CN111565821A - 从排出气体中除去氮气的低温方法 - Google Patents

从排出气体中除去氮气的低温方法 Download PDF

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CN111565821A
CN111565821A CN201880079693.4A CN201880079693A CN111565821A CN 111565821 A CN111565821 A CN 111565821A CN 201880079693 A CN201880079693 A CN 201880079693A CN 111565821 A CN111565821 A CN 111565821A
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gas stream
pressure
bar absolute
lean
gas
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保罗·泰里安
尼古拉斯·尚丹特
马林·安德里奇
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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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  • General Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

一种用于通过纯化生物气进料流(1)来生产生物甲烷(40)的方法，所述方法包括以下步骤：步骤a)：将所述进料气体流(1)引入预处理单元(5)，在所述预处理单元中所述气体流与其含有的CO2和氧气部分分离并在大于50巴绝对压力的压力P1下被压缩；步骤b)：通过将贫CO2的从步骤a)产生的待处理的气体流(22)引入蒸馏塔(26)对其进行低温分离，以便从待处理的所述气体流中分离氮气；步骤c)：在大于所述产物的临界压力的压力P2下通过泵送所述塔(26)的底部产物(37)回收由所述低温分离产生的富含CH4的流(27)，其特征在于，用于步骤b)的贫CO2的从步骤a)产生的所述气体流包含在0.3mol％与2mol％之间的CO2。

Description

从排出气体中除去氮气的低温方法
本发明涉及一种用于通过洗涤生物气、例如从非危险废物储存设施(NHWSF)获得的生物气来生产生物甲烷的方法。本发明还涉及一种用于实施所述方法的设施。
更确切地说，本发明涉及一种通过将至少含有甲烷、二氧化碳、大气气体(氮气和氧气)和污染物(H2S和挥发性有机化合物(VOC))的气体流的膜渗透和低温蒸馏结合的方法处理。目的是产生富含甲烷的气体流，其甲烷含量符合其使用要求，并使CH4排放到大气中的影响最小化(具有强烈温室效应的气体)。
本发明特别涉及从非危险废物储存设施(NHWSF)获得的生物气的洗涤，目的是生产符合注入天然气网络或在当地用作车辆燃料的生物甲烷。
NHWSF中存在的有机废物的厌氧消化在NHWSF的整个运行期间并且甚至在停止运行和关闭NHWSF之后的数年内，都会产生大量生物气。由于其主要成分-甲烷和二氧化碳-生物气是强有力的温室气体；同时，在越来越缺乏化石燃料的背景下生物气也并行地构成了相当可观的可再生能源的来源。
生物气含有若干种污染物化合物并且必须对其进行洗涤以实现商业利用。存在若干种用于进行生物气的回收和洗涤的方法。
生物气主要含有可变比例的甲烷(CH4)和二氧化碳(CO2)，这取决于生产方法。
在来自NHWSF的生物气的情况下，气体还含有一定比例的大气气体(氮气和氧气)，以及还有较小比例的水、硫化氢和挥发性有机化合物(VOC)。取决于降解的有机物质、所使用的技术以及每种NHWSF的特定条件(气候，类型等)，生物气组分的比例不同。然而，平均来说，生物气包括，在干燥气体基础上，从30％至60％的甲烷、从15％至50％的CO2、从0至30％的氮气、从0至6％的氧气、从0至1％的H2S和从每标准立方米几十毫克至几千毫克的VOC以及痕量的一定数量的其他杂质。
生物气以不同方式被有利地利用。在部分处理后，它可在生产现场附近被有利地利用，以提供热量、电力或两者组合(热电联产)。大含量的二氧化碳和氮气降低了其发热量，增加了压缩和运输成本，并将其有利的利用的经济利益限制在此附近使用。
生物气的更严格的洗涤使生物气得到了更广泛的使用。特别地，生物气的严格洗涤使得能够获得符合天然气规格并且可以替代天然气的洗涤的生物气。如此洗涤的生物气被称为“生物甲烷”。因此，生物甲烷向天然气资源补充在区域的中心处生产的可再生部分。它可以用于与化石来源的天然气完全相同的目的。它可以供给天然气网络或车辆加油站。
生物甲烷被有利地利用的方式是根据当地情况：尤其是当地能量需求、有利地利用生物甲烷作为生物甲烷燃料的可能性、附近的天然气运输或分配网络的存在确定的。通过产生在给定区域操作的各方(农民、制造商、城市当局)之间的协同作用，生物甲烷的生产有助于这些区域获取更大的能量自主性。
应该注意的是，取决于国家，环境法规通常会关于排放到大气中施加限制。
实际上，有必要采取用于限制生物气中含有的温室气体(CH4)和污染物(H2S和VOC)的影响的技术。因此，重要的是具有高CH4产量(质量上等于相对于生物气中含有的CH4的量被有利地利用的CH4的量)，并提供针对H2S和VOC的处理系统，这避免了大气排放。
此外，另外的问题仍然是O2的存在，在混合物的分离期间，O2可能在各个富集步骤期间产生爆炸性气氛。这种产生爆炸性混合物的风险使垃圾场生物气特别难以以安全和经济的方式洗涤。
US 8 221 524 B2描述了一种通过各个再循环步骤将气体的CH4富集至88％比例的方法。所述方法包括压缩气体流并且然后将其通过吸附剂以除去VOC。然后对气体流进行膜分离步骤并且然后进行变压吸附(PSA)步骤。PSA中使用的吸附剂是CMS(碳分子筛)类型的，并且使得能够除去氮气和一小部分氧气。
EP 1979446描述了一种生物气洗涤方法，所述方法包括除去H2S、压缩气体并将其过滤以除去颗粒。然后对气体进行膜分离步骤以除去CO2和O2，通过穿过PSA干燥并且然后穿过各种过滤器并且最后再次穿过PSA以除去氮气。气体最终被液化。
US 2004/0103782描述了一种生物气洗涤方法，所述方法包括除去压缩气体，将其过滤以除去颗粒，对其进行变压吸附(PSA)步骤以除去VOC，并且然后进行膜分离以除去大部分CO2以及还有一部分氧气。
US 5486227描述了一种用于洗涤和液化气体混合物的方法，所述方法包括对流进行变温吸附(TSA)以显著除去H2S，并且然后进行变压吸附(PSA)以显著除去CO2，并且最后进行低温分离以除去氮气并仅保留甲烷。
US 5964923和US 5669958描述了一种用于处理气态流出物的方法，所述方法包括使气体脱水，通过使其穿过交换器而将其冷凝，并对气体进行膜分离，并且然后进行低温分离。
US 2010/077796描述了一种洗涤方法，所述方法包括对气体流进行膜分离，在蒸馏塔中处理渗透物，并且然后在汽化之后将源自塔的甲烷气体与在膜分离结束时获得的渗余物混合。
US 3989478和FR 2917489描述了用于洗涤富含甲烷的流的低温系统。这两个系统使用吸附系统在液化步骤之前洗涤出CO2。
在US 3989478中，吸附系统的再生通过在蒸馏塔顶部回收的富含氮气的馏出物进行。在FR 2917489中，吸附系统的再生通过在蒸馏塔底部抽出的液态甲烷进行。
EP 0772665描述了使用低温蒸馏塔来分离主要由CH4、CO2和氮气构成的煤矿气体。
所引用的文献均没有使得能够解决提供生物甲烷而没有与O2相关的风险的问题，其中甲烷浓度大于95％，CO2浓度小于2.5％，并且甲烷产率大于85％。
因此，本发明解决的问题之一是提供一种符合上述约束条件的生物气洗涤方法，即一种安全、具有最佳产率、产生可替代天然气的高品质生物甲烷、并且符合尤其是关于污染物化合物(如VOC)和具有强烈温室效应的化合物(如CH4)的破坏的环境标准的方法。如此生产的气体将能够以气态形式通过注入气体网络或另外用于机动性应用而被有利地利用。
此外，在现有技术中，已知的做法是在气体洗涤单元中处理生物气，其可采用以下步骤：PSA(变压吸附)、吸附剂筛(以除去VOC)和膜级。
CO2主要在膜步骤被除去。这种不完美的分离在“洗涤的”气体中留下经常在0.5mol％与1.5mol％之间的CO2含量。通过使分离单元加大尺寸，可以减少在洗涤的气体中的CO2含量(需要更大压缩机消耗)。在任何情况下，在洗涤的气体中的CO2含量将永远不可能低很多(浓度的数量级相同)。
然后在低温单元中处理该洗涤的气体，其尤其含有其余的CO2、甲烷、少量的氧气和氮气(在1mol％与20mol％之间)。
在该单元中达到的温度为大约-100℃或甚至更低，这在低压下(在大气压与约30巴之间)导致待处理的气体中含有的CO2的凝固。
经常采用的一种解决方案是使用基于吸附技术(TSA，变温吸附)的洗涤步骤。该技术使得能够实现非常低的CO2含量(例如，在液化天然气的情况下50ppmv)。在这些含量下，即使在低压下，CO2在所考虑的温度下也不会凝固，因为它仍可溶于甲烷中。然而，该洗涤单元是相对昂贵的并且需要使用“再生”气体以便能够排出被捕集的CO2。经常使用的气体是在低温步骤中分离出的氮气，或在NRU(氮气排出单元)出口产生的甲烷。如果使用氮气，则可能有必要降低单元的产量或添加氮气以便设法获得所需的流量。如果使用生产甲烷，则可能出现与解吸相关的CO2浓度峰值，从而使气体不符合规格。
因此，需要改进如上所述的方法，而同时降低运行成本。
因此，本发明的诸位发明人开发了一种用于解决以上提出的问题的解决方案。
本发明的一个主题是一种用于通过洗涤生物气进料流来生产生物甲烷的方法，所述方法包括以下步骤：
步骤a)：将进料气体流引入预处理单元，在所述预处理单元中所述气体流与其含有的CO2和氧气部分分离并被压缩至高于25巴绝对压力、但优选高于50巴绝对压力的压力P1；
步骤b)：通过将从步骤a)获得的待处理的所述贫CO2的气体流引入蒸馏塔对其进行低温分离以从待处理的所述气体流中分离氮气，
步骤c)：在高于25巴绝对压力并且优选高于所述产物的临界压力的压力P2下，通过泵送来自所述塔的容器的产物，回收从所述低温分离获得的富含CH4的流，其特征在于，从步骤a)获得并用于步骤b)的所述贫CO2的气体流包含在0.3mol％与2mol％之间的CO2。
因此，作为本发明主题的解决方案是不进一步减少膜步骤出口处的CO2含量，而同时确保在待处理的气体(主要是甲烷)中CO2的足够溶解度以避免在方法中的任何时候结晶。
因此消除了用于主要洗涤CO2的TSA步骤。因此，进料低温区段的气体含有在0.3mol％与2mol％之间的CO2。
根据其他实施例，本发明的主题还是：
-如先前定义的方法，其特征在于，步骤a)还包括将水从压缩至压力P1的气体流中洗涤出的步骤。
-如先前定义的方法，其特征在于，在步骤a)期间，通过包括至少两个分离膜级的单元进行从所述进料气体流中分离CO2和氧气。
-如先前定义的方法，其特征在于，步骤c)的所述压力P2大于40巴绝对压力。
-如先前定义的方法，其特征在于，在步骤b)期间，从步骤a)获得的所述贫CO2的气体流在被引入所述蒸馏塔之前经历膨胀至在15巴绝对压力与40巴绝对压力之间的压力P3。优选地，P3大于25巴绝对压力。
-如先前定义的方法，其特征在于，在所述膨胀之前，将从步骤a)获得的所述贫CO2的气体流在热交换器中至少部分地冷凝。
-如先前定义的方法，其特征在于，将从步骤a)获得的所述贫CO2的气体流相对于从步骤c)获得的所述富含CH4的流和在步骤b)期间分离出的氮气流的至少一部分逆流在热交换器中至少部分地冷凝。
本发明的主题还是：
-一种用于通过使用如先前定义的方法洗涤从非危险废物储存设施(NHWSF)获得的生物气来生产生物甲烷的设施。
-如以上定义的用于通过如先前定义的洗涤从非危险废物储存设施(NHWSF)获得的生物气来生产生物甲烷的设施，所述设施依次包括：
ο生物气源；
ο预处理单元，用于从待处理的气体流中除去全部或部分VOC、水和硫化合物；
ο至少两个分离膜级，其能够从所述气体流中部分分离CO2和O2；
ο压缩机，其能够将所述气体流压缩至在50巴与100巴之间的压力；
ο热交换器，其能够冷却所述贫CO2的气体流；
ο蒸馏塔；
其特征在于，所述设施不包括除去小于0.3mol％的含量的CO2的TSA。
热交换器可以是适于允许一定数量的流通过的任何热交换器、任何单元或其他布置，并且因此允许一个或多个冷却剂流体管线与一个或多个进料流之间的直接或间接热交换。
将参考附图更详细地描述本发明，所述附图说明了由如附图中示意性表示的设施进行的根据本发明的方法的特定实施例。
相同的参考号表示液体流和输送所述液体流的管道，所考虑的压力是绝对压力并且所考虑的百分比是摩尔百分比。
在附图中，所述设施包括待处理的生物气源(1)，包括压缩单元(2)以及CO2和O2洗涤单元(23)的预处理单元(5)，VOC和水洗涤单元(3)，低温蒸馏单元(4)，以及最后是甲烷气体回收单元(6)。所有设备项目都通过管道连接在一起。
压缩单元(2)的上游是CO2洗涤单元(23)和任选的预先的预处理单元。
CO2洗涤单元(23)例如组合两个膜分离级。选择膜以允许分离至少90％的CO2和约50％的O2。然后将从第一分离获得的渗余物引导至第二膜分离。从第二膜分离获得的渗透物通过连接至压缩机上游主回路的管道进行再循环。该步骤使得能够生产具有小于3％的CO2和具有大于90％的CH4产率的气体(7)。该流的温度典型地是环境温度；必要时，可以结合用空气或水冷却的步骤。
压缩单元(2)例如是呈活塞压缩机的形式。
该压缩机将气体流(7)压缩至例如在50巴与80巴之间的压力。离开的流在附图中用参考号(8)表示。
用于洗涤VOC和水的单元(3)包括两个瓶(9、10)。它们填充有专门选择的吸附剂，以允许吸附水和VOC，以及在再生过程中随后解吸。瓶在生产模式和再生模式下交替地运行。
在生产模式下，向瓶(9、10)在其下部进料气体流。
气体流(8)在其中循环的管道分成两个管道(11、12)，每个管道配备有阀(13、14)，并且分别进料第一个瓶(9)和第二个瓶(10)的下部。阀(13、14)将根据瓶的饱和水平交替地关闭。实际上，当第一个瓶充满水时，阀(13)关闭并且阀(14)打开以开始填充第二个瓶(10)。分别从每个瓶的上部伸出管道(15和16)。它们中的每一个分别分成两个管道(17、18)和(19、20)。源自第一个瓶的水和VOC的洗涤流在管道(18)中循环，而源自第二个PSA的水和VOC的洗涤流在管道(20)中循环。两个管道接合以形成向低温单元(4)进料的单个管线(21)。
在再生模式下，再生气体在管道(17、19)中循环。它在瓶的下部伸出。
低温蒸馏单元(4)通过管道(21)进料，待洗涤的气体流(22)在所述管道中循环。它包括三个元件，分别是热交换器(24)、再沸器(25)和蒸馏塔(26)。
交换器(24)优选是铝或不锈钢钎焊板交换器。其通过与从蒸馏塔(26)中抽出的液态甲烷流(27)进行热交换来冷却在管线(21)中循环的气体流(22)。气体流(22)被冷却(28)至约-100℃的温度。由此产生的两相流(28)可以可替代地确保塔(26)的容器(25)的再沸器的再沸腾，并且所产生的热量(29)被传递到塔(26)的容器。
冷却的流体(28)通过阀(30)膨胀至例如在20巴绝对压力与45巴绝对压力之间的压力。将于是呈两相形式或呈液体形式(31)的流体在位于所述塔(26)的上部的级E1处在例如在-110℃与-100℃之间的温度下引入塔(26)。
液体(31)然后通过冷凝器(33)在塔(26)中分离以形成气体(32)。冷凝器(33)的冷却可以例如通过使用氮气和/或甲烷的制冷循环来进行。在-120℃与-90℃之间的温度下，离开蒸馏塔(26)的容器的液体(37)的一部分(36)被送至再沸器(25)，在所述再沸器中其部分汽化。所形成的气体(29)被送至塔(26)的容器。剩余的液体(37)的另一部分(38)通过泵(39)泵送以形成液态甲烷流(27)，所述液态甲烷流在交换器(24)中汽化以形成纯甲烷气体产物(40)。该泵送步骤是在高压下进行的，典型地高于25巴绝对压力，优先高于50巴绝对压力或流体的临界压力。该压力水平使得能够避免在交换管线的待汽化的最后液滴中CO2的积累。由于气体中的重烃非常少，因此低于临界压力的气体的露点非常低(典型地低于-90℃)。

Claims (8)

1.一种用于通过洗涤生物气进料流(1)来生产生物甲烷(40)的方法，所述方法包括以下步骤：
步骤a)：将所述进料气体流(1)引入预处理单元(5)，在所述预处理单元中所述气体流与其含有的CO2和氧气部分分离并被压缩至高于25巴绝对压力的压力P1；
步骤b)：通过将从步骤a)获得的待处理的贫CO2的气体流(22)引入蒸馏塔(26)对其进行低温分离以从待处理的所述气体流中分离氮气，
步骤c)：在高于25巴绝对压力并且优选高于所述产物的临界压力的压力P2下，通过泵送所述塔(26)的容器(37)中的产物，回收从所述低温分离获得的富含CH4的流(27)，
其特征在于，在步骤a)期间，通过包括至少两个分离膜级的单元进行从所述进料气体流中分离CO2和氧气，以便从步骤a)获得并用于步骤b)的所述贫CO2的气体流包含在0.3mol％与2mol％之间的CO2。
2.如前一项权利要求所述的方法，其特征在于，步骤a)还包括将水从压缩至所述压力P1的气体流(8)中洗涤出的步骤。
3.如前述权利要求中任一项所述的方法，其特征在于，P1大于50巴绝对压力。
4.如前述权利要求之一所述的方法，其特征在于，步骤c)的所述压力P2大于40巴绝对压力。
5.如前述权利要求之一所述的方法，其特征在于，在步骤b)期间，从步骤a)获得的所述贫CO2的气体流(22)在被引入所述蒸馏塔(26)之前经历膨胀(30)至在15巴绝对压力与40巴绝对压力之间的压力P3。
6.如前一项权利要求所述的方法，其特征在于，在所述膨胀(30)之前，将从步骤a)获得的所述贫CO2的气体流(22)在热交换器(24)中至少部分地冷凝。
7.如前一项权利要求所述的方法，其特征在于，将从步骤a)获得的所述贫CO2的气体流(22)相对于从步骤c)获得的所述富含CH4的流(27)和在步骤b)期间分离出的氮气流的至少一部分逆流在热交换器(24)中至少部分地冷凝。
8.一种用于通过采用如前述权利要求之一所述的方法洗涤从非危险废物储存设施(NHWSF)获得的生物气来生产生物甲烷的设施，所述设施依次包括：
ο生物气源(1)；
ο预处理单元(3)，用于从待处理的气体流中除去全部或部分VOC、水和硫化合物；
ο至少两个分离膜级(23)，其能够从所述气体流中部分分离CO2和O2；
ο压缩机(2)，其能够将所述气体流压缩至在25与100巴绝对压力之间的压力；
ο热交换器(24)，其能够冷却所述贫CO2的气体流(22)；
ο蒸馏塔(26)；
其特征在于，所述设施不包括除去小于0.3mol％的含量的CO2的TSA。
CN201880079693.4A 2017-12-21 2018-12-17 从排出气体中除去氮气的低温方法 Pending CN111565821A (zh)

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