。在再生循環結束時，在開始下一冷卻及凍結循環前，以純CO產物氣體吹掃該系統可為有利的。液氮(LN)源提供凍結CO2 所需的低溫。一旦CO2 自CO源氣體中除去，則CO氣體輸送至CO液化器及H2 移除容器。在此容器中，CO冷卻至液體溫度及H2 釋放且排出系統。液體CO接著可被壓縮且輸送至CO產物鋼瓶以分配給客戶。如圖1中所示，利用隔膜壓縮機壓縮CO以達到約200巴之產物鋼瓶壓力。圖2展示一個類似系統，唯一不同係CO利用低溫液體泵壓縮。 在另一實施例中，CO液化器及H2 移除容器可含有改良不同相之冷凝及/或分離的內部零件。在另一較佳實施例中，CO氣入口之位置可安置於內部零件之間。圖3展示一個與圖1類似之系統，唯一不同係CO液化器及H2 移除容器含有內部零件。 在操作所描述之本發明的一種較佳方法中，可純化0.1 Nm3 /hr至50 Nm3 /hr氣流。更佳地，氣流係在5 Nm3 /hr與10 Nm3 /hr之間或在6與8 Nm3 /hr之間。 用於凍結CO2 以及液化CO所需的低溫由液氮(LN)源提供。氮氣穿過系統且可被處理及再循環或釋放至大氣中。任何自系統釋放之廢N2 或H2 中CO2 或CO含量低。 為了具有在經濟上有效的程序，工作壓力及工作溫度較佳基於可用的液氮規格。在真空絕熱冷箱內部，氣流自約環境溫度(300 K)冷卻至約100 K(+/-5度）。 實例. CO自進料氣體鋼瓶提供，其中設置兩個具有自動轉換的鋼瓶庫。CO進料氣體可具有以下典型規格： CO 99.8% CO2 2,000 ppm N2 4 ppm O2 0.05 ppm H2 40 ppm H2 O ＜ 0.1 ppb CxHy ＜ 0.1 ppb 在利用本發明之系統處理CO進料氣體之後，產物CO氣體符合或超出以下規格： CO 99.9999% CO2 0.1 ppm N2 6 ppm O2 0.1 ppm H2 0.1 ppm H2 O 0.004 ppb CxHy 0.3 ppb 如上文所描述之本發明提供多個優點。詳言之，本發明提供一種具成本效益的純化CO以獲得電子工業所需的UHP CO的方法。相比於基於蒸餾技術之先前技術方法，藉由本發明之方法生產的UHP CO將在資金及操作成本兩個方面代價較低。 本發明的另外一個優點係，在反向熱交換器中其他雜質亦自CO源氣體中除去。羰基化合物之量減少至通常偵測水準以下的水準。對於五羰基鐵(Fe(CO)5 )或四羰基鎳(Ni(CO)4 )此為一特別優點，該等物質在CO接觸不鏽鋼的情況下形成。藉由謹慎選擇低溫純化程序下游之材料，可生成羰基化合物水準極低的CO氣體。 鑒於前文描述，預見到本發明之其他實施例及變化形式將為熟習此項技術者所易見，希望此等實施例及變化形式亦被包括在本發明之範疇內，如在隨附申請專利範圍中所陳述。
圖1係根據本發明之一實施例用於生產UHP CO之程序系統的示意圖。 圖2係根據本發明之另一實施例用於生產UHP CO之程序系統的示意圖。 圖3係根據本發明之另一實施例用於生產UHP CO之程序系統的示意圖。

Claims (8)

  1. 一種生產超高純度一氧化碳之方法，其特徵在於一氧化碳流在用於凍結移除二氧化碳之反向熱交換器中冷卻，及之後該氣流係引導至用於移除固體粒子之雪捕捉器，及在該雪捕捉器之後該氣流引導至液化器及氫氣移除容器，其中該一氧化碳經液化及氫氣保持氣態且經分離。
  2. 如請求項1之生產超高純度一氧化碳之方法，其中使用液氮作為冷卻劑在該反向熱交換器中、在該雪捕捉器中及在該液化器及氫氣移除容器中。
  3. 如請求項1之生產超高純度一氧化碳之方法，其中該一氧化碳流經隔膜壓縮機或低溫液體泵壓縮且儲存於氣體鋼瓶中。
  4. 如請求項1之生產超高純度一氧化碳之方法，其中二氧化碳及氫氣在該超高純度一氧化碳中的含量為0.1 ppm或小於0.1 ppm。
  5. 一種用於生產超高純度一氧化碳之裝置，其特徵在於該裝置包含熱交換器，其連接至雪捕捉器，其亦連接至液化器及氫氣移除容器。
  6. 如請求項5之用於生產超高純度一氧化碳之裝置，其中該熱交換器、該雪捕捉器、該液化器及氫氣移除容器及各別的連接管線置於真空絕熱冷箱中。
  7. 如請求項5之用於生產超高純度一氧化碳之裝置，其中該液化器及氫氣移除容器含有插入件。
  8. 如請求項5之用於生產超高純度一氧化碳之裝置，其中該裝置另外包含用於壓縮一氧化碳之隔膜壓縮機或低溫液體泵。
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