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CN116724208A - 用于液化氢气的方法和设备 - Google Patents

用于液化氢气的方法和设备 Download PDF

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CN116724208A
CN116724208A CN202280010999.0A CN202280010999A CN116724208A CN 116724208 A CN116724208 A CN 116724208A CN 202280010999 A CN202280010999 A CN 202280010999A CN 116724208 A CN116724208 A CN 116724208A
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hydrogen
heat exchanger
rich gas
cooled
rich
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A·盖特纳
M-K·戚
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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

在用于液化氢气的方法中，在不将富氢气体加热到0℃以上的温度的情况下，将富氢气体(27)从通过蒸馏和/或汽提和/或部分冷凝进行的分离装置(102)送到氢气液化器，离开分离装置的气体处于至多103K的温度和20‑30巴的压力下并且包含至少99.9摩尔％的氢气。

Description

用于液化氢气的方法和设备
技术领域
本发明涉及优选集成了包含一氧化碳和氢气的混合物的低温分离的氢气液化方法和设备。
背景技术
Jean Gallarda，J3603的章节“Techniques de l’Ingénieur”中描述了氢气的液化。
氢气被冷却，然后分以下三个阶段液化：
.通过制冷单元从环境温度降至230K；
.通过第一制冷循环从230K降至约80K；
.通过第二制冷循环从约80K将至约20K。
300K和20K之间的热交换通过铜焊铝制多通道板式换热器进行。
对应于待液化气体流的通道包含催化剂，并使得有可能进行氢气的连续转化，直到实现大于95％的仲氢含量。
冷却至约80K是在用珍珠岩绝热的室内进行的。这种冷却，称为预冷，其是通过使用闭环氮循环或利用称为“增压”的添加低温液体(通常是液氮)的冷却来实现的，两者都消耗大量的能量。
从约80K到20K的冷却是在维持在大约10-6mmHg的真空室中进行的，该室的设备被多层绝热材料包围。这种包括液化的冷却是使用氢或氦循环进行的。氮循环尤其不能在如此低的温度下使用。
发明内容
本发明的一个目的是减少该方法的能量消耗，并且可能地通过取消预冷却阶段来省掉一部分装置。
根据本发明的主题，提供了一种集成了包含氢气和另一组分的第一混合物(1)的低温分离的用于液化氢气的方法，其中：
i)将第一混合物在辅助热交换器中至少冷却到120K、在120K以下的温度下通过部分冷凝和/或蒸馏和/或汽提来分离经冷却的第一混合物，以生产处于20-30巴下的含有至少一种杂质的富氢流、以及在至多103K的低温下纯化所述富氢流，以降低其该至少一种杂质的含量，从而形成富氢气体；
ii)将来自用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置的富氢气体在不将所述富氢气体加热到0℃以上的温度的情况下送到氢气液化器，在至多103K的温度下从分离装置离开的该气体含有至少99.9摩尔％的氢气、优选至少99.99摩尔％的氢气、实际上甚至至少99.999摩尔％的氢气并且处于20-30巴的压力下；
iii)将富氢气体在液化器的第一热交换器中于20巴至30巴的压力下从至多103K的温度冷却，
其特征在于，使富氢流在液化器的第二热交换器中从高于103K、优选大于0℃的温度冷却，并且使经冷却的流随后在第二热交换器中冷却，使富氢气体与压力和组成与富氢气体基本相同并且在第二热交换器中被冷却至富氢气体的温度的富氢流混合，以形成第二混合物，并且使所述第二混合物在所述第一热交换器中液化或者在已于所述第一热交换器中冷却后液化，以形成液态氢。
根据本发明的其他可选方面，其可以与科学和逻辑兼容的任何方式组合：
·通过吸附来纯化所述富氢气体，以除去所述至少一种杂质，所述至少一种杂质是一氧化碳和/或氮气和/或甲烷；
·第一混合物包含氢气和一氧化碳作为主要成分并且可能还含有甲烷和/或氮气；
·富氢气体从蒸馏或汽提塔或相分离器中被提取出，所述塔或分离器在20-30巴的绝对压力下操作；
·该方法至少部分地通过制冷循环保持低温/冷量，该循环的流体在第一热交换器和任选的第二热交换器中被加热和冷却；
·液化氢储存在储罐中，其蒸发/气化气体在第一和第二热交换器中被加热；
·富氢气体在第一绝热室内部、在第一热交换器中或在第一热交换器下游被液化，并且在第二绝热室内部，第一混合物被冷却和/或分离，并且可选地，富氢流被纯化；
·富氢气体与具有基本相同的压力、温度和组成的富氢流混合，并且第二混合物在第一热交换器中液化或在于第一热交换器中被冷却之后液化；
.富氢流在第二热交换器中被冷却，并且随后与富氢气体混合；
.富氢气体不在第一热交换器上游与另外的气体混合。
根据本发明的另一主题，提供一种氢气液化设备，其包括液化器，该液化器包括：第一热交换器；用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置；用于将处于至多103K的温度和20-30巴的压力下的、来自所述用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置的富氢气体在不将所述富氢气体加热到0℃以上的温度的情况下输送至氢气液化器的机构，该富氢气体包含至少99.9摩尔％的氢气、优选至少99.99摩尔％的氢气、实际上甚至至少99.999摩尔％的氢气；和用于输送所述富氢气体以便在所述第一热交换器中于20-30巴的压力下从至多103K的温度冷却的机构，其特征在于，所述氢气液化设备包括：第二热交换器；用于输送富氢流以便在第二热交换器中冷却的机构；用于将富氢气体与已在第二热交换器中冷却并且具有与富氢气体基本相同的压力、温度和组成的富氢流混合以形成第二混合物的机构；以及用于输送第二混合物以便在所述第一热交换器中液化或在于所述第一热交换器中冷却后被液化以形成液态氢的机构。
优选地，所述第一交换器位于第一绝热室中，并且第二交换器位于第二绝热室中，富氢气体和富氢流的混合之处位于第一和第二室的外部。
所述设备可包括利用氦或氢以便冷却以及可选地液化第二混合物的制冷循环。
通过向液化过程供给在所需压力和所需温度下可获得的富氢气体，能减小预冷却的热交换器的尺寸，实际上如果所有进料气体都来自已经处于合适压力和合适温度下的外部来源，则甚至可完全去掉预冷却的热交换器。
用于液化经冷却的气体以形成液态氢的机构可由第一热交换器和/或由在第一热交换器下游的膨胀机构构成。
膨胀机构优选位于与热交换器相同的绝热室内，但也可位于专用绝热室内。
附图说明
将参照附图对本发明进行更详细的描述。
[图1]示出了用于生产氢气的低温分离方法。
[图2]和[图3]非常概略地示出了例如由[图1]的方法获得的氢气的液化方法。
具体实施方式
[图1]示出了使用相分离器9、甲烷洗涤塔15、汽提塔25和用于分离一氧化碳和甲烷的塔45的方法，这些塔包含例如用于塔的规整填料，并且能够在低温下操作。
含有甲烷和一氧化碳的合成气1在到达热交换器7之前，在纯化单元3中被纯化除去了水和/或二氧化碳，在热交换器7中，合成气1被冷却至低温并部分冷凝。
两相在相分离器9中分离，以形成富氢气体11和贫氢液体13。气体11被送到甲烷洗涤塔15的底部，该甲烷洗涤塔生产富氢气体19，该富氢气体19在交换器中被加热。该气体19的一部分用于再生纯化单元3。
从塔15中提取的至少一种中间气体210、211在热交换器23中通过与工艺流体(在这种情况下为液体51)进行热交换而被冷却。
来自塔15的底部液体17与来自分离器9的液体13合并，并且含有1摩尔％至3摩尔％的氢的混合物91被送至汽提塔25的顶部。来自汽提塔的顶部气体27包含至少95摩尔％的氢气并且还包括一氧化碳、氮气和甲烷。该来自汽提塔的顶部气体处于20巴至30巴下(这是塔25的操作压力)，并且具有103K至120K的温度。气体27不被加热，而是在于低温下操作的吸附单元29中被纯化，以除去一氧化碳和/或甲烷和/或氮气，从而提供能够液化的气体31，该能够液化的气体包含至少99.9摩尔％的氢气、优选至少99.99摩尔％的氢气、实际上甚至至少99.999摩尔％的氢气。这种类型的纯化描述于Kidnay等人的“The lowtemperature removal of small quantities of nitrogen or methane from hydrogengas by physical adsorption on a synthetic zeolite”，AIChE Journal，第12卷，第1期，1966年1月。
在汽提塔25底部提取的液体33在交换器7中冷却，并被送至分离塔45。相同的另一部分液体35在底部再沸器37中气化，并在汽提塔的底部返回。
分离塔包括用于通过蒸馏进行分离的多个区段和可选的容器99。它具有用于加热底部液体75的底部再沸器73，形成的气体返回到所述底部。富含甲烷的底部液体77被分成两部分。一部分83在交换器7中气化以形成燃料。剩余部分85由泵87加压，并被送到洗涤塔15的顶部。
来自塔的富含一氧化碳的顶部气体43被送至产品压缩机57，其生产富含一氧化碳的气体57。富含一氧化碳的气体中的一部分61被冷却并分成两部分。一部分65在涡轮机67中膨胀以提供冷量。经膨胀的气体89返回到压缩机57的入口。气体的剩余部分69在交换器7中继续冷却，并用来加热再沸器73和37(流93和73)。用于再沸的气体因此被部分冷凝，并作为流97供给分离塔45顶部的容器99。来自容器99的气体41供给压缩机57。来自容器99的液体47被送至相分离器49，来自分离器的液体51用作热交换器23中的制冷剂，以便冷却中间气体21A、21B、21C以及来自汽提塔的塔顶气体27。
从分离塔的分离区段提取的液体可以替代液体47或该过程/方法的另一种液体。
应当理解，存在许多方法，使得能够分离包含氢和一氧化碳作为主要组分并且可能还包含氮和/或甲烷的第一混合物。如果这些方法使得在低温和与液化器相容的压力下生产氢成为可能，那么所生产的氢可以在低温下被纯化并作为进料气体被送到液化器。
例如，在任选与蒸馏结合的部分冷凝过程中，可通过相分离器在20-30巴绝对压力下生产氢气27。
其它分离方法/过程也能够供应在低温和20-30巴的压力下的氢，例如从氨生产工艺中分离吹扫气。
与将氢加热至环境温度的过程相比，就氢在低温下离开冷过程的室而言，必须提供额外的冷量。这是通过增加冷的产生来实现的。对于一氧化碳和氢的低温分离，有必要增加一氧化碳(或N2)循环流量。
在低温和20-30巴压力下生产的氢可在绝热室中纯化，氢来自其的分离塔和/或相分离器位于该绝热室中。否则，特别是在修改现有设备的情况下，氢可从氢来自其的分离塔和/或相分离器所在的室中排出，并通过至少一个绝热管送入包含纯化设备的室102中，以降低其杂质例如一氧化碳、甲烷和氮中的至少一种的含量。
“冷”纯化是去除这样的所有杂质的必要阶段，即这些杂质可能沿着用于下降到大约20K的交换管线冻结，并因此堵塞热交换器。
[表1]
纯化前的平均摩尔纯度 纯化前可能的纯度范围 纯化后的纯度
H2 98％ 95％至99％ >99.999％
CO 0.4％ ppm至1％ <10ppb
CH4 1.2％ 0.5％至3％ <10ppb
N2 0.4％ ppm至1％ <10ppb
使用TSA(变温吸附)型单元纯化气态氢通常可在80K下进行(此温度下吸附能力高)。除去2％，实际上甚至1％的杂质需要短周期(几个小时)和高再生流量。
[图2]示出了根据本发明的方法的第一替代形式，其中[图1]的流27作为唯一的进料流体供给液化过程。
经纯化的气态氢27在20-30巴绝对压力下或者从氢来自其的分离塔和/或相分离器C所在的绝热室E中排出，或者从专用纯化室102中排出。
在没有加热到0℃以上、优选没有加热到-50℃以上、甚至没有加热到-100℃以上、甚至根本没有加热并且优选没有压缩的情况下，气态氢通过至少一个绝热管进入另一绝热室104，气态氢将在该另一绝热室处液化。
该室104包含铜焊铝制多通道板式热交换器101。
对应于待液化气体流的通道包含催化剂，并使得能够进行氢的连续转化，直到实现大于95％的仲氢含量。
室104处于维持在约10-6mmHg的真空下，室内的装置由多层绝热材料包围。在其中进行的冷却包括液化，并利用氢循环或氦循环进行。
交换器101可简单地包括：用于冷却和液化所述氢的至少一个通道，所有氢均以液体形式生产并作为产品111去除；以及针对一个或多个制冷循环所必需的通道。
可在热交换器101的热端引入已纯化的氢。
因此，可以理解，如果经纯化的氢是待液化的氢的唯一来源，或者如果所有的待液化的氢均可在待纯化的氢的温度下获得，则预冷是非必需的，并且也无需常规的第二交换器，该第二交换器用于利用其氮循环或其他制冷剂循环将氢冷却至约120K。
在其他情况下，如图3所示，将存在第二交换器103，但优选地，来自低温分离的经纯化的氢27将在用于第二交换器103的室106外部与已在第二交换器中冷却的富氢流127混合，并且所形成的混合物将随后在室104内部的液化热交换器101中冷却。
富氢流127通过从热端到冷端穿过第二交换器103而被冷却，并且公共循环105为第一和第二交换器提供冷量，而循环107仅为第二交换器103提供冷量。
图中的交换器101、103未给出冷却循环的细节，这些循环在文献中有大量描述，这些文献例如为，Walnum等人的“Principles for the liquefaction of hydrogen withemphasis on precooling processes”，IIR会议，2012，Berstad,D.O.，J.H.Stang和P.Large-scale hydrogen liquefier utilising mixed-refrigerant pre-cooling，国际氢能杂志，2010，35(10)，第4512-4523页，Quack,H.；Conceptual design ofa high efficiency large capacity hydrogen liquefier，低温工程进展：低温工程会议记录-CEC，2002，Madison,Wisconsin(USA):AIP；EP 3 339 605；EP 3 368 630；EP 3 368631；EP 3 368 844；EP 3 368 845和EP 3 759 192。
例如通常由H2循环承担的氢的液化本身可以是：
·a)直接使用剩余的将不被液化的气态氢(在29巴压力下，每50 000Nm3/h的氢气可液化约5000Nm3/h)进行。在这种情况下，这种过量的(和超纯的→不需要PSA)的氢气可在低压下或部分在中压下(例如在6巴下)被送至用户，或通过增加氢气压缩机，在至少20+巴的压力下被送至用户，
·b1)或通过独立的H2循环进行，例如在需要大量液态氢的情况下，
·b2)或通过独立的He循环进行。
本发明也可通过改进现有的合成气分离设备来使用。有必要增加制冷循环的尺寸、涡轮机的尺寸和循环压缩机冷却器的尺寸。
使用液氮增压可提供在低于环境温度下提取主要产品之一所需的冷量。
可选地，合成气1可在分离上游的热交换器103中至少部分冷却。
可选地，用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置的至少一部分可与第二热交换器布置在同一绝热室中。
待液化的氢气通常在冷却结束时于涡轮机和/或阀中膨胀。这最后一阶段并未示出。

Claims (12)

1.一种集成了包含氢气和另一组分的第一混合物(1)的低温分离的用于液化氢气的方法，其中：
i)将所述第一混合物在辅助热交换器(7)中至少冷却至120K、在120K以下的温度下通过部分冷凝和/或蒸馏和/或汽提来分离经冷却的第一混合物，以生产处于20-30巴下的含有至少一种杂质的富氢流、以及在至多103K的低温下纯化所述富氢流，以降低其所述至少一种杂质的含量，从而形成富氢气体；
ii)将来自用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置的富氢气体(27)在不将所述富氢气体加热到0℃以上的温度的情况下送到氢气液化器，在至多103K的温度下从分离装置离开的该气体含有至少99.9摩尔％的氢气、优选至少99.99摩尔％的氢气、实际上甚至至少99.999摩尔％的氢气并且处于20-30巴的压力下；
iii)将所述富氢气体在液化器的第一热交换器(101)中于20-30巴的压力下从至多103K的温度冷却，
其特征在于，使富氢流(127)在液化器的第二热交换器(103)中从高于103K的温度冷却，并且使经冷却的流随后在所述第二热交换器中冷却，使所述富氢气体(27)与压力和组成与所述富氢气体基本相同并且已在所述第二热交换器中被冷却至所述富氢气体的温度的富氢流(127)混合，以形成第二混合物，并且使所述第二混合物在所述第一热交换器(101)中液化或者在已于所述第一热交换器中冷却后液化，以形成液态氢(111)。
2.根据权利要求1所述的方法，其中，所述富氢气体(27)通过吸附(102)被纯化，以除去所述至少一种杂质，所述至少一种杂质是一氧化碳和/或氮气和/或甲烷。
3.根据权利要求1或2所述的方法，其中，所述第一混合物(1)包含氢气和一氧化碳作为主要组分并且可能还含有甲烷和/或氮气。
4.根据权利要求1、2或3所述的方法，其中，所述富氢气体(27)从蒸馏或汽提塔(C)或从相分离器中被提取出，所述塔或分离器在20-30巴的绝对压力下操作。
5.根据权利要求1至4中任一项所述的方法，其中，所述方法至少部分地通过制冷循环(105)保持低温，该循环的流体在所述第一热交换器(101)中并且可选地在所述第二热交换器(103)中被加热和冷却。
6.根据权利要求1至5中任一项所述的方法，其中，液化氢被储存在储罐中，所述液化氢的蒸发气体在所述第一热交换器和所述第二热交换器(101，103)中被加热。
7.根据权利要求1至6中任一项所述的方法，其中，所述富氢气体(27)在第一绝热室(104)内部、在所述第一热交换器(101)中或者在所述第一热交换器下游被液化，并且在第二绝热室(106)内部，所述第一混合物(1)被冷却和/或分离，并且可选地，所述富氢流(127)被纯化。
8.根据权利要求1-7中任一项所述的方法，其中，所述富氢流(127)在所述第二热交换器(103)中从0℃以上的温度冷却。
9.根据权利要求1至8中任一项所述的方法，其中，所述富氢流(127)在所述第二热交换器(103)中被冷却，并且随后与所述富氢气体(27)混合。
10.一种氢气液化设备，其包括液化器，该液化器包括：第一热交换器(101)；用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置(102)；用于将处于至多103K的温度和20-30巴的压力下的、来自所述用于通过蒸馏和/或汽提和/或部分冷凝进行分离的装置的富氢气体(27)在不将所述富氢气体加热到0℃以上的温度的情况下输送至氢气液化器的机构，该富氢气体包含至少99.9摩尔％的氢气、优选至少99.99摩尔％的氢气、实际上甚至至少99.999摩尔％的氢气；和用于输送所述富氢气体以便在所述第一热交换器中于20-30巴的压力下从至多103K的温度冷却的机构，其特征在于，所述氢气液化设备包括：第二热交换器(103)；用于输送富氢流(127)以便在所述第二热交换器中冷却的机构；用于将所述富氢气体(27)与已在所述第二热交换器中冷却并且具有与所述富氢气体基本相同的压力、温度和组成的富氢流(127)混合以形成第二混合物的机构；以及用于输送第二混合物以便在所述第一热交换器(101)中液化或在于所述第一热交换器中冷却后被液化以形成液态氢(111)的机构。
11.根据权利要求10所述的设备，其中，所述第一交换器(101)位于第一绝热室(104)中，并且所述第二交换器(103)位于第二绝热室(106)中，所述富氢气体和所述富氢流混合的点位于所述第一室和所述第二室的外部。
12.根据权利要求10或11所述的设备，其包括利用氦或氢以便冷却以及可选地液化所述第二混合物的制冷循环(105)。
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