CN1134640C - 制备超纯氮的方法及设备 - Google Patents

制备超纯氮的方法及设备 Download PDF

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CN1134640C
CN1134640C CNB991238044A CN99123804A CN1134640C CN 1134640 C CN1134640 C CN 1134640C CN B991238044 A CNB991238044 A CN B991238044A CN 99123804 A CN99123804 A CN 99123804A CN 1134640 C CN1134640 C CN 1134640C
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pressure column
nitrogen
tower
lower pressure
carbon monoxide
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CN1255619A (zh
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J��F�����ֹ�ķ
克里斯蒂安·孔茨
迪特里希·罗特曼
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Linde GmbH
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  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Removal Of Specific Substances (AREA)
  • Arrangement Of Elements, Cooling, Sealing, Or The Like Of Lighting Devices (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

本发明涉及一种通过具有至少一个蒸馏塔的空分装置制备超纯氮的方法，其中将来自于压力塔上部或液态氮储罐的无氧压缩氮馏份减压输入到在其底部被加热的低压塔中，由此在所述低压塔中形成上升的蒸汽，并借助于在该低压塔顶部用超纯氮进行的回流脱除一氧化碳，在所述低压塔的顶部抽出不含一氧化碳的顶部气体，然后在压力提高之后被部分液化，该已液化的部分减压进入在其底部被加热的He-Ne-H2塔中，从该塔液态地取出超纯氮。本发明还涉及用于实施上述方法的设备。

Description

制备超纯氮的方法及设备
技术领域
本发明涉及一种在具有至少一个精馏塔的精馏系统中通过低温分离空气来制备超纯氮的方法，其中将已压缩和纯化的使用空气输入到一个压力塔中，从该压力塔制备无氧的压缩氮馏份，然后输送到低压塔中，并且在该低压塔中制备作为顶部气体且不含一氧化碳的低压氮。本发明还涉及用于实施本发明方法的设备。
背景技术
在将要公布的第198 06 576号德国专利申请中知道了一种制备超纯氮的方法。从压力塔中得到无氧压缩氮馏份，其中所述压力塔具有至少160个理论底板，以便从这个压力塔中不含一氧化碳地取出压缩氮。尽管有160个理论底板，但是用于此的能源消耗还是一直很高。此外，该方法的缺点是纯氮的大部分是以气态制得的。
发明内容
因此，本发明的目的是避免这个缺点并降低能量消耗。
本发明的另一个目的是提供一种方法，这种方法可以有选择地用直接来自压力塔或者装有液态压缩氮的液态氮储罐的液态压缩氮馏份来进行。
按照本发明的一个方面，其提供一种通过低温分离无氧的压缩氮馏份来制备超纯氮的方法，其中所述无氧的压缩氮馏份或是从低温空气分离用压力塔的上部液态地制备或是从储存有液态氮的液态氮储罐中准备，该无氧的压缩氮馏份减压输入到在其底部(Sumpf)被加热的低压塔中，该方法的特征在于，
在所述低压塔中形成上升的蒸汽，并借助于在该低压塔顶部用超纯氮进行的回流脱除一氧化碳，以及
在所述低压塔的顶部抽出不含一氧化碳的顶部气体，然后在压力提高之后被部分液化，该已液化的部分减压进入在其底部被加热的He-Ne-H2塔中，从该塔液态地取出超纯氮；或者
低压塔中不含一氧化碳的顶部气体逆着液体冷却介质在一个冷凝器/蒸发器中被部分液化，并且在液体冷却介质蒸发时产生的气流在压力提高之后被部分液化，液化部分作为冷却介质被送回冷凝器/蒸发器中。
采用按照本发明的方法可液态制备超纯氮，并且可以以这个形式方便运输，所以可以容易地分配给用户。此外，这种方法可以通用。即：它可以接在空气分离设备后面使用(带有或者不带液态氮储罐)或者只与一个液态氮储罐(与空气分离设备在空间上是分开的)连接使用。此外，在带有液态氮储罐的空气分离设备上，空气分离设备不工作，也可以制备超纯液态氮。
在采用按照本发明方法的设备时，不含一氧化碳的顶部气体和He-Ne-H2塔的顶部气体汇集成一个不含一氧化碳的冷气体流。
可以有选择地将不含一氧化碳的顶部气体逆着可被蒸发的液体冷却介质在一个冷凝器/蒸发器中而被部分液化，而且在液体冷却介质蒸发时形成的气流和He-Ne-H2塔的顶部气体可以汇集成不含一氧化碳的冷气流。
本发明方法的优点是，在这两种情况下，不含一氧化碳的冷气流在一个热交换器中加热、压缩并在相同的热交换器内逆流重新冷却，并且紧接着一部分在低压塔中而另一部分在He-Ne-H2塔中用于所述塔的底部加热，且在这里被液化，但不包括气态的残余气流，并作为液体冷却介质输入到冷凝器/蒸发器中。
在加热He-Ne-H2塔和低压塔时液化的液流可以作为回流输入He-Ne-H2塔中。
在采用上述作为选择方法说明的冷凝器/蒸发器时，借助于在加热所述He-Ne-H2塔和低压塔时在低压塔的冷凝器/蒸发器中液化的液流，不包括残余气流，在低压塔中不含一氧化碳的顶部气体液化，而且至少部分作为回流输入He-Ne-H2塔中。与另外为冷凝器/蒸发器增加额外投资的缺点相比，该方法具有不可低估的优点：在压缩不含一氧化碳的气流时可能出现空气泄漏的情况下，不会使超纯液态氮含有杂质。
超纯氮液态从He-Ne-H2塔中抽出来，一部分作为低压塔的回流，而另一部分作为液态超纯氮产品制备。
超纯液态氮产品可以输送到一个产品罐中。
超纯液态氮产品可以用一个泵来加压，在使用冷却介质的情况下，在制备无氧压缩氮时蒸发、加热并作为气态压缩产品供给使用。
在这种情况下，采用上述制造超纯液态氮的方法也可以制造气态超纯氮产品，而且在这种情况下可以有意义地利用原先存在的液态产品的制冷性。
根据本发明的另一个方面，其还提供通过低温分离无氧的压缩氮馏份来制备超纯氮的设备，其包括：
用于将无氧的压缩氮馏份从低温空气分离用压力塔的上部或是从储存有液态氮的液态氮储罐中输入到在其底部被加热的低压塔中的装置，
在低压塔的顶部以回流的形式送入超纯氮的装置，
由低压塔的顶部抽出不含一氧化碳的顶部气体的装置，其与用于部分液化不含一氧化碳的顶部气体的装置相连，
用于向底部加热的He-Ne-H2塔中输入不含一氧化碳的顶部气体的液化部分的装置，
从He-Ne-H2塔中中取出液态超纯氮的装置，以及
具有使He-Ne-H2塔的顶部气体压力升高的装置的循环系统。
附图说明
以下将借助于5个构造及5张图详细说明本发明。
图1示出了一种按照本发明的方法，其中从液态氮储罐准备用于本方法的无氧氮。
图2示出了一种按照本发明的方法，其中从精馏系统的压力塔中准备用于本方法的无氧氮。
图3示出了与图1相同的方法，但是另外装有冷凝器/蒸发器。
图4示出了与图2相同的方法，但是另外装有冷凝器/蒸发器。
图5示出了与图2一样的方法，其可用于以后附加采用本发明方法的精馏系统这种情况。
具体实施方式
在图1至图5中用相同的参考符号标出了相同的工艺流和工艺步骤。
图1以示意图示出了按照本发明用于制备超纯氮的方法。包括少量mol-ppm之残余物的无氧液态压缩氮馏分1减压进入压力在4.5和5.5bar之间工作并已加热的低压塔2中。根据包括少量mol-ppb之残余物在内的纯度要求，通过在顶部以来自He-Ne-H2塔4的超纯氮3进行回流，使得在低压塔2中上升的蒸汽脱除一氧化碳并从而脱除比一氧化碳更难蒸馏的杂质如氩气和残余含量的氧。不含一氧化碳的顶部气体5和He-Ne-H2塔的顶部气体6汇集成不含一氧化碳的冷气流7，在热交换器8中加热，并且在压缩9之后在相同的热交换器8中重新冷却。冷却的气流10一部分11在低压塔2中而另一部分12在He-Ne-H2塔4中用于底部的加热13、14，并液化，但不包括气态的残余气流。液化的液流17、18作为回流输入He-Ne-H2塔4中。不含一氧化碳的超纯氮19液态地从He-Ne-H2塔中抽出，现在，根据数量级方面的要求，这种超纯氮只含有少量mol-ppb较容易蒸馏的氖和更容易蒸馏的成分——水蒸汽和氦。液态超纯氮19一部分3用作低压塔2的回流，而另一部分作为液态超纯液态氮产品20制备并输入产品罐21。
在如图1所示的按照本发明方法的结构中，作为塔内物料使用的液态压缩氮馏份1通过压力提高泵23从液态氮储罐22中取出，然后经过热交换器24进入低压塔2中。在热交换器24中，超纯液态氮产品20再次冷却并且紧接着没有气体减压损失地减压进入产品罐21。由于液态氮产品20的再冷却，产品罐21可以做成无压工作的液态氮储罐。
图2以示意图示出了与图1一样制备超纯液态氮产品20的方法。所不同的是，在按照图1的结构中，作为塔内物料使用的液态氮馏份1从精馏系统的压力塔25中取出，并通过热交换器24进入低压塔2中。超纯液态氮产品20用泵26加压，与液态氮馏份1逆流流过热交换器24，并且在使用冷凝器27和热交换器28中冷却介质的情况下，在制备无氧压缩氮馏份时使用，并由此蒸发、加热和作为气态超纯压力产品29供应给其它用途。
图3以示意图示出了本发明方法的一个实施方案，其中采用了冷凝器/蒸发器30。与图1结构不同的是，在按照图3的构造中，低压塔2中不含一氧化碳的顶部气体5(逆着通过汇集已液化的液流17、18而形成的、并在这里可蒸发的液体冷却介质31)在冷凝器/蒸发器30中被液化，但不包括液态的残余气流32，并且在He-Ne-H2塔4中作为回流33使用。在液体冷却介质蒸发时形成的气流5＇和He-Ne-H2塔4的顶部气体6汇集成冷的不含一氧化碳的气流7。
虽然采用冷凝器/蒸发器30会增加额外投资，但是可以分开塔2、4，使得在压缩时产生空气泄漏并进入不含一氧化碳的气体7、10的情况下，不会污染He-Ne-H2塔4并从而不污染超纯氮产品20。
图4以示意图示出了与图2一样的按照本发明的方法，但是采用了象图3中那样的冷凝器/蒸发器30。
图5以示意图示出了可以在现有的精馏系统上采用按照本发明的方法。从与图2那样的方法结构出发，在精馏系统中补充安装冷凝器27，而且热交换器8包括有两个附加通道用来在为精馏系统冷却和液化部分空气35流34时利用待加热之超纯氮20′的制冷性。这时，在热交换器8中加热的超纯氮作为气态超纯压力产品29供应其它用途。
图1至图5中的按照本发明方法结构的共同特点是，所有附带产生的残余气流(在图1、2、5中的15、16、36和在图3、4中的15、16、32、36)汇集成冷残余气流37在热交换器8中加热并且作为不纯净气体38排到大气中。
实施例
在这个示例中m3的意义为：在0℃和1.0133bar正常状态下的m3；也就是说，1m3相当于1.25kg。
采用图1结构中的本发明方法，从1750m3/h具有1mol-ppm一氧化碳的液态氮中可以产生1500m3/h具有20mol-ppb一氧化碳的超纯液态氮。在这里，压缩时损失100m3/h，还有150m3/h的残余气体。12500m3/h氮被从6.5bar压缩到7bar；压力提高泵在入口压力1bar和出口压力7bar之间工作。

Claims (9)

1、通过低温分离无氧的压缩氮馏份来制备超纯氮的方法，其中所述无氧的压缩氮馏份(1)或是从低温空气分离用压力塔的上部液态地制备或是从储存有液态氮的液态氮储罐中准备，该无氧的压缩氮馏份(1)减压输入到在其底部被加热(13)的低压塔(2)中，该方法的特征在于，
在所述低压塔中形成上升的蒸汽，并借助于在该低压塔顶部用超纯氮进行的回流(3)脱除一氧化碳，以及
在所述低压塔的顶部抽出不含一氧化碳的顶部气体(5、7)，然后在压力提高(9)之后被部分液化(13、14)，该已液化的部分(17、18)减压进入在其底部被加热(14)的He-Ne-H2塔(4)中，从该塔液态地取出超纯氮；或者
低压塔中不含一氧化碳的顶部气体(5)逆着液体冷却介质(31)在一个冷凝器/蒸发器(30)中被部分液化，并且在液体冷却介质蒸发(30)时产生的气流(5＇、7)在压力提高(9)之后被部分液化(13、14)，液化部分(17、18、31)作为冷却介质(31)被送回冷凝器/蒸发器(30)中。
2、按照权利要求1所述的方法，其特征在于，不含一氧化碳且上升流向压缩(9)的顶部气体(5)和所述He-Ne-H2塔(4)的顶部气体(6)汇集成不含一氧化碳的冷气流。
3、按照权利要求1所述的方法，其特征在于，在液体冷却介质蒸发(30)时产生的气流(5＇)和He-Ne-H2塔(4)的顶部气体(6)汇集成冷气流(7)。
4、按照权利要求2或3所述的方法，其特征在于是，所述冷气流(7、10)在一个热交换器(8)中加热，压缩(9)，并在相同的热交换器(8)中重新逆流冷却，然后紧接着一部分(12)在所述低压塔(2)中而另一部分(11)在所述He-Ne-H2塔(4)中用于加热底部(13、14)，并在其中液化，不包括气态的残余气流(15、16)。
5、按照权利要求4所述的方法，其特征在于，在低压塔的蒸发器/冷凝器(30)，所述低压塔中不含一氧化碳的顶部气体(5)被液化，不包括残余流(32)在内，并至少部分作为回流(33)输入He-Ne-H2塔(2)中。
6、按照权利要求4所述的方法，其特征在于，从所述He-Ne-H2塔中液态地抽出的超纯氮(19)，部分作为所述低压塔(2)的回流(3)使用。
7、按照权利要求1或6所述的方法，其特征在于，所述超纯液态氮产品(19、20)输入到产品罐(21)中。
8、按照权利要求7所述的方法，其特征在于，所述超纯液态氮产品用一个泵加压，在使用冷却介质的情况下，在制备无氧压缩氮馏份时蒸发、加热并作为气态压力产品供给其它用途。
9、通过低温分离无氧的压缩氮馏份来制备超纯氮的设备，其包括：
用于将无氧的压缩氮馏份从低温空气分离用压力塔的上部或是从储存有液态氮的液态氮储罐中输入到在其底部被加热的低压塔中的装置，
在低压塔的顶部以回流的形式送入超纯氮的装置，
由低压塔的顶部抽出不含一氧化碳的顶部气体的装置，其与用于部分液化不含一氧化碳的顶部气体的装置相连，
用于向底部加热的He-Ne-H2塔中输入不含一氧化碳的顶部气体的液化部分的装置，
从He-Ne-H2塔中中取出液态超纯氮的装置，以及
具有使He-Ne-H2塔的顶部气体压力升高的装置的循环系统。
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EP1001236A3 (de) 2000-11-08
JP2000180051A (ja) 2000-06-30
EP1001236A2 (de) 2000-05-17

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