TW200407B - Coproduction of a normal purity and ultra high purity volatile component from a multi-component stream - Google Patents

Abstract

A volatile component with normal purity and ultra high purity is coproduced from a stream containing a heavier component and contaminated with a lighter impurity which is more volatile than the volatile component by removing from a first distillation column a steam of the volatile component which is substantially free of the lighter impurity and then introducing this impurity-freed steam to a second distillation column for fractionation. The second distillation column is equipped with a rectification section wherein the impurity-freed stream is rectified and the volatile component obtained in ultra high purity as an overhead. The volatile component with normal purity is obtained from the first distillation column as an overhead.

Description

200407 Λ fi Η 0 經濟部屮央桴準局cx工消费合作杜印3i 五、發明説明（) 技術领 本發明係閣於從一氟體中共同生產出一昝通純度及一 超高純度揮發性成分的蒸餾分離。 相關申請案之參老 本案爲1991年11月15日申請，案號07/792,849美國專 利申請案的延續申請案。本案與該案具有相同之發明名稱 Ο 發明背棄 對一流例如爲較輕雜質污柴的空氟及天然氣流進行蒸 餘分離的技術爲智知的。典智地，一含有校輕污杂雜質的 揮發性成分的谓部產品，及包含有較重成分的一底部產品 被獲得。由於多種工業领域中的技術進步，需要比傳統蒸 餘方法所製得的產品純度更高的產品。此等純度更高的產 品的獲得需要進一步的程序及蒸餾以從該揮發性成分中有 效地移除該较輕污染雜質。因爲此等附加裎序步骑，於是 需要實f量的能量或附加設備或兩者同時以達成該揮發性 成分的一较高純化程度。例如超高純度產品被用於半導艘 及積體電路的產業领域。即使此等產業需要超高純度產品 ，然而在某些情形下被需求的量ϋ不足以支持一完全投入 超高純度產品生產的工廠。其它產業用途並不需要生產此 超南純度產品所必需的精心程序’也不能負擔生產超高純 度產品成分所必需的程序之有關成本因素。因此，在蒸询 本紙張尺度边用中Β國家標毕（CNS) f 4規格（210x297公处） (請先間讀背而之注意事項洱填寫本页) 裝. 訂- 線 ^00407200407 Λ fi Η 0 CX industry and consumer cooperation of the Ministry of Economic Affairs, CXC, Du Yin 3i V. Description of the invention () Technology leads the present invention to jointly produce Yitong purity and an ultra-high purity volatile from a fluorine body Distillation separation of sexual components. Participation in relevant application cases This case is an extension of the US Patent Application No. 07 / 792,849 filed on November 15, 1991. This case has the same invention title as this case. Invention abandonment The technology of steam separation and separation of first-class air fluoride and natural gas streams, such as lighter impurities, is well-known. Ingeniously, a predicate product containing volatile components that are lightly polluted and impurities, and a bottom product containing heavier components are obtained. Due to technological advances in various industrial fields, products with higher purity than traditional steaming methods are required. The acquisition of these higher purity products requires further procedures and distillation to effectively remove the lighter polluting impurities from the volatile components. Because of these additional steps, real energy or additional equipment or both are required to achieve a higher degree of purification of the volatile component. For example, ultra-high purity products are used in the field of semi-conductor ships and integrated circuits. Even though these industries require ultra-high-purity products, in some cases the amount required is not sufficient to support a plant that is fully engaged in the production of ultra-high-purity products. Other industrial uses do not require the meticulous procedures necessary to produce this ultra-nan purity product, nor can they afford the cost factors associated with the procedures necessary to produce ultra-high purity product ingredients. Therefore, please use the Chinese National Standards (CNS) f 4 specifications (210x297 public offices) for the size of this paper (please read the notes and fill in this page first). Binding-Line ^ 00407

Λ (i I5C 五、發明説明（） 领填中，尤其在冷凍蒸餾领域，對同時生產出一普通純度 及一超高純度的同成分存在有一實質上利益。如此，—校 大工廠可以被建造，工廠的產品可以被分銷到不同產業。 蒸餾及將一流的成分分離成不同組成分的代表性技藝如下 美國專利662,917號揭露了生產氮及氣的一單塔方 法。於此方法中，空氣被除去其雜質並冷卻至其露點溫度 ，並導入於一單塔而分離成其組成分。一富氮部分被從該 塔頂部移出。於一沸騰器/冷凝器中一部分爲該富氧校重 流所冷凝，並且其一部分作爲一回流而被送回，另一部分 作爲產品而被移出。 美囷專利4，871’382號揭露了適用於將空氣分離成其 組成分的一傳統雙塔方法，包括一用於獲得氬的支流塔。 於該方法中，空氟被注入於一高壓塔，其中一富氮部分於 該塔的頂部被產生，及—富氧部分於該塔的底部被產生。 該富氧部分及富氮頂部產品的一部分被導入於—低壓塔中 進一步進行分餾。一富於氮頂部產品從該低壓塔被移出作 爲產品，及氧（液態或氣態）從該低壓塔的底部被獲得。一 氬流接從該低壓塔移出一富氬支流而被獲得，並且於該支 流塔中被分餾，其中氣係作爲一頂部產品被移出，而氧係 作爲一底部產品被移出。 美國專利4,902 ’321號揭露了藉冷凍蒸餾一空氣流而 生產高純度氮的一方法。如同以上之前案，一富氣流係於 一蒸餾塔的底部被產生，而一富氮流於該塔的頂部作爲— -4 - ί4Λ11 a « t- iji(CH5) f (210X 297 ---~~- 200407 經沭部+央榀準而β工消合作社印31 五、發明説明（) 頂部產品被產生。 相對於前述所提的專利，該氮頂部產品的一部分於一 沸騰器/冷旋器中被冷凝，其中該頂部產品的雜質以一较 輕雜質形式被移除。從該沸騰器/冷敖器出來的冷凝物接 著被降壓並於同一彿騰器/冷凝器被蒸發而提供了一较高 純度氮產品流（具有较低滾度的較輕雜質）。很清楚地，此 系統的缺點在於該高純度氪產品的壓力低於該蒸餾塔壓力 〇 美國專利5，〇49,173號揭露了從一空氣流生產高純度 氧的方法。於此方法中，如同其它冷；東蒸你以分離空氣的 方法’一富氧底部產品及一富氪頂部產品係從該蒸餾塔中 產生。一基本上不含较重成分的含氧流被注入一第二分館 塔而於其中揮發性雜質被從氧中脱除，而獲得一超高純度 液態氧成分。 發明之總結 本發明關於蒸餘分離一多成分流的改良，該流包^^一 主要揮發性成分（A), —主要较重成分（B)，及至少一较輕 雜質（I)，該較輕雜質比該成分（A)具有一較高揮發性。於 一傳統方法中，成分（A)與成分（b)分離，並且成分（幻逹 同該較輕雜質（I)作爲一頂部產品部分被移出。一富於成 分（B)的流基本上不含較輕雜質（1)作爲一底部產品部分被 移出。同時生產出一含有普通純度成分（A〉及少量较輕雜 質（；〇的流，與一含有超高純度分分（A〉及實質上不含较輕 (請先閲請背而之注意帘項再项寫木頁) 裝· 線_ 本紙張尺度边用中a a家aiMCNS) ΤΊ規怙（2IdX297公及) 200407 Λ (； Π (： 經濟部屮央桴準而卩工消作合作社印驭 五、發明説明（） 雜質⑴的流之改良係藉由下列蒸始程序而達成。一多成 分流被注入於-第-蒸餘塔，該第一蒸館塔具有一用於有 效增泼成分（A)的上精魅，並從該區移出—頂部產品； 及-用於有效増泼成分⑻的下汽提區，並從該區移出一 底部產品部分。從該第一蒸餘塔的一點取出一流，該流含 有-實質量的成分（A〉及實質上不含任何較輕雜質⑴。此 流接著被導入-具有一精爾區的第二蒸館塔，該導入點係 低於該精舰，其中鱗發性成分⑷於錢够被増滚， 並從該精姆區上方終極取出該増泼部分。一富於成分⑻ 的底部產品部分從該精館區下方的—點被取出。從該第二 蒸館塔的精姆區上方出來的流比該第一蒸姆塔出來的頂部 產品具有一實質上较高純度。 除了可同時生產不同純度，例如一高純度及一超高純 度，的揮發性成分的事實外，以上所描述之蒸餘程序亦具 有下列的優點。該等優點包括： .可同時共同生產一揮發性成分且不會増加能量消托 的能力； .可同時共同生產壓力大小類似之一高純度及一超高 純度的成分（A)而不需要一附加再沸器及/或冷敖器；及 .可獲得高產量成分（A)的能力。 固示之簡 阖1爲用於同時生產出不同純度氮的多塔蒸餾系統的 方法流程圖。 -6 - 边 度 尺 本 一(CN 準 (請先間讀背而之注*苹項#塥寫本頁) 裝< 線 20040? 經濟部屮央楛準：：工消iv合作杜印ii Λ (i Η (i 五、發明説明（） 爲使用麋紊物膨服器的多塔蒸錄系統的方法流 程阑。 μ 爲使用廢棄物膨脹器的多塔蒸你系統的方法流 _除了其中支流塔在其精館部位的上方結合-汽提區 外與阖2相同。 之詳細效明 本案所播述<方法係特別用#從一含有一較重成分 (Β)及至少一较輕雜質（ι)的多成分流中共同生產出一揮發 f生成分（Α)，該较輕雜質（1)比該成分（幻具有一較高揮發 性0於許多情況下’該多成分流會含有其它成分。被用於 刀離的典型流包括空氣，其中高純度及超高純度氮爲想要 的共同產品。本發明方法亦通用於生產不同純度的破氩化 合物。 本發明可經由其最簡單喫態，參考圖i，而被最佳地 了解。於此具體實施例中，含有一揮發性主成分（A)，一 较重成分（B)及至少一較輕雜質（1)的一多成分流被蒸餾。 當使用空氣爲進料時，氮爲該揮發性之成分（A)，其滾度 爲78·12% ’氧爲主要較重成分（濃度爲2〇·95〇 ;然而其它 比氮重的成分例如氬（0.93%)等，典哩地被包括於一較重 成分（Β)。存在於空氣中比氪具有較高揮發性的较輕雜質 (1)爲氩（其濃度可高至l〇PPm)，氦（5.3ppm)及氖（Ιδρριη) 。當進料非爲空氣之一般情形時，较輕雜質（I)的滚度可 大大高於ppm的程度。 -7 - (請先間讀背而之注意事項再塡寫本IS ) 裝- 線.Λ (i I5C V. Description of invention () In the filling, especially in the field of refrigeration distillation, there is a substantial interest in the production of a common purity and an ultra-high purity of the same component at the same time. In this way, the school plant can be built The products of the factory can be distributed to different industries. Representative techniques for distillation and separation of first-class components into different components are as follows. US Patent No. 662,917 discloses a single-tower method for producing nitrogen and gas. In this method, air is Remove its impurities and cool to its dew point temperature, and introduce it into a single column to separate it into its components. A nitrogen-rich part is removed from the top of the column. A part of the oxygen-enriched calibration stream in a boiler / condenser Condensed, and a part of it is sent back as a reflux, and the other part is removed as a product. US Patent No. 4,871'382 discloses a traditional two-tower method suitable for separating air into its components, including A tributary column for obtaining argon. In this method, empty fluorine is injected into a high-pressure column, where a nitrogen-rich part is produced at the top of the column, and-an oxygen-rich part is The bottom of the column is produced. The oxygen-rich part and a part of the nitrogen-rich top product are introduced into a low-pressure column for further fractional distillation. A nitrogen-rich top product is removed from the low-pressure column as a product, and oxygen (liquid or gaseous) It is obtained from the bottom of the low-pressure column. An argon stream is obtained by removing an argon-rich side stream from the low-pressure column, and is fractionated in the side-stream column, in which the gas system is removed as a top product and the oxygen system as a The bottom product is removed. US Patent No. 4,902 '321 discloses a method of producing high-purity nitrogen by freeze distillation of an air stream. As in the previous case, a rich gas stream is generated at the bottom of a distillation column, and a nitrogen-rich Flowing to the top of the tower as-4-ί4Λ11 a «t-iji (CH5) f (210X 297 --- ~~-200407 by the Ministry of Shu + Central Standard and printed by the β Gongxiao Cooperative Society 31 V. Description of invention ( ) The top product is produced. Compared to the aforementioned patent, a portion of the nitrogen top product is condensed in a boiler / cold spinner, wherein the impurities of the top product are removed as a lighter impurity. From this Boiler / The condensate from the Ao device is then depressurized and evaporated in the same fortifier / condenser to provide a higher purity nitrogen product stream (lighter impurities with lower roll). Clearly, the The disadvantage is that the pressure of the high-purity krypton product is lower than the pressure of the distillation column. U.S. Patent No. 5, 〇 49,173 discloses a method of producing high-purity oxygen from an air stream. In this method, like other cold; East steam you to separate The air process'-an oxygen-rich bottom product and a krypton-rich top product are produced from the distillation tower. An oxygen-containing stream substantially free of heavier components is injected into a second branch tower where volatile impurities are removed from Oxygen is removed to obtain an ultra-high-purity liquid oxygen component. Summary of the Invention The present invention relates to the improvement of steam separation to separate a multi-component stream. The stream includes a main volatile component (A), a main heavier component (B), and at least one lighter impurity (I), which has a higher volatility than the component (A). In a traditional method, component (A) and component (b) are separated, and the component (phantom with the lighter impurity (I) is removed as a top product portion. A stream rich in component (B) does not substantially The lighter impurities (1) are partly removed as a bottom product. At the same time, a stream containing ordinary purity components (A> and a small amount of lighter impurities (; 〇, and an ultra-high purity fraction (A> and substance No lighter on the top (please read the curtain and write the wooden page first) Please install the line _ This paper size is used in the aa family aiMCNS) ΤΊ 訊 悙 (2IdX297 public) 200407 Λ (; Π ( ： The Ministry of Economic Affairs, the central government, and the work of the cooperative cooperative printing and control. 5. Description of the invention () The improvement of the flow of impurities (1) is achieved by the following steam initiation procedure. A multi-component stream is injected into the -di-steaming tower , The first steaming tower has an upper essence for the effective splash component (A), and is removed from the zone-the top product; and-the lower stripping zone for the effective splash component ⑻, and from the The bottom part of the product is removed from the zone. The first stream is taken from a point of the first steam residue column, and the stream contains The component (A> and substantially does not contain any lighter impurities ⑴. This stream is then introduced-the second steaming tower with a Jinger area, the introduction point is lower than the Jing ship, where the scaly component ⑷ is The money is rolled up, and the splashed part is finally taken out from above the Jingmu area. A bottom product part rich in ingredient ⑻ is taken out from the point below the Jingguan area. The refined from the second steaming tower The stream coming out of the um zone has a substantially higher purity than the top product from the first steam tower. In addition to the fact that volatile components of different purity, such as a high purity and an ultra-high purity, can be produced at the same time, The steaming process described above also has the following advantages. These advantages include: the ability to simultaneously produce a volatile component without increasing energy dissipation; the ability to simultaneously produce high purity and similar pressures An ultra-high-purity component (A) without the need for an additional reboiler and / or cold boiler; and. The ability to obtain high-yield components (A). The simple illustration 1 is used for simultaneous production of different Purity nitrogen in multi-tower distillation system Flow chart of the law. -6-One of the marginal scales (CN standard (please read back and forth at the first time * apple item # 塥 write this page) install &line; Cooperation Du Yin ii Λ (i Η (i V. Description of invention () is the method flow of the multi-tower steaming system using the moose turbulent expander. Μ is the method of multi-tower steaming your system using the waste expander Flow_ is the same as K2 except that the tributary tower is combined above the Jingguan-stripping area. The detailed effect is the same as that broadcast in this case. The method is specially used # 从 一 Contains a heavier component (B) and A multi-component stream of at least one lighter impurity (ι) co-produces a volatile f-generating component (Α), the lighter impurity (1) has a higher volatility than the component (magic has a higher volatility of 0 in many cases) Multi-component streams will contain other components. Typical streams used for knife separation include air, with high purity and ultra-high purity nitrogen being the desired common product. The method of the present invention is also commonly used to produce argon breaking compounds of different purity. The present invention can be best understood through its simplest eating state, referring to Figure i. In this particular embodiment, a multi-component stream containing a volatile main component (A), a heavier component (B) and at least one lighter impurity (1) is distilled. When using air as feed, nitrogen is the volatile component (A), and its rolling degree is 78 · 12% '. Oxygen is the main heavier component (concentration is 20.95%; however, other components heavier than nitrogen For example, argon (0.93%) is included in a heavier component (B). The lighter impurities (1) that exist in the air and have a higher volatility than krypton are argon (its concentration can be as high as 10). PPm), helium (5.3ppm) and neon (Ιδρριη). When the feed is not the general case of air, the roll of lighter impurities (I) can be much higher than the ppm. Contrary to the precautions, please write the IS)) Install-line.

200407200407

Λ Γ. Π G 五、發明説明 經 濟 部 中 k 標 準 局 工 消 fi- 合 Ρβ 杜 印 5i 該多成分流經管線10被送入一包含有一精餾區14及一 汽提區I6的蒸餾塔I2。訪進料係在介於該精餾區及該汽提 區問的位置被導入，於其中該揮發性成分（A〉及較輕雜質 (I)被増濃並以一頂部產品被產生，並經管線18被移出。 該頂部產品於冷凝器2〇中被凝_結，該获結的一部分經由管 線2 2被送回至該蒸餘塔1 2的頂部作爲回流。剩餘的获結頂 部產品經由管線24被移出，其主要成分爲成分（A)及污柴 該成分（A)的較輕雜質。選擇性地，該流18之一部分叮當 作氣體產品移出。當蒸餾空氣的情況時，氮（成分）係以一 大於99.5%的純度及最高至5〇ρριη的较輕雜質（1)例如氩、 氦、象等，被生產。 位於進料流10中的較重成分（B)於汽提區16被増滾， 並且一富於较重成分的液體產品經由管線26從該蒸餾塔12 的底部移出。此液體產品的一部分於再滞器/冷获器Μ中 被蒸發，並且所產生的蒸氣再進入該脱除區丨6的底部進行 脱除。該液體產品的其餘部分（富於较重成分（8))經由管 線3〇被移出。 藉從蒸館塔I2移出一含有大部分爲成分（A)及污染有 成分（B)但基本上不含任何較輕雜質（1)的流π而產生一超 咼純度成分（A)部分。於此流中的较輕雜質（1；)濃度比從輔 助精餾塔34頂部生產出的超高純度共同產品所要求者遺低 。例如，於空氣蒸餾以同時產生超高純度氮（較輕雜質氩 、氦及氖的全部滾度低於Sppb)時，該流之此等较輕雜質 的全部濃度應低於3ppb。移出此流的一點係從該脱除區“ (請先閲請背而之注意事項ΛΛ5寫本页) 裝- 訂 20040? Λ (i Η (i 五、發1V】説明（ 經濟部屮央標準灼Μ工消价合作杜印51 的一合遑位置。該流經由管線32被取出並送至一具有一精 餾區的輔助蒸餾塔34。帔送入之料於其中被純化而於精餾 區頂部產生一超高純度產品，及經由一管線％移出一超高 純度蒸氣。此蒸氟流接著於再沸器/冷凝器Μ中被至少部 分冷欢，並且該冷凝物的一部分被送回作爲從任何流有效 脱除较重成分，即成分（B)，的回流。其餘超高純度的成 分（A)經由管線U被取出。遴擇性地，位於管線％中的超 高純度蓁氣的一部分可以被取出以提供氣態超高純度共同 產品（A)。富於成分（B〉的底部產品部分經由管線从從該輔 助精餾塔Μ的底部移出並導入於該蒸餾塔1£的汽提區的一 合適點。 從此流程阖可簡單地觀察出成分（Α)，即氮，無論是 傳統純度遣是超高純度基本上具有相同壓力，並且鲁通純 度成分（Α)或氮與超高純度成分（幻或氮的共同生產係在未 進一步冷敖或蒸發其等各別之流下達成。此與美國專利 m號所示之流程阑明顯地不同。 阑2代表了本發明之另一具體實施例，其中牽涉到空 氣的冷凍蒸餾以獲得傳統純度及超高純度的氮產品。該方 法係藉由一具有氮再循環的傳統廢紊物膨脹器迴路，再依 本發明加予修飾變化而達成共同生產的效果。具有一氮再 循環的傳統廢棄物膨脹器迴路巳被描述於其闽專利第 4，4〇〇，188號。進而言之，於此修飾方法中空氣係經由管 線1〇〇導入並在進入一主熱交換器系列1〇2及1〇4之前先經 壓縮、冷卻、及爲一分子筛床吸附其中水及二氧化破。於 (請先間筇背而之汶Λ卞項ί'ί-Λ:ι,?ί木W) 訂 線· 1^紙5>：尺度边和肀明K家棕毕(CNS> T(210X297公及） Λ (i η ο 20040? 五、發明説叫（) 熱交換器1〇2及1〇4中，空氣被冷卻到接近其露點溫度，接 著經由管線1〇6送至一單塔蒸餾系統1〇8。於該塔頂部產生 一富氮成分的頂部產品，而於該塔底部產生一富氡成分。 該富氣蒸氣產品的一部分經由管線110取出並於熱交換器 104及1〇2中爲它流所加溫。該流的一部分被作爲普通純度 產品而取出，而一部分被再壓縮及於位在蒸餾塔1〇8底部 的沸騰器/冷莜器112中冷卻及凝結。此冷凝流接著被等拎 膨脹並導入該塔頂部作爲該塔的回流。該富氮蒸氟的另一 部分從管線被移出’於沸騰器/冷凝器1；16中被冷敖並 且至少一部分的冷熒物被送回該塔頂部作爲回流。其餘部 分可經由管線118移出而作爲遴擇性地昝通純度液氮產品 。蒸餾塔1〇8底部的粗液態氧由管線12〇取出並送至沸騰器 /冷凝器II6的蒸發側，而爲從塔頂取出的富氮蒸氟所蒸發 。被蒸發的粗液態氣經由管線〗22從該蒸發側移出，加溫 、膨脹、爲流程中的流再次加溫及最後當作一廢紊物被移 出〇 經？^部十央捣準而：^工消^八：作社印^ 超高純度氮係當作一共同產品從此方法取出，其包含 從蒸餾塔1〇8之汽提區位於該塔進料空氣下方的一點取出 一含氮流（經由管線I24取出）。此流基本上不含校輕雜質 ，例如高揮發性雜货如氩、氦及氖的體積含量低於5ΡΡΠ]， 較佳地係低於5Ppb(雜猜）。此流被導入一具有精你區的第 二蒸餾塔I26。該含氮流被導入該塔1Z6並且殘餘较重成分 被去除而在該塔頂部產生一超高純度氮產品。從蒸餾塔 I26顶部產生的頂部產品的一部分經由管線：28被送至沸騰 -10 - 本紙張尺度逡用中明》家標率（〇^)〒4枳怙（210;<297公;》) ^〇〇4〇7 Λ ίί η gΛ Γ. Π G V. Description of the Invention The Ministry of Economy, China, k Standard Bureau of Industry and Technology, Fi- and Ρβ Du Yin 5i The multi-component flow through line 10 is sent to a distillation column I2 that includes a rectification zone 14 and a stripping zone I6 . The incoming feed is introduced at a position between the rectification zone and the stripping zone, where the volatile components (A> and lighter impurities (I) are concentrated and produced as a top product, and It is removed via line 18. The top product is condensed in the condenser 20, and a portion of the cracked product is sent back to the top of the distillation column 12 via line 22 as reflux. The remaining top product of the cracked product It is removed via line 24, and its main components are component (A) and the lighter impurities of the component (A). Selectively, a portion of stream 18 will be removed as a gas product. When distilling air, nitrogen (Composition) is produced with a purity greater than 99.5% and lighter impurities (1) such as argon, helium, elephant, etc. up to 50 ρριη. The heavier composition (B) located in the feed stream 10 is steam The stripping zone 16 is rolled and a liquid product rich in heavier components is removed from the bottom of the distillation column 12 via line 26. A part of this liquid product is evaporated in the reslagger / cold catcher M and is produced The vapor enters the bottom of the removal zone 丨 6 for removal. The liquid product The remaining part (rich in heavier components (8)) is removed via line 30. By removing from the steaming tower I2 a component containing most of the component (A) and contaminated component (B) but basically does not contain any lighter The stream π of the impurity (1) produces an ultra-pure purity component (A). The concentration of lighter impurities (1;) in this stream is higher than that required for the ultra-high purity common product produced from the top of the auxiliary rectification column 34 For example, when air distillation produces ultra-high purity nitrogen at the same time (all lighter impurities such as argon, helium, and neon have a lower roll than Sppb), the total concentration of these lighter impurities in the stream should be less than 3ppb . The point to move out of this stream is from the removal zone "(please read the notes on the back ΛΛ5 to write this page first) Binding-Order 20040? Λ (i Η (i 五 、 发 1V) Description (Ministry of Economics The standard burner works at the combined position of Duin 51. The stream is taken out via line 32 and sent to an auxiliary distillation column 34 with a rectification zone. The feed material is purified and refined in it An ultra-high-purity product is produced at the top of the distillation zone, and an ultra-high-purity steam is removed through a pipeline%. It is at least partially cooled in the reboiler / condenser M, and a part of the condensate is sent back as a reflux to effectively remove the heavier component, component (B), from any stream. The remaining ultra-high purity components (A) is taken out via line U. Optionally, a part of the ultra-high-purity zeolite located in the line% can be taken out to provide the gaseous ultra-high-purity common product (A). The bottom product rich in ingredients (B>) Partially removed from the bottom of the auxiliary rectification column M via the pipeline and introduced to a suitable point in the stripping zone of the distillation column 1. From this process, the component (Α), namely nitrogen, whether traditional or not, can be simply observed Purity is that ultra-high purity basically has the same pressure, and the common production of Lutong purity component (A) or nitrogen and ultra-high purity component (magic or nitrogen) is achieved without further cooling or evaporation. This is obviously different from the flow stop shown in US Patent m. Lin 2 represents another specific embodiment of the present invention, which involves refrigeration distillation of air to obtain nitrogen products of conventional purity and ultra-high purity. This method uses a traditional waste turbulent expander circuit with nitrogen recycling, and is modified according to the present invention to achieve a common production effect. A conventional waste expander circuit with a nitrogen recirculation is described in its Fujian Patent No. 4,400,188. In addition, in this modification method, the air is introduced through line 100 and compressed, cooled, and adsorbed to a molecular sieve bed for water and two before entering a main heat exchanger series 102 and 104. Oxidation breaks. Yu (please look back and forth between Λ 卞 item ί'ί-Λ: ι,? Ί wood W) Threading · 1 ^ Paper 5>: Scale edge and the Ming K Family Brown Bi (CNS> T (210X297 (Public and) Λ (i η ο 20040? V. The invention is called () In heat exchangers 10 2 and 10 4, the air is cooled to a temperature close to its dew point, and then sent to a single column distillation via line 10 6 System 108. A nitrogen-rich component top product is generated at the top of the column, and a radon-rich component is generated at the bottom of the column. A portion of the gas-rich vapor product is withdrawn through line 110 and is passed through heat exchangers 104 and 102. It is heated by its stream. A part of this stream is taken out as a product of ordinary purity, and a part is recompressed and cooled and condensed in the boiler / cooler 112 at the bottom of the distillation column 108. This condensation The stream is then expanded by waiting and introduced into the top of the column as the reflux of the column. Another part of the nitrogen-enriched steam is removed from the pipeline in the boiler / condenser 1; 16 is cooled and at least a part of the cold phosphor It is sent back to the top of the tower as reflux. The rest can be removed via line 118 as a selective liquid nitrogen product The crude liquid oxygen at the bottom of the distillation column 108 is taken out from the line 12〇 and sent to the evaporation side of the boiler / condenser II6, which is evaporated by the nitrogen-rich steam removed from the top of the column. The evaporated crude liquid gas passes through Pipeline 22 is removed from the evaporation side, heated, expanded, reheated the flow in the process and finally removed as a waste turbulent matter. ^ Ministry Shiyang pounded and made: ^ 工 消 ^ 八: 作Sheyin ^ Ultra-high purity nitrogen is withdrawn from this process as a common product. It consists of withdrawing a nitrogen-containing stream (from line I24) at a point below the feed air of the distillation column 108. This stream is basically free of light-weight impurities, such as high volatile groceries such as argon, helium, and neon, whose volume content is less than 5PP (Pui), preferably less than 5Ppb (Miscellaneous guess). This stream is imported into a The second distillation column I26 of the zone. The nitrogen-containing stream is introduced into the column 1Z6 and the residual heavier components are removed to produce an ultra-high purity nitrogen product at the top of the column. Part of the top product produced from the top of the distillation column I26 is via the pipeline : 28 was sent to Boiling -10-The standard of this paper is used by "Ming Ming" Rate (square ^) 〒4 presume trifoliate orange (210; < 297 well; ") ^ Λ ίί η g 〇〇4〇7

五、發明說明（) 益/兮喊器116，並且所獲得冷凝物的至少 蒸餘塔I26頂部作爲回流。其蜍的超高純度氮產品經由管 線13〇被移出，並於其中爲流程中的流所加滠’再經由管 線I32移出作爲一產品。如果需要，從彿騰器/冷凝器n6 出來的冷敖流I28的一部分可以作爲一超高純度液態氮產 品而出產。被導入該蒸餾塔的前述流中所含的氧成分 從該塔底部以一液體形式從管線134移出。此部分被送回 蒸餾塔1〇8的汽提區。 阑2所示者爲用於分離空氣的一傳統廢棄物膨脹氮名 攝環方法被修飾成可共同生產出超高純度及普通純度氮的 情形。所生產出的超高純度氮與標準氮產品比較其壓力逢 無下降’並且除了該流程中的流所具有的能源外基本上才 需供應附加能源。 固2顯示了將圖1所提示的本發明應用於一具有廢音 物膨膝器及氣再雜環的氣產生器的情形。此概念亦可應用 於其它具有—汽提區的氣產生器。具有—汽提區的其它岸 塔氣產生㈣例子有美國專利4,464，188號；4 662 916_ 918號；4,594,〇85及4,867 773號所描述者，其等被引用 爲本案參考資料。於此㈣子中，蒸树底部之滞騰制 今贫-贼㈣齡而聽 用^藝中㈣雙㈣產生器。_產生器的例子可 5於英固專利第^15,377號，美國專利心，617,026及 =^7號，其等被_爲本案參考_。於 法中’峨(亦稱之爲上塔或中叫的汽提區提供了 -11 - 本 ^ ^ ^ ίΑ ———— 用中雄和家棋华(CNS) 簡S(21〇x297公幻 (請先間汸背而之注*事項/}-塡窩木1:30 裝- 線- 2004075. Description of the invention (1) Yi / Xi loudspeaker 116, and the condensate obtained is at least the top of the steam residue tower I26 as reflux. The ultra-high-purity nitrogen product of its toad was removed through line 13o, where it was added to the flow in the process and then removed through line I32 as a product. If necessary, a part of the cold stream I28 coming out of the fortuner / condenser n6 can be produced as an ultra-high purity liquid nitrogen product. The oxygen components contained in the aforementioned stream introduced into the distillation column are removed from the bottom of the column in line 134 in a liquid form. This part is sent back to the stripping zone of distillation column 108. Figure 2 shows a situation where a conventional waste expanded nitrogen photographic ring method used to separate air is modified to produce ultra-high purity and ordinary purity nitrogen together. Compared with standard nitrogen products, the pressure of ultra-high purity nitrogen produced is not reduced. 'In addition to the energy possessed by the flow in this process, additional energy is basically required. Gu 2 shows the case of applying the invention suggested in FIG. 1 to a gas generator having a waste sound knee expander and a gas re-heterocycle. This concept can also be applied to other gas generators with-stripping zone. Examples of other onshore tower gas generation with a stripping zone are described in U.S. Patent Nos. 4,464,188; 4,662,916-918; 4,594, 〇85 and 4,867 773, which are cited as references in this case. In this son, the stagnation system at the bottom of the steamed tree is impoverished-the thief is of age and listens to the ^ 艺 中 ㈣ 双 ㈣ generator. _An example of a generator can be found in Yinggu Patent No. ^ 15,377, U.S. Patent Center, 617,026 and = ^ 7, etc., which are referenced in this case. Yufa Zhong'an (also known as the upper tower or the middle-stripping stripping zone provides -11-Ben ^ ^ ^ ίΑ ———— Using Zhongxiong Hejia Qihua (CNS) 简 S (21〇x297 公 幻(Please note in advance * matters /)-Lanmu 1:30 installed-line-200407

經濟部+央標準局3工消价合作杜印驭 五、發明説明（） =助亀的進料’該精餘塔係用於共同生產出超高純 其中:3::1及圖2所建議之本案發明的-應用， = 的精館區上方結合有-汽提區。應用 變化，使得増進獲得量(即共同生產_ 揀2自女' 可増加）爲可能。爲了方便分折513所插 述之文良方法，（相對於固2)捋焦點專注在第二笨餘塔 心及其域料咖的關係。於所示之具时施例中，第 :桊餾塔126破分成"及日兩階段，其中精餾係在A區進行而 η提係在b區進行。相對_ 2所示之實_，位於管線 11二内的液態今爽物的—部分從比Β區高的—點被導入鼓第 -蒸館塔126 ’其中該冷κ於該標示爲β區的汽提區内被 除去任何輕雜質。如果情況需要，位料線118内之其餘 冷旋物可移出作爲產品。標示爲Β區的汽提區的上方所產 生的頂部錢經由管線128被移出並送回該㈣塔1。8的頂 部。管線128内的_產品的-部分或幾乎全部可從管線 110移出作爲產品。管線128內的謂部產品亦可如固2所示 者被夺冑騰器/冷徒器116，但此處流程所示則具较簡單 的製造設備其中經管線128從第二蒸祕126移出的领部產 品被直接導人❹塔1Q8。超高純歧產品以管以3〇從第 -蒸館塔126介於精與汽提區_的一餘出。如果 情況需要’―超高純朗液態該可從㈣塔126的相同 位置被取出作爲產品（未示於囷中）。 藉在第二蒸餾塔^6的精餾區的上方設置一汽提區及 12 本紙张&度边用中Η國家標準（CNS)T4Mtft〇in (請先間請背而之：;-£-事項再艰"7木狂) 裝· 線i 200407Ministry of Economic Affairs + Central Bureau of Standards 3 Industry and Consumer Price Cooperation Du Yinyu V. Description of invention () = Feed of the help 'This Jingyu tower is used to jointly produce ultra-high purity among them: 3 :: 1 and Figure 2 The proposed application of the invention in this case is combined with the stripping zone above the Jingguan area of the. The application of changes makes it possible to increase the amount of gains (that is, co-production _ pick 2 self-daughter can be increased). In order to facilitate the Wenliang method interpolated in 513, (relative to Gu 2), the focus is on the relationship between the second stupid tower and its domain materials. In the illustrated embodiment, the first: the distillation tower 126 is divided into two stages: "daily" and "daily", in which the rectification system is carried out in zone A and η is carried out in zone b. Relative to the fact shown in FIG. 2, the liquid present in the pipeline 11—part of which is higher than the area B—is introduced into the Gudi-Steaming Tower 126 ′ where the cold kappa is marked as the area β Any light impurities are removed in the stripping zone. If necessary, the remaining cold spinners in the feed line 118 can be removed as products. The top money produced above the stripping zone labeled Zone B is removed via line 128 and sent back to the top of the tower 1.8. A part or almost all of the product in the pipeline 128 can be removed from the pipeline 110 as a product. The predecessor product in the pipeline 128 can also be taken out of the container / cooler 116 as shown in Gu 2, but the process shown here has a simpler manufacturing equipment in which the pipeline 128 is removed from the second steamer 126 The collar products are directly guided to the tower 1Q8. The ultra-high-purity manifold product is discharged from the first-steaming tower 126 in the fine and stripping zone with a tube 30. If the situation requires, 'Ultra-high purity Lang liquid can be taken from the same position of the tower 126 as a product (not shown in Fig. 2). By setting a stripping zone and 12 sheets of paper & edging in the second distillation column ^ 6 above the rectification zone with the national standard (CNS) T4Mtft〇in (please please turn back:;-£- The matter is more difficult " 7 Wood Madman) outfit · line i 200407

Λ (i It G 經濟部屮央榣準局A工消费合作社印製 五、發明説明（） 利用從蒸餾塔108頂部產品所獲得冷敖物的一部分，經由 管線I28從該第二蒸餾塔I26移出的頂部產品的實質上全部 可以被送回至主蒸餾塔108。此尤許位於管線丨36内流至該 蒸餾塔I26的液態流大於管線I28内之蒸氣。於是使得經由 管線13〇移出的超尚純度氣產品増多。於阖2所示之實施 例中，從第二蒸餾塔I26產生的頂部產品被分成兩部分， 一部分經管線I28被送回沸騰器/冷蔹器116，而其餘部分 經管線13〇移出作爲超高純度氪產品。 吾人可療解不同的修飾變化可以應用在以上所描述的 方法流程以獲得想要的結果。例如，於闽i所插述的流程 串聯另一系統可以被用於分離一多成分進料流。 雖然圖1顯示了兩成分進料之分離例子，但是該方法 亦可應用於具有超過兩主要成分的分離。例如，其可應用 於巳知之任何三成分蒸姆流程。當使用一含有三個主要成 分u〉、⑻及（〇並污染有至少—校輕雜質⑴的進料流， 該三個主要成分中，⑷爲最具揮發性者，接著爲⑻，再 接著爲⑹，而該较輕雜質⑴比成分⑷更具揮發性，來 共同生產一超高純度產品流A(實質上無較輕㈣⑴）時， 此三成分蒸館一般使用至少兩主蒸。由围^示範之 觀念，很明顯地含有⑷但幾乎不含较輕雜質⑴的一合通 流可從該主蒸館塔的至少—個的1提區被取出〇此流接 著可於-輔助精餘塔中被蒸始而共同生產出超高純度產品 (A) 〇 衣紙張尺度边用中SH家規tft(210x297公Λ) 裝- 訂_ 線· • ....... —tmmi 13Λ (i It G Printed by the Industrial and Consumer Cooperatives of the Central Bureau of Economics and Trade of the Ministry of Economic Affairs V. Description of the invention) The part of the cold product obtained from the top product of the distillation tower 108 is removed from the second distillation tower I26 via the pipeline I28 Substantially all of the top product can be sent back to the main distillation column 108. This allows the liquid stream flowing to the distillation column I26 in line 丨 36 to be larger than the vapor in line I28. Thus, the superfluid removed through line 13〇 There are many products with high purity gas. In the embodiment shown in Figure 2, the top product produced from the second distillation column I26 is divided into two parts, and a part is sent back to the boiler / cold water separator 116 via line I28, while the rest Removed as ultra-high-purity krypton product via pipeline 13〇. We can treat different modifications and changes can be applied to the method described above to obtain the desired results. For example, the process described in Mini is connected in series with another system It can be used to separate a multi-component feed stream. Although Figure 1 shows an example of separation of a two-component feed, the method can also be applied to separations with more than two main components. For example, it can be applied Any three-component steaming process known in the market. When using a feed stream containing three main components u>, ⑻ and (〇 and contaminated with at least-school light impurities ⑴, of the three main components, ⑷ is the most Volatile, then ⑻, then ⑹, and the lighter impurity ⑴ is more volatile than component ⑷ to jointly produce an ultra-high-purity product stream A (substantially without lighter ㈣ ⑴), these three components The steaming hall generally uses at least two main steams. From the concept demonstrated by the ^^, the one-pass flow which obviously contains ⑷ but contains almost no lighter impurities ⑴ can be removed from at least one of the main steaming tower towers. Take out this stream and then it can be steamed in the auxiliary finishing tower to jointly produce ultra-high-purity products (A). The size of the paper sheet is packed with a medium SH home regulation tft (210x297 g).-Order_Line ...... —tmmi 13

Claims (1)

A7 〇· 〇〇4〇,7 B7 C7 D7 經濟部中央螵準局R工消費合作社印製 #、申請專利範圍 1. 一種蒸你分離一多成分流的方法，該流包含一主揮發 性成分（A)，一主要較重成分（B)及至少一比成分（A)更具 揮發性的較輕雜質（I)，其中一富於成分（A)的部分以一頂 部產品部分被產生’及一富於成分（B)的部分以一底部產 品部分被產生’其共同生產出一含有普通純度成分（幻之 流及一含有超高純度成分（A)、實質上不含较輕雜質（I)之 流的改良之處包含： 捋該多成分流的至少一部分作爲進料導入一第一 蒸館塔’其具有可有效増濃主揮發性成分的一精 始區，並從該區移出一頂部流，此頂部流的一部分作 爲普通純度產品被獲得；一有效増濃成分（B〉的汽提 區，並從該區移出一底部產品部分； 從該汽提區移出一包含成分（A)及（B)及實質上不 含任何雜質（I)的一被汽提流； 將該被汽提流導入一第二蒸餾塔，其具有可有效 將主揮發性成分（A)從主要較重成分（B)分離的一精餾 區； 於該第二蒸餾塔的精餾區分離成分（A)及成分（B) ;及 獲得比從該第一蒸餾塔生產者更高純度的成分 (A) 〇 2—種藉冷凍蒸餾而分離空氟以至少生產一氮成分的方 法，其中進料空氣被壓缩、冷卻至其露點並於一多塔蒸館 -14 - (請先閲讀背面之注意事項再塡寫本頁) 裝， 訂_ 夂紙張疋度適用中國國家標準(cn^· 規格（210 X 297 公^·) 200407 A7 B7 C7 D7 申請專利範圍 系統中被冷凍蒸餾，其中氪從該蒸餾系統中日勺至少一塔以 一頂部流被產生益作爲產品被移出，及氧從該蒸餾系統中 的至:> 一塔作爲一底部產品部分被移出，其共同生產出一 昝通純度氮及一超高純度氮的改良之處包含： 於該多塔蒸餾系統的一第一塔的汽提區中產生一 含兔及氧及實質上不含较輕雜質的進料流； 從該汽提區移出該氪/氣部分並捋其導入該多塔 蒸餾系紇的一第二蒸餾塔，該第二蒸餾塔具有至少一 精餾區； 於該第二蒸餾塔的該精餾區内將氮及氡分雊並因 而產生一比該第一蒸餾塔生產者较高純度的含氮頂部 產品部分’及含氧的一底部產品部分；及 獲得該较高純度氮產品。 (請先閲讀背面之;±意事項再頌寫本頁) .丨装· 訂. 蛭 濟 部 中 央 樣 準 局 Ά 工 消 作 社 印 轚 3依申請專利範固第1項所述的多成分流蒸餾分離方法， 其中該第二蒸餾塔具有可有效將主揮發性成分（A)從一主 要较重成分（B)分離的一精餾區及位於該猜餾區上方的一 汽提區； 將從第一蒸餾塔出來的該被汽提流導入該第二蒸 餘塔的精餾區下方的一點，其中該主揮發性成分（A) 在該第二蒸餾塔的精餾區上方及介於該精餾區與該汽 提區之間作爲一頂部產品被產生，而一主要較重成分 (B)作爲該第二蒸餾塔的一底部產品被產生； 將該主要较重成分（B)回流至該第一蒸餾塔； -15 -A7 〇 · 〇〇4〇, 7 B7 C7 D7 Ministry of Economic Affairs, Central Bureau of Industry and Commerce R Rong Consumer Cooperatives printed #, patent scope 1. A method of steaming you to separate a multi-component stream, the stream contains a main volatile component (A), a main heavier component (B) and at least one lighter impurity (I) that is more volatile than component (A), where a part rich in component (A) is produced as a top product part ' And a part rich in component (B) is produced as a bottom product part 'which together produces a component containing ordinary purity (magic flow and a component containing ultra-high purity (A), which is substantially free of lighter impurities ( I) The improvement of the stream includes: pressing at least a part of the multi-component stream as a feed into a first steaming tower, which has a refined starting area where the main volatile components can be effectively concentrated, and is removed from the area A top stream, a part of this top stream is obtained as a product of ordinary purity; a stripping zone with effective enriched ingredients (B>, and a bottom product part is removed from the zone; a contained ingredient (A is removed from the stripping zone ) And (B) and one that does not substantially contain any impurities (I) Stripping stream; introducing the stripped stream into a second distillation column, which has a rectification zone that can effectively separate the main volatile component (A) from the main heavier component (B); in the second distillation column Separation of component (A) and component (B) in the rectification zone of the plant; and obtaining component (A) of higher purity than that from the producer of the first distillation column Ingredients method, in which the feed air is compressed, cooled to its dew point and steamed in Yiduota-14-(Please read the precautions on the back before writing this page). Standards (cn ^ · Specification (210 X 297 g ^ ·)) 200407 A7 B7 C7 D7 The scope of patent application system is refrigerated distillation, in which at least one tower of krypton from the distillation system is produced with a top stream as a product. Removed, and oxygen from the distillation system to: > One tower was removed as a bottom product portion, which together produced Yitong purity nitrogen and an ultra-high purity nitrogen. Improvements include: In the multi-tower distillation In the stripping section of a first column of the system, a rabbit containing And oxygen and feed streams substantially free of lighter impurities; removing the krypton / gas portion from the stripping zone and introducing it into a second distillation column of the multi-column distillation system, the second distillation column having at least A rectification zone; separating nitrogen and radon in the rectification zone of the second distillation column and thus producing a higher purity nitrogen-containing top product portion and oxygen-containing one than the producer of the first distillation column Bottom product part; and obtain the higher purity nitrogen product. (Please read the back side first; ± Importance and then write this page). 丨 Installation and ordering. Central Sample Bureau of the Ministry of Economic Affairs Ά 工 消 作 社 印 訚 3 The multi-component stream distillation separation method as described in item 1 of patent application Fan Gu, wherein the second distillation column has a rectification zone that can effectively separate the main volatile component (A) from a main heavier component (B) And a stripping zone located above the guessing zone; introducing the stripped stream from the first distillation column to a point below the rectification zone of the second distillation column, where the main volatile component (A) is Above the rectification zone of the second distillation column and between the rectification zone and the stripping zone Room is generated as a top product, and a primary heavier component (B) a bottom product of the second distillation column as is generated; the heavier the main component (B) is returned to the first distillation column; -15-- A720040^ B7 C7 D7 六、申請專利範圍 將從該第一蒸餾塔獲得的一含有成分（A)及（I)佴 實質上不含主要较重成分（B)的一液體部分導入該第 二蒸餾塔的汽提區上方的一點，其中一富於成分（I) 的頂部產品在該汽提區的上方被產生；及 捋於該第二蒸餾塔的汽提區上方產生的該頂部產 品之至少一部分送®至該第一蒸餾塔的頂部。 (請先閲讀背面之注意事項再塡寫太頁) 烴濟部中央樣準局®:工消费合作社印* -16 - 本纸張尺度適用中國國家標準（CNS)甲4规格（210 X 297公釐〉 -Γ—, .|f- P.f| ---------------------------------------------- minillMimr Τ·ΐη·ΊΐηΐΊ>Ι>Ιΐ I UlilBMltfmi'nn -TlBi-.lllinni1 — ^ — ΐ'ΛΗΒΪΙϋ.Η·-···". 丨丨_ΙΙ»·Μ"ΙΙΗΙΒ· +WI .....A720040 ^ B7 C7 D7 VI. Scope of patent application A liquid part containing components (A) and (I) obtained from the first distillation column that does not substantially contain the main heavier component (B) is introduced into the second distillation A point above the stripping zone of the column, wherein a top product rich in component (I) is produced above the stripping zone; and at least at least the top product produced above the stripping zone of the second distillation column A portion is sent to the top of the first distillation column. (Please read the precautions on the back before writing the page.) Central Prototype Bureau of the Ministry of Hydrocarbon Economy®: Printed by the Industrial and Consumer Cooperatives * -16-The paper size is in accordance with the Chinese National Standard (CNS) Grade 4 (210 X 297 %〉 -Γ—,. | F- Pf | -------------------------------------- -------- minillMimr Τ · ΐη · ΊΐηΐΊ > Ι > Ιll I UlilBMltfmi'nn -TlBi-.lllinni1 — ^ — ΐ'ΛΗΒΪΙϋ.Η ·-·· ". 丨 丨 _ΙΙ »· Μ " ΙΙΗΙΒ · + WI ...