CN105008835B - 在低于环境的温度下分离包含二氧化碳和较轻杂质的气态混合物 - Google Patents

在低于环境的温度下分离包含二氧化碳和较轻杂质的气态混合物 Download PDF

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CN105008835B
CN105008835B CN201480009699.6A CN201480009699A CN105008835B CN 105008835 B CN105008835 B CN 105008835B CN 201480009699 A CN201480009699 A CN 201480009699A CN 105008835 B CN105008835 B CN 105008835B
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phase
splitter
gas
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admixture
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A·布里格利亚
M·莱克勒克
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

一种用于分离气体混合物的设备，所述气体混合物包含至少35mol％的二氧化碳并且还包括至少一种比二氧化碳更轻的气体，所述设备包括：第一分相器(15)；用于将第一部分地冷凝的流从交换线路传送到第一分相器的导管；冷却装置(23)；用于运送来自第一分相器的、比气体混合物包含更少二氧化碳的气体使其被冷却装置冷却以形成第二部分地冷凝的流的导管；第二分相器(27)；用于将第二部分地冷凝的流送到第二分相器的导管；第一阀(21)；用于运送从第一分相器抽出的、比所述气体混合物包含更多二氧化碳的液体使其在所述第一阀中膨胀以将该液体的压力减小最多300mbar并形成第一膨胀液体的导管；以及用于将第一膨胀液体与来自第三阀上游的第二分相器的第二液体混合的混合装置。

Description

在低于环境的温度下分离包含二氧化碳和较轻杂质的气态混 合物
本发明涉及在低于环境的温度下分离包含二氧化碳和较轻气体的气体混合物。具体地，包括用于分离包含至少35mol％的二氧化碳和至少一种较轻气体的气体混合物的方法和设备。较轻气体可以从以下列表中选取：一氧化碳、氢气、甲烷、氧气、氮气、氩气。
气体混合物可以包括至少45mol％的二氧化碳或至少55mol％的二氧化碳或至少65mol％的二氧化碳或至少75mol％的二氧化碳。
分离的目的是产生比被分离的混合物更富含二氧化碳的流体。该流体可以是处于环境压力下的气体、处于比环境压力更高的压力下的气体或加压液体。可以通过蒸发液体来产生气体。
可以通过根据本发明的方法来分离的混合物的示例有：
-来自产生富氢流的吸附过程的残余气体以及包含至少35mol％的二氧化碳和至少氢气的残余气体；
-来自氧-燃料燃烧过程的残余气体，在该过程中燃料在存在氧的情况下燃烧以产生包含至少55mol％的二氧化碳和至少氧气和氮气的残余气体。
用于在低于环境的温度下分离二氧化碳的单元包括在低于环境的温度下的步骤(有时称为低温步骤)，其中加压并干燥的混合物从至少一种其它气体分离。
低于环境的温度下的步骤基本上至少包括一个冷却步骤和一个部分冷凝步骤。具体地，在低于环境的温度下的步骤中处理的气体必须被冷却到接近二氧化碳的三相点的温度，在-56℃附近。在这些温度下，气体将部分冷凝，液体特别地富含二氧化碳。然后需要利用分离罐将液体与气体分离。来自该分离罐的液体通常膨胀，随后被送到蒸馏塔以在其中被净化。
塔的选择压力可以远低于分离罐的压力。以示例的方式，在关于来自SMR(蒸汽甲烷重整器)PSA H2的残余气体来捕获二氧化碳的情况下，部分冷凝压力选为50bara附近，而塔的压力为11bara附近。由罐产生的平衡的液体在阀中的膨胀将产生部分气化，导致阀出口处温度大幅下降。如果阀之前液体的温度接近CO2的三相点，阀的出口处的温度可能变为低于CO2的三相点的温度。恐怕存在液体中包含并集中的CO2冻结的重大风险。
用于限制该冷却和相关的冻结风险通常选择的方案在于在来自罐的液体膨胀之前对其进行加热。但是该方案具有一个主要缺点：由于来自罐的液体处于平衡，对其进行的加热将产生部分气化。因此两相混合物将进入膨胀阀。后者将更难以控制：调节阀的开度的物理参数(例如压力、流量)的测量将被气体的出现中断，气体的物理特性与液体显著不同；由该受中断的测量导致的阀的打开和关闭将对阀出口处流体特性产生不可预知的作用。由于阀的入口处气体和液体各自的速度以及特别地由于两相流模式，阀也可能更迅速地退化。
根据本发明的一个主题，提供了一种用于分离气体混合物的方法，所述气体混合物包含至少35mol％的二氧化碳或甚至至少45mol％的二氧化碳，并且还包括至少一种比二氧化碳更轻的气体，其中：
i)所述混合物被冷却以形成第一部分地冷凝的流，
ii)所述第一部分地冷凝的流被送到第一分相器，
iii)来自所述第一分相器的、比所述气体混合物包含更少的二氧化碳的气体在未经压缩的情况下被冷却，以形成第二部分地冷凝的流，
iv)所述第二部分地冷凝的流被送到第二分相器，
v)从所述第一分相器抽出的、比所述气体混合物包含更多二氧化碳的液体在未经加热的情况下在第一阀中膨胀以将其压力减小最多300mbar，以形成第一膨胀液体，
vi)所述第一膨胀液体与来自所述第二分相器的第二液体混合，以形成包含至少99.9％的液体的流体，所述第二液体在与所述第一膨胀液体混合之前没有膨胀或被加热，所述第一膨胀液体的温度大于所述第二液体的温度，
vii)第三流体在第二阀中膨胀至一压力，使得膨胀的第三流体中二氧化碳的分压大于5.28bar(绝对压力)并且膨胀的第三流体的温度高于-54.5℃，以及
viii)膨胀的第三流体在未经加热的情况下至少部分地被送到腔室和/或间接热交换器，来自所述第二分相器的所述第二液体如果在没有与第一膨胀液体混合的情况下膨胀到所述腔室和/或所述间接热交换器的压力，其将达到低于-54.5℃的温度。
根据本发明的其它可选方面：
-膨胀的第三流体的至少一部分被送到粗/简单蒸馏塔的顶部以对所述塔进行供应并在所述塔中进行分离，从所述塔的顶部抽出气体，并且从所述塔的底部抽出相对于所述气体混合物富含二氧化碳的液体；
-来自所述塔的富含二氧化碳的液体通过与来自所述第一分相器的所述气体的热交换而被加热，或至少部分蒸发，所述气体在步骤iii)中被冷却，优选地在专用的间接热交换器中被冷却；
-富含二氧化碳的液体通过与步骤i)中被冷却的所述气体混合物的热交换而蒸发；
-膨胀的第三流体的至少一部分被送到第三分相器，并且通过与步骤i)的所述气体混合物的热交换，来自所述第三分相器的气体被加热和/或来自所述第三分相器的液体蒸发；
-膨胀的第三流体的至少一部分被送到间接热交换器而被加热或蒸发，以形成富含二氧化碳的气体；
-第一分相器和第二分相器以及适当情况下的第三分相器是执行相当于单个理论塔板的分离的分相器。
根据本发明的另一主题，提供了一种用于分离气体混合物的设备，所述气体混合物包含至少35mol％的二氧化碳或甚至至少45mol％的二氧化碳，并且还包括至少一种比二氧化碳更轻的气体，所述设备包括：交换线路，用于将要被冷却的混合物送到所述交换线路以形成第一部分地冷凝的流的导管；分相器；用于将所述第一部分地冷凝的流从所述交换线路送到第一分相器的导管；冷却装置；用于传送来自所述第一分相器的、比所述气体混合物包含更少二氧化碳的气体以使其在未经压缩的情况下通过所述冷却装置被冷却以便形成第二部分地冷凝的流的导管；第二分相器；用于将所述第二部分地冷凝的流送到所述第二分相器的导管；第一阀；用于传送从所述第一分相器抽出的、比所述气体混合物包含更多二氧化碳的液体使其在所述第一阀中膨胀以将该液体的压力减小最多300mbar并形成第一膨胀液体的导管，其中在所述第一阀的上游和所述第一分相器的下游没有加热装置；用于将所述第一膨胀液体与来自所述第二分相器的第二液体混合以形成包含至少99.9％的液体的流体的混合装置，其中在所述混合装置的上游不包括用于膨胀或加热所述第二液体的装置，所述设备配置为使得在使用中所述第一膨胀液体的温度大于所述第二液体的温度；第二阀，其用于将第三流体膨胀至一压力，使得膨胀的第三流体中二氧化碳的分压大于5.28bar绝对压力并且膨胀的第三流体的温度高于-54.5℃；用于将膨胀的第三流体从所述第二阀至少部分地送到腔室和/或间接热交换器的导管，其中在所述第二阀和所述腔室或间接热交换器之间没有加热装置。
根据其它可选的特征，该设备包括：
-粗蒸馏塔，所述第二阀连接到所述塔的顶部，以对所述塔供应膨胀的第三流体的至少一部分并使其在所述塔中进行分离；用于从所述塔的顶部抽出气体的导管；以及用于从所述塔的底部抽出相对于所述气体混合物富含二氧化碳的液体的导管；
-用于传送来自所述塔的富含二氧化碳的液体以使其在所述冷却装置中通过与来自所述第一分相器的气体的热交换而被加热，或至少部分蒸发的装置；
-作为腔室的第三分相器、用于将膨胀的第三流体的一部分送到所述第三分相器的导管、以及用于传送膨胀流的一部分使其通过与来自所述第一分相器的气体混合物的热交换而被加热的导管；
-第三分相器、用于将膨胀的第三流体的至少一部分送到所述第三分相器的导管、以及用于传送来自所述第三分相器的液体以使其通过与步骤i)的所述气体混合物的热交换而被加热的装置；
-第三分相器、用于将膨胀的第三流体的至少一部分送到所述第三分相器的导管、以及用于传送来自所述第三分相器的气体使其通过与步骤i)的所述气体混合物的热交换而被加热的装置；
-间接热交换器和用于将膨胀的第三流体的至少一部分传送到所述间接热交换器以在其中被加热的导管。
本发明可以获得在阀入口处充分热的液体以避免膨胀阀出口处过低的温度。问题是以第一温度T1执行第一部分冷凝，随后以接近CO2的三相点的第二温度T2执行第二部分冷凝(T1>T2)。来自第一罐的液体和来自第二罐的液体的混合物将处于介于T1和T2之间的中间温度，并且不产生蒸气，因为来自混合物的液体将也处于平衡。实际上，混合物的组分将处于来自第一罐的液体的组分和来自第二罐的液体的组分之间。本发明中也将有更少的能量损失，因为用于加热阀入口处液体的热交换借助直接接触发生。
两个部分冷凝步骤可以在两个独立的交换器中执行，或在技术允许的情况下在相同的交换器中执行(例如钎焊式铝交换器)。
将参照附图更详细描述本发明，图中示出了根据本发明的用于分离气体混合物的方法。
在图1中，气体混合物1在压缩机3中被压缩到23bar的压力。在冷却器5中冷却后，冷却流7在提纯单元9中去除水以产生干燥的气体混合物11。应理解，如果混合物1是干燥的并且加压的，这些步骤则是可选的。对于该示例，流11包含87％的CO2、4％的氧气、5％的氮气、3.9％的氩气和0.1％的一氧化碳。处于环境温度的气体流11被送到钎焊式铝板热交换器13，在此被冷却到-36℃并部分冷凝。部分冷凝的流被送到第一分相器15，产生顶部气体19和底部液体17。底部液体包含98％的二氧化碳、0.6％的氧、0.7％的氮、0.8％的氩和少量一氧化碳。气体19富含轻质污染物/杂质并仅包含64％的二氧化碳。气体19在交换器23中被冷却到-52.5℃的温度，接近二氧化碳的三相点的温度。因此，气体部分冷凝。部分冷凝的流25被送到第二分相器27。形成的气体29在交换器13和加热器31中被加热以在涡轮机35中从23bar膨胀以提供冷量。膨胀的流37在交换器13的冷端处被再次引入，被加热，然后被加热器39加热，以便能够以已知方式再生提纯单元9。已经用于再生的气体41被送到大气。
交换器23可以是钎焊式铝板交换器或壳管式交换器。气体19在其中经历约0.2bar的小压降。
从分相器27产生的液体43包含97％的二氧化碳并处于22.9bar和-52.5℃。如果该液体膨胀到较低的压力以被送到后续步骤，形成的液体的温度将低于三相点，导致形成固体颗粒。
为了避免该问题，液体43(27 700kg/h)与来自第一分相器的液体45混合。液体45通过膨胀来自第一分离器15的底部液体17(131 969kg/h)产生，以将交换器23中的压降考虑在内。该0.2bar的小膨胀在阀21中执行。膨胀的液体45处于-36℃。
因此，通过混合液体43、47，形成的液体(称为第三流体)处于-39℃。
当第三流体在第二阀47中膨胀时，形成的流是处于-47℃的温度和11bar绝对压力的两相流。流49被送到汽提塔51的顶部，其构成汽提塔51的唯一进气流。来自塔51的顶部气体81在交换器13中被加热并被送到压缩机3。底部液体53被一分为二。一部分55在阀57中膨胀后在交换器23中部分蒸发。蒸发的部分59在交换器13中被加热，在产物压缩机67中被压缩并在冷却器69、73中被冷却至冷凝。剩下的液体部分61在泵75中加压并与冷凝后的流59混合以形成富含二氧化碳的液体产物76，其包含至少70％的二氧化碳或甚至至少90％的二氧化碳。该产物76在泵77中加压以形成加压的产物79。
底部液体的另一部分在热交换器13中蒸发并且形成的气体一分为二。一部分63被送回塔以用于执行再沸腾，并且余下的部分65被送到压缩机67。
图2与图1的不同在于不存在汽提塔51。这里，两个存在形成固态二氧化碳的风险的阀是阀56、57。来自第二分相器27的液体43如图1那样与膨胀的液体45混合以增大温度。形成的第三流体46一分为二，一部分55被送到阀57以在其中膨胀，另一部分被送到阀56。由于加热，阀56、57下游的温度没有降到三相点。在阀57中形成的液体在交换器23中部分蒸发，如图1。来自阀56的液体58是两相液体并被送到第三分相器60。来自第三分相器60的气体62在交换器中被加热并且液体64在其中蒸发。形成的两股气体混合以形成在产物压缩机67中被加压的流65。
根据本发明的方法和设备也可以用于分离比示例更少富含CO2或更多富含CO2的混合物。
例如通过将在第二阀中膨胀的流的一部分送到蒸馏塔并将另一部分送到间接热交换器和/或第三分相器，可以结合图1和图2的各方面。

Claims (13)

1.一种用于分离气体混合物(1、7、11)的方法，所述气体混合物(1、7、11)包含至少35mol％的二氧化碳，以及至少一种比二氧化碳轻的气体，其中：
i)所述混合物被冷却以形成第一部分地冷凝的流，
ii)所述第一部分地冷凝的流被送到第一分相器(15)，
iii)来自所述第一分相器的、比所述气体混合物包含更少二氧化碳的气体(19)在未经压缩的情况下被冷却，以形成第二部分地冷凝的流，
iv)所述第二部分地冷凝的流被送到第二分相器(27)，
v)从所述第一分相器抽出的、比所述气体混合物包含更多二氧化碳的液体(17)在未经加热的情况下在第一阀(21)中膨胀以将其压力减小最多300mbar，以形成第一膨胀液体，
vi)所述第一膨胀液体(45)与来自所述第二分相器的第二液体(43)混合，以形成包含至少99.9％的液体的第三流体，所述第二液体在与所述第一膨胀液体混合之前没有膨胀或被加热，所述第一膨胀液体的温度大于所述第二液体的温度，
vii)所述第三流体在第二阀(47、56、57)中膨胀至一压力，使得膨胀的第三流体中二氧化碳的分压大于5.28bar绝对压力并且所述膨胀的第三流体的温度高于-54.5℃，以及
viii)膨胀的第三流体在未经加热的情况下至少部分地被送到腔室(51、60)和/或间接热交换器(23)，来自所述第二分相器的所述第二液体如果在没有与所述第一膨胀液体混合的情况下膨胀到所述腔室和/或所述间接热交换器的压力，其将达到低于-54.5℃的温度，
其中，所述方法包括下列步骤(a)和(b)中的一者：
(a)膨胀的第三流体(49)的至少一部分被送到粗蒸馏塔(51)的顶部以供给所述粗蒸馏塔并在所述粗蒸馏塔中进行分离，从所述粗蒸馏塔的顶部抽出气体(81)，并且从所述粗蒸馏塔的底部抽出相对于所述气体混合物富含二氧化碳的液体(53)，富含二氧化碳的液体(53)通过与在步骤i)中被冷却的所述气体混合物(11)的热交换而蒸发；
(b)膨胀的第三流体的至少一部分被送到第三分相器(60)，并且通过与步骤i)的所述气体混合物(11)的热交换，来自所述第三分相器的气体(62)被加热和/或来自所述第三分相器的液体(64)蒸发。
2.根据权利要求1所述的方法，其中，来自所述粗蒸馏塔(51)的富含二氧化碳的液体(53)通过与步骤iii)的来自所述第一分相器的被冷却的所述气体(19)的热交换而被加热，或甚至至少部分蒸发。
3.根据权利要求1或2所述的方法，其中，膨胀的第三流体的至少一部分被送到交换线路(13)而被加热或甚至蒸发，以形成富含二氧化碳的气体(65)。
4.根据权利要求1或2所述的方法，其中，第一分相器(15)和第二分相器(27)以及在适当情况下第三分相器(60)是执行相当于单个理论塔板的分离的分相器。
5.根据权利要求1所述的方法，其中，所述气体混合物(1、7、11)包含至少45mol％的二氧化碳。
6.根据权利要求2所述的方法，其中，来自所述粗蒸馏塔(51)的富含二氧化碳的液体(53)在间接热交换器(23)中通过与来自所述第一分相器的所述气体(19)的热交换而被加热，或甚至至少部分蒸发。
7.一种用于分离气体混合物的设备，所述气体混合物包含至少35mol％的二氧化碳，并且还包括至少一种比二氧化碳轻的气体，所述设备包括：交换线路(13)；用于将要被冷却的混合物送到所述交换线路以形成第一部分地冷凝的流的导管；第一分相器(15)；用于将所述第一部分地冷凝的流从所述交换线路传送到所述第一分相器的导管；冷却装置；用于传送来自所述第一分相器的、比所述气体混合物包含更少二氧化碳的气体以使其在未经压缩的情况下通过所述冷却装置被冷却以便形成第二部分地冷凝的流的导管；第二分相器(27)；用于将所述第二部分地冷凝的流送到所述第二分相器的导管；第一阀(21)；用于传送从所述第一分相器抽出的、比所述气体混合物包含更多二氧化碳的液体使其在所述第一阀中膨胀以将该液体的压力减小最多300mbar并形成第一膨胀液体的导管，其中在所述第一阀的上游和所述第一分相器的下游没有加热装置；用于将所述第一膨胀液体与来自所述第二分相器的第二液体混合以形成包含至少99.9％的液体的流体的混合装置，其中在所述混合装置的上游不包括用于膨胀或加热所述第二液体的装置，所述设备配置为使得在使用中所述第一膨胀液体的温度大于所述第二液体的温度；第二阀(47、56、57)，其用于将第三流体膨胀至一压力，使得膨胀的第三流体中二氧化碳的分压大于5.28bar绝对压力并且膨胀的第三流体的温度高于-54.5℃；用于将膨胀的第三流体从所述第二阀至少部分地送到腔室(51、60)和/或间接热交换器(23)的导管，其中在所述第二阀和所述腔室或间接热交换器之间没有加热装置，
其中，所述设备还包括下面(a)和(b)中的一者：
(a)粗蒸馏塔(51)，所述第二阀(47)连接到所述粗蒸馏塔的顶部，以将膨胀的第三流体的至少一部分传送到所述粗蒸馏塔的顶部以供给所述粗蒸馏塔并使其在所述粗蒸馏塔中进行分离；用于从所述粗蒸馏塔的顶部抽取气体(81)的导管；用于从所述粗蒸馏塔的底部抽取相对于所述气体混合物富含二氧化碳的液体(53)的导管；以及用于传送来自所述粗蒸馏塔的富含二氧化碳的液体(53)以使其在所述交换线路(13)中蒸发的装置；
(b)第三分相器(60)、用于将膨胀的第三流体的至少一部分(58)送到所述第三分相器的导管、以及用于传送来自所述第三分相器的液体(64)以使其通过与步骤i)的所述气体混合物(11)的热交换而被加热的装置。
8.根据权利要求7所述的设备，包括用于传送来自所述粗蒸馏塔(51)的富含二氧化碳的液体(53)以使其通过在所述冷却装置中与来自所述第一分相器的气体(19)的热交换而被加热，或至少部分蒸发的装置。
9.根据权利要求7所述的设备，包括作为所述腔室的第三分相器(60)、用于将膨胀的第三流体的一部分(58)送到所述第三分相器的导管、以及用于传送膨胀流的一部分(55)以使其通过与来自所述第一分相器(15)的气体混合物的热交换而被加热的导管。
10.根据权利要求7或9所述的设备，包括第三分相器(60)、用于将膨胀的第三流体的至少一部分(58)送到所述第三分相器的导管、以及用于传送来自所述第三分相器的气体(62)以使其通过与步骤i)的所述气体混合物(11)的热交换而被加热的装置。
11.根据权利要求7至9中任一项所述的设备，其中，所述冷却装置是交换线路(13)。
12.根据权利要求7至9中任一项所述的设备，其中，所述冷却装置是除交换线路(13)以外的热交换器。
13.根据权利要求7所述的设备，其中，所述气体混合物包含至少45mol％的二氧化碳。
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