CN1133428A - 纯一氧化碳馏份的提取方法 - Google Patents

纯一氧化碳馏份的提取方法 Download PDF

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CN1133428A
CN1133428A CN95116109A CN95116109A CN1133428A CN 1133428 A CN1133428 A CN 1133428A CN 95116109 A CN95116109 A CN 95116109A CN 95116109 A CN95116109 A CN 95116109A CN 1133428 A CN1133428 A CN 1133428A
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carbon monoxide
hydrogen
methane
tower
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H·鲍尔
R·法比安
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Abstract

从一种在必要时分离掉水与二氧化碳并至少含有氢、一氧化碳及甲烷的进料馏份中提取纯CO馏份的方法，其中将进料馏份冷却并使之部分冷凝，用过冷的液态甲烷洗出一氧化碳和氢，汽提所洗出的氢，并接着对如此提取得的富CO/CH4馏份进行精馏分离，以此分离成纯CO馏份和富CH4馏份，其间用作洗涤剂的过冷液态甲烷至少含2-15％(摩尔)一氧化碳，优选含7-10％(摩尔)一氧化碳。氢汽提塔和甲烷洗涤塔可组装在一个塔中。

Description

纯一氧化碳馏份的提取方法
本发明涉及从一种在必要时分离掉水与二氧化碳并至少含氢、一氧化碳和甲烷的进料馏份中提取纯CO馏份的方法，其中将进料馏份冷却并使之部分冷凝，用过冷的液态甲烷洗出一氧化碳和氢，汽提所洗出的氢，并接着对如此提取得的富CO/CH4馏份进行精馏分离，以此分离成纯CO馏份和富CH4馏份。
基于对分离产物的纯度要求提高、设备运行成本的重要性越来越大，以及可供使用的热力学数据的不断完善，近年来H2/CO分离领域不断发生着技术上的变化。
作为H2/CO进料馏份的主要供应来源，始终须提及蒸汽重整器(Steam-Reformer)。但是，用氧使重油汽化——即部分氧化——以有廉价氧来源为先决条件，近年来，以氧来汽化重油作为H2/CO的供应者有着重大意义。
绝大部分如此制得的一氧化碳，都用于甲酸和乙酸的生产中。另外的买主出现在聚碳酸酯化学领域中，该化学领域要求以高纯度光气为原料，而光气又要求最高纯度的一氧化碳为原料。此时，一氧化碳中的甲烷含量须＜10ppm(摩尔)、氢含量须＜1000ppm(摩尔)。制造纯CO时产生的氢，在必要时经接续精细净化后，用于各种氢化目的。
R.Fabian在LINDE公司科技报告书第55期(1984年)第38-42页上和R.Berringer博士在LINDE公司科技报告书第62期(1988年)第18-23页上发表的文章，对制备一氧化碳和副产品氧所使用的方法作了概述。由后面所述的LINDE公司报告书中的附图6及附图说明已知一种借助甲烷洗涤和必不可少的N2/CO分离来提纯CO的方法。在此已知方法中，以过冷的液态甲烷在第一洗涤塔中将一氧化碳、氢及氮从进料气流中洗涤出来。在后置的一个氢汽提塔中，使洗涤塔塔底抽出的馏份与氢分离。接着在另一个分离塔中，将从上述汽提塔塔底抽出的无氢混合物分离成N2/CO馏份(塔顶产物)和CH4重馏份(塔底产物)。此液态CH4馏份被泵至原料气的压力，并供入洗涤塔，作洗涤剂用。接着，在第4个塔中，分离成CO产物馏份和富N2馏份。倘若进料混合气中不含氮，则可取消该第四个塔。CO产物馏份温热后，同所谓的循环CO一起压缩，并以所需的产品压力供货。为对该过程供冷，用一个一氧化碳循环同制冷涡轮机一起工作。
为了能在洗涤塔中尽可能完全地洗出一氧化碳和氮，有必要将作洗涤剂的甲烷以尽可能纯的形式供入洗涤塔。但是，为在洗涤馏份中获得尽可能高的CH4纯度，就需要富CH4洗涤馏份回收塔再沸效率高。
本发明赖以为基础的目的是，避免现有技术中的上述缺点。
按本发明，此目的以下述措施来实现：用作洗涤剂的过冷的液态甲烷至少含有2-15％(摩尔)一氧化碳，优选含有7-10％(摩尔)一氧化碳。
下面以附图来尽详阐明本发明方法以及本发明装置与其它发展。
下文中所有对工艺流的数量说明，均以摩尔百分比表示。
下表中举例性地列出了标有标号的各管道中的温度、压力、流量及气体或混合气体的液化分量(Flüssiganteil)。
    管道     T[K]    p[bara]     流量[Nm3/h]     液化分量
    11′22′2″33′455′66′77′7″899′1010′10″111′11″121313′     308，088，894，092，0300，0124，4108，0124，497，4305，0125，7125，0125，7126，188，8305，0305，088，888，887，8300，088，889，488，3100，2108，0129，0     13，112，812，74，94，512，74，712，74，54，14，74，64，713，712，79，924，224，024，02，04，224，04，52，17，94，84，7     2720272021152115223484684617898318317567567267267265761049104961361379443625618090486486     0，00，1180，00，00，01，00，821，00，00，01，00，981，01，01，00，00，01，01，00，9880，01，01，00，9881，00，820，0
附图中概括示出一种经分离至少含氢、一氧化碳及甲烷且优选来源于蒸汽重整器的进料馏份来提取一氧化碳产品物流和氢副产品物流的方法。
在必要时用吸附法分离掉水和二氧化碳的进料馏份，经由管道1输过两个换热器E1和E2。进料馏份的组成为72.9％(摩尔)H2、24.5％(摩尔)CO、2.4％(摩尔)CH4及0.3％(摩尔)其它组分如N2。在上述两个换热器中，将进料馏份冷却到大部分一氧化碳和甲烷已冷凝。已冷却并部分冷凝的进料馏份经由管道1′输向塔T1上部的下部。塔T1是一个由氢汽提塔和甲烷洗涤塔构成的联合塔。此时，根据本发明，该塔的上部为甲烷洗涤塔，而该塔的下部为氢汽提塔。富H2馏份在顶部经由管道2从塔T1引出，该富H2馏份由93.7％(摩尔)H2、4.2％(摩尔)CO、2.9％(摩尔)CH4和0.1％(摩尔)N2组成。在阀a中使此馏份减压，并接着经由管道2′逆着冷却过的工艺物流输过两个换热器E2和E1。富H2馏份经由管道2′抽出。需要时，还可单独在加压下将此富H2馏份稍微加热，并例如在变压吸附过程中再提纯为纯氢或最纯氢。在塔T1的塔底，将由46.8％(摩尔)CO、52.8％(摩尔)CH4、0.4％(摩尔)N2及10ppmH2组成的富CO/CH4馏份，经由管道3抽出。一部分此馏份经由管道4输入再沸器，使之蒸发，并接着再供入塔中。为一目了然起见，在附图中该位置上标出也同样标以E2的一个独立的换热器。但实践上，图中所示的这两个换热器E2构成了一个换热器。从塔T1底部引出的馏份经由二条路线抵达CO/CH4分离塔T2。也即，一部分该馏份在阀b中减压——而且这部分几平全为液态——并接着经由管道3′输到分离塔T2。另一部分在阀b′中减压，并经由管道13输到换热器E2。在该换热器中，此馏份完全蒸发，并接着经由管道13′同样输到分离塔T2，但在第一分流输入处的下部位置处输入。经由塔顶并借助管道5从该分离塔T2引出纯一氧化碳产品馏份，并在换热器E2和E1中将之逆着冷却过的工艺物流稍予温热。该纯一氧化碳馏份的组成为99.2％(摩尔)CO、0.8％(摩尔)N2、23ppmH2及10ppmCH4。理论上，H2和CH4可继续任意从纯一氧化碳馏份中分离掉。富CH4馏份从分离塔T2的底部引出，其组成为93.0％(摩尔)CH4、7.0％(摩尔)CO及0.04％(摩尔)N2。该纯CH4馏份不需用于洗涤的那部分，经由管道6引出，在阀c中减压，并接着经由管道6′与管道2′中的纯H2馏份混合。由88.7％(摩尔)H2、4.2％(摩尔)CO、2.9％(摩尔)CH4和0.9％(摩尔)N2组成的富H2混合气经由管道2″引出。需用于洗涤的纯CH4馏份经由管道7引入泵P，在该泵中纯CH4馏份被泵至原料气的压力。接着，使该纯CH4馏份在换热器E2中过冷，并经由管道7″输至塔T1上部(即甲烷洗涤塔部分)的塔顶。根据本发明，该用作洗涤剂的过冷的富CH4馏份至少含2-15％(摩尔)一氧化碳，优选含7-10％(摩尔)一氧化碳。这意味着，分离塔T2中再沸效率可保持得任意的低。甚或可将其完全取消。为一目了然起见，附图中未将其示出。本发明方法所需的能量用附设的CO循环来产生。为此，将经由管道5′从换热器E1输出的纯一氧化碳产品馏份输至三级活塞式压缩机V的第二级。在现有情况下，第一级压缩到4.5bar bara，第二级压缩到10.0bar bara，而第三级压缩到24.5bar bara。纯一氧化碳产品馏份可在第二或第三压缩级后引出。在第三压缩级之后，将分流(即形成一氧化碳冷循环的分流)经由管道9引出，在换热器E1中将之冷却、在换热器E2中使之冷凝并过冷，接着经由管道9′输至分配该一氧化碳馏份的地点。其中第一股分流经由管道10输至阀d，并在其中减压。接着，将该股分流经由管道10′输过换热器E2和E1，并在其中逆着待冷却的工艺料流蒸发并稍受加温。接着，将该分流经由管道10″输至第一压缩级。第二股分流经由管道11输至分配该分流的另一个地点。该物流的一部分在阀e中减压，并经由管道11′以回流形式输至分离塔T2的塔顶。另一部分在阀f中减压，并接着经由管道11″作为冷却剂输至塔T1的上部。接着将自塔T1引出并已稍予温热的冷却剂在进入换热器E2之前混入管道10′。可能有必要的是，为进行制冷，将液氮经由管道12混入管道2′。代之以经管道12输入液氮，也可考虑在一氧化碳冷循环中设置一台减压涡轮机。
同现有技术中的已知方法相比，本发明具有一些重大优点。由于或许可以取消对分离塔T2加热，所以不纯CH4馏份在分离塔T2底部提取的这种事实要求小得多的一氧化碳冷循环量。基于分离塔T2的再沸效率(Aufkocherleistung)很小或根本不需要再沸，特有的能耗就相应减少。现在可以把甲烷洗涤塔和氢汽提塔一起建造在一个塔内，这能使建造费用比迄今常用的方法更为便宜。以本发明方法运作的装置只需大约80％具有甲烷洗涤功能的常规装置所需的零部件。正如本发明中所记载，进行这样一种方法，对于一氧化碳生产能力较小的、尤其是低于1000Nm3/h的工艺和装置尤为有意义。虽然分离塔T2底部提取到的不纯CH4馏份确实除了甲烷之外基本上还含有一氧化碳，而且塔T1顶部所提取的富氢馏份同样也含有百分之几的一氧化碳，这对收率起着不良作用，但是这一缺点由于可以不使用高成本工艺过程而得补偿。如此，本实施例所达到的一氧化碳收率为85.8％。

Claims (3)

1.从一种在必要时分离掉水和二氧化碳并至少含有氢、一氧化碳及甲烷的进料馏份中提取纯CO馏份的方法，其中将进料馏份冷却并使之部分冷凝，用过冷的液态甲烷洗出一氧化碳和氢，汽提所洗出的氢，并接着对如此提取得的富CO/CH4馏份进行精馏分离，以此分离成纯CO馏份和富CH4馏份，其特征在于，用作洗涤剂的过冷的液态甲烷至少含2-15％(摩尔)一氧化碳，优选含7-10％(摩尔)一氧化碳。
2.权利要求1所述的方法，其特征在于，用精馏分离所得的富CH4馏份作洗涤剂。
3.实施前列诸权利要求中任何一项所述方法用的装置，其特征在于，氢汽提塔构成塔的下部，而该塔的上部是甲烷洗涤塔。
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