CN1502552A - 从空气生产氪/氙混合物的方法和装置 - Google Patents

从空气生产氪/氙混合物的方法和装置 Download PDF

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CN1502552A
CN1502552A CNA200310115448XA CN200310115448A CN1502552A CN 1502552 A CN1502552 A CN 1502552A CN A200310115448X A CNA200310115448X A CN A200310115448XA CN 200310115448 A CN200310115448 A CN 200310115448A CN 1502552 A CN1502552 A CN 1502552A
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tower
xenon
krypton
materials flow
liquid
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F・芬特斯
F·芬特斯
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

本发明涉及一种从空气生产氪/氙混合物的方法，其中：(a)空气在至少一个空气蒸馏设备(8)中蒸馏，以便从空气生产含有大多数氪和氙的液氧料流，和该液氧料流被汽化；(b)用步骤(a)中获得的至少一部分气态氧进行至少一种烃的部分氧化，以便生产含有至多0.1ppm摩尔氧的合成气；和(c)从合成气中除去除氪和氙之外的组分。

Description

从空气生产氪/氙混合物的方法和装置
发明领域
本发明涉及一种从空气生产氪/氙混合物的方法和装置。
背景技术
氪和氙的主要来源是大气，其中它们以痕量存在，即分别是1.135ppm和0.086ppm(ppm：百万分之一份)。
通常使用的提纯方法包括从低温空气分离装置提取富集的混合物，通常在液氧再沸器中进行，然后通过低温蒸馏浓缩该混合物。因此获得了约99％的氪和氙总含量。该混合物然后分离成氪和氙，通常在实验室中进行。
该方法的主要问题在于安全性。这是因为，由于氪和氙的沸点，作为重金属稀有气体的氪和氙基本上是在液氧中存在，同时烃类以痕量存在于空气中。所以，在一步中富集存在导致爆炸性烃/氧比例的危险。
所以必须通过蒸馏进行第一部分富集，然后去除烃，这是以化学方式在非深冷温度下完成的，然后进行新的低温蒸馏。另外，由于化学反应生成可能在混合物蒸馏温度下固化的化合物(特别是CO2或H2O)，所以必要的是在反应器下游插入吸收(或等价)步骤以去除烃类。
还应该注意的是，氪/氙提纯设备的尺寸是显著的，因为这些组分在液氧中的低含量(几ppm至几十ppm)。
发明概述
本发明的目的是提供一种从空气生产氪/氙混合物的方法，该方法是安全的并需要较小尺寸的设备。
为此，本发明的主题是提供一种从空气生产氪/氙混合物的方法，其特征在于：
(a)空气在至少一个空气蒸馏设备中蒸馏，以便从空气生产含有大多数氪和氙的液氧料流，和该液氧料流被汽化；
(b)用步骤(a)中获得的至少一部分气态氧进行至少一种烃的部分氧化，以便生产含有小于0.1ppm摩尔氧的合成气；和
(c)从合成气中除去除氪和氙之外的组分。
本发明的方法可以包括一个或多个以下特征：
-通过使氧气与过量的烃和任选地与蒸汽反应来进行部分氧化；
-通过使氧气与天然气、甲烷、石脑油或煤反应来进行部分氧化；
-步骤(c)包括干燥/脱碳步骤，然后进行低温分离；
-低温分离操作包括一系列步骤，生产富集氪/氙的料流、氢气料流、一氧化碳料流和废料流，所述富集氪/氙的料流另外含有基本上甲烷和一氧化碳；
-所述系列步骤包括将液态一氧化碳送入第一塔的顶部的步骤，塔底液体从该塔膨胀，从第二塔去除氢气，在该塔的顶部加入所述膨胀的塔底液体，塔底液体从该第二塔膨胀，并将膨胀的液体注射入低压塔中，在低压塔的顶部加入液态一氧化碳，并生产作为塔顶产品的一氧化碳和作为塔底产品的所述富集氪/氙的料流；和
-此外，低温分离包括任选地在立即加热富集氪/氙的料流之后，将氪和氙与该料流中除氪/氙之外的其它组分进行低温分离。
本发明的另一个目的是提供一种从空气生产氪/氙混合物的装置，其特征在于该装置包括：
-空气蒸馏设备，该装置从空气生产含有大多数氪和氙的液氧料流，该装置与用于汽化该液氧料流的再沸器组合使用；
-部分氧化反应器，在该反应器中一方面加入汽化的氧气流，另一方面加入含有至少一种烃的气体，该反应器生产出含有至多0.1ppm摩尔氧的合成气；和
-用于从合成气中除去除氪和氙之外的组分的装置(3-7)。
根据其它任选的方面：
-所述去除装置包括干燥/脱碳装置，然后是低温分离装置；
-低温分离装置包括适于生产富集氪/氙的料流、氢气料流、一氧化碳料流和废料流的塔的组合，所述富集氪/氙的料流另外含有基本上甲烷和一氧化碳；
-低温分离装置包括第一塔，用于将液态二氧化碳送入第一塔顶部的装置，用于使来自该第一塔的塔底液体膨胀的装置，用于去除氢气的第二塔，在所述第二塔的顶部加入所述膨胀的塔底液体，用于使来自所述第二塔的塔底液体膨胀的装置，和低压塔，在该低压塔的中间水平处加入来自第二塔的膨胀塔底液体，和在该低压塔的顶部加入液体一氧化碳，该低压塔生产出作为塔顶产品的一氧化碳和作为塔底产品的所述富集氪/氙的料流；和
-低温分离装置还包括用于将氪和氙与该料流中除氪/氙之外的其它组分分离的塔。
附图简述
将通过以下附图来描述本发明的实施方案：
图1是根据本发明装置的全视图；
图2显示了该装置的一部分；和
图3是一个变型实施方案的部分示意图。
本发明的具体实施方案
图1所示的装置包括包含双塔空气蒸馏装置的低温试验箱1，部分氧化反应器2，冷凝器3，胺洗涤脱碳装置4，吸收型干燥-脱碳装置5，用于生产一氧化碳CO、氢气、第一废料流W1和富集氪/氙的混合物的低温试验箱6，和用于分离氪/氙混合物和第二废料流W2的低温试验箱7。
在操作中，大气空气预先经压缩提纯出水和二氧化碳，该空气在低温试验箱1中冷却，并在该试验箱中所含的双蒸馏塔8中蒸馏，该蒸馏塔具有常规的结构，即中压塔和低压塔经由再沸器-冷凝器连接。从低压塔底取出的液氧LOX被低温泵9泵压到高压，通常是20巴，并在该高压下汽化，以便形成气态氧料流GOX，它含有基本上全部的在进入空气中所含的氪和氙。液氧通常在空气分离装置(ASU)的主换热器或在指定换热器中通过与加压空气流或氮气流之间的热交换而被汽化。
该氧气经由管线10进入反应器2中，该反应器也经由管线11接收过量的天然气(通常为98％CH4/2％N2)。任选地，如果部分氧化是ATR型的(自热重整型)，则蒸汽参与该反应。
氧气可以来自数个ASU。
因此，经由管线12生产含有小于0.1ppm摩尔氧的合成气。该合成气在3中冷却之后，在4中汽提出其中的二氧化碳CO2，并在5中汽提出其中的水和痕量二氧化碳CO2。
因此，含有氪/氙和基本上痕量氮和氩并含有氢气、CO、未反应的甲烷的混合物经由管线13进入低温试验箱6。
低温试验箱6的出料是经由管线14的CO、经由管线15的氢气、经由管线16的基本由CO和氢气组成的废料流W1以及经由管线17的富集氪/氙的混合物。
低温试验箱7中(经由管线17加料)基本包含蒸馏塔，该蒸馏塔在其顶部经由管线18生产作为塔顶产品的氪/氙混合物，和经由管线19生产作为塔低产品的废料流W2，废料流W2基本由甲烷、CO、氮气和氩气组成。
如图2所示，低温试验箱6基本上包括：
-逆流型的主换热器20；
-用于洗涤CO的高压塔21，在该塔之上配有相分离器22；
-中压闪蒸塔23，配有塔底再沸器24；
-低压塔25，配有塔底再沸器26；
-中压闪蒸塔27，配有塔底再沸器28；
-辅助换热器29；
-高压相分离器30；和
-膨胀汽轮机31。
在操作中，经由管线13输送并在换热器20的加热部分被冷却的合成气被引入塔21的底部。轻质组分基本上是作为塔顶产物生产的氢气和一氧化碳，该轻质组分在换热器20的冷却部分被冷却和部分冷凝，然后加入相分离器22。来自该分离器的基本上由CO组成的塔底液体以回流方式送到塔21的顶部，而汽相从换热器29的热端到冷端被再次冷却和部分冷凝，该汽相引入相分离器30。后者生产了作为塔顶产物的高压氢气和作为塔底产物的高压CO。
在换热器29中受热的高压氢气在汽轮机31中被膨胀到接近大气压，然后通过换热器29和进而换热器20，被加热，从而保持低温试验箱6的冷却。该料流然后经由管线15回收。
在分离器30中收集的并含有痕量氢气的液体CO在膨胀阀32中被膨胀到中等压力，并引入塔27的顶部。该塔产生作为塔顶产物的H2/CO混合物和作为塔底产物的液体CO。
来自塔21的并基本由甲烷和CO组成且含有氪/氙和痕量氢气的底部液体在膨胀阀35中被膨胀到中等压力，并引入塔23的顶部。从该塔顶部取出H2/CO混合物。
来自塔23和27的H2/CO料流在各膨胀阀33和34中被膨胀到接近大气压之后，进入同一管线，形成废料气体W1，它在20中被加热，并经由管线16排出。
来自塔23的塔底液体再次在膨胀阀36中被膨胀到低压，然后引入塔25的中部。从塔27底部取出的液体CO在膨胀阀37中被膨胀到低压，并引入塔25的顶部。因此，该塔一方面分离了来自塔顶并然后在20加热和经由管线14回收的CO，另一方面分离了含有氪/氙和痕量氮和氩的甲烷/CO混合物。
该混合物任选在膨胀阀38中被膨胀到接近大气压之后在20中加热，然后经由管线17回收，然后在低温试验箱7中处理，如上所述。
应该理解的是，可以预见许多替换的实施方案。例如，底部再沸器24、26和28可以被任何在装置中可获得的处于适宜压力的适宜料流加热，例如被合成气加热。相似地，一氧化碳循环可以用于保持塔23、25和27的冷却状态和/或用于其中的再沸腾，如本身已知的那样。
此外，低温试验箱1、6和7可以在其安装方式和/或保持冷却方式方面组合至或多或少的程度。例如，如果低温试验箱6和7组合，则来自塔25的底部液体可以直接送到用于分离出氪/氙的最终的塔，不需要中间加热。
因此，氧气根据上述方法生产，它经过压缩，从而从空气进行氪/氙的第一次浓缩。接着，生产了不含氧气并具有低甲烷含量且含有全部氪/氙的合成气，这进而允许使用小型的氪/氙富集装置。因为在合成气中没有氧气，所以在该装置中没有爆炸的危险。
处于中等压力的两个闪蒸塔23和27用于除去溶解在要进入塔25的一氧化碳中的氢气。
应该注意的是，氪/氙的回收可以容易地在现有的氢气/一氧化碳生产装置中实施。该装置可以基于从CO分离氢气的工艺，它不同于图2所示的工艺，例如基于“甲烷洗涤”工艺。但是，图2的工艺特别适合于回收氪/氙。
图3显示了低温试验箱1的另一实施方案，其中送入反应器2的氧气一部分是由来自双塔8的低压塔底部取出的气态氧形成的，和一部分是由来自相同塔底部取出液态氧形成的，在低温试验箱1的换热器39中汽化并与气态氧料流合并。

Claims (12)

1.一种从空气生产氪/氙混合物的方法，其特征在于：
(a)空气在至少一个空气蒸馏设备(8)中蒸馏，以便从空气生产含有大多数氪和氙的液氧料流，和该液氧料流被汽化；
(b)用步骤(a)中获得的至少一部分气态氧进行至少一种烃的部分氧化，以便生产含有至多0.1ppm摩尔氧的合成气；和
(c)从合成气中除去除氪和氙之外的组分。
2.根据权利要求1的方法，其特征在于通过使氧气与过量的烃和任选地与蒸汽反应来进行部分氧化。
3.根据权利要求1或2的方法，其特征在于通过使氧气与天然气、甲烷、石脑油或煤反应来进行部分氧化。
4.根据权利要求1-3中任一项的方法，其特征在于步骤(c)包括干燥/脱碳步骤，然后进行低温分离。
5.根据权利要求4的方法，其特征在于低温分离操作包括一系列生产富集氪/氙的料流、氢气料流、一氧化碳料流和废料流的步骤，所述富集氪/氙的料流另外含有基本上甲烷和一氧化碳。
6.根据权利要求5的方法，其特征在于所述系列步骤包括将液态一氧化碳送入第一塔(21)顶部的步骤，塔底液体从该塔膨胀(35)，从第二塔(23)去除氢气，在该塔的顶部加入所述膨胀的塔底液体，来自第二塔(23)的塔底液体进行膨胀(36)，并将膨胀的液体注射入低压塔(25)中，在低压塔的顶部加入一氧化碳，并生产作为塔顶产品的一氧化碳和作为塔底产品的所述富集氪/氙的料流。
7.根据权利要求5或6的方法，其特征在于低温分离还包括任选地在立即加热富集氪/氙的料流之后，将氪和氙与该料流中除氪/氙之外的其它组分进行低温分离。
8.一种从空气生产氪/氙混合物的装置，其特征在于该装置包括：
-空气蒸馏设备(8)，该装置从空气生产含有大多数氪和氙的液氧料流，该装置与用于汽化该液氧料流的再沸器组合使用；
-部分氧化反应器(2)，在该反应器中一方面加入汽化的氧气流，另一方面加入含有至少一种烃的气体，该反应器生产出含有至多0.1ppm摩尔氧的合成气；和
-用于从合成气中除去除氪和氙之外的组分的装置(3-7)。
9.根据权利要求8的装置，其特征在于所述去除装置(3-7)包括干燥/脱碳装置(4，5)，然后是低温分离装置(6，7)。
10.根据权利要求9的装置，其特征在于低温分离装置(6，7)包括适于生产富集氪/氙的料流、氢气料流、一氧化碳料流和废料流的塔(21，23，25，27)的组合，所述富集氪/氙的料流另外含有基本上甲烷和一氧化碳。
11.根据权利要求9或10的装置，其特征在于低温分离装置(6，7)包括第一塔(21)，用于将液体一氧化碳送入第一塔顶部的装置，用于使来自该第一塔的塔底液体膨胀的装置(35)，用于去除氢气的第二塔(23)，在所述第二塔的顶部加入所述膨胀的塔底液体，用于使来自所述第二塔的塔底液体膨胀的装置(36)，和低压塔(25)，在该低压塔的中间水平处加入来自第二塔(23)的膨胀塔底液体，和在该低压塔(25)的顶部加入液体一氧化碳，该低压塔(25)生产出作为塔顶产品的一氧化碳和作为塔底产品的所述富集氪/氙的料流。
12.根据权利要求10或11的装置，其特征在于低温分离装置(6，7)还包括用于将氪和氙与该料流中除氪/氙之外的其它组分分离的塔。
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CN113003553A (zh) * 2019-12-18 2021-06-22 气体产品与化学公司 从液态氧中回收氪和氙
CN113003553B (zh) * 2019-12-18 2023-10-27 气体产品与化学公司 从液态氧中回收氪和氙
CN112250050A (zh) * 2020-10-27 2021-01-22 深圳市博纯半导体材料有限公司 一种氙气生产制备装置及方法
CN113465292A (zh) * 2021-07-05 2021-10-01 乔治洛德方法研究和开发液化空气有限公司 一种增加空气精馏装置氪/氙产量的方法

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FR2847568B1 (fr) 2005-02-11

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