CN100420908C - 利用空气低温蒸馏制取稀有气体和氧气的方法和装置 - Google Patents

利用空气低温蒸馏制取稀有气体和氧气的方法和装置 Download PDF

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CN100420908C
CN100420908C CNB038209675A CN03820967A CN100420908C CN 100420908 C CN100420908 C CN 100420908C CN B038209675 A CNB038209675 A CN B038209675A CN 03820967 A CN03820967 A CN 03820967A CN 100420908 C CN100420908 C CN 100420908C
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destilling tower
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L·若瓦尼
F·茹达斯
B·索尼耶
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

本发明涉及利用低温空气蒸馏制取稀有气体和氧气的方法和装置。在包括至少一个中压蒸馏塔(K01)，一个低压蒸馏塔(K02)和一个辅助蒸馏塔(K05)的蒸馏塔系统内制取稀有气体和氧气的方法包括：在中压蒸馏塔的中间层抽出中间排放流体(LR1)，将其导入低压蒸馏塔；从中压蒸馏塔中导出排放流体(LR2)，该流体富含氧，将其导入辅助蒸馏塔的罐；从低压蒸馏塔的顶部导出富含氮的排放流体(WN2)；从低压蒸馏塔的罐中导出富含氧的液态排放流体(CL)，形成产品，可在蒸发阶段后将流体导出以制成气态产品；并从辅助蒸馏塔中导出富含氪和氙的富氧排放流体(PURGE)，使含有至少78%mol氮的液态流体(5，15)作为回流返回到辅助蒸馏塔中。

Description

利用空气低温蒸馏制取稀有气体和氧气的方法和装置
本发明涉及利用空气蒸馏方式来制取氧气和稀有气体的方法和装置。
通常用位于复式空气分离塔主蒸发器处的驱气来制取稀薄的氪/疝混合物(参见“Tieftemperaturtechnik”，作者：Hausen和Linde，1985年版，337-340页；“气体的分离”，作者：Isalski，1989年版，96-98页)。然后将氧产物从蒸发器上方几级处的低压蒸馏塔中抽出。如果氧以气态形式抽出，则这种设置导致大量的氪馏分存在于空气中而所有的氙都有待回收。
然而，在利用被称之为“泵送”的方法来制取氧的装置中，存在于空气中的大约30％的氪和氙“流失”于从低压蒸馏塔中抽出的液态氧中。
DE-A-2603505公开了一种空气分离装置，在该装置中在净化塔内制取含有氪和氙的流体，所述净化塔以从中压蒸馏塔排出的两股富液为原料，这两股富液在净化蒸馏塔中的再沸腾是由蒸发器提供的，该蒸发器以来自氩蒸馏塔的塔顶气为原料。
本发明的一个目的是提供一种提高下述装置氪和氙产量的系统，所述装置为利用泵送和蒸发液态氧的方式来制取气态氧的装置(或者更一般地说该装置为从低压蒸馏塔的底部抽出大量液氧的装置)。而且，优选该装置也制取氩。
本发明的另一个目的是发明一个高含氧量和整体净化的主蒸发器，并因此极大的降低碳氢化合物/杂质的浓度(泵送“oxytonne”的好处)，这一点与常规制取稀薄氪和氙的方案不同。
本发明的主题之一是在蒸馏塔系统中通过蒸馏制取氧气和稀有气体的方法。该蒸馏塔系统包括至少一个中压蒸馏塔，一个低压蒸馏塔和一个辅助蒸馏塔。在此方法中：
i)将至少一股被冷却和提纯的空气流送至中压蒸馏塔，在中压蒸馏塔中将上述空气流分离；
ii)至少将第一股富氮流体从中压蒸馏塔中抽出，并且至少将这股流体的一部分直接或者间接地导入低压蒸馏塔中；
iii)从中压蒸馏塔的中间层将中间流体抽出；
iv)将与中间流体相比富含氧的第二股富氧流体从中压蒸馏塔的底部抽出并将其导入辅助蒸馏塔的底部；
v)将富含氮的流体从低压蒸馏塔的顶部抽出；
vi)将富含氧的液态流体作为产品从低压蒸馏塔抽出，或者在蒸发阶段后将流体抽出以制成气态的产品；并且
vii)将第三股富氧流体从辅助蒸馏塔中抽出，与第二股富氧的流体相比这股流体还富含氪和氙，
其特征在于，将中间流体导入低压蒸馏塔中，并且一股含有至少78mol％氮的液态流体作为回流返回到辅助蒸馏塔中。
优选地，作为回流返回辅助蒸馏塔中的液态流体是液化空气和/或与导入中压蒸馏塔中的液化空气流相比富含氮的液体。
根据可选择的方案：
-借助从氩蒸馏塔中导出的塔顶气体对辅助蒸馏塔的底部进行加热；
-所述的液化空气和/或与空气相比富含氮的液体是通过与来自低压蒸馏塔底部的富含氧的液态流体进行热交换而制成的，或者可选择在压缩阶段以后进行上述热交换；
-富氮流体包含至少80mol％的氮；
-液化空气不是来自中压蒸馏塔，被导入辅助蒸馏塔顶部的液态流体的含氮量高于中间流体；将制取的至少10％的氧以液态形式从低压蒸馏塔中抽出。
本发明的另一个主题是在蒸馏塔系统中通过蒸馏来制取氧气和稀有气体的装置，该蒸馏塔系统包括：至少一个中压蒸馏塔，一个低压蒸馏塔和一个辅助蒸馏塔。所述装置包括：
i)将至少一股被冷却和提纯的空气流送至中压蒸馏塔的机构，在中压蒸馏塔中将上述空气流分离；
ii)至少将第一股富氮流体从中压蒸馏塔中抽出的机构，和将至少一部分这股流体直接或者间接地导入低压蒸馏塔中的机构；
iii)将富含氮的流体从低压蒸馏塔的顶部抽出的机构；
iv)将中间流体从中压蒸馏塔的中间层抽出的机构；
v)将与中间流体相比富含氧的第二股富氧流体从中压蒸馏塔的底部送至辅助蒸馏塔底部内的机构；
vi)使液态流体作为回流返回辅助蒸馏塔的机构；
vii)将富氧的液态流体作为产品从低压蒸馏塔底部抽出的机构，或者可选择在蒸发阶段后将流体抽出以制成气态的产品；和
viii)将与第二股富氧流体相比还富含氪和氙的第三股富氧流体从辅助蒸馏塔中抽出的机构；
其特征在于上述使液态流体作为回流返回辅助蒸馏塔的机构用于输送液化空气或与导入中压蒸馏塔中的液态空气流相比富含氮的液态流体作为回流，且该装置还包括将中间流体从中压蒸馏塔送到低压蒸馏塔的机构。
根据所选择的其他方案，该装置包括：
-净化蒸馏塔，将第三股富氧流体导入净化蒸馏塔顶部的机构，和在塔中至少下行几个理论级将第四股富氧流体抽出的装置，第四股富氧流体为富含氪和氙的混合物；和
-热交换管，在该管中，液化空气和/或与空气相比富含氮的液体通过与低压蒸馏塔底部导出的富含氧的液态流体进行热交换制成，或者可选择在加压阶段以后进行上述热交换。
现在将参照图1-9来对本发明进行说明，这些图是表示本发明所述装置原理的示意图。
在图1所示的实施例中，复式空气分离塔包括中压蒸馏塔K01和低压蒸馏塔K02，这两个蒸馏塔通过主蒸发器E02热连接，该蒸发器用于通过与来自蒸馏塔K02底部的氧进行热交换，使至少部分蒸馏塔K01高处的气态氮冷凝。
氩蒸馏塔K10以来自低压蒸馏塔K02的富氩流体7为原料，富氩流体9从氩蒸馏塔K10返回到低压蒸馏塔K02中。将富含氩的流体ARGON从氩蒸馏塔K10的顶部抽出。
在泵送装置中，部分干燥和脱碳的空气在空气增压机(图中未示出)中被压缩到足以允许任意泵送的氧蒸发的压力。接着这些空气在主热交换管中冷凝(图中未示出)。在主热交换管的冷端，这股流体在阀或者水轮机中膨胀。然后可以分别在中压蒸馏塔K01、低压蒸馏塔K02和辅助蒸馏塔K05之间将这股流体的液相LIQ AIR分配成流体1、3和5。该液体包含78％mol的氮。
中压空气MP AIR的另一部分在主热交换管中冷却，并被导入中压蒸馏塔K01的底部。
本发明的原理是在富液RL2中收集氪和氙，接着在辅助蒸馏塔K05中处理该富液。
因此两股富液RL1和RL2都从中压蒸馏塔K01中抽出，即从中压蒸馏塔底部上方几级的中间层抽出含有少量氪和氙的“常规”富液RL1，和富集氪和氙的底部富液RL2。在使这股“常规”富液RL1过冷后接着可以将其送到蒸馏塔K02中。
在底部富液RL2过冷(图中未示出)后，将其导入K10的氩混合物冷凝器E10中。为了在氩混合物冷凝器中提浓氪和氙，在上述装置上方设置了多个级。上述组件构成蒸馏塔K05。该塔的部分回流是由液态空气LIQ AIR中没有流入蒸馏塔K01的部分5在过冷后提供的，回流的另一部分由中间流体11的部分15提供，通常经过管道13将所述中间流体导入蒸馏塔K02中，并且该流体包含至少80％mol的氮。将气体16从蒸馏塔K05回流注入点下方的中间层抽出，而且该气体组成气化的富液。接着该气体将在蒸馏塔K02中再循环。来自蒸馏塔K05的顶部气体WN2’组成离开冷箱的废气WN2的一部分。
来自混合物冷凝器E10的驱气PURGE包含大部分存在于空气中的氪和氙，这些氪和氙已经由蒸馏塔K01和K05处理过。为了集取稀有气体，而使这股流流入一个装置中。例如，可以使这股流体流入稀薄的氪/氙混合物蒸馏塔(K90)中。该塔的塔底包括待受益的产品。从蒸馏塔K90中出来的蒸汽17被送回蒸馏塔K05的底部。
形成部分MP AIR的空气流对蒸馏塔K90进行加热。因而可以将形成的液化空气送回中压蒸馏塔K01和/或低压蒸馏塔K02。
液态氧LO产品作为残留物从蒸馏塔K02抽出，与主蒸发器E02在同一平面。因而和传统制取氪和氙的方案的不同：此主蒸发器被整体净化。
优选采用泵对液态氧LO加压，然后液态氧在热交换管或者专用的蒸发器中通过与压缩空气进行热交换而蒸发，或者可选择地，可以利用氮循环使液态氧LO蒸发。
接下来的附图示出由图1衍变而成的几个不同的实施例。与图1相同的元件不再重复说明。
如图2所示的实施例，从主热交换管出来的所有液态空气LIQ AIR都被导入蒸馏塔K01中，将以液态形式的中间流体1’从蒸馏塔K01中抽出(最好在引入液态空气的平面或者高于这个平面的水平处)。接着，在过冷后，将上述中间流体在蒸馏塔K02和蒸馏塔K05之间分成两股流体3和5。将包括至少80％mol氮的流体11导入蒸馏塔K05的顶部。
在图3中，在图2的基础上，将蒸馏塔K05的一个顶部部分去除。。这个蒸馏塔的回流仅由液态空气5，最好是过冷的液态空气，提供。该液态空气是通过蒸发在热交换管中加压的液态氧LO来制取的。所有的低品味液体13都被导入低压蒸馏塔K02中。
另外，所有出现在热交换管出口的液态空气LIQ AIR都可以从蒸馏塔K01中(最好是在引入液态空气的点处)抽出，在过冷之后接着将该空气在蒸馏塔K02和蒸馏塔K05之间进行分配，如图4所示。
在图5和图6中，在图3和图4的基础上，将从蒸馏塔K05出来的废气WN2’在低于低品味液体13的注入点处送回蒸馏塔K02中。
在图7中，在图5的基础上，将流体16省略并用废氮流WN2’取代，这股废氮流从辅助蒸馏塔K05的顶部导入低压蒸馏塔的中部。
在上面所述的所有图中(图1-7)，可以用传统的方案连接上述装置来制取氪和氙。而要这么做，需要安装几个级来富集蒸馏塔K02中的残留物。在主蒸发器E02上方的几级处将液态氧LO制取出来。在与主蒸发器E02齐平的平面处将驱气21抽出。该驱气包括蒸馏塔K02中的70％mol的氪和全部的氙。将这股流体送入蒸馏塔K90中以回收稀有气体。
图8示出一个实施例。
在上面所示的所有图中(图1-8)，提到了同时生产氩。然而，也可以将上述装置安装到不生产氩的设备中。例如，安装热交换器来冷凝从蒸馏塔K02中抽出的部分气体7就足够了。这股气体一旦液化，就将其(9)送入蒸馏塔K02中。这使其将在蒸馏塔K05中再沸腾。
图9示出一个实施例。
在有鼓风式涡轮机的具体方案中，将鼓送的空气送入蒸馏塔K05的底部以回收流体中含有的氪和氙。
另外，图1-9所示的方案也可以包括蒸馏装置，例如Etienne塔(一种可以在中压和低压之间的压力下运行并以富液为原料的蒸馏塔)。在这种情况下，就可以依据相同的原理，通过将图1-9所示的氩蒸馏塔K10换成Etienne塔，来改进Etienne蒸馏塔的顶部冷凝器，这种相同的原理为：在冷凝器的上方增加几个级来收集稀有气体。
不将所有的液态空气送至辅助蒸馏塔的顶部，而是此蒸馏塔的入口处仅引入能够确保氪和氙在K05底部富集所需的L/V(蒸馏部分中下降的液体流速和增大的气体流速的比值)，从而限制K05底部氧气浓度的气流量，这或许也是有利的。将剩余的液态空气流和富液RL2一起导入辅助蒸馏塔的底部。

Claims (11)

1. 一种在蒸馏塔系统中通过蒸馏制取氧气和稀有气体的方法，该蒸馏塔系统包括至少一个中压蒸馏塔(K01)，一个低压蒸馏塔(K02)和至少一个辅助蒸馏塔(K05)，在该方法中：
i)将至少一股被冷却和提纯的空气流(1)送至中压蒸馏塔，在中压蒸馏塔中将上述空气流分离；
ii)至少将第一股富氮流体(11)从中压蒸馏塔中抽出，并且至少将这股流体的一部分直接或者间接地导入低压蒸馏塔中；
iii)从中压蒸馏塔的中间层将中间流体(RL1)抽出；
iv)将与中间流体相比富含氧的第二股富氧流体(RL2)从中压蒸馏塔的底部抽出并将其导入辅助蒸馏塔的底部；
v)将富含氮的流体(WN2)从低压蒸馏塔的顶部抽出；
vi)将富含氧的液态流体(LO)作为产品从低压蒸馏塔抽出，或者在蒸发阶段后将流体抽出以制成气态的产品；和
vii)将第三股富氧流体(PURGE)从辅助蒸馏塔中抽出，与第二股富氧流体相比这股流体还富含氪和氙；
其特征在于，将中间流体(RL1)导入低压蒸馏塔中，并且至少一股含有至少78mol％氮的液态流体(5，15)作为回流返回到辅助蒸馏塔中。
2. 如权利要求1所述的方法，其中将第三股富氧流体(PURGE)导入净化蒸馏塔(K90)的顶部，组成富含氪和氙的混合物的第四股富氧流体(MIXTURE)在塔的至少下行几个理论级被抽出。
3. 如权利要求1或2所述的方法，其中作为回流返回辅助蒸馏塔(K05)的液态流体(5)是液化空气和/或与导入中压蒸馏塔中的液化空气流相比富含氮的液体。
4. 如权利要求1或2所述的方法，其中利用氩蒸馏塔(K10)塔顶气体对辅助蒸馏塔的底部进行加热。
5. 如权利要求1或2所述的方法，其中通过与来自低压蒸馏塔底部的富含氧的液态流体(LO)进行热交换来制取液态空气(5)和/或与空气相比富含氮的液体，或者可选择压缩阶段以后进行上述热交换。
6. 如权利要求3所述的方法，其中作为回流返回辅助蒸馏塔的富氮流体(15)包含至少80mol％的氮。
7. 如权利要求1或2所述的方法，其中被导入辅助蒸馏塔顶部的液态流体(5，15)的含氮量高于所述中间流体。
8. 如权利要求1或2所述的方法，其中将制取的至少10％的氧以液态形式从低压蒸馏塔中抽出。
9. 一种在蒸馏塔系统中通过蒸馏制取氧气和稀有气体的装置，该蒸馏塔系统包括至少一个中压蒸馏塔(K01)，一个低压蒸馏塔(K02)和一个辅助蒸馏塔(K05)，该装置还包括：
i)将至少一股被冷却和提纯的空气流(1)送至中压蒸馏塔中的机构，在中压蒸馏塔中将上述空气流分离；
ii)至少将第一股富氮流体(11)从中压蒸馏塔中导出的机构，和将至少一部分这股流体直接或者间接地导入低压蒸馏塔中的机构；
iii)将富含氮的流体(WN2)从低压蒸馏塔顶部抽出的机构；
iv)将中间流体(RL1)从中压蒸馏塔的中间层抽出的机构；
v)将与中间流体相比富含氧的第二股富氧流体从中压蒸馏塔的底部送至辅助蒸馏塔底部内的机构；
vi)使液态流体(5，15)作为回流返回辅助蒸馏塔的机构；
vii)将富含氧的液态流体(LO)作为产品从低压蒸馏塔底部导出的机构，或者可选择地在蒸发阶段后将流体抽出以制成气态的产品；和
viii)将与第二股富氧流体相比还富含氪和氙的第三股富氧流体(PURGE)从辅助蒸馏塔中抽出的机构，
其特征在于上述使液态流体作为回流返回辅助蒸馏塔的机构用于输送液化空气或与导入中压蒸馏塔中的液态空气流相比富含氮的液态流体作为回流，且该装置还包括将中间流体从中压蒸馏塔送到低压蒸馏塔的机构。
10. 如权利要求9所述的装置，还包括一个净化蒸馏塔(K90)，将第三股富氧流体(PURGE)导入净化蒸馏塔顶部的机构，和将组成富含氪和氙的混合物的第四股富氧流体(MIXTURE)在塔的至少下行几个理论级抽出的装置。
11. 如权利要求9或10所述的装置，还包括热交换管，其中通过与低压蒸馏塔底部导出的富含氧的液态流体进行热交换，或者在压缩阶段以后进行热交换，产生液化空气和/或与空气相比富含氮的液体。
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