CN101107489A - 通过低温蒸馏生产一氧化碳的方法和装备 - Google Patents

通过低温蒸馏生产一氧化碳的方法和装备 Download PDF

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CN101107489A
CN101107489A CNA2006800031287A CN200680003128A CN101107489A CN 101107489 A CN101107489 A CN 101107489A CN A2006800031287 A CNA2006800031287 A CN A2006800031287A CN 200680003128 A CN200680003128 A CN 200680003128A CN 101107489 A CN101107489 A CN 101107489A
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carbon monoxide
wash
absorber
methane
gas
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CN100582621C (zh
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G·特谢拉
J·佩龙
J·劳赫
N·艾克-贝劳德
J·比利
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

本发明涉及一种用于生产一氧化碳的方法，在吸附步骤期间，使用N个吸附器(4A，4B)，N等于或大于2，各吸附器按交错序列以相同的时间周期T工作，在该时间周期期间相继发生吸附阶段和再生阶段；在吸附阶段开始时，各吸附器被置于洗脱阶段，在洗脱阶段期间，仅混合物名义流量的一部分被送至所述吸附器，直到所述吸附器对一氧化碳基本达到饱和，而同时其它吸附器中的至少一个维持在吸附阶段；在整个周期中，净化后的气体混合物被部分液化生成经液化的气体混合物，所述混合物存储在一容器(7)中，并且将该经液化的气体混合物从所述容器送至至少一个用于分离出富含一氧化碳的产品的塔(11)；在吸附器洗脱阶段的至少一段时间内，所述容器中的液位下降，在周期中除洗脱阶段外的至少一段时间内，所述液位上升。

Description

通过低温蒸馏生产一氧化碳的方法和装备
技术领域
本发明涉及一种通过低温蒸馏生产一氧化碳的方法和装备。
背景技术
在通过低温蒸馏生产一氧化碳和/或氢气的方法中，必须净化待分离的气体混合物，以除去易于在低温下冻结并因此堵塞冷箱的热交换器的湿气和残存的二氧化碳。
湿气和二氧化碳通常是通过使供给气体通过容纳有多种吸附剂的干燥单元包括分子筛来截留。
事实上，分子筛具有吸附大量一氧化碳的特性。只要分子筛对一氧化碳的吸附未饱和，这一特性就会严重影响每个吸附周期起始的(一氧化碳)生产率。这些生产波动可能对下游单元不利。
WO 03/049839中所述的一种解决办法是，在每个吸附周期前进行所谓的洗脱程序(洗提程序，séquence d′élution)，在该洗脱程序中，吸附床吸附一氧化碳而逐渐达到饱和，从而在一定程度上消除生产中一氧化碳的减少。洗脱阶段是指，在该阶段期间吸附剂之一仅接收待净化流的一小部分，例如待净化流的2-10mol％。
冷箱中的另一种解决办法在EP-A-1497989中进行了说明：例如，将液态一氧化碳的容器用作一缓冲容积，从而使在洗脱阶段外积聚的一氧化碳在洗脱期间在热交换管路中再蒸发，以补偿干燥器中的损耗。不幸的是，为此所作的测试表明，由于冷平衡失调而难以实施。
发明内容
本发明在于，使用位于洗涤器(colonne de lavage)底部的缓冲容器。在冷箱的这一高度，一氧化碳作为经液化的合成气体的一部分而存在，并在洗脱阶段外积聚。当在干燥器中发生洗脱时，将缓冲容器排空，从而使一氧化碳的生产率得以稳定。
在经液化的合成气体在洗涤器底部积聚阶段期间，在一氧化碳和甲烷分离器底部液态甲烷的滞留量不断减小。相反，在洗脱阶段期间，经液化的合成气体的消耗通过液态甲烷滞留量的增加得以补偿。必要时，也可调节汽提塔(colonne d′épuisement)的液位和在热交换器中蒸发的甲烷的流速。
本发明的主要优点在于，由于总体维持了通过冷箱的低温液体的总量，因此使得冷平衡状况得以保持平衡。可调整一氧化碳透平以确保冷平衡的精确性。
本发明的第二优点在于，本发明用于使闪蒸塔及一氧化碳和甲烷分离器中部分一氧化碳的流速维持恒定。这有利于稳定运行。但是，也可通过调节CO容器(例如CO/CH4分离器顶部的一氧化碳容器)代替对合成气体在洗涤器底部的滞留量的调节。
本发明的主要目的在于，提供一种通过分离气体混合物来生产一氧化碳、可选地生产氢气的方法，该方法包括吸附分离步骤，该吸附分离步骤之后进行低温分离步骤，其中：
i)在吸附步骤期间，使用N个吸附器，N等于或大于2，各吸附器按交错序列以相同的时间周期T工作，在该时间周期中相继发生吸附阶段和再生阶段；在吸附阶段开始时，将各吸附器置于洗脱阶段；在洗脱阶段期间，仅混合物名义流量的一部分被送至吸附器，直到该吸附器对一氧化碳基本达到饱和，同时使其它吸附器中的至少一个维持在吸附阶段，
ii)其特征在于，在整个周期中，将净化后的气体混合物部分液化，以生成经液化的气体混合物，所述混合物存储在一容器中，将经液化的气体混合物从该容器送至至少一个用于分离出富含一氧化碳的产品的塔；在吸附器洗脱阶段的至少一段时间内，所述容器中的液位下降，在周期中除洗脱阶段外的至少一段时间内，所述液位上升。
根据本发明的其它可选方面：
-所述容器为低温分离塔的底部；
-所述容器中经液化的气体混合物的液位在整个周期中除洗脱阶段外上升，和/或所述容器中经液化的气体混合物的液位仅在洗脱阶段期间下降；
-所述气体混合物至少包含一氧化碳、氢气和甲烷，将净化后的气体混合物的一部分送至甲烷洗涤器，富含氢气的气体在甲烷洗涤器顶部流出，将富含一氧化碳的液体从甲烷洗涤器送至汽提塔的顶部，富含一氧化碳的液体在该汽提塔的底部流出并将其送至一氧化碳和甲烷分离器，富含甲烷的液体在该一氧化碳和甲烷分离器的底部流出并将其至少一部分送至甲烷洗涤器的顶部，并且富含一氧化碳的气流在该一氧化碳和甲烷分离器的顶部流出；
-将气体混合物从所述容器送至所述汽提塔；
-在一氧化碳和甲烷分离器底部富含甲烷的液体的体积在周期中除洗脱阶段外的至少一段时间内减少，并且该体积在洗脱阶段的至少一段时间内增加；
-在汽提塔底部的富含一氧化碳的液体体积在周期中除洗脱阶段外的至少一段时间内减少，和/或该体积在洗脱阶段的至少一段时间内增加。
本发明的第二个目的在于，提供一种用于通过分离气体混合物生产一氧化碳和/或氢气的装备，该装备包括一吸附单元和一低温分离单元，其中：
i)该吸附单元包括：N个吸附器，N等于或大于2；用于将气体混合物送至吸附器的装置；以及用于将净化后的气体混合物从吸附器送至低温分离单元的装置；
ii)该低温分离单元包括一冷箱和位于该冷箱中的甲烷洗涤器、汽提塔、一氧化碳和甲烷分离器和经液化的气体混合物容器以及用于以吸附周期的函数控制容器中液位的装置。
根据本发明的其它方面：
-所述经液化的气体混合物容器与所述甲烷洗涤器的底部及所述汽提塔相连通；
-所述经液化的气体混合物容器内置于所述甲烷洗涤器中。
根据本发明的第三方面，提供一种用于通过分离气体混合物生产一氧化碳和/或氢气的装备，该装备包括一吸附单元和一低温分离单元，其中：
a)该吸附单元包括：N个吸附器，N等于或大于2；用于将气体混合物送至吸附器的装置；以及用于将净化后的气体混合物从吸附器送至低温分离单元的装置；
b)该低温分离单元包括一冷箱和位于该冷箱中的构成经液化的气体混合物容器的相分离器、至少一个汽提塔、用于使富含一氧化碳的流体从汽提塔之一流出的装置以及用于以吸附周期的函数控制容器中液位的装置。
附图说明
下面参考附图详细说明本发明，附图中：
图1示出本发明的一氧化碳和氢气第一生产单元；
图2和3示出容器和CO/CH4分离器的底部在周期T内液位的变化；以及
图4示出本发明的一氧化碳和氢气第二生产单元。
具体实施方式
在图1中，将合成气体流1送至净化单元3，以除去大部分杂质、尤其是湿气和二氧化碳。该气体混合物包括作为主要成分的氢和一氧化碳，以及可选地包括次要成分如氮和甲烷，并包括作为杂质的湿气和二氧化碳。
净化单元3包括并列放置的两个吸附器4A、4B，它们交替用于通过吸附来净化气体混合物。各吸附器包括设置成层状的吸附材料。未用于吸附的吸附器利用气体、可选地利用来自低温蒸馏单元的气体进行再生。在第一步骤即洗脱阶段期间，吸附器4A仅接收待净化流的一部分，约为该流的5％，其余的待净化流被送至吸附器4B。当吸附器4A对一氧化碳达到吸附饱和时，开始进行第二步骤——其中两吸附器4A、4B各接收50％的待净化流。而后，在第三步骤中，吸附器4A处于吸附阶段而吸附器4B处于再生阶段。在第四步骤期间，吸附器4A处于吸附阶段末期而吸附器4B转入洗脱阶段，吸附器4A接收95％的待净化流，而吸附器4B接收5％的待净化流，直到吸附器4B对一氧化碳达到饱和。在第五步骤中，两吸附器各接收50％的待净化气体混合物，以及在第六步骤即最后的步骤中，吸附器4B发生吸附而吸附器4A发生再生。
因此，在一周期中，如有N个吸附器就有N个洗脱阶段，从而使得各吸附器在从所有待净化流中吸附杂质之前已对一氧化碳达到饱和。
在洗脱步骤期间，由于一氧化碳的滞留，送往蒸馏的气体混合物的流量减少约1％。
然后，送至冷箱F的饱和气体在热交换器5中冷却并在部分液化后从该热交换器输出。随后将该流送至甲烷洗涤器9下方的容器7。来自容器7的蒸气到达洗涤器9的底部。在整个周期中，将该容器中的液体在中间高度送至汽提塔，而该汽提塔的顶部供有来自甲烷洗涤器的底部液体。阀V1用于将液体输送至汽提塔11，位于该容器中的液位检测器控制该阀V1的开启。富含氢气的气体15在甲烷洗涤器9的顶部流出，并在热交换器5中加热。
容器7可如图所示内置于洗涤器9中，也可与之分开或由洗涤器9的底部构成。
富含甲烷的液体在汽提塔11的底部流出，并将其送至甲烷和一氧化碳分离器13的中间高度。阀V2用于将液体输送至CO/CH4分离器13，位于汽提塔11底部的液位检测器控制该阀V2的开启。
富含氢气的气体17在汽提塔11的顶部流出。该被称为FG的流体在热交换器5中加热。
来自CO/CH4分离器13底部的液体，一部分17被泵送至甲烷洗涤器的顶部，而一部分19经由一受CO/CH4分离器底部18中的液位控制的阀V3泵送以生产富含甲烷的液体产品。CO/CH4分离器的顶部利用一氧化碳循环21按已知的方式冷却。富含一氧化碳的气体23在CO/CH4分离器的顶部流出，并在热交换器5中加热。
除洗脱阶段外，送至甲烷洗涤器的净化后的气体流量6保持恒定。至少在吸附器之一处于吸附阶段而另一个吸附器处于再生阶段时，离开容器7的流8受到控制，从而使得液位上升，如图2所示。在洗脱阶段期间，净化后的气体混合物的流量6减小，且该流量6与周期其余阶段内的流量相比，其中一氧化碳被消耗。至少在各洗脱阶段的一段时间内、优选在各洗脱阶段开始时，更多液体8流出，从而使得容器中的液位降低。在随后的步骤中，当待处理的气体的流量在两吸附器4A和4B之间以50％平均分配时、以及其后至少在吸附器之一处于吸附阶段时，该液位重新上升。
这样，在各洗脱阶段的至少一段时间内从所述容器输送额外液体，从而补偿送往低温蒸馏的气体混合物在洗脱阶段期间一氧化碳的消耗。
为使所述冷平衡状况得以平衡，控制CO/CH4分离器底部18的液位，以使其在洗脱阶段上升而在周期其余阶段内下降，如图3所示。
也可通过控制下述特征中的至少一个来代替或补充这一平衡手段：
-汽提塔中的液位，
-甲烷洗涤器中的液位，
-一氧化碳循环的透平23的速度。
这样即可使得一氧化碳的流速基本保持不变。
本发明还适用于一种通过局部冷凝生产一氧化碳的装备。来自吸附单元4A、4B的净化后的合成气体流1A进入冷箱F，在热交换器D中冷却并部分液化。在构成根据本发明的容器的相分离器(séparateur de phases)A中进行相分离。来自该相分离器的富含氢气的气体2A被送至热交换器D。来自该相分离器的液体8A在阀V1的控制下被送至第一汽提塔B，并在该汽提塔中分离出将在热交换器D中被加热的富含氢气的流6A。液体6A发生膨胀并被送至第二汽提塔，该第二汽提塔生产出作为上部气体的富含一氧化碳的气体5A和作为底部液体的富含甲烷的液体7A。
容器A中的液位检测器控制用于将液体8A输送至第一汽提塔B的阀V1的开启。除洗脱阶段外，送至容器A的净化后的气体1A的流量保持恒定。至少在吸附器之一处于吸附阶段而另一吸附器处于再生阶段时，控制离开容器7的流量8A，从而使得液位上升，如图2所示。在洗脱阶段期间，净化后的气体混合物1A的流量减小，该流量1A与周期其余阶段内的流量相比，其中一氧化碳被消耗。至少在各洗脱阶段的一段时间内、优选在各洗脱阶段开始时，更多液体8A流出，从而使得容器中液位下降。在随后的步骤中，当待处理的气体的流量在吸附器4A和4B之间以50％平均分配时、以及随后至少在吸附器之一处于吸附阶段时，所述液位重新上升。

Claims (11)

1.一种通过分离气体混合物生产一氧化碳、以及可选地生产氢气的方法，该方法包括吸附分离步骤，该吸附分离步骤之后进行低温分离步骤，其中：
i)在吸附步骤期间，使用N个吸附器(4A，4B)，N等于或大于2，各吸附器按交错序列以相同的时间周期T工作，在该时间周期期间相继发生吸附阶段和再生阶段；在吸附阶段开始时，将各吸附器置于洗脱阶段，在该洗脱阶段期间，仅混合物名义流量的一部分被送至该吸附器，直到该吸附器对一氧化碳基本达到饱和，同时使其它吸附器中的至少一个维持在吸附阶段，
ii)其特征在于，在整个周期中，将净化后的气体混合物部分液化以生成经液化的气体混合物，所述混合物存储在一容器(7，A)中，将经液化的气体混合物从该容器送至至少一个用于分离出富含一氧化碳的流体的塔(11，B)，并且，在吸附器洗脱阶段的至少一段时间内，该容器中的液位下降，而在周期中除洗脱阶段外的至少一段时间内，所述液位上升。
2.根据权利要求1所述的方法，其特征在于，所述容器为一低温分离塔(9)的底部部分。
3.根据权利要求1或2所述的方法，其特征在于，所述容器中经液化的气体混合物的液位在整个周期中除洗脱阶段外上升，和/或所述容器中经液化的气体混合物的液位仅在洗脱阶段期间下降。
4.根据权利要求1或2所述的方法，其特征在于，所述气体混合物至少包含一氧化碳、氢气和甲烷，将所述净化后的气体混合物的一部分送至甲烷洗涤器(9)，富含氢气的气体在该甲烷洗涤器的顶部流出，将富含一氧化碳的液体从甲烷洗涤器送至汽提塔(11)的顶部，富含一氧化碳的液体在该汽提塔的底部流出并被送至一氧化碳和甲烷分离器(13)，富含甲烷的液体在该一氧化碳和甲烷分离器的底部流出并至少部分地被送至所述甲烷洗涤器的顶部，并且富含一氧化碳的气流在所述一氧化碳和甲烷分离器的顶部流出。
5.根据权利要求4所述的方法，其特征在于，将所述经液化的气体混合物从所述容器(7)送至所述汽提塔(11)。
6.根据权利要求4或5所述的方法，其特征在于，所述一氧化碳和甲烷分离器(13)的底部(18)中富含甲烷的液体的体积在周期中除洗脱阶段外的至少一段时间内减少，且该体积在洗脱阶段的至少一段时间内增加。
7.根据权利要求4、5和6之一所述的方法，其特征在于，所述汽提塔底部(18)中富含一氧化碳的液体的体积在周期中除洗脱阶段外的至少一段时间内减少，和/或该体积在洗脱阶段的至少一段时间内增加。
8.用于通过分离气体混合物生产一氧化碳和/或氢气的装备，该装备包括一吸附单元和一低温分离单元，其中：
i)所述吸附单元包括：N个吸附器(4A，4B)，N等于或大于2；用于将气体混合物送至所述吸附器的装置；以及用于将净化后的气体混合物从所述吸附器送至所述低温分离单元的装置；并且
ii)所述低温分离单元包括一冷箱(F)和位于该冷箱中的甲烷洗涤器(9)、汽提塔(11)、一氧化碳和甲烷分离器(13)、经液化的气体混合物容器(7)以及用于以吸附周期的函数控制所述容器中液位的装置(V1)。
9.根据权利要求8所述的装备，其特征在于，所述经液化的气体混合物容器(7)与所述甲烷洗涤器(9)的底部及所述汽提塔(11)相连通。
10.根据权利要求9所述的装备，其特征在于，所述经液化的气体混合物容器内置于所述甲烷洗涤器中。
11.用于通过分离气体混合物生产一氧化碳和/或氢气的装备，该装备包括一吸附单元和一低温分离单元，其中：
i)所述吸附单元包括：N个吸附器(4A，4B)，N等于或大于2；用于将气体混合物送至所述吸附器的装置；以及用于将净化后的气体混合物从所述吸附器送至所述低温分离单元的装置；以及
ii)所述低温分离单元包括：一冷箱(F)和一位于该冷箱中构成经液化的气体混合物容器的相分离器(A)、至少一个汽提塔(B，C)、用于使富含一氧化碳的流体从汽提塔之一流出的装置以及用于以吸附周期的函数控制所述容器中液位的装置(V1)。
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EP1844282B1 (fr) 2013-04-17
FR2881063B1 (fr) 2007-04-20
US20100055021A1 (en) 2010-03-04
WO2006079736A1 (fr) 2006-08-03
US8192525B2 (en) 2012-06-05
FR2881063A1 (fr) 2006-07-28

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