CN1419097A - 一种通过空气低温分馏生产氪和/或氙的方法和装置 - Google Patents

一种通过空气低温分馏生产氪和/或氙的方法和装置 Download PDF

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CN1419097A
CN1419097A CN02146975A CN02146975A CN1419097A CN 1419097 A CN1419097 A CN 1419097A CN 02146975 A CN02146975 A CN 02146975A CN 02146975 A CN02146975 A CN 02146975A CN 1419097 A CN1419097 A CN 1419097A
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krypton
xenon
evaporator
condenser
tower
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CN100346119C (zh
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迪尔克·施文克
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Linde GmbH
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Linde GmbH
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
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    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
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    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
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    • F25J3/04672—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
    • 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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    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
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    • F25J3/04703—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 being arranged in more than one vessel
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    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
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Abstract

本发明涉及用于通过空气低温分馏生产氪和/或氙的方法和装置。将加压和清洁的装填空气(1)引入一用于氮氧分离的分馏***，该***至少包括一高压塔(2)和一低压塔(3)。从高压塔(2)去除含氪和氙的馏分(13，14，15，16，416)。将含氪和氙的馏分(13，14，15，16，416)引入第一冷凝蒸发器(17)的蒸发空间中，在此部分蒸发。从冷凝蒸发器(17)的蒸发空间萃取净化液体(26)，并输送到一氪氙浓缩塔(24)。从该氪氙浓缩塔(24)去除氪氙浓缩物(30)。将来自氪氙浓缩塔底部区域的液体引入与该第一冷凝蒸发器(17)分开的一第二冷凝蒸发器(27)中。

Description

一种通过空气低温分馏生产氪和/或氙的方法和装置
发明领域
本发明涉及一种根据本专利权利要求1前序部分所述的方法，用于通过空气低温分馏生产氪和/或氙。
背景技术
空气低温分馏的一般基本原理以及特别用于氮氧分离的分馏***的结构，在Hausen/Linde的专题论文“低温工程”[Tieftemperaturtechnik](1985年第2版)以及Latimer在“化学工程发展”[Chemical Engineering Progress]上的一篇论文(1967年第2期第63卷第35页)中作了描述。高压塔的操作压力高于低压塔；两个塔最好通过一主冷凝器处于相互热交换关系，该主冷凝器中来自高压塔的顶部气体逆着来自低压塔的蒸发底部液体液化。本发明的分馏***可设计成常规的双塔***，但也可以设计成三塔或多塔***。除用于氮氧分离的塔之外，还可以有用于生产其它空气成分，特别是稀有气体的装置，如氩生产装置。
从DE1000007A1中知道一种用于通过空气的低温分馏来生产氪和/或氙的方法以及相应的装置。在该方法中，来自用于氮氧分离的双塔中的高压塔的含氪和氙的馏分，具体地说是底部液体，在没有任何改变浓度的措施的情况下输送到用于生产氪-氙的另一塔中。
DE2605305A中描述了一种前言中所述类型的通过空气低温分馏生产氪和/或氙的方法和装置。该文件中，第一冷凝蒸发器由来自天然氩塔的冷凝顶部气体加热，同时形成氪-氙浓缩塔的底部加热器。在氪-氙浓缩塔中上升的全部蒸发都是在第一冷凝蒸发器中产生的。
发明内容
本发明基于进一步改进氪和氙的生产，特别是以特别经济的方式完成该生产的目的。
该目的是通过下述事实实现的，来自氪氙浓缩塔底部区域的液体引入与第一冷凝蒸发器分开的第二冷凝蒸发器。
因此在本发明中，有一个单独的热交换器，“第二热交换器”，用于氪氙浓缩塔的上升蒸气独立于第一冷凝蒸发器生成，且挥发性相对较低的组分以这种方式进一步浓缩。第二冷凝蒸发器最好设计成氪氙浓缩塔的底部加热器。它可设置在该塔内部或一个单独容器中。
第二冷凝蒸发器在第一冷凝蒸发器中建立了一个较高的氧浓度，因此考虑到相应减小的温差，第一冷凝蒸发器的整体尺寸可以减小。另外，第一冷凝蒸发器中挥发性相对较低的组分的加强浓度较小，在该位置由于操作原因，这是不期望的。在本发明的范围内，可根据需要选择用于第二冷凝蒸发器的加热装置。原理上，可使用任何适当的工艺馏分，例如可能来自高压塔的氮，来自高压塔的任何其它馏分，来自与低压塔联接的天然氩塔的增压空气的一局部气流或馏分，特别是来自这种天然氩塔顶部的天然氩。
第一冷凝蒸发器的“净化液体”用作氪氙浓缩塔的增压馏分。在本发明的范围内，术语“氪氙浓缩塔”理解为表示逆流质量传递塔，其中产生一馏分，其氪和/或氙的浓度高于该塔中的每个增压馏分。作为例子，氪氙浓缩物的氪和/或氙摩尔水平高于输送到氪氙浓缩塔中的“净化液体”。该塔例如可设计成如DE1000017A1中所述的传送塔，和/或可同时用于排除甲烷。
净化液体最好引入例如位于底部正上方的底部区域中。在这种情况下，将一液体填加到氪氙浓缩塔的顶部，以迫使存在于上升蒸气中的氪向下运行，并迫使甲烷向上运行。该液体例如可从该高压塔的底部或其上方的少量板从高压塔中去除。一种可能的替换方案或者附加源是纯氩塔的顶部冷凝器的蒸发空间。在氪氙浓缩塔的底部，向下流动的液体可通过一底部蒸发器而沸腾。这使得氪氙浓缩物中的氪氙含量进一步提高。底部蒸发器例如可用来自高压塔顶部的压缩空气或压缩氮操作。
本发明中，可在从高压塔萃取含氪和氙的馏分与将该馏分输送到氪氙浓缩塔之间完成一中间步骤，即在第一蒸发器中部分蒸发。该步骤用于在到达氪氙浓缩塔之前浓缩氪和/或氙。进一步的效果是，挥发性低于氧的所有其它成分用部分蒸发的净化液体导引到氪氙浓缩塔中，并以这种方式与设备的其它部件分开，特别是低压塔。
产生于氪氙浓缩塔中的氪氙浓缩物具有的氪含量例如是600到5000ppm，最好是1200到4000ppm，氙含量例如是60到500ppm，最好是120到400ppm。另外，它主要含有氧和一般最多约10摩尔％的氮。
本发明可特别有利地作为生产氩的空气分馏工厂的一部分实施，其中来自低压塔的含氩馏分引入天然氩分馏台中。天然氩分馏台特别用于氩氧分离，并可在一个或多个塔中完成(例如参见EP377117B2或EP628777B1)。在任何情况下都需要的对天然氩分馏台的冷却，在本发明的范围内是由含氪和氙的馏分完成的，来自天然氩分馏的富含氩的蒸气与第一冷凝蒸发器中蒸发的含氪和氙的馏分间接接触。因此作为氪氙生产一部分的部分蒸发同时还用于在天然氩分馏台中产生回流和/或液体产品。
在许多情况下，在一个或多个产品的内部压缩中例如有一液体装填的气流。液化空气经常通过例如引入设置在高压塔中的容器中，从该容器中再次去除部分流体，并输送到低压塔中而在高压塔与低压塔之间分开。在本发明的范围内，下面的情况是有利的，从高压塔中萃取含氧液体并引入低压塔中，该含氧液体起始于一第二中间点，该第二中间点设置于液体装填空气引入高压塔中的第一中间点的上方。这确保了存在于液体装填空气中的氪和氙朝高压塔底部流动，而不是进入低压塔中，这会对氪氙生产造成损失。另外，还使其它低挥发性污物远离主冷凝器。根据本发明的这个方面，液体空气(或具有相似成分的含氧液体)基本上是通过高压塔的无氪和氙的回流液体形成的。
本发明的这个方面可以有利地应用于来自高压塔的馏分输送到氪氙生产台的任何工艺中。其用途并不局限于含氪氙馏分部分蒸发的方法和装置。它还可以应用于相应的其它结构。
在第一中间点与第二中间点之间最好没有质量传递元件，如板或包装物。结果，除了沸点温度高于氧的不期望的成分以外，该含氧液体的组分基本上与空气相同。
在压力塔中，可以有隔板，含氪和氙的馏分在这些隔板下面萃取，富含氧的液体在这些隔板上方去除。因此，富含氧的液体中氪和氙的含量远小于含氪和氙的馏分，且例如可以直接输送到低压塔中和/或用于冷却纯氩塔的顶部冷凝器，而氪和氙的量不会有显著损失。隔板的数量例如可以是一到九个，最好是二到六个(理论板)。
除净化液体之外，气流可从第一冷凝蒸发器蒸发空间萃取，并例如在与净化液体相同的点同样输送到氪氙浓缩塔。结果，仍存在于含氪氙馏分的蒸发部分中的氪也被输送到氪氙生产台。
在本发明方法中，可通过空气在中间压力涡轮机中工作执行膨胀到大致高压塔的操作压力而发生致冷，这经常包含空气的部分液化。在本发明的范围内，已经以工作执行方式膨胀的空气可输送到相分离器，至少部分来自相分离器的液体馏分可输送到氪氙浓缩塔和/或第一冷凝蒸发器的蒸发空间中。
作为替换或填加，空气可例如在低压塔中以工作执行方式膨胀到大致低压塔压力。如果低压气流输送到汽提塔，来自汽提塔的底部液体最好在顶部或者其下方几个板的中间点处输送到氪氙浓缩塔，则存在于该气流中的氪和氙可以回收。此外，汽提塔还保持有其它低挥发性成分，例如在低压塔中不期望的N2O。
与空气的工作执行膨胀相联系的本发明这些方面的优点并不局限于含氪氙馏分部分蒸发的方法和装置。而是，这些工艺步骤还可用在氪氙生产的其它工艺中。
本发明还涉及一种根据专利权利要求9和10通过空气低温分馏生产氪和/或氙的装置。
附图描述
参照在附图中图表表示的示例性实施例对本发明及本发明的细节进行了更详细的描述，其中：
图1示出本发明的第一实施例，
图2示出一修改，隔板位于高压塔中，
图3示出具有一中间压力涡轮机的另一示例性实施例，
图4示出具有低压涡轮机的第四个示例性实施例，及
图5示出另一变形，一涡轮机位于高压塔与低压塔之间。
具体实施方式
已经大致冷却到露点的清洁空气以气体形式流过图1中的管线1，进入用于氮氧分离的整流***的高压塔2中，该整流***还包括一低压塔3和一主冷凝器4，在当前例子中该主冷凝器4设计成降膜式蒸发器。来自高压塔顶部的气态氮5的第一部分6输送到主冷凝器4的冷凝空间中。形成于该空间中的凝汽7的第一部分8作为回流填加到高压塔中。第二部分9在一过冷反流热交换器10中进行过冷，并输送通过管线11和节流阀12到达低压塔3的顶部。该液体的一部分92可作为液态氮产品(LIN)获得。
来自高压塔2的富含氧的底部液体13同样在过冷反流热交换器10中冷却。已过冷的富氧液体14以两个局部液流向外移动。第一个局部液流15-16作为“含氪和氙的馏分”引入代表天然氩整流台18/19的顶部冷凝器的“第一冷凝蒸发器”17的蒸发空间中。第二局部液流15-20输送到纯氩塔22的顶部冷凝器21的蒸发空间中。
第一冷凝蒸发器17设计成强制循环蒸发器，即蒸发空间中含有热交换块部分没入其中的液浴。(优选地，热交换块-与附图不同-完全没入液浴中。)液体在蒸发通道的底端通过热虹吸效果吸入。蒸气与未蒸发液体的混合物在其上端浮出，未蒸发液体流回液浴中。含氪和氙的馏分16在第一冷凝蒸发器17中部分蒸发，作为例子，引入的液体16的0.5到10摩尔％，最好是1到5摩尔％，作为净化液体26从第一冷凝蒸发器17的蒸发空间中以液体形式萃取。这种部分蒸发提高了液体中挥发性相对较低成分，特别是氪和氙的浓度，并减少了它在蒸气中的含量(每种情况下与含氪和氙的馏分16的成分相比)。在部分蒸发过程中产生的蒸气作为气流25从第一冷凝蒸发器17的蒸发空间中萃取。残留的液体作为“净化”液体26从液浴中排出，并输送到位于紧靠底部上方的氪-氙浓缩塔24。
氪-氙浓缩塔24具有一可用任何适当馏分加热。该示例性实施例中，来自高压塔2顶部的加压氮28用作加热手段。(可替换地，可使用来自高压塔的任何其它馏分，排放空气的部分流或来自第二天然氩塔19顶部的一部分天然氩50。已经在底部蒸发器27中液化的氮29与来自主冷凝器4的液体7混合。来自纯氩塔22的顶部冷凝器2 1的蒸发器的净化液体的部分流23作为回流液体填加到氪-氙浓缩塔24的顶部。从底部蒸发器27上升的蒸气与氪-氙浓缩塔中含较少氪和氙的液体23进行逆流质量传递。结果，这些成分冲刷到底部，而多数甲烷与顶部气体30一起排出。本示例性实施例中，后者在一适当的中间点输送到低压塔3。从氪-氙浓缩塔24底部去除液体形式的氪-氙浓缩物30(LOX/Kr/Xe)，该浓缩物例如具有大约2400ppm的氪含量和大约200ppm的氙含量：此外，浓缩物30主要包含氧，还包含大约10摩尔％的氮。浓缩物30可储存在一液体罐中，或直接输送用于进一步生产纯的氪和/或氙。
除液体氮92之外，位于顶部的纯气态氮32，同样为气态的不纯的氮33，以及液体形式的氧34，都至少部分作为产品从低压塔3萃取。气态产品32、33在过冷逆流热交换器10中，然后在一主热交换器(未图示)中加热。液态氧34共分成三部分。第一部分和第二部分初始地一起输送通过管线35和泵36。第一部分37流到主冷凝器4的蒸发空间中，在此部分蒸发。形成的气-液混合物38流回低压塔3的底部。如果在过冷热交换器10中过冷后合适，则第二部分作为液体产品(LOX)通过管线39和40萃取。
来自低压塔3底部的液体氧34的第三部分41由于在泵42中到达所需产品压力而受到内部压力，并通过管线43(LOX-IC)输送到一个或多个热交换器，在其中蒸发(或者在超临界状态下假蒸发)并加热到大致大气温度。蒸发和加热例如可通过与高压气流的直接热交换而完成。液化的(或超临界)高压空气膨胀(未图示)并作为液化空气44在“第一中间点”输送到高压塔2。其数量至少对应于一部分液态空气44的含氧液体45在设置于第一中间点正上方的“第二中间点”从高压塔中萃取；液流45还可大于液流44。在第一中间点与第二中间点之间没有板或其它质量传递元件。在过冷逆流热交换器10中过冷后，其成分基本上对应于空气的含氧液体45通过管线46和节流阀47输送到低压塔3。
来自低压塔3的含氩馏分通过氩传送管线48输送到天然氩整流台，在当前例子中整流是在两个串联的天然氩塔18和19中完成的。含氩馏分18以气体形式输送到位于底部紧上方的第一天然氩塔18。上升蒸气中的氩含量提高。来自第一天然氩塔18的顶部气体通过管线49向前输送到第二天然氩塔19的底部。
富含氩的蒸气(天然氩)50在第二天然氩塔19顶部产生，并在第一冷凝蒸发器17中大量冷凝。液体51作为逆流液体填加到第二天然氩塔19。产生于第二天然氩塔19底部的流体52通过一泵53输送经过管线53，到达第一天然氩塔18的顶部。来自第一天然氩塔18的底部液体55通过另一泵56和管线57流回低压塔3。
来自第一冷凝蒸发器17的液化空间的保持气体形式的天然氩58在纯氧塔中进一步被打破，特别将挥发性相对较高的组分，如氮去除掉。纯氩产品(LAR)以液体形式通过管线59和60萃取。底部液体中另一部分61在与分离器62联接的纯氩蒸发器63中蒸发，并作为上升蒸气通过管线64返回纯氩塔22。纯氩蒸发器63通过与在热交换器中过冷的来自高压塔2的底部液体15的至少一部分进行间接热交换而被加热。如已经描述过的，纯氩塔的顶部冷凝器21用该过冷液体的一部分20冷却。蒸气66以及残留液体23、65从顶部冷凝器21的蒸发空间萃取，并在适当的中间点输送到低压塔3中和/或填加到氪氙浓缩塔24。纯氩塔22的顶部气体67在液化空间中部分冷凝。该过程中产生的逆流液体68填加到纯氩塔。残留蒸气69排放到大气中。
在图1中所示的示例性实施例中，在高压塔2中产生的全部富含氧的液体都从底部(管线13)萃取。这使高压塔2的结构相对不复杂。图2示出该过程的一个修改，其中进一步提高了氪和氙的产量。在这种情况下，对于来自高压塔2的液体270有另一个即刻卸料，该卸料与底部卸料213由大约四个隔板271分开。这些板将大部分低挥发性组分，特别是氪和氙保留在高压塔2的底部。结果，液流270的氪氙含量远低于底部液体213。该液流的一部分220通过过冷逆流热交换器10输送到纯氩塔22的顶部冷凝器21的蒸发空间中。残留物223流到氪氙浓缩塔24顶部。结果从顶部冷凝器3流出到达低压塔3以及回流液体223中的馏分265、266中的氪氙含量都特别低。这都使氪氙产量特别高。
空气中存在的大部分氪和氙(一般是90摩尔％)与底部液体231一起流动经过过冷逆流热交换器10和管线215、纯氩蒸发器63、管线216以及第一冷凝蒸发器17，向前经过管线215和226到达氪氙浓缩塔24，在此处几乎与氪氙浓缩物30一起回收。
如果需要，来自中间卸料的一部分流体270可通过旁通管线272与底部液体213混合。作为例子，在该中间卸料与第一中间点之间有2到14个，最好是5到8个理论板，来自内部压力的液体44在该第一中间点引入。
图1和2中没有图示致冷生产，图3中所示的***与图1中所描绘的不同之处在于，致冷是通过一介质压力涡轮机获得的。该涡轮机本身没有图示，而只图示了来自其出口且处于两相混合物形式的局部液流373。它引入一分离器(相分离器)274中。来自分离器374的蒸气375通过与引导空气1一起输送到高压塔2中。相反，氪和氙含量提高的液体376与来自高压塔2的一部分过冷底部液体14一起，通过管线416输送到第一冷凝蒸发器17的蒸发空间中。过冷底部液体14的另一部分323填加到氪氙浓缩塔24的顶部。当然，也可以将图3中的附加特征与图2中所示的变量相结合。
图4中，过程致冷是通过低压涡轮机生产的。来自该涡轮机出口的空气477大致处于低压塔3的操作压力下，但在这种情况下并不是直接输送到该塔，而是引入到一汽提塔478，挥发性相对较低的馏分被冲刷到底部。底部液体479然后被输送到氪氙浓缩塔24上的一适当中间点。它形成了用于氪氙浓缩塔的一部分回流液体。只有来自汽提塔478的低氪和低氙顶部气体480直接流入低压塔3中，通过这种方式绕过氪氙生产。在每种情况下，过冷底部液体14的一局部液流423、492填加到氪氙浓缩塔24和汽提塔478的顶部。
为简单起见，图5中高压塔2、低压塔3和主冷凝器4图示为双塔。在这种情况下，致冷是通过来自隔板271上方的中间点的气态中间馏分581的工作执行扩张器而产生的。该馏分可在主热交换器582中对抗将冷却的增压空气583而被加热，可以通过管线584输送到一再压缩机585，然后向前输送到主热交换器582的暖端。它在中间温度下通过管线587从主热交换器582中去除，并输送到工作执行扩张器588。涡轮机588最好通过直接机械耦合驱动再压缩机585。已经过工作执行扩张的气流最后在适当点(589)引入低压塔3中。可替换地，如果通过由点划线所示的管线590的气流只加热到主热交换器582中涡轮机588的入口温度然后直接输送到该涡轮机(管线587)，则再压缩以及整个加热都可省略。
图5中没有图示氩生产和氪氙生产。它们的完成方式与图1或2相同。图5中没有内部压力。

Claims (10)

1.一种通过空气低温分馏生产氪和/或氙的方法，其中
将加压和清洁的装填空气(1)引入一用于氮氧分离的分馏***，该***至少包括一高压塔(2)和一低压塔(3)，
从高压塔(2)去除含氪和氙的馏分(13，14，15，16，416)，
将含氪和氙的馏分(13，14，15，16，416)引入第一冷凝蒸发器(17)的蒸发空间中，在此部分蒸发，
从第一冷凝蒸发器(17)的蒸发空间萃取净化液体(26，266)，并
输送到一氪氙浓缩塔(24)，并
从该氪氙浓缩塔(24)去除氪氙浓缩物(30)，
其特征在于，
将来自氪氙浓缩塔(24)底部区域的液体引入与该第一冷凝蒸发器(17)分隔开的一第二冷凝蒸发器(27)中。
2.根据权利要求1所述的方法，其特征在于，将来自低压塔(3)的含氩馏分(48)引入天然氩分馏台(18，19)，使来自天然氩分馏台(18，19)的富含氩的蒸气(50)与第一冷凝蒸发器(17)中蒸发的含氪和氙的馏分(16)间接接触。
3.根据权利要求1或2所述的方法，其特征在于，装填空气的一局部流在液体状态下在一第一中间点输送到高压塔(2)中，在设置于该第一中间点上方的一第二中间点从高压塔(2)中萃取含氧液体(45)，并引入低压塔(3)中。
4.根据权利要求3所述的方法，其特征在于，在第一中间点与第二中间点之间没有质量传递元件。
5.根据权利要求1至4中任一所述的方法，其特征在于，在高压塔(2)中设有隔板(271)，含氪和氙的馏分(213)在隔板(271)下方萃取，在隔板上方去除富含氧的液体(270)。
6.根据权利要求1至5中的一项所述的方法，其特征在于，从第一冷凝蒸发器(17)的蒸发空间中萃取气流(25，255)，并同样输送到氪氙浓缩塔(24)。
7.根据权利要求1至6中任一所述的方法，其特征在于，装填空气的一局部流(373)以工作执行方式膨胀到大约高压塔(2)的操作压力，然后输送到相分离器(374)，至少部分来自相分离器(374)的液体馏分(376)输送到氪氙浓缩塔(24)和第一冷凝蒸发器(17)的蒸发空间中。
8.根据权利要求1至7中任一所述的方法，其特征在于，装填空气的一局部流(477)以工作执行方式膨胀到大致低压塔的压力，并输送到一汽提塔(478)，来自汽提塔(478)的底部液体(479)输送到氪氙浓缩塔(24)。
9.一种通过空气低温分馏生产氪和/或氙的装置，具有
一装填空气管线(1)，用于将加压和预清洁的装填空气引入一用于氮氧分离的分馏***，该***至少包括一高压塔(2)和一低压塔(3)，
具有一去除管线(13，14，15，16，416)，用于从高压塔(2)去除含氪和氙的馏分，
用于含氪和氙的馏分的去除管线(13，14，15，16，416)与第一冷凝蒸发器(17)的蒸发空间相联，
一净化液体管线(26，266)与冷凝蒸发器(17)的蒸发空间及一氪氙浓缩塔(24)相联，及
该氪氙浓缩塔(24)具有用于氪氙浓缩物的生产线(30)，
其特征在于，
一与该第一冷凝蒸发器(17)分开的第二冷凝蒸发器(27)，其蒸发空间与氪氙浓缩塔(24)的底部区域流体联通。
10.根据权利要求9所述的装置，其特征在于，该低压塔(3)通过一氩传送管线(48)与一天然氩分馏台(18，19)相联，该第一冷凝蒸发器(17)的液化空间与该天然氩分馏台(18，19)流体联通。
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