CN1043196A - 空气分离方法及装置 - Google Patents

空气分离方法及装置 Download PDF

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CN1043196A
CN1043196A CN89108846A CN89108846A CN1043196A CN 1043196 A CN1043196 A CN 1043196A CN 89108846 A CN89108846 A CN 89108846A CN 89108846 A CN89108846 A CN 89108846A CN 1043196 A CN1043196 A CN 1043196A
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威廉·罗德
霍斯特·科杜安
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Linde GmbH
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Abstract

本发明记载了一种藉空气低温精馏来分离空气的工艺和装置，其中氩仅藉精馏来制取。粗氩塔(24)中至少配置150块理论精馏板，才有可能在其中完全分离掉氧。

Description

本发明涉及一种藉空气低温精馏来分离空气的方法和装置，其中将空气压缩、预净化、冷却、输至两级精馏段，并分离成一种富氧馏份和一种富氮馏份，同时由精馏段低压级抽出另一种富集氩的氧馏份，并在粗氩精馏段中分离成粗氩和一种难于沸腾的残余馏份。
空气分离的主产物氧和氮，可直接从两级精馏段抽出。而沸点在氧沸点和氮沸点之间的氩，却富集于精馏段低压级的中间区域。在此部位，抽出一种基本由氧组成的馏份，大部分含于原料空气中的氩就随之而抽出。该馏份藉在粗氩塔中进行的精馏，分离成粗氩和一种液态残余馏份。该残余馏份则被回输至低压级。
由联邦德国专利局公开说明书DE-OS-3436897，已知一种本说明书开头所提及的那种方法。其中在两级空气精馏之后，而粗氩塔中得到气态粗氩，它约有95%由氩组成，而且主要杂质为约3%的氧和2%的氮（各百分比均为体积比）。用迄今已知的工艺，在通常只有约60块精馏塔板的粗氩塔中进行精馏，只能不完全地除去氧，这是由于氩的沸点和氧的沸点挨得极近之故。这两个沸点之差，例如在压力为1bar时，为2.9K。
要制备含杂质少于1%的纯氩，就必须在将易挥发的氮于纯氩塔中精馏分离出去之前，先将沸点比氩高得极为有限的氧，从以已知方法制得的粗氩中除去。
在已知方法中，从粗氩中分离出氧，是在所谓的Deoxo装置中进行的。在该装置中，使氧同与之混合的氢燃烧，并将由此产生的水在干燥器中分离掉。这样一种工艺，举例来说，已在联邦德国专利局公开说明书DE-OS-3428968中予以公开。
这种Deoxo装置是一种昂贵的装置，并由于消耗相当多的氢而首先使生产成本提高。当在空气分离装置中进行的各化学过程中，无论如何也不产生氢时，要提供氰是特别费钱的事。
本发明的任务是，研制一种本说明书开头所提及的那种以设备投资小和生产成本低为特色的工艺和装置。
该任务通过至少使用150块理论板进行粗氩精馏而得以解决。本发明尤为有利的发展是，将来自粗氩精馏段的粗氩，在纯氩精馏段中分离成纯氩和一种易于沸腾的残余馏份。
迄今，在设计空气分离装置时，尚未认真考虑在氧约为1%的条件下来精馏分离氧和氩。这是由于这样一种工艺因这两种物质的沸点差极小而极难实现，而且花销很大。这种谨慎是以下面所要简短阐明的、暂时明白易懂的论据为基础的。
在其中要进行这样一种分离的精馏塔中，其塔顶必须予以冷却，以产生回流。对于这种塔顶冷却，只能考虑采用来自增压级的塔底馏份进行间接换热，就象通常在粗氩精馏时也采用的那样。在此情况下，塔底馏份在塔顶冷凝器中减压，并在其中液化。来自所冷凝气体的热量在粗氩精馏塔塔顶中，经间接换热而予吸收。汽化的塔底馏份则被导入低压塔。用此方法可产生回流的前提条件自然是，待冷却塔的塔顶处气体冷凝温度要高于汽化的塔底液体汽化温度。该温度由各馏份的压力所确定。其值均受低压塔的压力制约，这一方面因为待精馏的含氩馏份来源于低压塔之故，另一方面因为用于冷却的馏份紧接着被输入低压塔之故。对这两股气流中的任一股进行辅助压缩，这在经济上是不合理的，因为这牵涉到比所得氩量大得多的输送量。
空气分离装置中精馏塔的分离级几乎仅靠塔板来实现分离。然而，一座能从氩中完全分离掉氧的精馏塔，必须包含数目大得可在塔内产生很大压差的塔板。因此，塔顶处压力的下降，要大得使塔顶气的冷凝温度低于增压塔塔底液体（30-40%氧）在低压塔压力（约1.4bar）时的气体温度。从而，不再有可能产生回流液体，在该塔中不能进行精馏。
按本发明，仍保留仅以精馏法来分离氧。在本发明装置中放弃精馏板，以具特定结构且在精馏塔内仅产生极小压降的填料或填充体抵之，藉此可使仅以精馏法分离氧成为可能。由于丝毫没有关于具特定结构的填料或填充体在空气精馏时效果的经验值，所以可先凭在较大试压装置中所得的经验来评估，在此领域中，特别在粗氩塔中，采用填料的可行性，经多次试验已知，使用150至200之间，较佳约180的理论板数，可在符合经济要求的氩收率时，使粗氩中的氧含量小于1ppm。
尤为有利的是，这种氩精馏在粗氩塔就已进行。因此，粗氩塔虽然须建造得带有高数目的分离级，并达较高的建筑高度。但是，由于不含氧的氩可直接输给纯氩精馏段，故而所产生的节约要比辅助支出大得多。不需要安装用来消除残留氧的Deoxo装置。然而，本发明的主要优点则在于，可完全省去Deoxo装置的大笔运行费用及由该装置所致的较大控制费用。
下面用附图中示意表示的实施例来更详细地阐明本发明。该图以简化形式，示出一种按本发明仅用精馏法进行的空气分离，并接着制取氩的工艺。
空气经由管道1被吸进缩气机2，并在净化级3中除去水蒸汽和二氧化碳。该空气接着在换热器4中为产品气体逆流冷却，并有一部分经由管道5被输入两级精馏塔9的增压塔10。该空气的另一部分则在换热器4中，在中等温度时分出（管道6），在涡轮机7中作功减压，并经由管道8输向低压塔11。
在冷凝蒸发器12中，出自增压塔顶部的气体逆蒸发着的低压塔塔底液体而冷凝，并以回流形式供向增压塔。氮以气态（管道15）及液态（管道14）从增压塔抽出。一部分以液体状态被抽出的氮，经由管道18作为回流液体供入低压塔。塔底液体经由管道18被抽出增压塔，并在一部分经由管道16被输至低压塔的中间部位。
气态氮（管道20）和气态氧（管道21）作为产物流从低压塔被抽出，并接着在换热器4中加热到接近环境温度。另一馏份经由管道22离开低压塔。该馏份含氧87-92%，较佳90%，含氩8-13。较佳10%，此外还含约0.05%氮，并被供入粗氩塔24的下部，粗氩塔24的塔顶冷凝器26籍经由管道17从增压塔10的塔底引过来的蒸发液体来冷却。道管17中的塔底液体含35-40%氧，并在引入塔顶冷凝器26之前，被减压到大约低压塔的压力。蒸发的部分经由管道19被引入低压塔。
粗氩塔24按本发明，装有具特定结构并相当于理论板数为170-200，较佳约180的填料，并在1.2-1.6bar，较佳1.3bar的低压塔压力下工作。代替该填料，也可使用相似的低压力损填料。仅还含约1ppm氧的氩以气态形式经由管道25被抽出。该氩的一部分在塔顶冷凝器26中予以液化，并以回流形式送回到粗氩塔中。其余部分的氩在粗氩液化器28中，在与来自增压塔的蒸发氮29进行换热的过程中，被冷凝。
由于按本发明建造的粗氩塔建筑高度很高（约30m），所以可在管道40中利用从粗氩塔塔顶所抽出粗氩的流体静位压，来产生在纯氩塔30中进行精细纯化所需的压力。
在同样可象高大精馏塔9那样，以常规方法用塔板建造的纯氩塔中，留在粗氩中的氮被分离出来。该塔的塔底用经由管道15从增压塔引过来的氮气来加热。此时冷凝下来的氮31同从增压塔以液态形式抽出的氮32一起用来冷却纯氩塔的塔顶。在纯氩塔的塔顶处，气体经由管道34被抽出，并部分地在塔顶冷凝器33中液化，然后回流到纯氩塔30中。其余部分经由管道37作为残余气体予以排放，该残余气主要由氮组成。总计还含1-10ppm杂质，最好还含3ppm杂质的液态纯氩，经由管道39被抽出。

Claims (3)

1、藉空气低温精馏来分离空气的方法，其中将空气压缩、预净化、冷却、输至两级精馏段，并分离成一种富氧馏份和一种富氮馏份，同时由精馏段低压级抽出另一富集氩的氧馏份，并在粗氩精馏段中分离成粗氩和一种难于沸腾的残余馏份，其特征在于，粗氩精馏用至少150块理论板来进行。
2、权利要求1所述的方法，其特征在于，将来自粗氩精馏段的粗氩，在纯氩精馏段中分离成纯氩和一种易于沸腾的残余馏份。
3、实施权利要求1所述方法用的装置，该装置包括一座由增压塔和低压塔组成的两级精馏塔和一座粗氩塔，其特征在于，粗氩塔中装有具有特定结构的填料或填充体。
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