CN102317207A - 通过在涡轮中固体冷凝缩而俘获co2的方法 - Google Patents

通过在涡轮中固体冷凝缩而俘获co2的方法 Download PDF

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Publication number
CN102317207A
CN102317207A CN2009801569303A CN200980156930A CN102317207A CN 102317207 A CN102317207 A CN 102317207A CN 2009801569303 A CN2009801569303 A CN 2009801569303A CN 200980156930 A CN200980156930 A CN 200980156930A CN 102317207 A CN102317207 A CN 102317207A
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gas
solid
fluid
turbine
poor
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F·洛克伍德
A·拉沃
J-P·特拉尼耶
C·韦伯
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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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Publication of CN102317207A publication Critical patent/CN102317207A/zh
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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Abstract

本发明涉及一种由包含CO2和至少一种比CO2更具挥发性的化合物的待加工流体生产至少一种贫CO2气体和一种或多种富CO2初级流体的方法，其包括：a)将待加工流体通过无状态改变地热交换而第一次冷却；b)将至少一部分在步骤a)期间冷却的待加工流体第二次冷却以得到至少一种主要包含CO2的固体和至少一种贫CO2气体；和c)包括将至少一部分所述固体液化和/或升华以得到所述一种或多种富CO2初级流体的步骤；其中本方法的特征在于步骤b)在至少一个膨胀涡轮中进行，固体在所述涡轮内部形成。

Description

通过在涡轮中固体冷凝缩而俘获CO2的方法
本发明涉及在包含至少一种比二氧化碳CO2更具挥发性的化合物如甲烷CH4、氧气O2、氩气Ar、氮气N2、一氧化碳CO、氦气He和/或氢气H2的流体中俘获二氧化碳的方法。
本发明可特别地应用于由碳燃料如煤、烃(天然气、燃料油、石油化学残留等)、家庭废物、生物质生产电和/或蒸汽的装置，但也可应用于来自精炼厂、化工厂、炼钢厂或水泥厂的气体，处理离开生产井的天然气。它也可应用于来自用于加热建筑物的锅炉的烟道气或甚至来自运输车辆的废气，更通常应用于产生包含CO2的烟道气的任何工业方法。
二氧化碳是温室气体。由于环境和/或经济原因，日益理想的是通过俘获CO2，然后将它储存在适当地质层中或通过实现它作为产品的资产价值而降低或甚至消除CO2向大气中的排放。
已知一定量的俘获二氧化碳的技术，例如基于用通过化学反应分离CO2的化合物的溶液洗涤流体，例如使用MEA洗涤的方法。这些方法通常具有以下缺点：
-高能量消耗(与用于与CO2反应的化合物的再生有关)，
-与二氧化碳反应的化合物的降解，
-由于化合物与二氧化碳反应而导致的腐蚀。
在冷凝缩，即冷却直至固体CO2出现的领域中，可提到文献FR-A-2820052，其公开了一种通过反升华，即通过没有经过液态而由气体固化而提取CO2的方法。所需冷通过冷冻液分馏而提供。该方法消耗大量能量。
文献FR-A-2894838公开了相同类型的方法，其中一些所产生的液体CO2再循环。冷可通过使LNG(液化天然气)蒸发而提供。该协同作用降低了该方法的比能耗，但是尽管这样，能耗仍然是高的并需要LNG接收站。
文献US-A-3614872描述了一种分离方法，其中二氧化碳绝热和等熵膨胀得到冷冻液。
本发明的目的是提供从包含CO2和至少一种比CO2更具挥发性的化合物的流体中俘获二氧化碳的改进方法。
本发明首先涉及由包含CO2和至少一种比CO2更具挥发性的化合物的工艺流体生产至少一种贫CO2气体和一种或多种富CO2初级流体的方法，其进行以下步骤：
a将所述工艺流体通过不改变状态地热交换而第一次冷却；
b)将在步骤a)中冷却的至少一部分所述工艺流体第二次冷却以得到至少一种主要包含CO2的固体和至少所述贫CO2气体；和
c)包括将至少一部分所述固体液化和/或升华并可得到所述一种或多种富CO2初级流体的步骤；
所述方法的特征在于步骤b)在至少一个膨胀涡轮中进行，所述固体在所述涡轮内部形成。
工艺流体通常来自锅炉或任何产生烟道气的装置。这些烟道气可以已经受各种预处理，特别是着眼于除去NOx(氮的氧化物)、粉尘、SOx(硫的氧化物)和/或水。
在分离以前，工艺流体为单相、气体或液体形式，或多相的。“气体”形式意指“基本上为气体”形式，即它可明显含有粉尘、固体粒子如烟灰和/或液滴。
工艺流体含有要通过冷凝缩与所述流体的其它成分分离的CO2。这些其它成分包含一种或多种在冷凝方面比二氧化碳更具挥发性的化合物，例如甲烷CH4、氧气O2、氩气Ar、氮气N2、一氧化碳CO、氦气He和/或氢气H2。工艺流体通常包含主要氮气或主要CO或主要氢气。
工艺流体通常来自锅炉或任何产生烟道气的装置。这些烟道气可以已经受各种预处理，特别是着眼于除去NOx(氮的氧化物)、粉尘、SOx(硫的氧化物)和/或水。
在分离以前，工艺流体为单相、气体或液体形式，或多相的。“气体”形式意指“基本上为气体”形式，即它可明显含有粉尘、固体粒子如烟灰和/或液滴。
工艺流体含有要通过冷凝缩与所述流体的其它成分分离的CO2。这些其它成分包含一种或多种在冷凝方面比二氧化碳更具挥发性的化合物，例如甲烷CH4、氧气O2、氩气Ar、氮气N2、一氧化碳CO、氦气He和/或氢气H2。工艺流体通常包含主要氮气或主要CO或主要氢气。
在步骤a)中，首先将工艺流体不改变状态地冷却。该冷却可有利地至少部分通过与来自该分离方法的富CO2流体热交换而进行。另外或作为选择，它可有利地至少部分通过与来自该分离方法的贫CO2气体热交换而进行。来自该分离方法的这些冷流体被加热，同时工艺流体冷却。这使得可降低冷却操作所需的能量。
步骤b)在于通过使工艺流体升高至低于CO2三相点的温度，同时工艺流体中的CO2分压低于CO2三相点而使初始气体CO2固化。例如，工艺流体的总压力接近大气压力。该固化操作有时称为CO2的“冷凝缩”或“反升华”和通过工艺流体膨胀。
根据一个具体实施方案，在步骤a)中不固化或没有与固体CO2集合在一起的所有工艺流体组分保持为气态。这些构成贫CO2气体。
某些比CO2更具挥发性的化合物不固化并保持气态。这些与未固化的CO2一起构成所述贫CO2气体，即构成所述包含小于50体积％CO2，优选小于10体积％CO2的气体。根据一个具体实施方案，所述贫CO2气体含有小于1体积％CO2。根据另一具体实施方案，它含有大于2％的CO2。根据另一具体实施方案，它含有大于5％的CO2。形成主要包含CO2，即如果考虑气态的，则含有至少90体积％，优选含有至少95体积％，更优选仍含有至少99体积％CO2的固体。
该固体可包含除CO2外的化合物。例如可提及也可能已固化的其它化合物，或作为选择包含在所述固体块中的流体泡和/或滴。这解释了为何固体可能不仅由固体CO2组成。该“固体”可含有非固体部分，例如流体包体(滴、泡等)。
然后在冷凝缩以后将该固体与未固化的化合物分离并回收。接着，在步骤c)中，它恢复温度和压力条件使得它变为流体、液体和/或气体状态。然后可将至少一部分所述固体液化。这然后产生一种或多种富CO2初级流体。这些流体称为“初级”以将它们与称为“二次”的处理流体区别。“富CO2”意思有点像上文定义的“主要包含CO2”。
发明人已证明特别有利的是使用一个或多个冷冻循环进行工艺流体的第一和/或第二次冷却，每个冷冻循环包括至少一个气体的近等熵膨胀。这些冷冻循环由几个步骤组成，其导致所谓的“工作”流体经过以给定组成、温度、压力等条件为特征的几种物理状态。在循环的各步骤中，至少一个近等熵膨胀，即导致膨胀流体的熵提高小于25％，优选小于15％，仍更优选小于10％的膨胀的存在使得可改善分离方法的能量消耗。按照惯例，认为熵在0K(开尔文)的温度下为0。
取决于情况，本发明方法可包括一个或多个以下特征：
-所述固体为二氧化碳霜形式。
-所述膨胀涡轮包含至少一个转子部件和至少一个位于所述转子部件上游的定子部件，且步骤b)在所述转子部件中进行。所述转子部件是位于转子叶片前缘与后缘之间的区域；它包括转子旋转时转子位移的容积。
-包含CO2和至少一种比CO2更具挥发性的化合物的所述工艺流体在所述定子部件中保持为蒸气态。
-所述工艺流体在位于所述转子部件上游的所述定子部件中为过饱和蒸气态。
-所述膨胀涡轮为向心径流式涡轮或离心径流式涡轮或轴流式涡轮或冲击波超声涡轮。
-该方法还包括在步骤b)以后，将步骤b)中得到的所述主要包含CO2的固体和所述贫CO2气体分离成至少一种富CO2部分和贫CO2部分的步骤b1)，所述步骤b1)在位于所述转子部件下游的区域中进行。“所述转子部件下游”意指转子叶片后缘的下游。
-在步骤b)中，赋予所述主要包含CO2的固体和所述贫CO2气体旋转运动，并且在步骤b1)中，均在步骤b)中得到的所述主要包含CO2的固体与所述贫CO2气体的分离包括通过在步骤b)中赋予所述主要包含CO2的固体的旋转运动引发的离心效应而分离。
-将所述涡轮的某些部件加热。这些部件例如为与转子上游的定子部件、转子部件和/或转子下游的定子部件的流体接触的那些。
-所述涡轮包含被磨光和/或涂有给定材料的表面，这旨在限制所述主要包含CO2的固体在所述表面和/或所述涂料上异相成核。
-所述工艺流体包含比CO2更小挥发性的化合物，并且所述方法包括在步骤b)之前将所述工艺流体(40)纯化以除去所述较小挥发性化合物的一个或多个步骤。如果不除去这些化合物，则它们会带来在高于CO2的固体冷凝缩温度的温度下形成固体化合物和因此可能引发CO2较早成核的风险。
-所述比CO2更小挥发性的化合物包括H2O、SO2、NxOy和在环境温度下存在于工艺气体中的固体化合物。
-将1mg/m3以下，优选100μg/m3以下的固体化合物从工艺流体中除去(在单元103中)。
-所述涡轮包含钛。
-用于涡轮主体中或作为涂层的物质对由主要包含CO2的固体粒子导致的腐蚀有抗性。可例如使用钛。
-将吹扫气体注入所述涡轮中，所述吹扫气体与所述工艺流体接触。该吹扫气体可例如为空气或氮气并防止固体CO2存在于转子部件的背面；如果固体聚集在该区域中，可腐蚀转子部件。
-所述涡轮具有超过50％的反应度，即在转子部件中流体的焓下降大于50％(涡轮入口与出口之间的焓的差)。
此外，步骤b1)可使用两个同心圆锥，意欲回收所述富CO2部分和所述贫CO2部分。作为选择，在步骤b1)中，也可将均在步骤b)中得到的所述主要包含CO2的固体和所述贫CO2气体减速，然后在重力作用下分离成所述富CO2部分和所述贫CO2部分。
为提供进行第一和/或第二次冷却所需的另一部分冷，可依赖于一个或多个包括非近等熵膨胀的流体膨胀的循环，例如逆兰金循环。由于这些循环用作冷冻循环，所以它们称为逆循环。作为使用近等熵膨胀的冷冻循环的补充，它们的优点是它们不需要大量工作流体。相反，它们能效更小。
根据一个实施方案，一个或多个冷冻循环的一些近等熵膨胀提供功。
工作流体可以为各种类型的。根据各个实施方案，这些流体可包含氮气和/或氩气。它们也可包含所有或部分所得贫CO2气体或者所有或部分工艺流体。这些流体可与其它流体混合或已经受压缩、膨胀等中间步骤。
当冷冻循环的工作流体包含所有或部分工艺流体时，不提供外功的一个或多个近等熵膨胀可导致工作流体冷却使得出现固体CO2。这可构成工艺流体的所有或部分第二次冷却。根据一个具体实施方案，这些近等熵膨胀通过文丘里管(具有文丘里效应的喉管)进行。
上述流体旋转可通过任何常规方法，例如通过适当取向的叶片得到。速度的提高通过文丘里效应实现。工作流体的温度下降。出现CO2的固体粒子。流体围绕基本平行于流动方向的轴做旋转运动，像螺旋形。这产生离心效应，使得这些固体粒子在流的周边被回收。
根据优选实施方案，任何可通过一个或多个近等熵膨胀产生的功部分用于在该方法的其它步骤中压缩流体。
本发明还涉及应用于工业烟道气的目的在于俘获CO2的方法。
根据一个具体实施方案，这些烟道气来自生产能量(蒸汽、电)的装置并且可能已经经受预处理。
阅读参考附图给出的以下描述，其它特性和优点会变得清晰，其中：
-图1示意性地描绘使用本发明纯化CO2的方法的装置，其中冷冻循环使用辅助流体作为工作流体，
图2示意性地描绘使用本方法的替代形式的部分装置，其具有使用贫CO2气体作为工作流体的冷冻循环，并且包括产生功的近等熵膨胀，
-图3示意性地描绘使用本方法的替代形式的部分装置，其具有使用贫CO2气体作为工作流体的冷冻循环，并且包括产生功的近等熵膨胀，
-图4示意性地描绘使用本方法的替代形式的部分装置，其具有使用工艺流体作为工作流体的冷冻循环，并且包括产生功的近等熵膨胀，在此期间不存在CO2的冷凝缩，
-图5示意性地描绘使用本方法的替代形式的部分装置，其具有使用工艺流体作为工作流体的冷冻循环，并且包括产生功的近等熵膨胀，在此期间存在CO2的冷凝缩，
-图6示意性地描绘使用本方法的替代形式的部分装置，其具有使用工艺流体作为工作流体的冷冻循环，并且包括没有产生功的近等熵膨胀，在此期间存在CO2的冷凝缩，
-图7示意性地描绘使用本方法的替代形式的部分装置，其中第二次冷却还包括液化，并且还包括使用工艺流体作为工作流体的冷冻循环，并且包括没有产生功的近等熵膨胀，在膨胀期间存在CO2的冷凝缩，
-图8示意性地描绘本发明方法在基于煤在空气中燃烧而发电的装置中的使用。
-图9示意性地描绘本发明方法在基于煤混合燃烧或在氧气中燃烧而发电的装置中的使用。
-图10示意性地描绘本发明方法在炼钢厂中的使用。
-图11示意性地描绘本发明方法在基于氧气操作的生产合成气的装置中的使用。
-图12示意性地描绘本发明方法在由来自合成气蒸汽重整的合成气生产一氧化碳的装置中的使用。
-图13示意性地描绘本发明方法的使用，其具有一方面使用固体CO2的熔融冷产生能量的循环，和另一方面通过蒸馏比CO2更小挥发性的化合物，然后比CO2更具挥发性的化合物的另外纯化。
-图14和15描绘根据本发明用于进行生产外功的工艺流体近等熵膨胀的涡轮。
图1所述装置执行以下所述步骤。
将由烟道气组成的流体24在压缩机101中压缩，特别以补偿装置中各个设备部件中的压力损失。我们注意到该压缩也可与已知为产生烟道气的锅炉通风压缩的压缩组合。它也可在该方法的其它步骤之间进行，或在CO2分离方法的下游进行；
将压缩流体30注入过滤器103中以除去粒子使其降至1mg/m3以下，优选100μg/m3以下的浓度水平。
接下来将无粉尘流体32冷却至接近0℃，通常0-10℃的温度，以将它所包含的水蒸气冷凝。该冷却在塔105中进行，该塔具有以两个水平注入的水，冷水36和温度接近环境温度的水34。也可设想间接接触。塔105可具有或不具有填料。
使用以下方法中一种和/或另一种将流体38送入除去残余水蒸气的单元107中：
-在固定床、流化床和/或旋转干燥器上吸附，其中吸附剂可以为活性氧化铝、硅胶或分子筛(3A、4A、5A、13X、...)；
-在直接接触或间接接触交换器中冷凝。
然后将干流体40引入交换器109中，流体在其中冷却至接近，但在所有情况下均高于CO2固化的温度的温度。该温度可由本领域技术人员了解压力和工艺流体40的组成而确定。如果工艺流体的CO2含量为约15体积％且压力接近大气压力，则该温度位于约-100℃左右。
然后将已经受第一次冷却109的流体42引入容器111中，它在其中连续冷却至提供所需CO2俘获水平的温度。包含在流体42中的至少一部分CO2的冷凝缩一方面产生贫CO2气体44，另一方面产生主要包含CO2的固体62。气体44在约-120℃的温度下离开容器111。该温度根据目标CO2俘获水平选择。在该温度下，气体44的CO2含量为约1.5体积％，即90％的俘获水平起始于包含15％CO2的工艺流体。存在可用于该容器111的各种技术：
-连续固体冷凝缩交换器，其中固体CO2以二氧化碳霜(carbondioxide snow)的形式产生，例如使用螺杆提取并加压以将它引入液体CO2的浴121中，其中得到高于CO2的三相点压力的压力。该加压也可在料仓系统中分批进行。连续固体冷凝缩本身可以以各种方式进行：
-刮面式交换器(scraped surface exchange)，其中刮板例如为螺杆形式以促进固体的提取；
-流化床交换器以运送二氧化碳霜并使用例如密度大于二氧化碳霜的粒子清理管；
-通过振动、超声、气动或热效应(间歇式加热以导致二氧化碳霜降落)提取固体的交换器；
-在光滑表面上累积，定期“自然”落入槽中；
-分批固体冷凝缩：在这种情况下，可交替地使用几个并联的交换器。然后将它们分离，加压至高于CO2的三相点压力的压力以将固体CO2液化，它可能部分蒸发。
然后将流体46在交换器109中加热。当它离开时，流体48还特别用于使除去残余蒸气的单元107再生，和/或用于通过在直接接触塔115中蒸发而产生冷水36，将干流体50引入所述塔中，其然后变得水饱和，其中一些蒸发。然后可使冷水在冷冻机单元119中经受另外的冷却。
将主要包含CO2的固体62转移至液体CO2的浴121中。
需要将该浴121加热以保持液体，补偿由固体62加入的(熔化潜热和显热)。这可以以各种方式进行：
-通过与更热的流体72热交换。来自流体74的冷能可用于该方法的别处，
-通过直接交换，例如通过从浴121中放出流体80，将它在交换器109中加热，并将它再注回浴121中。
将主要包含CO2的液体64从浴121中放出。该液体分成三种料流。在该实施例中，第一种通过膨胀65-5.5绝对巴得到，产生二相气-液流体66。第二种68通过压缩67例如至10巴得到。第三种70例如被压缩至55巴。5.5巴水平提供温度接近CO2三相点温度的冷。10巴水平允许在-40℃左右转移流体68的蒸发潜热。最后，在55巴下，流体70在交换109期间不蒸发。在交换109期间有效地使用包含在流体64中的冷能，同时限制生产纯化且压缩的CO2料流5所需的能量。
第一次冷却109和第二次冷却111所需的部分冷通过使用工作流体51(其为氩气)的冷冻循环200提供。它依次包括：压缩129、可能两个压缩56和57、通过间接交换109冷却、产生冷却的近等熵膨胀131、在容器中加热111和加热109。在冷却109期间，部分工作流体被放出，然后经受近等熵膨胀130，其后间接交换109，在到达压缩段129以前最后压缩128。近等熵膨胀130和131提供部分可用于压缩56和57的功。
该循环200产生约-100℃至-120℃之间的冷用于冷凝缩111和约5℃至-100℃之间的冷以弥补交换109期间冷的不足。
第一次冷却109所需的另一部分冷通过例如逆兰金型的另外冷冻循环181、183提供。
第二次冷却111所需的另一部分冷通过例如逆兰金型的另外冷冻循环191、193提供。
在间接交换109以后，将富CO2初级流体66、68、70在段141、142、143中压缩。例如第一段压缩气态料流。如果需要的话，将压缩的CO275通过间接接触交换器冷却以将它转化成液体形式。然后将它与料流73混合。将该液体混合物抽至运输压力(流体5)。由于运输压力通常为超临界的，通过延伸，超临界流体被认为是温度低于CO2的临界点的液体。
图2-7描绘了根据本发明具体实施方案的实施例，没有描绘在将工艺流体40第一次冷却109以前应用于该工艺流体40的步骤，也没有描绘在热交换109以后富CO2初级流体的压缩。仅描绘了与图1相比主要涉及提供用于交换109和111的冷的冷冻循环的变化。
图2阐述产生功的近等熵膨胀的替代形式，其中工作流体为贫CO2气体44。冷凝缩方法与图1中相同。以下仅详述变化。
将贫CO2气体44例如通过多级压缩机315压缩。当离开时，如果需要的话通过交换器316将流体303冷却至交换器109的入口温度。这可以为直接接触交换器或间接接触交换器。
将压缩的贫CO2气体304在交换器109中冷却使得它可在涡轮312中膨胀(近等熵膨胀)以提供交换111所需的一些冷。离开交换器111的流体307再一次膨胀(近等熵膨胀)以借助流体308为交换器111提供功和冷。其中贫CO2气体膨胀的该回路可根据需要重复多次。
在交换器111以后，将贫CO2气体46在交换器109中加热。将输出流体48如图1中的流体48加工。
交换器111所需的一些冷可通过兰金型冷冻循环191、193提供。
图3阐述产生功的近等熵膨胀的另一替代形式。
贫CO2气体44在交换器111和109中放出冷能。然后通过多级压缩机415将它压缩。接着，如果需要的话将它在交换器416中冷却至交换器109的入口温度。这可以为直接接触交换器或间接接触交换器。
在贫CO2气体404通过涡轮412膨胀以前将它在交换器109中再一次冷却。该近等熵涡轮产生补偿交换器111中冷能的部分亏损所需的冷。
接着，通过近等熵涡轮414使流体407再次膨胀。流体408放出其冷能以补偿交换器111中冷能的部分亏损。其中贫CO2气体膨胀的该回路可根据需要重复多次。
在交换器111以后，将贫CO2气体46在交换器109中加热。最后，将输出流体48如图1中的流体48加工。
图4阐述产生功的近等熵膨胀的另一替代形式。
将工艺流体40通过可以为多级压缩机的压缩机512压缩。使贫CO2气体在近等熵涡轮514中膨胀。流体503的温度必须保持在CO2的冷凝缩温度以上。
包含在流体503中的部分CO2然后在容器111中冷凝。将固体CO262倒入液浴121中，接下来的步骤与图1所述那些(从浴121和料流64向上)相同。贫CO2气体44将其冷能传送至交换器111和109。将输出流体48如图1的流体48加工。
图5阐述产生功的近等熵膨胀的另一替代形式，其中工作流体为工艺流体。
产生功的近等熵膨胀在涡轮612中在流体42上进行以将流体冷却至CO2的冷凝缩温度以下的温度，因此产生二氧化碳霜形式的固体CO2以及贫CO2气体602。
需要非常仔细地设计该膨胀涡轮612。它必须适于高流速，例如工业装置的烟道气40的那些，具有良好的等熵效率并且对于由于固体CO2的存在而导致的潜在另外腐蚀具有抗性。为实现这一点，容许二氧化碳霜存在于涡轮的转子部件(图14和15中包含在前缘951与后缘954之间的区域)中，并在转子部件上游的定子部件960(包含在定子叶片950后缘上游的区域)中被禁止或最小化以便特别是不导致转子部件的叶片952前缘的腐蚀。不同地，优选CO2在定子部件中为蒸气或超饱和蒸气状态或它具有足够小(小于10μm，优选1μm水力直径)的二氧化碳霜核以避免腐蚀转子部件。
涡轮可以为径流式涡轮(向心或离心的)。它可以为超声冲击波涡轮。它可以为轴向的。
后一种技术最适于高流速，但需要大量连续的定子和转子段。为避免腐蚀，优选在流体进入下一个定子段以前将二氧化碳霜从各个转子段下游分离出来。前两种技术的优点是保持高膨胀比(超过10)有效，因此可避免必须进行大量分离操作。
此外，优选采取其它预防法以产生这种涡轮：
-需要例如通过将这些表面中的一些加热或通过施加特殊涂层使异相成核(在定子和转子表面上)最小化；
-需要在比CO2更小挥发性的化合物(包括固体粒子)进入涡轮中以前通过除去它们而延迟成核，使得它们不形成促进固体CO2成核的核；
-需要通过使用更强的金属如钛或通过使用特殊涂层或表面处理而提高表面的耐腐蚀性；
-在向心径流式涡轮的情况下，优选使吹扫气体953横穿过叶轮962的背面。该气体与膨胀气体在定子部件(叶片)和转子部件(叶轮)之间的界面上混合，因此避免固体在叶轮后面形成和积累。
然后在分离器612中将该二氧化碳霜与贫CO2气体分离以得到主要包含CO2的固体62和贫CO2气体44。
该分离可在转子部件下游通过使转子部件中的流体旋转和通过使用离心效应以将处于周边的富CO2部分与处于中心的贫CO2部分分离而进行。也可有利地提高速度，因此实现会聚喷嘴956(称作Laval涡轮的涡轮)中流体的另外膨胀。通过在使气体减速以前降低压力，可提高固化CO2的量。大多数贫CO2气体在流的中心959回收，大多数固体CO2在周边958回收，与气体部分混合。
用于进行固体冷凝缩的涡轮的优点是大量固体CO2可以以与间接交换系统相比非常小的体积产生。
如果需要的话，兰金型或包括产生或不产生功的工作流体近等熵膨胀的其它冷冻循环191、193提供具有冷能的分隔带612。将主要包含CO2的固体62倒入液浴121中，接下来的步骤与图1所绘那些相同。
在交换器109中将贫CO2气体44通过与工艺流体热交换而加热。然后将流体605压缩至高于或等于大气压力的压力。最后，如图1中加工输出流体48。
图6阐述不产生功的近等熵膨胀的一个实施方案。
仍在容器111中将工艺流体42冷却至CO2的冷凝缩温度以下以产生冷却的贫CO2气体701。该容器可位于该方法的“膨胀/文丘里”部件702以后，现在描述它。
待俘获的一些CO2以主要包含CO2的固体62的形式固化并从容器111中提取。为改善CO2俘获，使用固定叶片系统717使流体701围绕基本平行于它流动方向的轴旋转。
当离开叶片时流体703膨胀并冷却至CO2的冷凝缩温度以下，其中没有产生功。该膨胀可通过文丘里效应通过使流体通过界限718而进行。形成主要包含CO2的固体粒子并由于流体旋转导致的离心效应而在流的周边回收。
回收主要包含CO2的固体和气体的混合物705。输出的不可冷凝物44、46在交换器111和109中放出它们的冷能。
料流705主要由固体构成，但可能需要在分离器731中将残余气体与固体分离。不可冷凝的部分然后在交换器111和109中放出其冷能。
将主要包含CO2的固体62倒入液浴121中并经受与图1所述那些相同的步骤。
料流48用于以与图1中的料流50相同的方式将水冷却。
图7阐述不产生功的近等熵膨胀的另一实施方案。
使工艺流体40处于压力，例如高达60巴下(通过压缩机101或通过另外的压缩机进行压缩)。它的CO2能到可能比在其他实施例中更浓，通常含有50-90体积％。
交换809包括与图1中的交换109相同的特征。交换器811将工艺流体42冷却至CO2的液化温度以下的温度。由此形成冷却的工艺流体801，将其送入分离器812中。
通过分离器812提取富CO2液体816。通过固定叶片系统817使残余流体802围绕基本平行于其流动方向的轴旋转。当离开803旋转的叶片时它膨胀并冷却至CO2的冷凝缩温度以下，其中没有产生功。该膨胀可通过文丘里效应通过使流体通过界限818而进行。
形成主要包含CO2的固体粒子并由于流体旋转导致的离心效应而在流的周边被回收。料流805主要由固体构成，但可能需要在分离器841中将残余气体与固体分离。不可冷凝的部分44然后在交换器811和809中放出它们的冷能。
为改善CO2俘获水平，可添加第二(或甚至第三或更多)步骤，其中使流体806经受具有文丘里效应的近等熵膨胀。该步骤与前一个相同：
-使用固定叶片系统807使流体806围绕基本平行于其流动方向的轴旋转；
-在使它旋转以后，使离开叶片808的流体膨胀以将它冷却至CO2的冷凝缩温度以下的温度，其中没有产生功。该膨胀可通过文丘里效应通过使流体通过界限822而进行。
将在分离器841和可能的851出口处回收的主要包含CO2的固体62倒入液浴121中并如图1加工。料流48用于以与图1中料流50相同的方式将水冷却。
图8描绘一种用于由煤发电的装置，其使用各个单元4、5、6和7用于纯化烟道气19。
使第一气流15通过单元3，在其中将煤15粉化并送向锅炉1的燃烧器。将第二气流16直接施加在燃烧器上以提供煤的近完全燃烧所需的其它氧气。将进料水17送入锅炉1中以产生蒸汽18，其在涡轮8中膨胀。
使由煤的燃烧产生，包含氮气、CO2、水蒸气和其它杂质的烟道气19经受各种处理以除去一些所述杂质。单元4例如通过在氨的存在下催化而除去NOx。单元5例如使用静电过滤器除去粉尘，单元6为用于除去SO2和/或SO3的脱硫系统。取决于所需产物的组成，单元4和6可以是多余的。然后将来自单元6(或如果不存在6的话5)的纯化流24送入低温冷凝缩纯化单元7中以产生相对纯的CO2流26和富氮残余流25。该单元7也称为CO2俘获单元并进行例如如图1-7所述形成本发明主题的方法。
图9描绘一种用于由煤发电的装置，执行各个单元5和7以纯化烟道气19。
使第一气流15通过单元3，在其中将煤15粉化并送向锅炉1的燃烧器。将第二氧化剂流16直接供入燃烧器中以提供煤的近完全燃烧所需的其它氧气。该第二氧化剂为使用鼓风机91再循环的烟道气94与通过用于分离空气的单元10产生的氧气90混合的结果。将进料水17送入锅炉1中以产生蒸汽18，其在涡轮8中膨胀。
使由煤的燃烧产生，包含氮气、CO2、水蒸气和其它杂质的烟道气19经受各种处理以除去一些所述杂质。单元5(ESP)例如使用静电过滤器除去粉尘，将来自单元5的无粉尘流24送入低温冷凝缩纯化单元7中以产生相对纯的CO2流26和富氮残余流25。该单元7也称为CO2俘获单元并进行例如如图1-7所述的形成本发明主题的方法。
在这种情况下，用于分离空气的单元的存在用于在单元7中在低CO2的固体冷凝缩水平下提供冷，和优选通过与工艺气体直接交换而进行冷凝缩。流体93可以为液体、气体或二相形式，并由冷却空气的混合物组成。例如这可以为冷气态氮或空气(在-56℃与-196℃之间)，或作为选择为液体氮或空气。预期将它引入图1-4和图6中参考号为111，图5中参考号612，图6中731，和图7中841、851的容器中。
单元7也可以生产流体92，其将用于分离空气的单元中。这可例如为一部分离开图1-4和6中容器111，图5中612，图7中731，和图8中841、851的贫气的一部分。该贫气以一些途径在高于通过流体93由单元10获得的温度水平下将冷返还给单元10。这对于随时间变化的该流体93注入的流速而言是有利的。例如当能量是可得且便宜的时，可产生液氮并在夜间储存，然后可在白天注入液氮以降低能量消耗。单元10产生冷的时间(例如液氮)与它用于单元7中的时间分开。在这种情况下，气体的近等熵膨胀可在单元10，而不是单元7中进行。
该方案可证明良好适于改进现有装置的情况，其中用再循环烟道气加上氧气的混合物代替一次空气送入碎煤机可证明是复杂的，这部分是由于水含量的提高、包含比湿空气多得多的水的烟道气，部分是由于安全原因，但是这不应过高估计。
此外，可证明有利的是单元7和10组合成单一单元，特别是通过在两个单元的流体之间进行一次(或多次)热交换。
图10示意性地描绘本发明方法在炼钢厂中的使用。用于分离空气的单元10为高炉900提供氧气90，还向该炉中引入铁矿901和碳产品902(煤和焦炭)。在这种情况下，高炉在很少氮气的存在下操作。
由例如47％CO、36％CO2、8％N2和9％其它化合物如H2和H2O构成的高炉煤气903可分成两部分。多数905进入CO2俘获单元中，另一部分904用于降低回路中的氮气浓度。将流体905在直接接触交换器906中预先冷却，在过滤器103中除去粉尘，然后通过压缩机901压缩，在交换器105中冷却并在进入低温交换器109中以前在干燥器107中干燥，在所述低温交换器中将它冷却，然后部分液化至接近CO2的三相点的温度，其中没有形成固体。在分离器928中将所得二相气-液流体912分离成气体部分502和液体部分920。然后将气体部分502通过例如在涡轮514中近等熵膨胀而冷却，以得到二相气-固流体503。这在容器111中分离成气体部分44和富CO2固体部分62。将固体部分62例如通过蜗杆压缩并与液体920在浴121中混合，其通过在交换器109中蒸发液体74而产生的气体72加热。将液体CO264通过泵69压缩以得到加压液体70并在交换器109中加热，其中如果压力在超临界压力以上，则没有经受蒸发或拟蒸发。将贫气通过压缩机315和交换器109连续地加热。
本发明还适合于基于富空气(enriched air)操作的高炉类型，例如通过添加使用低温蒸馏的CO/N2分离，将气体44冷却至所要求的温度。
图11示意性地描绘本发明方法在由氧气方法(部分氧化、气化、自热重整器等)生产合成气的装置中的使用。用于分离空气的单元10提供氧气90给反应器900，向其中引入碳产品902(煤、天然气、生物质、家庭废物等)。
合成气903主要包含化合物CO、CO2、H2和H2O。CO可在水蒸气的存在下(在所谓的变换反应中)转化成CO2和H2：
Figure BDA0000083905490000161
流体905可在过滤器103中除去粉尘，然后通过压缩机101压缩，在交换器105中冷却并在进入低温交换器109中以前在干燥器107中干燥，在所述低温交换器中在接近CO2的三相点的温度下将它部分液化。在分离器928中将该二相气-液流体912分离成气体部分502和液体部分920。然后将气体部分502通过例如在涡轮514中近等熵膨胀而冷却，以得到二相气-固料流503。这在容器111中分离成气体部分44和富CO2固体部分62。将固体部分62与液体920在浴121中混合，其用通过在交换器109中蒸发液体72而产生的气体74加热。将液体CO264通过泵压缩并在交换器109中加热，其中如果压力在超临界压力以上，则没有蒸发或拟蒸发。将贫气44借助压缩机924和交换器109连续地加热。可将基本由氢气组成的贫气送入燃气轮机中燃烧，其中不排放CO2。单元10可提供热氮90a和/或冷氮90b，将热氮在干燥器910下游引入，将冷氮直接引入容器111中以提高俘获的CO2的量。在第一种情况下，存在于料流502中的热氮在涡轮514中的膨胀提供另外的冷能用于涡轮514中CO2的固体冷凝缩；在第二种情况下，通过经与流体503接触而被加热的冷氮90b导致CO2的固体冷凝缩。热氮90a的另一优点是它提高气体502的分子量，这可以在降低膨胀514和/或压缩924的费用方面证明是有利的。实际上发生的是当这些气体非常富含氢气时，使用最适于高流速的技术，即轴向、径向或超声冲击波类型的技术不容易使这些气体压缩/膨胀。然后需要使用正位移类型的技术，例如使用活塞或螺杆，其对于进行而言非常昂贵。
图12示意性描绘本发明方法在由蒸汽重整生产合成气的装置中的使用。将碳产品902(天然气、甲醇、石脑油等)引入反应器900中。
反应器900中产生的合成气903主要包含化合物CO、CO2、H2和H2O。可将流体905通过压缩机101压缩，在交换器105中冷却并在进入低温交换器109中以前在干燥器107中干燥，可以在所述低温交换器109中在接近CO2的三相点的温度下将它部分液化。在分离器928中将所得二相气-液流体912分离成气体部分502和液体部分920。然后将气体部分502通过例如在涡轮514中近等熵膨胀而冷却，以得到气-固二相混合物503。这在容器111中分离成气体部分44和富CO2固体部分62。将固体部分62与液体920在浴121中混合，其用通过在交换器109中蒸发液体72而产生的气体74加热。将液体CO264通过泵压缩并在交换器109中加热，其中如果压力在超临界压力以上，则没有蒸发或拟蒸发。然后将贫气44在引入低温单元924中用于生产CO以前，在低温下例如通过使用分子筛13X吸附而在CO2方面纯化。该单元例如通过甲烷洗涤或CO部分冷凝而操作。单元924产生富氢气体929和富CO气体925。可将该单元的一种或多种流体在低温下压缩，然后再引入换热器926中。
在这种情况下，固体冷凝缩代替用胺(MDEA或MEA)吸附除去CO2。如果需要生产纯氢气，则可在该固体冷凝缩纯化上游，即在合成气冷却以后在重整器900的出口侧，或在富H2气体929上将H2PSA加入该方案中。
可假定这些固体冷凝缩方法缺乏冷。实际上，情况并不是这样。相反，工艺气体近等熵膨胀的这些固体冷凝缩方法产生过量冷，如果该方法还提供外功的话尤其如此。问题则是富CO2流体和贫CO2气体在低温下排出，这说明明显的能量损失。为了使该方法的能量消耗最小，可进行一种或多种以下操作：
-在内部：
○将冷凝缩方法的一种流体冷压缩：
■在压缩以前冷却至低温的工艺气体；
■在低温下压缩的贫CO2气体(参见图2)。它然后可再次膨胀或在真空下压缩以使它恢复大气压力或它可在产生工艺气体的方法的热部件中加热以后膨胀；
○在交换器中间接固体冷凝缩；
-在外部：
○冷压缩装置的任一种流体；
○产生液氮和/或液态空气；
○在CO2上跨临界兰金循环。
图13示意性地描绘使用本发明方法在CO2上进行跨临界兰金循环。它也包括本发明的特征，其中液体冷凝缩，然后固体冷凝缩依次进行，且其中使用两个蒸馏塔改善产生的CO2的纯度，它们中的一个用于除去比CO2更小挥发性的化合物(NO2或N2O4、SO2等)，另一个用于除去更具挥发性的化合物。
流体24由烟道气组成并可为约150℃的温度，将其注入过滤器103中以除去粒子使其降至1mg/m3以下，优选100μg/m3以下的浓度水平。
将无粉尘的流体30冷却至接近0℃，通常0-10℃的温度以使它所包含的水蒸气冷凝。该冷却在塔105b中进行，该塔具有以两个水平注入的水，冷水36b和温度接近环境空气的湿球温度的水34b。也可设想间接接触。塔105可具有或不具有填料。该塔也可用作SO2的洗涤塔。
当离开该第一塔时，将可能已去饱和的流体在压缩机101中压缩至5-50绝对巴的压力。将流体32冷却至接近0℃，通常0-10℃的温度以将它所包含的水蒸气冷凝。该冷却在塔105中进行，该塔具有以两个水平注入的水，冷水36和温度接近环境空气的湿球温度的水34。也可设想间接接触。塔105可具有或不具有填料。
将流体38送入单元107中，其例如使用以下方法中一种和/或另一种除去残余水蒸气：
-在固定床、流化床和/或旋转干燥器上吸附，其中吸附剂可以为活性氧化铝、硅胶或分子筛(3A、4A、5A、13X等)；
-在直接接触交换器或间接接触交换器中冷凝。
将工艺流体40冷却，然后使其在蒸馏塔79中与纯CO2接触，以回收包含CO2和例如NO2(或其二聚物N2O4)的液体形式的比CO2更小挥发性的化合物。可将该液体抽吸并在单元78中蒸发，然后送入燃烧室中以将NO2还原或送入用于通过SO2的低压洗涤而纯化料流30的单元中，其中它直接以NO2的形式或以已与水反应的硝酸的形式充当试剂。
然后将工艺流体74a冷却，部分冷凝成液体形式并送入分离器76中。将液体部分76a送入浴121中。将气体部分76b送入膨胀涡轮以在那里产生气-固二相料流42，然后将其送入容器111中，在其中将它分离成贫CO2气体44和固体CO262。例如来自空气分离单元的辅助流体93可提供用于固体冷凝缩的其它冷。当它这样做时，可有利地从贫CO2气体44中放出流体92，使其返回提供流体93的单元中。将固体62例如通过蜗杆压缩并注入液体CO2的浴121中，从其中放出液体64。可将该液体抽吸并引入蒸馏塔75中，在其中除去比CO2更具挥发性的化合物。将纯液体68加热，其中如果它为超临界的，则没有蒸发或拟蒸发。可再一次将它抽吸以得到准备运输的流体5。可将一部分流体5抽出以在单元72中蒸发或拟蒸发。单元72例如为生产工艺流体的装置的任何随意热源。这部分流体80然后在用于生产电或机械功的涡轮73中膨胀，然后在交换器109中冷却，并通过在浴121中直接交换而冷凝，同时将固体CO2熔融。
当离开交换器109时，流体48仍可特别是用于使除去残余蒸气的单元107再生，和/或用于通过在直接接触塔115中蒸发而生产冷水36a，干流体50引入其中并变得水饱和，一部分蒸发。可能地，冷水可在冷冻单元119中经受另外的冷却。其后，该冷水可用于一个和/或另一个塔105和105b中以将工艺气体在压缩以前和/或以后冷却。
图14和15描绘用于进行根据本发明产生外功的工艺流体的近等熵膨胀的涡轮。上游定子部件960以螺旋形开始(未描绘)，其后是叶片950，其可以为固定或可变的。接下来是转子部件960，其例如包括具有前缘951和后缘954的叶片952，其中转子部件960在前缘开始，在后缘结束。
在转子部件下游，如果离心力不用于固体部件上，则转子部件可由简单的减速圆锥组成。
如果下游定子部件961用于实现第一次分离，则在转子部分中已使流体旋转这一事实和离心效应可用于将处于周边的富CO2部分与处于中心的贫CO2部分分离。也可有利地提高速度，因此在会聚喷嘴956(所谓的“Laval”涡轮)中进行流体的另外膨胀。通过在使气体减速以前降低压力，可提高固化的CO2的量。多数贫CO2气体在流的中心959回收，多数固体CO2在周边958回收，与气体部分混合。

Claims (13)

1.一种由包含CO2和至少一种比CO2更具挥发性的化合物的工艺流体(40)生产至少一种贫CO2气体(44)和一种或多种富CO2初级流体(66、68、70)的方法，其进行以下步骤：
a)将所述工艺流体(40)通过不改变状态地热交换而第一次冷却(109)；
b)将在步骤a)中冷却的至少一部分所述工艺流体(42)第二次冷却(111)以得到至少一种主要包含CO2的固体(62)和至少所述贫CO2气体(44)；和
c)包括将至少一部分所述固体(62)液化和/或升华并可得到所述一种或多种富CO2初级流体(66、68、70)的步骤；
所述方法的特征在于步骤b)在至少一个膨胀涡轮(612、71、514)中进行，所述固体(62)在所述涡轮(612、71、514)内部形成。
2.根据权利要求1的方法，其特征在于所述固体(62)为二氧化碳霜的形式。
3.根据权利要求1和2中任一项的方法，其特征在于所述膨胀涡轮(612、71、514)包含至少一个转子部件(962)和至少一个位于所述转子部件(962)上游的定子部件(960)，且步骤b)在所述转子部件(962)中进行。
4.根据权利要求3的方法，其特征在于包含CO2和至少一种比CO2更具挥发性的化合物的所述工艺流体(40)在所述定子部件(960)中保持为蒸气态。
5.根据权利要求3的方法，其特征在于所述工艺流体(40)在位于所述转子部件(962)上游的所述定子部件(960)中为过饱和蒸气态。
6.根据权利要求3-5中任一项的方法，其特征在于它还包括在步骤b)以后，将步骤b)中得到的所述主要包含CO2的固体(62)和所述贫CO2气体(44)分离成至少一种富CO2部分(958)和贫CO2部分(959)的步骤b1)，所述步骤b1)在位于所述转子部件(962)下游的区域(961)中进行。
7.根据权利要求6的方法，其特征在于在步骤b)中，赋予所述主要包含CO2的固体(62)和所述贫CO2气体(44)旋转运动，并且在步骤b1)中，均在步骤b)中得到的所述主要包含CO2的固体(62)与所述贫CO2气体(44)的分离包括通过在步骤b)中赋予所述主要包含CO2的固体(62)的旋转运动引发的离心效应而分离。
8.根据权利要求1-7中任一项的方法，其特征在于将所述涡轮(612、71、514)的某些部件加热。
9.根据权利要求1-8中任一项的方法，其特征在于所述涡轮(612、71、514)包含被磨光和/或涂有给定材料的表面，这旨在限制所述主要包含CO2的固体(62)在所述表面和/或所述涂料上异相成核。
10.根据权利要求1-9中任一项的方法，其特征在于所述工艺流体(40)包含比CO2更小挥发性的化合物，并且所述方法包括在步骤b)之前将所述工艺流体(40)纯化以除去所述较小挥发性化合物的一个或多个步骤。
11.根据权利要求1-10中任一项的方法，其特征在于所述涡轮(612、71、514)包含钛。
12.根据权利要求1-11中任一项的方法，其特征在于将吹扫气体(953)注入所述涡轮(612、71、514)中，所述吹扫气体(953)与所述工艺流体(40)接触。
13.根据权利要求1-12中任一项的方法，其特征在于所述涡轮(612、71、514)具有超过50％的反应度。
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FR2940413B1 (fr) 2013-01-11
WO2010076467A1 (fr) 2010-07-08
EP2379971B1 (fr) 2014-02-12
CN102326044A (zh) 2012-01-18
US20110302955A1 (en) 2011-12-15
FR2940413A1 (fr) 2010-06-25
WO2010076466A1 (fr) 2010-07-08
EP2379199A1 (fr) 2011-10-26
EP2379971A1 (fr) 2011-10-26
US20110252827A1 (en) 2011-10-20
CN102326044B (zh) 2015-08-19
EP2379970A1 (fr) 2011-10-26

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