CN106468498B - 用于通过低温分馏空气来制备氧气的蒸馏塔系统和装置 - Google Patents

用于通过低温分馏空气来制备氧气的蒸馏塔系统和装置 Download PDF

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CN106468498B
CN106468498B CN201610860977.XA CN201610860977A CN106468498B CN 106468498 B CN106468498 B CN 106468498B CN 201610860977 A CN201610860977 A CN 201610860977A CN 106468498 B CN106468498 B CN 106468498B
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column
mass transfer
argon
condenser
liquid
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CN106468498A (zh
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D·格卢贝夫
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Linde GmbH
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Linde GmbH
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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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Abstract

本发明的蒸馏塔系统和装置用于通过低温分馏空气来制备氧气。蒸馏塔系统具有高压塔(101)和低压塔(102)，主冷凝器(103)，和具有氩气塔顶部冷凝器(155)的氩气塔(152)。低压塔(102)包括上部传质区(131)，下部传质区(132)和中部传质区(130)。氩气塔顶部冷凝器(155、255)被设置在低压塔(102)内，位于上部和中部传质区之间，并被构建为强制流动蒸发器。

Description

用于通过低温分馏空气来制备氧气的蒸馏塔系统和装置
本发明涉及根据权利要求1前序部分、用于通过低温分馏空气来制备氧气的蒸馏塔系统。
在Hausen/Linde(第二版，1985)的专题论文“Tieftempereturtechnik”[Cryogenic Technology]以及Chemical Engineering Progress(第63卷第2期，1967，第35页)中总体描述了低温分馏的基础，并特别描述了双塔装置的构造。双塔的高压塔和低压塔之间的热交换关系通常通过主冷凝器的方式来实现，其中高压塔的塔顶气体被液化，而低压塔的塔底液体被蒸发。
本发明的蒸馏塔系统原则上可被构建为具有高压塔和低压塔的常规双塔系统。除了用于氮气-氧气分离的两个分离塔，其还可以包括用于获得其它空气组分、特别是稀有气体例如氪气-氙气回收的其它设备。
本发明中的主冷凝器称为冷凝器-蒸发器。“冷凝器-蒸发器”意指一种换热器，其中第一冷凝流体料流与第二蒸发流体料流进行间接热交换。每个冷凝器-蒸发器都具有液化空间和蒸发空间，其分别由液化通道和蒸发通道构成。在液化空间中进行第一流体料流的冷凝(液化)，并在蒸发空间中进行第二流体料流的蒸发。蒸发空间和液化空间由通道组形成，所述的通道组相互之间呈热交换关系。
典型地，主冷凝器被构建为液浴蒸发器，特别是级联蒸发器(例如描述于EP1287302B1＝US 6748763B2中的)。其可以通过在常规压力容器中设置的单个换热器模块(block)或者多个换热器模块形成。
“氩气排料塔”在这里意指用于氩气-氧气分离的分离塔，其并不用于回收纯的氩气产物，而是用于由正在高压塔和低压塔中分馏的空气排出氩气。其与通常具有70至180个理论塔板的常规粗氩气塔的连接方式仅存在轻微的不同之处；然而，其包含少得多的理论塔板，即少于40个，特别是15至35个。就像粗氩气塔，氩气排料塔的底部区域连接至低压塔中的中间点，并且氩气排料塔典型地通过顶部冷凝器而冷却，其中源自高压塔的膨胀塔底液被引入至蒸发侧；氩气排料塔通常并不具有再沸器。
术语“氩气塔”在这里用作为覆盖性术语，用于氩气排料塔、全部范围的粗氩气塔和其间所有的中间阶段。
任何分馏装置的蒸馏塔系统均被设置于一个或多个冷箱中。“冷箱”在这里理解为是指绝热壳，其由外壁完全包围热绝缘内部；在内部中设置的是所要绝热的装置部件，例如一个或多个分离塔和/或换热器。绝热作用可以通过外壁的恰当设置和/或通过在装置部件和外壁之间的中间空间填充绝热材料而形成。在后者的变例中，优选使用粉状材料，例如珍珠岩。用于低温空气分馏装置的氮气-氧气分离的蒸馏塔系统和主换热器及其它的冷装置部件必须要由一个或多个冷箱包封。冷箱的外部尺寸典型地决定了在预制装置的情况下包装的运输尺寸。
“主换热器”用于冷却与源自蒸馏塔系统的回流进行间接热交换的进给空气(feedair)。所述主换热器可以由一个单独的或者多个并联和/或串联连接的换热器部分形成，例如由一个或多个板式换热器模块形成。特别是用于蒸发或者伪蒸发单独液体或者超临界流体、而不会部分加热和/或蒸发其它流体的分离型换热器并不形成主换热器的一部分。这样的分离型换热器例如可以通过用于在升高的压力下蒸发或伪蒸发液体料流的次级冷凝器或者分离型换热器来形成。除了主交换器，某些空气分馏装置例如包含用于蒸发或者伪蒸发以液体形式由进给空气的一部分形成的高压空气流来加压的产品的次级冷凝器或者高压交换器。
相对空间术语“顶部”、“底部”、“在…之上”、“在…之下”、“上方”、“下方”、“竖直”、“水平”等涉及在常规操作中装置的空间排列。
在文章开始时提及类型的蒸馏塔系统从US 5235816已知。这种类型的装置在生产时尽可能按计划预制，并将预制部件运输至施工现场并最终相互连接。根据装置的尺寸，例如，整个双塔可以与其冷箱一起运输。如果装置的尺寸并不允许这样，那么双塔就不与冷箱和管道一起运输，如果合适的话其可以分为两个部分运输。其它塔例如氩气塔会由于分离的冷箱而产生额外的复杂性。这种塔被单独地运输至施工现场，并在现场连接至装置的其它部分，这具有相当高的复杂性。为了避免额外的低温泵，这种塔(位于其自身的冷箱内)被置于复杂的框架上。这种框架尤其会导致整个装置占地面积的增加。
EP 1108965A1的图1公开了一种氩气塔，其已被组装于低压塔中，并且其具有的顶部冷却器设置在低压塔的外部。
本发明的目的在于以最大的密实度来构建在本文开始时所提及类型的蒸馏塔系统，从而简化其构造，并开发操作特别可靠的控制方法。
这种目的通过权利要求1的技术特征来实现。据此，氩气塔顶部冷却器被设置于低压塔内。氩气排料顶部冷凝器被构建为强制流动(直通式)蒸发器；在其顶部末端，蒸发空间连接于低压塔的内部，从而使得其中产生的气体可以流至上部传质区中。在本发明中，氩气塔顶部冷凝器无需设置在氩气塔上方的中部(如果氩气塔全部或者部分组装于低压塔内)；取而代之的是，其能够利用低压塔的整个横截面。
在强制流动蒸发器中，液流在其自身压力下强制经过蒸发空间，并在其中部分蒸发。这种压力例如通过液体柱的方式在通向蒸发空间的入口管道内产生。这种液体柱的高度相应于蒸发空间内的压力降。离开蒸发空间的通过相分离的气体-液体混合物直接向前地被导向至下一个方法步骤，并且更特别地，其不被引入至冷凝器-蒸发器的液浴中，而以液体形式保持的部分会由所述冷凝器-蒸发器再次吸入(“直通式”)。
液体在强制流动蒸发器的蒸发空间内部分蒸发。将流出出口的两相混合物优选在中部传质区的顶部引入至液体分配器中。已蒸发的馏分(fraction)向上流至上部传质区内；以液体形式保持的馏分形成回流的至少一部分，用于中间传质区的至少一部分，其特别地形成低压塔的氩气部分。
原则上，如在标准的氩气方法中，强制流动蒸发器能够在只有源自高压塔的粗氧气的情况下运行。然而，在本发明的内容中，已经发现使用源自低压塔的上部传质区的液体来进料(charge)氩气塔顶部冷凝器的蒸发空间是更加有利的。出于此目的，液体收集器在上部传质区的下方连接至经由入口将液体收集器的液体引入至氩气塔顶部冷凝器的蒸发空间内的设备。由上部传质部分流出的液体在液体收集器中混合，并例如经由管道被引入至氩气塔顶部冷凝器的蒸发空间内。所述液体由此用于冷却氩气塔的顶部。其为比源自高压塔的粗氧气更加富氧的，据此能够在氩气塔顶部冷凝器中产生更小的温差以及相应更小的热力学损失。
根据本发明(“控制方法3”)，源自氩气冷凝器蒸发空间的两相混合物被引入至作用为相分离单元和液体缓冲器的容器中。在所述容器中分离出的液体被导向至下方的液体分配器中。液体体积通过位于容器底部内的固定隔膜或者相应的孔或者通过液体管道内的控制阀来控制。气体经由气体管道由容器排出。所述管道包含控制阀，蒸发空间内的压力通过所述控制阀而被调节，由此，氩气冷凝器内的温差及其性能会被调节。
原则上，除了强制流动冷凝器，还可使用降膜蒸发器，在这种情况下，向下流至上部传质部分内的所有或者几乎所有的液体会同样流经所述降膜蒸发器的蒸发空间。
DE 1272322B公开了通过圆柱形分隔壁的方式将粗氩气塔组装至低压塔内；顶部冷凝器被构建为常规液浴蒸发器，其第一部分设置于低压塔内。此外，在这里使用其它容器用于顶部冷凝器的第二部分。
优选地在本发明中，氩气冷凝器经构建以使得其产生用于氩气塔的整个回流料流。因此，不存在将被设置于低压塔外部的其它氩气冷凝器。
总的来说，氩气塔被构建为氩气排料塔。然而，如果需要氩气制品，那么其还可被构建为粗氩气塔，其中，在顶部获得耗尽氧气或者不含氧气的原始氩气制品。原始氩气产物会被导出或者经传送，以在纯氩气塔内进一步进行后处理(workup)。
在本发明的其它改进中，氩气塔或其一部分也设置于低压塔内，特别是位于中部传质区内。出于此目的，后者被构建为分隔壁(dividing wall)部分，意味着其包含竖直的分隔壁，所述竖直的分隔壁将低压塔的氩气部分(“第一传质空间”)和氩气塔(“第二传质空间”)分开。第一传质空间在向上的方向朝上部传质区以及在向下的方向朝下部传质区均为敞开的。这意味着上升的气体可以在不存在显著妨碍的情况下在底部流至第一传质空间内，并在顶部流出第一传质空间。
第二传质空间在向上的方向朝上部传质区以气密的方式密封。由下部传质区在底部流入的气体由此在第二传质空间内精馏(在氩气塔中)之后，并未被引回至低压塔内，而是经由一个或多个特定的气体管道向前被导向和/或引入至氩气塔顶部冷凝器的液化空间内。
如果仅氩气塔的一部分被设置于低压塔内，那么在低压塔的外侧，氩气塔还具有分离的粗氩气塔。
在本发明的一个实施方式中，第二传质空间在向下的方向朝下部传质区是敞开的。源自下部传质区的上升气体由此流至第二传质空间内，并在其中进行氩气-氧气的分离。
可替换地，第二传质空间在向下的方向朝下部传质区是闭合的，从而使得在第二传质空间的下部区域与在下部传质区的上部末端可以存在不同的浓度。由此在精馏领域中，氩气塔的“上部”部分可被结合至分隔壁部分中，而在下部末端连接至低压塔的氩气塔的其余部分则单独地实施。
对于全范围的氩气生产来说，可以加入分开的粗氩气塔。在这种情况下，氩气塔由粗氩气塔和第二传质空间的组合构成，在精馏领域中，可以将第二传质空间连接至粗氩气塔的上部或下部末端。在任一种情况下，氩气塔的顶部与氩气塔顶部冷凝器的液化空间流体连接。
如果低压塔不包含分隔壁部分，那么氩气塔就仅由分离粗氩气塔形成。在这种情况下，其以常规方式连接，其中氩气塔的头部与氩气塔顶部冷凝器的液化空间流体连接，并且氩气塔的底部与低压塔的中间区流体连接，特别是与位于中部和下部传质区之间的区域流体连接。当将源自液体收集器的液体引入至氩气塔顶部冷凝器的蒸发空间内的设备经构建，以将在常规操作中流至液体收集器内的液体体积的至少80摩尔％、优选至少90摩尔％引入至氩气塔顶部冷凝器的蒸发空间内时，也是有利的。
在本发明的内容中，在所述装置的常规操作中，源自液体收集器的尽可能接近100％的液体应当被引入至蒸发空间内。
优选地，粗氧气管道经提供以用于将源自高压塔底部的粗氧气引入至低压塔的上部传质区内；可替换地，粗氧气可被直接供给至蒸发空间上游的液体收集器内。在引入至低压塔内的情况下，这种本身也是常规操作的将源自高压塔的底部液体引入至低压塔内并未经由氩气塔顶部冷凝器来进行，而是直接进入上部传质区内。引入至氩气塔顶部冷凝器的蒸发空间内的液体由此是比在常规方法中更富氧的，因为在这里使用了位于上部部分下方收集的液体。
在一种实施方式中，蒸馏塔系统具有旁通(bypass)管道，用于利用在所述旁通管道内设置的控制阀，将源自位于上部传质部分下方的液体收集器的液体在下部传质部分的顶部引入至液体分配器内。
在本发明范围之外，通过这种旁通管道的方式，就可以控制氩气塔顶部冷凝器的性能。如果合适的话，控制阀为开启的，少量相对富含氮气的液体直接流至分配器内，并由此旁通通过中部传质部分。作为结果，氩气顶部冷凝器的液化空间内(或者出口处的两相混合物内)的氮气含量有所增加，平均冷凝温度下降，且作为驱动温差下降的结果，冷凝器的性能会下降(控制方法1)。
作为根据本发明进行控制的一种替换，还可以在原始氩气冷凝器上游的气流中的阀的帮助下，控制粗氩气塔中的转化。在这种情况下，气体入口被用于将源自氩气塔的气体引入至氩气塔顶部冷凝器的液化空间内，并包含控制阀(控制方法2)。
恰位于控制阀下游的气体出口可以连接至启动管道，该启动管道经构建以用于控制源自低压塔的气体的去除。
启动管道在容器壁外部连接至气体入口，并且仅当装置冷启动的时候才会使用。所述启动管道包含控制阀，控制阀在稳态运行时是闭合的。在启动时，确保在分隔壁的任一侧上均等地冷却传质空间是必要的。这样的两个部分之间大的温差应当被避免，从而由此最小化热感应应力在隔壁上的负载。启动管道要么连通于空气，要么连接至主换热器上游的不纯(impure)氮气管道。根据分隔壁右侧和左侧的温度，控制阀在启动时开启至更大或更小的角度。对于启动管道来说，在塔上不提供单独的短管是有利的；相反，启动管道直接结合至用于氩气塔顶部冷凝器的控制阀下游的气体入口内，即所述塔的外部。这种启动技术不仅可被用于本发明中，而且原则上还可用于在其上具有冷凝器的分隔壁塔部分的情况下。
本发明还涉及根据权利要求8至12、通过低温分馏空气来制备氮气的装置，所述装置包括主空气压缩机、空气预冷单元、空气清洁单元和主换热器，并且包括两个如上所述的蒸馏塔系统，这两个蒸馏塔系统均接收源自共同的主换热器的进给空气。
在这种情况下，用于双蒸馏塔系统的进给空气的至少一部分可以在主换热器中一起冷却，并在组合的压缩空气管道中由主换热器排出。组合的压缩空气管道随后分支为通向第一蒸馏塔系统的第一压缩空气子料流管道，和通向第二蒸馏塔系统的第二压缩空气子料流管道。可替换地，两个压缩空气子料流管道直接连接至主换热器。
除了主换热器，如果根据本发明的装置具有高压交换器，那么后者同样可用于两个蒸馏塔系统，这意味着源自高压交换器的处于高压下的冷压缩空气被分配于两个蒸馏塔系统之间，并且送往高压交换器的产品料流以液体形式由两个蒸馏塔系统排出、混合并被送至所述高压交换器。
出于制造的原因，主换热器在任意情况下通常由多个并联连接的模块构成。在这种情况下，将模块分为两个对称的组从而能够更好地控制主换热器就是明智的。将在第一蒸馏塔系统分馏的空气和源自相同蒸馏塔系统的相应的不纯氮气料流在这里均被引导经过第一交换器组。用于第二蒸馏塔系统的和/或源自第二蒸馏塔系统的相应料流流经第二组。剩余的料流(产品和涡轮流)均匀地分配于两个组的模块之间。
US 612892确实公开了在共同的冷箱中运行相互并排的两个并联连接的双塔；然而，这篇文献的目的在于不同地构建两个双塔。本领域技术人员在检索最大化装置生产力的方式时将不会参考这篇公开物。在任意情况下，至于多线(multistrand)系统如何能够以如上所述目的的方式进行改变，该技术人员并未获得任何建议。
双蒸馏塔系统的上游和下游的装置特别地可以由单预冷操作、单空气清洁操作和/或单换热器形成。
在所述装置中，当第一蒸馏塔系统和第二蒸馏塔系统具有相同的装配尺寸时，并且更特别地，当高压塔、低压塔和氩气塔具有相同的尺寸时，其为有利的。“相同的装配尺寸”在这里理解为是指相互之间的相应塔高和直径的差值不大于10％，特别是不大于5％。这种比较涉及第一和第二高压塔、第一和第二低压塔以及氩气塔之间的成对的相应部分。
双蒸馏塔系统中的每个均可容纳于单独的冷箱中。可替换地，第一和第二蒸馏塔系统可设置于共同的冷箱中。
在两种情况下，双蒸馏塔系统相互之间均可以单独地操作。热装置部件和主换热器以及任选存在的高压交换器例如可以一起使用。出于此目的，用于源自双蒸馏塔系统的产品的一个、多于一个或者所有的排出管道如果并不意图用于直接导出液体产物，那么它们应成对地组合成连接至主换热器冷端的组合管道，随后在共同的管道中导向至主换热器或者任选地导向至高压交换器。可替换地，双蒸馏塔系统中的每一个均具有其自身的主换热器，并且任选地具有其自身的高压换热器。
对于独立操作来说，双蒸馏塔系统中的每一个均具有单独的过冷冷却(subcooling)逆流换热器，其可以独立于另一个蒸馏塔系统的过冷冷却逆流换热器进行操作，并且更特别地，所述过冷冷却逆流换热器并不连接至源自蒸馏塔或通向另一个蒸馏塔系统的管线。
更特别地，这意味着双蒸馏塔系统为可相互独立操作的。
本发明还涉及根据权利要求13至15、通过低温分馏空气来获得氧气的方法。根据本发明的方法可以通过与单独的、数个或者所有从属权利要求装置的技术特征相应的方法特征来补充。
本发明的优点特别是在具有多线构造的特别大型的装置中证明。
本发明以及本发明进一步的细节在下文通过参考以示意的形式示出的工作实施例和附图来详细说明。附图示出：
图1所示为根据本发明具有蒸馏塔系统的完整装置的第一工作实施例，其具有双涡轮系统，
图2所示为仅具有一个制冷涡轮、一个空气喷射涡轮的第二工作实施例，
图3所示为具有加压氮气涡轮的第三工作实施例，
图4所示为具有不纯氮气涡轮的第四双塔系统，
图5所示为根据本发明具有双蒸馏塔系统(“双塔”)的第五工作实施例，
图6所示为对于具有液体旁通的氩气塔冷凝器，具有第一闭合回路控制概念的低压塔的详细视图，
图7所示为对于氩气塔内的转化，具有闭合回路控制阀的其它闭合回路控制概念，
图8所示为对于源自高压塔的粗氧气、图7的不具有单独填充物部分的改进例，
图9至11所示为具有完整氩气回收的三种实施方式，和
图12所示为衍生自图6和7的第三闭合回路控制概念。
图1示出了具有单蒸馏塔系统的装置。这种蒸馏塔系统的低压塔构造在图6中详细示出(在下文中提及的某些附图标记仅在图6中示出)。图1的工作实施例的蒸馏塔系统具有高压塔101、低压塔102、主冷凝器103和氩气塔152。
主冷凝器103在所述实施例中由三级级联蒸发器、即多层袋式蒸发器形成。塔对101/102以双塔的形式来设置。氩气塔152置于低压塔102的中部传质区130内。氩气塔顶部冷凝器155位于低压塔102内、中部传质区130的上方。低压塔102还具有上部传质区131和下部传质区132(特别是参见图6)。
图1中所示的装置具有用于环境空气(AIR)的入口过滤器302，主空气压缩机303，空气预冷单元304，空气清洁单元305(典型地由一对分子筛吸附器形成)，具有下游冷却器307的空气增压压缩机306(BAC)，以及主换热器308。主换热器308容纳于专用冷箱内，所述专用冷箱与围绕蒸馏塔系统的冷箱隔离。源自主换热器308冷端的组合的压缩空气料流100被引入至高压塔101内。
在增压压缩机306内增压至其最终压力的空气在主换热器308内液化(或者，如果其压力处于超临界，那么就是伪液化)，并经由管道311/111供给至蒸馏塔系统。
源自高压塔101的氮气料流104、114被引入至主冷却器103的液化空间内。在主冷却器103的液化空间内，液氮115由此形成，并且其至少第一部分作为第一液氮料流105导向至第一高压塔101。
源自低压塔102的液氧料流106由低压塔102的最下端传质层107的下端流出，并由此被引入至主冷凝器103的蒸发空间内。气态氧在主冷凝器103的蒸发空间形成。所述气态氧的至少第一部分被引入至第一低压塔102内，其中，其向下流至低压塔102的最下端传质层107内；根据需要，第二部分可以以气态氧产物直接获得，并在主换热器308内温热(在本实施例中未示出)。
用于低压塔102的回流液109由富氮液体120形成，其在高压塔101内由中间点排出(或者可替换地由顶部直接排出)，并在过冷冷却逆流换热器123中冷却。不纯氮气110由低压塔102的顶部排出，并作为残留气体导向经过过冷冷却逆流换热器123，并经过管道32到达主换热器308。
富氧底液料流151由高压塔101排出，并在过冷冷却逆流换热器123中冷却。在本实施例中，整个已冷却的底液153被供给至低压塔102的上部传质区。其与源自上方的回流液一起流至上部传质区的最下端部分。由这一部分流出的液体通过液体收集器133收集，并被引入至氩气塔顶部冷凝器155的蒸发空间内。氩气塔顶部冷凝器155在这里根据本发明而被构建为强制流动蒸发器。在顶部冷凝器155内蒸发的馏分回流至上部传质区131，并且以液体形式保持的馏分157被供给至低压塔102的中部传质区130内。氩气塔的富氩“产物”163以气态形式由氩气塔152或者其顶部冷凝器155移除，并通过管道164经由单独通道组引导经过主换热器308。
可替换地，可以将富氩馏分163和不纯氮气混合，并将混合物引导经过主换热器。
源自主换热器的液态空气111经由管道111在中间点供给至高压塔101。至少一部分127立即被再次排出，并经由过冷冷却器123引入，并经由管道128进入低压塔102的上部传质区内，并且特别是位于底部馏分153的进料之上。经由管道129，源自空气喷射涡轮137的气态空气还可被引入至低压塔102内，与粗氧气153处于相同的水平。
由蒸馏塔系统排出的主产物为源自主冷凝器103的蒸发空间的液态氧141，并且其经由管道14至少部分地供给至内部压缩。这就涉及通过泵15的方式将液态氧14泵送至高产物压力，在主换热器308内在高产物压力下使之蒸发或者(如果压力处于超临界的话)伪蒸发，将其温热至约为环境温度，并最终作为气态压缩氧产物GOXIC而排出。这是本实施例装置的主产物。
所述装置的另一种产物为压缩氮气，其直接由高压塔101的顶部排出(管道104、142)，经由管道42导引至主换热器308，在其中温热并最终作为气态压缩氮气产物MPGAN而获得。其一部分可被用作为密封气体。此外，在主冷凝器103内产生的液态氮的一部分143可以经由管道43供给至内部压缩(泵16)，并作为气态高压氮气产物GANIC而获得。所述装置还可以供给液体产物LOX、LIN。
在一个具体的实施例中，低压塔102内的传质元件仅由结构化填充物形成。低压塔102的氧气部分107所装备的结构化填充物的比表面积为750m2/m3，或者可替换地为1200m2/m3；在其它部分中，所述填充物的比表面积为750或500m2/m3。此外，低压塔102可以具有氮气部分，位于附图中所示的传质区的上方；其同样可装备有特别致密的填充物(例如，出于降低塔高的目的，比表面积为1200m2/m3)。与之不同的是，其能够在任意所提及部分内组合具有不同比表面积的结构化填充物。在本工作实施例中，氩气塔152独有地包含比表面积为1200m2/m3或者可替换地为750m2/m3的填充物。
在高压塔101内，传质元件仅由比表面积为1200m2/m3或者750m2/m3的结构化填充物形成。可替换地，高压塔101内传质元件的至少一部分可以由常规的蒸馏塔板形成，例如由筛板形成。
图1的系统构建为双涡轮方法，其具有中压涡轮138和空气喷射涡轮137。
图2的工作实施例与图1的不同之处在于，其被构建为单涡轮系统。其仅具有一个空气喷射涡轮，不具有中压涡轮。
图3与图2几乎相同，但是使用压缩氮气涡轮337来代替空气喷射涡轮。其对以气态形式由高压塔101的顶部排出的压缩氮气142的一部分342进行操作。
在图4中，所替代的是，涡轮料流442由高压塔101的中间点排出，并在不纯氮气涡轮437内做功膨胀。
图5示出根据本发明构造的具有双蒸馏塔系统的装置。
图5的工作实施例的第一蒸馏塔系统具有第一高压塔101、第一低压塔102、第一主冷凝器103和第一氩气塔152。第二高压塔201、第二低压塔202、第二主冷凝器203和第二氩气塔252形成在图1中所示装置中的第二蒸馏塔系统的一部分。
在本实施例中，主冷凝器103、203中的每一个均由三级级联蒸发器形成。塔对101/102、201/202以两个双塔的形式来设置。氩气塔152/252设置于低压塔102、202的中部传质区内。氩气塔顶部冷凝器155、255在各个低压塔102、202内，位于中部传质区113、213上方，并根据本发明构建为强制流动蒸发器。低压塔102、202的每个还具有位于氩气塔顶部冷凝器155、255上方的上部传质区，以及位于氩气塔152/252或中部传质区113、213下方的下部传质区。特别地，图6中清楚地示出传质区在低压塔内的设置。
双蒸馏塔系统中的每一个均独立地控制。低压塔内的压力例如可被单独地设定和控制。这种去耦还降低了总体闭合回路控制的复杂性，并允许在两个双塔内的任何制造公差可更好地补偿。
在图5中所示的装置具有用于环境空气(AIR)的入口过滤器302、主空气压缩机303、空气预冷单元304、空气清洁单元305(典型地由一对分子筛吸附器形成)、具有下游冷却器307的增压空气压缩机306(BAC)、和主换热器308。主换热器308容纳于专用冷箱内，其与围绕蒸馏塔系统的冷箱隔离。源自主换热器308冷端的组合的压缩空气料流99被分支为第一压缩空气子料流100和第二压缩空气子料流200。第一压缩空气子料流100被引入至第一高压塔101内，并且第二压缩空气子料流200被引入至第二高压塔201内。
在增压压缩机306内增压至其最终压力的空气在主换热器308内液化(或者如果其压力为超临界的，那么会被伪液化)，并经由管道311供给至蒸馏塔系统，并在其中分支为料流111和112。
源自第一高压塔101的第一氮气料流104、114被引入至第一主冷凝器103的液化空间内。液氮115在第一主冷凝器103的液化空间内制成，并且其至少第一部分作为第一液氮料流105被导向至第一高压塔101。
源自第二高压塔201的第二氮气料流204、214被引入至第二主冷凝器203的液化空间内。液氮215在第二主冷凝器203的液化空间内制成，并且其至少第一部分作为第二液氮料流205被导向至第二高压塔201。
源自第一低压塔102的第一液氧料流由第一低压塔102的最下端传质层107的下端流出，并由此被引入至第一主冷凝器103的蒸发空间内。气态氧于第一主冷凝器103的蒸发空间内形成。所述气态氧气的至少第一部分作为第一氧气料流引入至第一低压塔102内，其中，其由下方流至第一低压塔102的最下端传质层107内；根据需要，第二部分可以直接作为气态氧产物获得，并在主换热器308内被温热。
源自第二低压塔202的第二液氧料流由第二低压塔202的最下端传质层207的下端流出，并由此被引入至第二主冷凝器203的蒸发空间内。气态氧于第二主冷凝器203的蒸发空间内形成。所述气态氧的至少第一部分作为第二氧气料流被引入至第二低压塔202内，其中，其由底部流至第二低压塔202的最下端传质层207内；根据需要，第二部分可以直接作为气态氧产物获得，并在主换热器308(未示出)内被温热。
用于两个低压塔102、202的回流液109、209中的每一个均由富氮液体120、220形成，所述富氮液体120、220在两个高压塔101、201内从中间点(或者可替换地直接从顶部)排出，并在过冷冷却逆流换热器123、223内被冷却。不纯氮气110、210从两个低压塔102、202的顶部排出，并在每种情况下作为残留气体被导向经过一个过冷冷却逆流换热器123、223，并经由共同的管道32被导向至主换热器308。
一个富氧底液料流151、251从两个高压塔101、201的每一个排出，并在各自的过冷冷却逆流换热器123、223中冷却。在本实施例中，整个已冷却的底液153、253被供给至低压塔102、202的上部传质区。其与源自上方的回流液一起流至上部传质区的最下端部分内。由所述部分向下流动的液体通过液体收集器133、233来收集，并被引入至氩气塔顶部冷凝器155、255的蒸发空间内。氩气塔顶部冷凝器155、255在这里根据本发明被构建为强制流动蒸发器。在顶部冷凝器155、255内已蒸发的馏分流回至上部传质区131、231内，并且以液体形式157、257保持的馏分被供给至低压塔102、202的中部传质区130内。氩气塔的富氩“产物”163、263以气态形式由氩气塔152、252或其顶部冷凝器155、255收回，并经由管道164经过分离通道组，导向通过主换热器308。
可替换地，可以将富氩馏分163、263和不纯氮气110、210混合，并传导混合物经过主换热器。
源自主换热器的液体或者超临界空气311经由管道111、211在中间点供给至高压塔101、201。至少一部分127、227会立即再次收回，并被引导经过过冷冷却器123、323，并经由管道128、228进入低压塔102、202的上部传质区内，位于底部馏分153、253供料的上方。源自空气喷射涡轮137的气态空气也经由管道129、229而被引入至低压塔102、202内，与粗氧气153、253处于相同的水平。
由蒸馏塔系统排出的主产物为液氧141，其源自主冷凝器103、203的蒸发空间，并且其被组合和经由管道14至少部分地供给至内部压缩。这涉及通过泵15的方式将液氧14泵至高产物压力，在主换热器308内、在所述高产物压力下使之蒸发或者(如果其压力为超临界的)伪蒸发，温热至约为环境温度，并最终作为气态压缩氧气产物GOXIC而被排出。这是本工作实施例装置的主产物。
源自所述装置的另一种产物为压缩氮气，其直接由高压塔101、201的顶部(管道104、142和204、242)排出，经过管道42一起被传导至主换热器308，在其中被温热并最终作为气态压缩氮气产物MPGAN而获得。其一部分可被用作为密封气体。此外，在主冷凝器103、203中制造的液氮的一部分143、243可以经由管道43而被供给至内部压缩(泵16)，并作为气态高压氮气产物GANIC而获得。
所述装置还可以供给液体产物LOX、LIN。这些可以如所示的由每个蒸馏塔系统单独地移除。
在一个特别的实施例中，两个低压塔102、202内的传质元件仅由结构化填充物形成。两个低压塔102、202的氧气部分107、207所装备的结构化填充物的比表面积为750m2/m3，或者可替换地为1200m2/m3；在其它部分中，所述填充物的比表面积为750或500m2/m3。此外，两个低压塔102、202可以具有氮气部分，其位于在附图中所示的传质区的上方；其同样可装备有特别致密的填充物(例如，出于降低塔高的目的，比表面积为1200m2/m3)。与之不同的是，可以在任意所提及部分内组合具有不同比表面积的结构化填充物。在本工作实施例中，氩气塔152、252仅包含比表面积为1200m2/m3或者可替换地为750m2/m3的填充物。
在高压塔101、201内，传质元件仅由比表面积为1200m2/m3或者750m2/m3的结构化填充物形成。可替换地，两个高压塔101、201内传质元件的至少一部分可以由常规蒸馏塔板形成，例如由筛板形成。
图5的系统与图1相类似地构建为双涡轮方法，具有中压涡轮138和空气喷射涡轮137。可替换地，在图5的具有双蒸馏塔系统的系统中，其还可以将使用图2、3或4的涡轮构型。
双蒸馏塔系统中的每一个均单独地控制。低压塔内的压力例如可被分开地设定和控制。这种去耦还降低总体闭合回路控制复杂性，并允许在两个双塔内的任何制造公差更好地得到补偿。
参考图6所示的细节，现在将说明氩气塔和氩气塔顶部冷凝器及其闭合回路控制的确切功能。所述细节可用于任意前述的工作实施例。
图6仅示出双塔101、102的一部分，其由高压塔101的上端延伸至低压塔的上部传质区131的第二填充物层，并且更特别地，其包含氩气塔152和氩气塔顶部冷凝器155。可以理解的是，图6的工作实施例还用于其它的双塔系统，例如低压塔与高压塔并排设置和/或主冷凝器设置于低压塔外部的那些。
在主冷凝器103内，液氧被蒸发，其由下部传质区132向下流动，或者在低压塔的底部由液浴65吸入；与之相反，源自高压塔101顶部的气态氮被蒸发。(氮气管道在图6中未示出。)
液体收集器和分配器在图6中并未示出，除以下示出的外，收集器133位于上部传质区131和氩气塔顶部冷凝器155之间，两个液体分配器44、420位于第一和第二传质空间134、135的顶部，液体分配器45位于底部传质区132的顶部。对于其余的，图6为非常示意性的，并且通常不应当被认为是按尺寸的。
低压塔的中部传质区130由竖直的扁平分隔壁136以气密的方式分隔为第一传质空间134和第二传质空间135。第一传质空间134在向上的方向朝上部传质区131敞开，并在向下的方向朝下部传质区132敞开，意味着源自下部传质区132的气体可以流至中部传质区131的第一传质空间134内，源自第一传质空间134的气体可以向上流出，进入低压塔的上部传质区内。第一传质空间134实现低压塔的氩气部分的功能，即传质区的功能，在常规装置中，其恰位于氩气转变之上，包含氩气的馏分将通过其而被传至外部的粗氩气塔或者氩气塔。
形成氩气塔152的第二传质空间135还同样在向下的方向朝下部传质区132敞开；上升气体流出低压塔的下部传质区132，并以这种方式进入第二传质空间135。然而在其上端，第二传质空间135以气密的方式与上部传质区131密封。向上方向的密封通过水平板36来实现-除了引导经过其的管道37、37、41以外-所述水平板36为气密的。在上部传质区131和中部传质区130之间的是氩气塔顶部冷凝器155，其被构建为冷凝器-蒸发器，在这里根据本发明被构建为强制流动蒸发器。在本工作实施例中，其由单板式换热器模块构成。可替换地，其还可以由并联设置的两个或更多个板式换热器模块形成。氩气塔顶部冷凝器155的液化空间与氩气塔152的顶部经由气体管道37和液体管道62、41流体连接。在这种情况下，源自氩气塔152的顶部气体经由气体管道37由第二传质空间135的上端流至液化空间，并在其中至少部分地液化。所产生的液体经由管道62排出，经由管道41回收至第二传质空间135内，并通过液体分配器420的方式作为回流液在第二传质空间135的横截面上分配至氩气塔。以气态形式保持的部分163由低压塔102的容器排出，并如在图1至5中所示的进一步处理。
由中部传质区130的两个传质空间134、135流出的液体在液体收集器(未示出)内收集。所述液体向前流至液体分配器45，所述液题分配器45将液体分配于整个塔的截面之上，并将其施加至下部传质区132。
类似于图1，源自高压塔101底部的粗氧气153被引入至上部传质区131的两个填充物部分之间。空气料流129在相同的位置引入，其已在先膨胀至约为低压塔的压力，以此来执行作业(参见图1、2和5中的空气喷射涡轮137)。
此外，液态空气128被引入至上部传质区131内。实际上，源自上部传质区131的所有液体均收集于液体收集器133内，并通过管道71引入至氩气塔顶部冷凝器155的蒸发空间内。这具有两个优点：
-经由管道71流经蒸发空间的液体量为特别大的。在氩气塔顶部冷凝器中，优选35％至55％、例如约45％的该液体量被蒸发。
-这种液体具有相对高的氧含量，由此具有相对高的蒸发温度。这使得能够实现特别小的温差；在三个特定的实施例中，其为0.8K、1.0K或1.5K。这使得冷凝器内的热力学损失能够保持为特别小。
对于强制流动蒸发器的效率来说，由此的高度过量的液体为显著重要的。
两相混合物经由管道73从冷凝器155的蒸发空间显现。液体组分L在第一传质空间134的顶部流至液体分配器44内。蒸发的组分V向上回流至上部传质部分131内。
氩气塔顶部冷凝器155的闭合回路控制通过闭合回路控制方法1在图6的工作实施例中实施，其需要旁通管道49/50以及闭合回路控制阀48。以此方式，氩气塔顶部冷凝器155的性能得到控制。
少量相对富氮的液体流至分配器45内，提高上升流出下部部分132的蒸气中的氮气含量，并据此还提高在整个氩气塔152内以及额外地在氩气塔顶部冷凝器155的液化空间内的氮气含量。由此，在其中设置的这种控制管道和阀能够控制冷凝器性能的降低。在本工作实施例中，在上部传质区131的下端从收集器133出来相对富氮的液体。
闭合回路控制阀48在稳态运行时是闭合的，或者仅非常少量的液体流动经过它。在偏离稳态操作时，例如在负载变化时，通常小于5％的源自液体腔室133的全部液体71/49会流经旁通管道，并在任意情况下均小于15％。
可替换地，其它闭合回路控制方法可采用，其中之一在下文详细描述。
图7示出一种替换方式的闭合回路控制方法2，在通向氩气塔顶部冷凝器155的液化空间的气体入口37内具有闭合回路控制阀700。所述阀可被用于通过使用恰当的冷凝温度来调节冷凝压力。这会直接影响冷凝器155内的驱动温差，并相应地还影响冷凝器性能或者氩气塔152内的转化。所述阀可以通过氩气塔内的压力差来控制(PDIC＝压力差指示和控制，未示出)。
图8与图7的不同之处仅在于在由高压塔的底部引入原始液氧153和位于上部传质区131下端的液体收集器133之间缺少传质区。换句话说，原始液氧被直接引入至液体收集器133内，并据此进入冷凝器155的蒸发空间内。
在图12中示出闭合回路控制方法3。在这里，源自氩气冷凝器155的蒸发空间的两相混合物被引入至额外的容器1250内。经由管道1251，气态组分V返回至低压塔，从而使得其能够作为上部传质部分131内的上升蒸气。液体组分L经由管道1254在(氩气部分的)第一传质空间134的顶部被引入至液体分配器44内。借助于闭合回路控制阀1252，氩气冷凝器155的蒸发空间内的压力以及由此其性能可被调节。
液体管道1254还同样可以具有闭合回路控制阀。可替换地，液流通过在容器1250底部例如开口形式的固定隔膜来控制。其尺寸应为这样的，即根据容器内的压力，容器中的液位可以在容器上限和下限之间变化。
图9为基于图2的，但是其完全回收氩气，其中，源自氩气塔的顶部产物963中的氧含量例如下降至0.1至100ppm。基本上不含氧气的氩气963随后会被供给至纯氩塔，在所述纯氩塔中进行氩气-氮气分离。出于低氧含量是所必要的这一目的，在分隔壁部分135内的几个理论塔板是不够的。因此，使用几乎标准长度的粗氩气塔900，利用低压塔102的分隔壁部分内的第二传质空间135作为原始氩气精馏的最上端传质区。出于此目的，第二传质空间135必须在其下端例如通过半圆形板气密密封。在所述板的下方，包含氩气的气体901由低压塔102排出，并供给至粗氩气塔900的底部。源自粗氩气塔900的底液902以相反的方向在低压塔102内的相同位置传导。粗氩气塔的顶部经由管道903(用于气体)和904(用于液体)与第二传质空间135的下端流体连接。如根据图1至7所知的，其上端连接至氩气塔顶部冷凝器155。
在图10的工作实施例中，第二传质空间135在底端敞开，并且在这一方面，与图1至5相类似地进行操作。然而，其顶部并未直接连接至氩气顶部冷凝器155，而是经由管道905和906连接至粗氩气塔900的底部。粗氩气塔的顶部经由管道907和908与氩气塔顶部冷凝器的液化空间流体连接。
图11示出在低压塔内不具有分隔壁部分的工作实施例。氩气塔在这里仅由单独的粗氩气塔900构成，类似于图10，其顶部连接(907、908)至氩气塔顶部冷凝器155。类似于图9，图11的粗氩气塔900的底部连接(901、902)至低压塔102内恰当的中间点。

Claims (16)

1.通过低温分馏空气来获得氧气的蒸馏塔系统，包括- 高压塔（101；201）和低压塔（102；202），- 主冷凝器（103；203），其被构建为冷凝器-蒸发器，主冷凝器的液化空间与高压塔的顶部流体连接（104、105、114、115；204、205、214、215），- 并且包括氩气塔（152；252），其- 与低压塔（102）内的中间点流体连接，并且- 具有排出富氩料流的设备（37，163），和- 氩气塔顶部冷凝器（155、255），其被构建为冷凝器-蒸发器，并与氩气塔（152、252）的顶部流体连接（37、62、41），- 所述低压塔具有上部传质区（131），下部传质区（132）和中部传质区（130），- 中部传质区（130）具有至少一个第一传质空间（134），其在向上的方向朝上部传质区（131）敞开，并在向下的方向朝下部传质区（132）敞开，其特征在于，- 上部传质区（131）在其底端具有液体收集器（133），- 第一传质空间（134）在其顶部具有液体分配器（44），- 氩气塔顶部冷凝器（155、255）设置于低压塔（102）内，位于上部和中部传质区之间，并且其中，- 氩气塔顶部冷凝器（155）被构建为强制流动蒸发器，其具有蒸发空间，所述蒸发空间在其底端具有入口并且在其顶端具有出口，并且所述出口连接至第一传质空间（134）的液体分配器（44），所述系统进一步包括- 在上部传质区（131）的下方、将源自液体收集器（133）的液体引入至氩气塔顶部冷凝器（155）的蒸发空间的入口内的设备（71），和-容器（1250），连接至氩气冷凝器（155）的蒸发空间的出口以及容器（1250）的入口的两相管道（73），用于由容器（1250）排出气体并包含控制阀（1252）的气体管道（1251），和在中部传质部分（152）的顶部将液体由容器（1250）引入至液体分配器（44）内的液体管道（1254）。
2.根据权利要求1所述的蒸馏塔系统，其特征在于，氩气冷凝器（155）经构建以使得其产生用于氩气塔的整个回流料流。
3.根据权利要求1或2所述的蒸馏塔系统，其特征在于，氩气塔被构建为粗氩气塔，并具有70至180个理论塔板。
4.根据权利要求1或2所述的蒸馏塔系统，其特征在于，- 中部传质区（130）被竖直的分隔壁、特别是扁平分隔壁（136）以气密的方式分隔为第一传质空间（134）和第二传质空间（135），- 其中，第二传质空间（135）在向上的方向朝上部传质区（131）以气密的方式（36）密封，并形成氩气塔（152）的至少一部分，- 其中，第二传质空间（135）特别是在向下的方向朝下部传质区（132）敞开。
5.根据权利要求4所述的蒸馏塔系统，其特征在于，氩气塔由第二传质空间（135）和分开的粗氩气塔（900）的组合形成，并且，特征还在于以下情形的任选其一- 分开的粗氩气塔（900）的顶部与氩气塔顶部冷凝器（155）的液化空间流体连接（907、908），并且- 分开的粗氩气塔（900）的底部特别地与第二传质空间（135）的顶部流体连接（905、906），或者- 分开的粗氩气塔（900）的顶部与第二传质空间（135）的下端流体连接（903、904），并且第二传质空间（135）特别地在朝下部传质区（132）的下端（901）闭合。
6.根据权利要求1或2所述的蒸馏塔系统，其特征在于，所述氩气塔仅由分开的粗氩气塔（900）形成；并且- 氩气塔的顶部与氩气塔顶部冷凝器（155）的液化空间流体连接（907、908），并且氩气塔的底部与低压塔（102）的中间区域、特别是与中部和下部传质区（130、132）之间的区域流体连接（901、902）。
7.根据权利要求1或2所述的蒸馏塔系统，其特征在于，将液体由液体收集器（133）引入至氩气塔顶部冷凝器的蒸发空间内的设备（71）经构建，以用于将至少80摩尔%、特别是大于90摩尔%体积的在正常运行时流至液体收集器内的液体引入至氩气塔顶部冷凝器的蒸发空间内。
8.根据权利要求1或2所述的蒸馏塔系统，其特征在于，粗氧气管道（153）用于将源自高压塔（101）底部的粗氧气引入至低压塔（102）的上部传质区（131）内。
9.通过低温分馏空气来制造氧气的装置，包括- 主空气压缩机（303），用于压缩进给空气，
- 空气预冷单元（304），用于预冷在主空气压缩机内压缩的进给空气，- 空气清洁单元（305），用于清洁预冷却的进给空气，- 主换热器（308），用于冷却已清洁的进给空气，
- 第一蒸馏塔系统，根据权利要求1至7任一项所述来构建，- 第二蒸馏塔系统，根据权利要求1至7任一项所述来构建，- 第一压缩空气子料流管道（100），用于将已冷却的进给空气由主换热器（308）引入至第一蒸馏塔系统的高压塔（101）内，并且包含- 第二压缩空气子料流管道（200），用于将已冷却的进给空气由主换热器（308）引入至第二蒸馏塔系统的高压塔（201）内。
10.根据权利要求9所述的装置，其中主换热器（308）被分为第一组换热器模块和第二组换热器模块，所述换热器模块为并联连接的，主换热器经设计为使得在所述装置运行时，
- 用于第一蒸馏塔系统的进给空气仅经过第一组，- 用于第二蒸馏塔系统的进给空气仅经过第二组，- 第一不纯氮气料流（110）由第一低压塔（102）排出，并完全引入至第一组内，并且- 第二不纯氮气料流（210）由第一低压塔（202）排出，并完全引入至第一组内，并且
其中，所述装置具有第一总体产物管道（14、42、43），用于组合源自第一蒸馏塔系统的第一产物料流（114、142、143）和源自第二蒸馏塔系统的第二产物料流（214、242、243），以及在主换热器的第一组和第二组之间分开源自总体产物管道的总体产物料流的设备。
11.根据权利要求9或10所述的装置，其中，第一蒸馏塔系统和第二蒸馏塔系统具有相同的组装尺寸。
12.根据权利要求9或10所述的装置，其特征在于，对应于双蒸馏塔系统中的每一个的一个单独的过冷冷却逆流换热器（123；223），其中的一个换热器可相对于另一个蒸馏塔系统的过冷冷却逆流换热器独立地操作，并且其特别地未连接至源自蒸馏塔或者通向另一个蒸馏塔系统的管线。
13.根据权利要求9或10所述的装置，其特征在于，双蒸馏塔系统相互之间能够独立地操作。
14.通过使用蒸馏塔系统低温分馏空气来获得氧气的方法，包括- 高压塔（101；201）和低压塔（102；202），- 主冷凝器（103；203），其被构建为冷凝器-蒸发器，主冷凝器的液化空间与高压塔的顶部流体连接（104、105、114、115；204、205、214、215），- 并且包括氩气塔（152；252），其- 与低压塔（102）内的中间点流体连接，并且- 具有排出富氩料流的设备（37，163），和- 氩气塔顶部冷凝器（155、255），其被构建为冷凝器-蒸发器，并与氩气塔（152、252）的顶部流体连接（37、62、41），其中- 进给空气（100；200）被引入至高压塔（101；201）内，并且- 氧气产物料流（14，GOXIC）由低压塔（102；202）排出，
- 低压塔具有上部传质区（131）、下部传质区（132）和中部传质区（130），- 中部传质区（130）具有至少一个第一传质空间（134），其在顶部朝上部传质区（131）敞开，并在底部朝下部传质区（132）敞开，其特征在于，- 上部传质区（131）在其底端具有液体收集器（133），-第一传质空间（134）在其顶部具有液体分配器（44），- 氩气塔顶部冷凝器（155、255）设置于低压塔（102）内，位于上部和中部传质区之间，- 氩气塔顶部冷凝器（155）被构建为强制流动蒸发器，其具有蒸发空间，所述蒸发空间在其底端具有入口并且在其顶端具有出口，并且所述出口连接至第一传质空间（134）的液体分配器（44），- 富氩馏分（163；263）由氩气顶部冷凝器（155；255）的液化空间排出，- 将源自设置于上部传质区（131）下方的液体收集器（133）的液体引入至氩气塔顶部冷凝器（155）的蒸发空间内，并且其特征在于，- 对氩气塔顶部冷凝器（155）通过由氩气冷凝器（155）的蒸发空间收回两相混合物（73）并将其引入至容器（1250）内、经由控制阀（1252）从容器（1250）排出气体料流（1251）、以及从容器（1250）排出液体料流（1254），并在中部传质部分（152）的顶部将其引入至液体分配器（44）内来控制。
15.根据权利要求14所述的方法，其特征在于，至少80摩尔%、特别是大于90摩尔%体积的流入液体收集器（133）内的液体被引入至氩气塔顶部冷凝器的蒸发空间内。
16.根据权利要求14或15所述的方法，其特征在于，通过液体收集器（133）从上部传质区（131）收集的整个回流液被引入至氩气塔顶部冷凝器（155）的蒸发空间内。
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