CN109311665B - 用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物以及还有一氧化碳的方法和设备 - Google Patents

用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物以及还有一氧化碳的方法和设备 Download PDF

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CN109311665B
CN109311665B CN201780034465.0A CN201780034465A CN109311665B CN 109311665 B CN109311665 B CN 109311665B CN 201780034465 A CN201780034465 A CN 201780034465A CN 109311665 B CN109311665 B CN 109311665B
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column
liquid
nitrogen
methane
carbon monoxide
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CN109311665A (zh
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伯特兰·德蒙莱恩斯
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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

用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物以及一氧化碳的方法，其中在洗涤塔(15)的第一中间高度处引入富甲烷液体(45)作为第一次洗涤液并且在高于该洗涤塔的第一高度的高度处引入至少一种富氮液体(73)作为第二洗涤液，并且从该洗涤塔中抽取出作为塔顶气体(27)的氢气和氮气的混合物。

Description

用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物 以及还有一氧化碳的方法和设备
技术领域
本发明涉及一种用于通过低温蒸馏和低温洗涤联合生产任选地构成氨合成气的氢气和氮气的混合物、以及还有一氧化碳和任选的甲烷的方法和设备。
背景技术
已知使用EP 0 465 366中描述的甲烷洗涤型工艺，以便将合成气分离成其各种组分。该工艺具体地是基于使用在CO/CH4塔底部处回收的富甲烷流体的一部分作为前两个塔的洗涤流体，然后该流体的其他部分以甲烷吹扫的形式被回收。
通过洗涤甲烷与塔的塔顶气体之间的热力学平衡，然后在这两个塔的塔顶气体中损失一部分甲烷。在EP 0 317 851中描述了洗涤汽提塔以便增加产率。
因此，必须在任何时刻在有待处理的气体中具有足够量的甲烷以便补偿这些甲烷损失。如果有待处理的合成气不含有足够的甲烷，则将不可能按原样使用该工艺。因此，必须使用富甲烷气体的补充，以便人为地增加有待处理的进入气体中的甲烷含量，以能够进行如DE 37 41 906 A1中所述的甲烷洗涤。
与甲烷洗涤相比，使用部分冷凝工艺显著降低了CO提取率。在这种情况下，必须消耗更多的上游“燃料”(天然气、石脑油、煤等)以生产合成气，以便获得相同的一氧化碳产量。
还已知使用在洗涤塔中用液氮处理富氢气体以便产生合成氨所需的气体混合物，该气体混合物具有在3H2/1N2附近的化学计量。
某些文献，诸如EP 0 937 681 A1，已解决了CO和用于氨的气体的共生产问题。然而，其主要缺点在于：
·降低CO提取率(典型地在洗涤塔中间的液体吹扫中损失约8％-10％的CO)
·或使CO产物被氮气污染(然后需要另外的塔和能量来重新分离该混合物)。
发明内容
本发明的目的是将一氧化碳的生产与用于生产氨的混合物的生产相结合。向洗涤塔的顶部添加另外的区段，以便依次用(从顶部到底部)氮气和甲烷洗涤合成气。在CO产物中将不会发现添加的氮气。然而，在没有脱氮塔的情况下，在出口处在CO产物中将发现入口处合成气中存在的氮气。还可以添加汽提塔，这将使得可以回收一部分甲烷，这些甲烷原本将随洗涤塔塔顶气体而损失掉。该汽提塔可以由具有单个理论塔板的室形成，该室例例如为能够实现相当于几个理论塔板的分离的分离容器或分离室。
该甲烷的另外回收可以使得可能：
在合成气中使用用少量甲烷进行的甲烷洗涤工艺。典型地，由ATR产生的合成气在甲烷中非常贫乏，为约1mol％。
在入口处的合成气中低于0.4mol％的甲烷含量变得足以进行甲烷洗涤。
·否则
o将必须进行部分冷凝工艺，具有显著的CO产率损失
o将必须输入另外的气体G1，以便人为地增加有待处理的进入气体中的甲烷含量，以能够进行如DE 37 41 906 A1中所述的甲烷洗涤。因此，对于相同的CO生产处理了更多的气体，这需要更大的设备和/或更大的能量消耗：这可能潜在地输入气体G1中存在而不是合成气中存在的杂质，然后将必须处理这些杂质。
o还可以进行如EP 0 790 212 A1中所述的甲烷的内部再循环，这也使得可以帮助
·回收更多的甲烷，以便然后能够将其作为液体或气体生产。
将这两个工艺相结合还使得可以仅使用单个冷箱而不是两个冷箱，并且相对于常规甲烷洗涤还可以减小CO涡轮机的尺寸，并且因此减少CO循环流量(并且因此消耗更少能量)。实际上，氮气和氢气的混合是吸热的，这使得可以通过除CO涡轮机之外的装置产生冷量。
根据本发明的一个主题，提供了一种用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物、一氧化碳以及任选的甲烷和任选的氮气的方法，其中：
i)将至少含有氢气、一氧化碳和甲烷的气体混合物在热交换器中冷却，
ii)将冷却的混合物送至洗涤塔，
iii)在洗涤塔的第一中间高度处引入富甲烷液体作为第一洗涤液，
iv)在高于洗涤塔的第一高度的高度处引入至少一种富氮液体作为第二洗涤液，
v)将氢气和氮气的混合物作为塔顶气体从洗涤塔中抽取出，
vi)将底部液体从洗涤塔中抽取出并送至汽提塔，
vii)将与洗涤塔的中间区段处于同一高度的液体抽取出，将该液体送至热交换器、或汽提塔塔顶气体管线、或第二汽提塔，
viii)将底部液体从汽提塔中抽取出并送至用于分离一氧化碳和甲烷的塔，
ix)来自分离塔的底部液体的至少一部分构成步骤iii)的液体，并且
x)将富含一氧化碳的流体从分离塔中抽取出。
根据本发明的其他任选的方面：
-该方法至少部分地通过在涡轮机中膨胀富含一氧化碳的流体的至少一部分或来自汽提塔的塔顶气体的至少一部分来保持冷却，
-该方法至少部分地通过在热交换器的中间温度下和/或热交换器的冷端温度下将来自洗涤塔的塔顶气体与源自外部源的富氮液体混合来保持冷却，
-洗涤塔、汽提塔和分离塔在同一个隔热外壳中，
-该气体混合物含有至多0.4mol％的甲烷，并且构成用于该方法的甲烷的唯一来源，但不构成内部再循环的甲烷的唯一来源，
-来自分离塔的底部液体的一部分在热交换器中蒸发后，以液体形式或气体形式作为富甲烷产物回收，
-来自步骤iv)的富氮液体源自外部源并且不包含在热交换器上游的气体混合物中，
-来自步骤iv)的富氮液体不源自外部源并且包含在热交换器上游的气体混合物中，
-来自步骤iv)的第一富氮液体源自外部源并且不包含在热交换器上游的气体混合物中，并且来自步骤iv)的第二富氮液体不源自外部源并且包含在换热器上游的气体混合物中，
-将该至少一种富氮液体送至洗涤塔的顶部，
-将从洗涤塔的中间区域中抽取出的气体用从分离塔抽取出的富含一氧化碳的液体冷却，并且将冷却的气体送回洗涤塔，
-来自洗涤塔的塔顶气体每一份氮气含有至少五份、或甚至至少九份氢气，并且任选地富含氮气以达到三份氢气，
-气体混合物含有氮气，并且送至洗涤塔的富氮液体的至少一部分源自脱氮塔，该脱氮塔净化氮气的富含一氧化碳的流体，
-产生的富甲烷液体含有至少一种其他重烃，诸如乙烷。
根据本发明的另一主题，提供了一种用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物、一氧化碳以及甲烷和任选的氮气的设备，该设备包括热交换器，洗涤塔，汽提塔，用于分离一氧化碳和甲烷的塔，用于输送有待冷却的至少含有氢气、一氧化碳和甲烷的气体混合物的管线，用于将冷却的混合物从热交换器送至洗涤塔的管线，用于在洗涤塔的第一中间高度处引入富甲烷液体作为第一洗涤液的管线，至少一条用于在高于洗涤塔的第一高度的高度处引入富氮液体作为第二洗涤液的管线，用于将氢气和氮气混合物作为塔顶气体从洗涤塔中抽取出的管线，用于将底部液体从洗涤塔中抽取出并将底部液体从洗涤塔送至汽提塔的管线，用于将与洗涤塔的中间区段处于同一高度的液体抽取出并将该液体送至热交换器、或汽提塔塔顶气体管线、或第二汽提塔的管线，用于将底部液体从汽提塔中抽取出并将该底部液体送至用于分离一氧化碳和甲烷的塔的管线，来自分离塔的底部液体的至少一部分构成富甲烷液体，以及用于将富含一氧化碳的流体从分离塔中抽取出的管线。
本发明的原理是，以甲烷洗涤工艺开始，在洗涤塔的顶部处添加区段。洗涤塔的第一(底部)区段以常规方式用液体甲烷处理合成气。然后气体将继续到第二区段。在整合第二区段之前，可以将气体用液体CO冷却至-181℃，以便回收将被冷凝的甲烷(以与FR 2 807505中所述方式类似的方式)。将洗涤塔底部液体常规地送至汽提塔，然后送至CO/CH4塔。
在第二(顶部)区段中，将气体用氮气洗涤。然后回收来自该第二区段的底部液体并且将该底部液体直接蒸发(图1)、或送至第二汽提塔(图2)。该第二汽提塔在大约3巴的压力下操作。将该第二汽提塔的底部再加热，以便降低液体的氮浓度，从而不使CO产物被氮气污染。将来自该塔底部的液体送至CO/CH4塔。在传递中回收了一小部分CO(进入CO流量的约0.1％)，这也使得可以增加CO产率。将来自第二汽提塔的塔顶气体在主交换器中再加热，然后吹扫。
因此，将在氮气洗涤之后不再含有甲烷的洗涤塔塔顶气体直接送至交换器7，或送至蒸发器-冷凝器，以便从LP CO产生液体CO。(具体地，N2/H2混合是吸热的并且该气体的温度是大约-193℃。)
可以混合调节H2/N2比率所需的氮气：
i)直接在低温下(即没有在交换器中或在冷端处再加热富氢洗涤塔塔顶气体)和/或
ii)在交换器的中间高度处(即在主交换器中部分再加热洗涤塔塔顶气体之后)。
这两种解决方案使得可以产生冷量并且因此减少通过涡轮机的冷量补充。
还可以在高温下进行混合，也就是说在主交换器的下游进行混合，这通常使得可以减少投入。
可以将该气体混合物以与塔顶部相同的方式直接送至交换器7，或送至蒸发器-冷凝器以便从LP CO产生液体CO，或者用于以与FR 2 807 504类似方式冷却甲烷洗涤塔区段。
还可以在低温下或在交换器的中间高度处部分地加入氮气并且进行最终混合，以便在高温下实现期望的化学计量。
附图说明
将参照示出根据本发明的方法的三个图更详细地说明本发明。
具体实施方式
根据图1的方法，在净化单元3中使至少含有氢气、一氧化碳和甲烷的合成气流1净化掉水、二氧化碳、甲醇和其他杂质，并且然后在热交换器7中冷却干合成气流5，该热交换器优选地是钎焊铝板交换器。将冷却的气体送至相分离器9，并且将形成的气体11送至洗涤塔15的底部。在洗涤塔15的中间高度(称为第一中间高度)处向该洗涤塔供给富甲烷液体45作为第一洗涤液。在高于洗涤塔15的第一高度的高度处引入富氮液体73作为第二洗涤液。将氢气和氮气的混合物作为塔顶气体27从洗涤塔15中抽取出，并且将底部液体从洗涤塔中抽取出。来自洗涤塔的塔顶气体27每一份氮气含有至少五份、或甚至至少九份氢气，并且富含氮气以达到三份氢气。
将来自洗涤塔的底部液体17与来自相分离器9的液体13混合，并且将混合物29送至汽提塔31的顶部。将中间液体28在洗涤塔51的第一中间高度处抽取出并且送至在热交换器7中蒸发。如果没有该抽取出，则富含一氧化碳的产物将被氮气污染。将底部液体35从汽提塔31中抽取出并在热交换器7中冷却之后送至用于分离一氧化碳和甲烷的塔37的中间高度处。来自分离塔37的底部液体41的至少一部分45在泵47中加压之后构成第一洗涤液。在分离塔37的顶部处抽取出富含一氧化碳的流体53。分离塔37在塔顶部处包括液体一氧化碳的储器39。将气体53和来自储器的气体作为气体55送至一氧化碳压缩机57，以便提供富含一氧化碳的产物59。一氧化碳的一部分61在热交换器7中冷却并分成两部分；一部分63在涡轮机67和阀69中膨胀，以便再加热并送回压缩机57。剩余部分65用于使塔31和37再沸腾并供给储器39。
将来自储器39的液体一氧化碳49用于在第一洗涤液的入口下方的某一点处冷却洗涤塔的中间流体。室21接收该液体，并且将液体23送至交换器19，以便冷却中间流。将来自该室的气体25送回压缩机57。
闪蒸气体33离开汽提塔31的顶部，并且富甲烷产物43任选地以液体形式从CO/CH4塔37中抽取出并在交换器7中蒸发。
图2的方法与图1的方法的不同之处在于添加了第二汽提塔77，该第二汽提塔在约3巴下操作。在顶部处供给在第一洗涤液的入口上方取出的液体，该液体通过一氧化碳循环加热。将底部液体79在与流35相同的高度处送至CO/CH4塔37。
为了达到所需的氢气和氮气的比率，可以将来自外部源的氮气在热交换器上游和/或热交换器的中间高度处和/或热交换器下游添加到来自洗涤塔的塔顶气体中。
在这两个附图的实例中应理解，来自洗涤塔的塔顶气体可以含有氢气和氮气，氢气和氮气处于氨或非氨合成气所需的3:1比率。在存在的氮气不足的情况下，如图2所示可以在该塔的出口处添加氮气，以便实现所需的比率。
在图3中，添加了脱氮塔89。在底部处供给源自压缩机57的一氧化碳65，该脱氮塔在底部处产生供给压缩机57的无氮一氧化碳。将在塔89的顶部处产生的富氮流膨胀、液化并作为洗涤液送至塔15的顶部。在这种情况下，可以减少流73，或甚至不需要供应除供给气体1之外的氮气。在该实例中，将液体91在液体73的入口下方引入到塔15中。

Claims (12)

1.一种用于通过低温蒸馏和低温洗涤联合生产氢气和氮气的混合物、一氧化碳的方法，其中：
i)将至少含有氢气、一氧化碳和甲烷的气体混合物在热交换器(7)中冷却，
ii)将冷却的混合物送至洗涤塔(15)，
iii)在该洗涤塔的第一中间高度处引入富甲烷液体(45)作为第一洗涤液，
iv)在高于该洗涤塔的该第一中间高度的高度处引入至少一种富氮液体(73，91)作为第二洗涤液，
v)将氢气和氮气的混合物作为塔顶气体(27)从该洗涤塔中抽取出，
vi)将底部液体(17)从该洗涤塔中抽取出并送至汽提塔(31)，
vii)将液体(28，75)从该洗涤塔的该第一中间高度处抽取出，将该液体送至该热交换器、或汽提塔塔顶气体管线、或第二汽提塔，
viii)将底部液体(35)从该汽提塔中抽取出并送至用于分离一氧化碳和甲烷的分离塔(37)，
ix)来自该分离塔的底部液体(41)的至少一部分构成该步骤iii)的富甲烷液体，并且
x)将富含一氧化碳的流体(53)从该分离塔中抽取出。
2.如权利要求1所述的方法，其中该方法通过以下方式保持冷却
i)至少部分地通过在涡轮机(67)中膨胀该富含一氧化碳的流体的至少一部分或来自该汽提塔的该塔顶气体的至少一部分，和/或
ii)至少部分地通过在该热交换器(7)的中间温度下和/或该热交换器的冷端和/或热端温度下将来自该洗涤塔的该塔顶气体与源自外部源的富氮液体(73A，73B，73C)混合。
3.如前述权利要求中任一项所述的方法，其中该洗涤塔(15)、该汽提塔(31)和该分离塔(37)在同一个隔热外壳中。
4.如权利要求1或2所述的方法，其中该气体混合物含有至多0.4mol％的甲烷并且构成用于该方法的甲烷的唯一来源。
5.如权利要求1或2所述的方法，其中来自该分离塔的该底部液体的一部分在该热交换器(7)中蒸发后，以液体形式或气体形式作为富甲烷产物回收。
6.如权利要求1或2所述的方法，其中来自步骤iv)的该富氮液体(73)源自外部源并且不包含在该热交换器(7)上游的气体混合物中。
7.如权利要求1或2所述的方法，其中将该富氮液体(73，91)送至该洗涤塔的顶部。
8.如权利要求1或2所述的方法，其中将从该洗涤塔的中间区域抽取出的气体用从该分离塔抽取出的富含一氧化碳的液体冷却，并且将该冷却的气体送回该洗涤塔。
9.如权利要求1或2所述的方法，其中来自该洗涤塔的该塔顶气体(27)每一份氮气含有至少五份氢气。
10.如权利要求9所述的方法，其中来自该洗涤塔的该塔顶气体(27)每一份氮气含有至少九份氢气。
11.如权利要求9所述的方法，其中来自该洗涤塔的该塔顶气体(27)富含氮气以达到三份氢气。
12.一种用于通过低温蒸馏联合生产氢气和氮气的混合物、一氧化碳的设备，该设备包括热交换器(7)，洗涤塔(15)，汽提塔(31)，用于分离一氧化碳和甲烷的分离塔(37)，用于输送有待冷却的至少含有氢气、一氧化碳和甲烷的气体混合物的管线，用于将冷却的混合物从该热交换器送至该洗涤塔的管线，用于在该洗涤塔的第一中间高度处引入富甲烷液体作为第一洗涤液的管线，用于在高于该洗涤塔的第一中间高度的高度处引入富氮液体作为第二洗涤液的管线，用于将氢气和氮气的混合物作为塔顶气体从该洗涤塔中抽取出的管线，用于将底部液体从该洗涤塔中抽取出并将该底部液体从该洗涤塔送至该汽提塔的管线，用于将液体(28，75)从该洗涤塔的该第一中间高度处抽取出并将该液体送至该热交换器、或汽提塔塔顶气体管线、或第二汽提塔(77)的管线，用于将底部液体从该汽提塔中抽取出并将该底部液体送至该用于分离一氧化碳和甲烷的分离塔的管线，来自该分离塔的底部液体的至少一部分构成该富甲烷液体，以及用于将富含一氧化碳的流体从该分离塔中抽取出的管线。
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