CN105745506A - 用于使至少包含一氧化碳、氢气和氮气的混合物深冷分离的方法和装置 - Google Patents

用于使至少包含一氧化碳、氢气和氮气的混合物深冷分离的方法和装置 Download PDF

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CN105745506A
CN105745506A CN201480063530.9A CN201480063530A CN105745506A CN 105745506 A CN105745506 A CN 105745506A CN 201480063530 A CN201480063530 A CN 201480063530A CN 105745506 A CN105745506 A CN 105745506A
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nitrogen
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A·费尔南德斯
P·马蒂
B·普拉萨德
M-P·维克托
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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使一氧化碳、氢气和氮气的混合物深冷分离的装置，其包括汽提塔(2)和脱氮塔(4)、用于将液体形式的混合物(13)送至汽提塔顶部的管道、连接到汽提塔的用于移除脱除氢气的液体(15,16)的管道、用于由汽提塔移除富含氢气的气体(14)的管道、用于将脱除氢气的液体(16)或由所述液体得到的流体送至脱氮塔的设备、用于由脱氮塔取出富含一氧化碳的液体(22)的管道、用于由脱氮塔顶部取出富含氮气的气体(21)的管道以及用于将至少一部分富含氢气的气体送至脱氮塔的设备。

Description

用于使至少包含一氧化碳、氢气和氮气的混合物深冷分离的方法和装置
本发明涉及用于使至少包含一氧化碳、氢气和氮气的混合物深冷分离的方法和装置。氮气含量可波动。
已知的做法是使用至少一个用于降低CO中的H2含量的汽提塔和随后的为CO/N2分离塔的氮脱除塔通过深冷蒸馏分离该混合物。
在CO/N2塔顶部的顶部冷凝器为“水浴汽化器”类型。
当混合物中的N2含量(其意指进入CO/N2塔的N2含量)远低于作为设计CO/N2塔的基础使用的含量时，安装的冷凝器实际上具有导致所有CO/N2混合物在罐底部冷凝的过量热交换表面积，其结果是不能再维持塔操作压力。然后，不再可能维持待产生的CO的纯度并且导致单元停车的风险。减少冷凝器的交换表面积的一种方法是降低浴液面(液体CO-部分“未淹没”冷凝器)，但受限于由以下事实引起的这种原则：冷凝器为“热虹吸”型，即设计用于要求最小液体进料的再循环速率以使得正确操作，所需液体的最小压头不一定对应其需要设定以控制非常低的N2含量的压头。
在CO/N2塔中与极低N2含量相关的风险通常通过将气态N2导入和注入供给塔的不纯CO管线的可能性而补偿，以保证“水浴汽化器”冷凝器的操作稳定性和塔中操作压力的稳定性。
FR-A-2895067和WO-A-2008/099124描述了如果混合物中的氮气含量下降，则使用氮气加料的解决方法。
EP-A-0928936和由LindeAG所著的“CryogenicGasSeparation:Themosteconomicandexperiencedseparationprocessforproductionofcarbonmonoxideandhydrogenfromrawsynthesisgas”描述了根据最近的现有技术的方法。
本发明的一个主题提供了一种用于使至少包含一氧化碳、氢气和氮气的混合物深冷分离的方法，其中：
将液体形式的混合物送入汽提塔顶部，其中它分离形成贫氢液体和富氢气体，并且将贫氢液体或由该液体得到的流体送至氮脱除塔，其中它分离形成富一氧化碳液体和包含大部分存在于混合物中的氮气的富氮气体，
其特征在于：
-如果混合物和/或富氮气体和/或者变体ii)的情况下的富一氧化碳气体的氮气含量在阈值以下，则
i)将来自汽提塔的富氢气体的至少一部分送至氮脱除塔的中间点，或者
ii)如果流体在分离塔中通过蒸馏而由贫氢液体得到，则将来自汽提塔的富氢气体的至少一部分送至塔的中间点而送至分离塔，将富一氧化碳气体由分离塔顶部移除并将来自分离塔顶部的顶部冷凝器的未冷凝的气体送至氮脱除塔。
根据其他任选主题：
-在变体ii)中，混合物包含甲烷，并且将贫氢液体送至分离塔，后者在顶部具有顶部冷凝器，在底部产生富甲烷液体，并且在塔的顶部将富一氧化碳气体分离出来。
-富氮气体流速的检测器引发将富氢气体送至分离塔或者送至氮脱除塔。
-在变体ii)的情况下，氮脱除塔顶部的富氮流速度的检测器引发将在冷凝器中未冷凝的气体送至氮脱除塔。
-在变体ii)的情况下，通过分离塔顶部的富一氧化碳气体上的压力检测器，使分离塔与氮脱除塔在压力方面解耦。
-在变体ii)的情况下，其中使冷凝器中未冷凝的气体与富一氧化碳气体混合。
-在变体ii)的情况下，其中仅在混合物和/或富一氧化碳气体和/或富氮气体的氮气含量在阈值以下时，将富氢气体的至少一部分在分离塔中间点送至分离塔并将来自顶部冷凝器的在其中未冷凝的气体送至氮脱除塔。
-在变体ii)的情况下，混合物为来自甲烷洗涤塔的底部液体，洗涤液体来自分离塔底部。
-混合物为来自相分离器的液体。
-在变体i)中由贫氢液体得到的流体通过借助阀使该液体膨胀而产生。
本发明的另一主题提供一种用于使一氧化碳、氢气和氮气以及可能的甲烷的混合物深冷分离的装置，其包括汽提塔、氮脱除塔和可能的在顶部具有顶部冷凝器的分离塔、用于在汽提塔顶部运送液体形式的混合物的管道、用于移除贫氢液体的管道(该管道连接到汽提塔)、用于由汽提塔移除富氢气体的管道、用于将贫氢液体或由该液体得到的流体送至氮脱除塔的设备、用于将富一氧化碳液体由氮脱除塔分离的管道和用于将富氮气体由氮脱除塔顶部分离的管道，其特征在于它包括用于将富氢气体的至少一部分或由该气体得到的流体送至氮脱除塔的设备。
该装置可包括在顶部具有顶部冷凝器的分离塔且其中用于将由富氢气体得到的流体送至氮脱除塔的设备包括用于将富氢气体的至少一部分送至贫氢液体分离塔的管道，该管道连接到分离塔的中间点，以及用于将来自顶部冷凝器的在其中未冷凝的气体送至氮脱除塔的管道。
该装置可包括在顶部具有顶部冷凝器的分离塔、用于由汽提塔移除贫氢液体的连接到分离塔的管道、用于移除富氢气体的连接到分离塔的管道，以及包括用于由分离塔顶部移除富一氧化碳气体的管道和用于将来自分离塔顶部的顶部冷凝器(6)的未冷凝的气体送至氮脱除塔的管道。
该装置可包括用于检测混合物和/或富氮气体和/或富一氧化碳气体的氮气含量的设备，以及用于调整送至氮脱除塔的富氢气体的至少一部分或由该气体得到的流体的流速的设备。
该装置可包括用于使用混合物和/或富一氧化碳气体和/或富氮气体的氮气含量的检测器和/或混合物和/或富一氧化碳气体和/或富氮气体的流速的检测器，将富氢气体的至少一部分在分离塔中间点送至分离塔或者送至氮脱除塔的设备。
本发明创新性特征在于其通过将一些来自CO/N2塔上游的汽提塔的顶部气体输入CO/N2塔中而补偿氮气的减少：来自汽提塔的顶部气体包含氢气可使得提高至CO/N2塔的不可冷凝物的流速。
该新管线的流速通过流速控制设备(FIC)控制。
在汽提塔和CO/N2塔之间装配不可冷凝物的旁通管道提供以下优势：
·CO/N2塔的操作压力不再取决于不纯CO中的氮气含量(由供入合成气产生单元的天然气导致的)。
·当冷箱进料气体中N2含量证明为太低时，不存在气态氮气输入。
本发明将通过参考显示本发明装置的附图更详细地说明。
在图1中，将一氧化碳、氮气和氢气的混合物10在交换器9中冷却并送至蒸馏塔1(或分离器)。富氢顶部气体12离开塔1的顶部并在交换器9中加热。使底部液体13膨胀且然后送至在底部通过再沸器8加热的汽提塔2的顶部。将富氢顶部气体14在交换器9中加热且然后燃烧。使主要包含氮气和一氧化碳的底部液体15膨胀并送至氮脱除塔4的中部。将富一氧化碳底部液体送至交换器18，其中其用于使来自氮脱除塔的顶部气体冷凝。在氮脱除塔4中，富氮气体21离开塔的顶部。
如果氮气21的流速降至给定阈值以下，则管道26的阀打开并将富氢气体由汽提塔顶部送至氮脱除塔4，优选将其与通过借助阀使来自管线16的液体膨胀而形成的气体混合。
根据图2，待分离的混合物包含氮气、氢气、甲烷和一氧化碳。
已知的做法是使用深冷蒸馏，使用CO/CH4分离塔和随后的CO/N2分离塔分离该混合物。
不使用来自CO/CH4塔的不可冷凝物(H2-N2)：将它们直接送至火炬或者送至燃料网络。
CO/CH4和CO/N2塔在相等压力下操作。
创新性特征在于通过将来自CO/CH4塔上游的汽提塔的顶部气体(其包含氢气)输入CO/CH4塔且然后通过将来自CO/CH4塔的不可冷凝物输入CO/N2塔而补偿氮气的减少。
将所有或部分来自汽提塔的顶部气体(其包含氢气)收集从而送至CO/CH4塔的进料。
由于该新管线，可提高至CO/CH4塔的不可冷凝物的流速。
然后在CO/CH4塔的顶部(其包含氢气且不包含甲烷)回收所有或一些不可冷凝物从而经由供入CO/N2塔的不纯CO管线导入CO/N2塔。由于该其他新管线，如果在CO中氮气不足，则也可维持CO/N2塔中的压力：氢气的存在补偿氮气的不足。
新管线各自的流速通过FIC控制。
CO/CH4塔中的压力需要略微提高，从而使得确保不可冷凝物的料流将确实导入CO/N2塔。
不纯CO的流速通过附加至CO/CH4塔的PIC控制，以使塔的两个操作压力可彼此解耦。
然后，使在CO/N2塔的顶部的不可冷凝物借助经由交换管线通过的N2净化管线导入燃料网络。
一氧化碳、氮气、氢气和甲烷的混合物10在交换器9中冷却并送至顶部供有液体甲烷11的甲烷洗涤塔1或者送至分离器。富氢顶部气体12离开塔1的顶部并在交换器9中加热。使底部液体13膨胀且然后送至在其底部通过再沸器8重新加热的汽提塔2的顶部。使富氢顶部气体14在交换器9中加热且然后燃烧。使主要包含甲烷和一氧化碳的底部液体15膨胀并送至具有底部再沸器7和顶部冷凝器6的蒸馏塔3的中部。不可冷凝的气体的料流22离开该冷凝器6。富一氧化碳顶部气体16离开塔3并送至氮脱除塔4。通过泵5泵送富甲烷底部液体并分成两部分。一部分20在交换器9中汽化，并且将剩余部分作为料流11供至洗涤塔1。
在氮脱除塔4中，富氮气体21离开塔顶部并且富含一氧化碳的液体22离开底部。一氧化碳在为水浴汽化器的顶部冷凝器18中汽化。
管道26将塔2的顶部气体出口14连接到进入塔3的液体管道15。同样，管道24容许将不可冷凝气体由冷凝器6送至氮脱除塔，特别是使其与气体16混合。
仅在料流10或者16中的氮气减少时，操作这两个管道。当检测到氮气减少时，将所有或部分来自汽提塔2顶部的顶部气体送至CO/CH4塔3的进料。借助该新管道，可提高至CO/CH4塔的不可冷凝物的流速。
然后，回收所有或部分来自CO/CH4塔3顶部的顶部冷凝器6的不可冷凝物从而经由供入CO/N2塔的不纯CO管线16送至CO/N2塔。借助该其他新管道26，在CO中的氮气不足时，可由此维持CO/N2塔4中的压力：氢气的存在补偿了氮气的不足。
新管道24、26各自中的流速通常在通过交换管线9之后通过检测来自CO/N2塔4顶部的氮气净化21中氮气的最小纯度的检测器控制。
CO/CH4塔3的压力需要略微升高，从而使得确保不可冷凝物的料流将确定导入CO/N2塔4。
不纯CO16的流速通过附加至CO/CH4塔的压力控制器控制，以使得塔的两个操作压力可彼此解耦。
然后，使CO/N2塔顶部包含氢气的不可冷凝物借助经由交换管线通过的氮气净化管道21导入燃料网络。
附图中的元件列表
1洗涤塔或分离器
2汽提塔
3甲烷/一氧化碳分离塔
4一氧化碳/氮气分离塔
5甲烷泵
6甲烷/一氧化碳分离塔冷凝器
7甲烷/一氧化碳分离塔再沸器
8汽提塔再沸器
9热交换器
10合成气进料
11洗涤甲烷进料
12富氢气体
13汽提塔进料
14汽提塔顶部气体
15甲烷/一氧化碳分离塔进料
16一氧化碳/氮气分离塔进料
17液体一氧化碳回流
18一氧化碳/氮气分离塔冷却器
19泵送的液体甲烷
20液体甲烷净化
21氮气净化
22低压一氧化碳
23不可冷凝物
24将富氢气体带入塔3的管道
26将不可冷凝物带入塔4的管道
30冷箱

Claims (13)

1.一种用于使至少包含一氧化碳、氢气和氮气的混合物深冷分离的方法，其中：将液体形式的混合物(13)送至汽提塔(2)的顶部，其中它分离形成贫氢液体(15,16)和富氢气体(14)，将贫氢液体(16)或由该液体得到的流体(16)送至氮脱除塔(4)，其中它分离形成富一氧化碳液体(22)和包含大部分存在于混合物中的氮气的富氮气体(21)
其特征在于：
-如果混合物和/或富氮气体和/或在变体ii)的情况下富一氧化碳气体(16)的氮气含量在阈值以下，则
i)将来自汽提塔的富氢气体(26)的至少一部分送至氮脱除塔的中间点，或者
ii)如果流体在分离塔(3)中通过蒸馏而由贫氢液体得到，则将来自汽提塔的富氢气体(14)的至少部分(26)送至分离塔的中间点，使富一氧化碳气体由分离塔顶部移除，并且将来自分离塔顶部的顶部冷凝器(6)的未冷凝的气体(24)送至氮脱除塔。
2.如权利要求1所述的方法，其中，在变体ii)中，混合物包含甲烷，并且将贫氢液体(15)送至分离塔(3)，后者在顶部具有顶部冷凝器，在底部产生富甲烷液体(19)，并且使富一氧化碳气体(16)在塔的顶部分离。
3.如前述权利要求中任一项所述的方法，其中富氮气体(21)流速的检测器引发将富氢气体(26)送至分离塔(3)或送至氮脱除塔(4)。
4.如前述权利要求中任一项所述的方法，其中，在变体ii)的情况下，在氮脱除塔顶部的富氮流速度的探测器引发将在冷凝器(6)中未冷凝的气体(24)送至氮脱除塔。
5.如前述权利要求中任一项所述的方法，其中，在变体ii)的情况下，其中通过在分离塔顶部的富一氧化碳气体(16)上的压力检测器(PIC)，使分离塔(3)与氮脱除塔(4)在压力方面解耦。
6.如前述权利要求中任一项所述的方法，对于变体ii)，其中使在冷凝器中未冷凝的气体(24)与富一氧化碳气体(16)混合。
7.如前述权利要求中任一项所述的方法，对于变体ii)，其中仅在混合物和/或富一氧化碳气体和/或富氮气体的氮气含量在阈值以下时，将富氢气体(26)的至少一部分在分离塔的中间点送至分离塔(3)并且将来自顶部冷凝器的在其中未冷凝的气体(24)送至氮脱除塔(4)。
8.如前述权利要求中任一项所述的方法，其中，在变体ii)的情况下，混合物为来自甲烷洗涤塔(1)的底部液体(13)，洗涤液体(11)来自分离塔(3)的底部。
9.如权利要求1所述的方法，其中在变体i)中由贫氢液体得到的流体通过借助阀使液体(16)膨胀而产生。
10.一种用于使一氧化碳、氢气和氮气以及可能的甲烷的混合物深冷分离的装置，其包括汽提塔(2)、氮脱除塔(4)和可能的在顶部具有顶部冷凝器(6)的分离塔(3)、用于运送汽提塔顶部的液体形式的混合物(13)的管道、用于移除贫氢液体(15,16)的连接到汽提塔的管道、用于由汽提塔移除富氢气体(14)的管道、用于将贫氢液体(16)或由该液体得到的流体送至氮脱除塔的设备、用于使富一氧化碳液体(22)由氮脱除塔分离的管道和用于使富氮气体(21)由氮脱除塔顶部分离的管道，其特征在于其包括用于将富氢气体的至少一部分或由该气体得到的流体送至氮脱除塔的设备。
11.如权利要求10所述的装置，其包括在顶部具有顶部冷凝器(6)的分离塔(3)、用于由汽提塔移除贫氢液体(14)的连接到分离塔的管道、用于移除富氢气体的连接到分离塔的管道，并且包括用于由分离塔顶部移除富一氧化碳气体(16)的管道和用于将来自分离塔顶部的顶部冷凝器(6)的未冷凝的气体(24)送至氮脱除塔的管道。
12.如权利要求10或11所述的装置，其包括用于检测混合物和/或富氮气体和/或富一氧化碳气体(16)的氮气含量的设备以及用于调整送至氮脱除塔的富氢气体的至少一部分或由该气体得到的流体的流速的设备。
13.如权利要求10、11或12所述的装置，其包括用于利用混合物和/或富一氧化碳气体和/或富氮气体的氮气含量的检测器和/或混合物和/或富一氧化碳气体和/或富氮气体的流速的检测器，将富氢气体的至少一部分在分离塔的中间点送至分离塔或者送至氮脱除塔的设备。
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