CN1406661A - 通过变压吸附的气体纯化 - Google Patents

通过变压吸附的气体纯化 Download PDF

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CN1406661A
CN1406661A CN02127830A CN02127830A CN1406661A CN 1406661 A CN1406661 A CN 1406661A CN 02127830 A CN02127830 A CN 02127830A CN 02127830 A CN02127830 A CN 02127830A CN 1406661 A CN1406661 A CN 1406661A
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R·库马尔
邓曙光
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BOC Inc
Linde LLC
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Abstract

公开一种从气体原料流除去杂质的方法，在容器有吸附剂材料和氧化催化剂的反应区中，从气体原料流除去如氢、水、一氧化碳和二氧化碳的杂质。该方法优选是在低温蒸馏单元之前的变压吸附法。

Description

通过变压吸附的气体纯化
发明领域
本发明涉及一种在变压(pressure swing)吸附单元中除去气体原料流中的气态杂质方法。具体而言，本发明提供一种从气体原料流中除去氢、一氧化碳、水和二氧化碳，再将该气体原料流通入低温蒸馏单元的方法。
发明背景
很好建立了吸附单元操作，能用于纯气体制备、气体纯化和其混合物上前处理(up-front)、进一步的物理和/或化学处理，以及用于处理废弃物料流。广泛使用吸附方法的主要领域之一是大气空气的纯化和分离。为提高这些方法的效率，人们会一直寻求新的吸附剂配方及其使用方法。
工业和技术上最关注的领域之一是在低温蒸馏之前空气的预纯化。通过空气低温分离生产氮气(N2)和氧气(O2)，以及生产氩气(Ar)的常规空气分离单元(ASUs)主要包括分别由两个或至少3个在很低温度下操作的联合蒸馏塔。由于这些低温，必须从将送入ASU的压缩空气原料中除去水蒸汽(H2O)和二氧化碳(CO2)。如果不这样的话，ASU的低温部分会冻结，必须中断生产，加热堵塞部分，再蒸发和除去造成中断的冻结的气体的固体块。这样做的成本很高。一般认为，为防止ASU的冻结，压缩空气原料中的H2O和CO2的含量必须分别小于0.1ppm和小于等于1.0ppm。此外，其它杂质如低分子量烃和一氧化二氮(N2O)也存在于送入低温蒸馏塔的空气进料中，这些杂质也必须在所谓分离方法之前除去，防止有害的过程状态。
空气预纯化使用的方法和设备必须具有稳定满足杂质的上述含量的能力，并且有希望能超过相关的要求含量，必须能以有效的方式进行。这点尤其重要，因为预纯化的成本直接增加了ASU的气体产品的成本。
目前，空气预纯化的工业方法包括逆转热交换器(reversing heatexchanger)、变温吸附、变压吸附和催化剂预纯化方法。
逆转热交换器通过在通道中交替冷冻和蒸发，除去水蒸汽和二氧化碳。这样的体系需要大量的通常为50％或更高的产品气体用于清洁，再生其通道。所以，产品的产率被限制在约为进料的50％。这种明显的缺陷与特定的机械和噪音问题合并，其结果是，近年来，使用逆转热交换器作为ASU之前的空气预纯化的手段已稳步下降。
在空气的变温吸附(TSA)预纯化中，在相对低的环境温度通常约(5-15℃)下从空气除去杂质，在升高温度如约150-250℃范围进行吸附剂的再生。再生所需的产品气体量通常仅为产品气体的约10-25％。因此，TSA法比使用逆转热交换器法有了相当的改进。然而，TSA法需要用于冷却进料气体的蒸发冷却或冷冻单元以及用于加热再生气体的加热单元。因此，尽管比逆转热交换器的原理在成本上更低，但它们在投资成本和能耗方面都存在缺陷。
变压吸附(PSA)法(加压—真空变换吸附(PVSA))由于吸附和通过脱附的再生通常都在环境温度进行，因此是对TSA法的很有吸引力的替代法，例如作为空气预纯化的手段。PSA法一般确实需要大大多于TSA法的再生气体。如果要求高回收低温分离的气体，这也是缺陷。如果PSA空气预纯化单元结合到低温ASU装置中，来自在接近环境压力下操作的低温部分的废物流用作再生吸收床的吹扫流。进料空气压力下通过活性氧化铝颗粒层，除去大量H2O和CO2，然后通过沸石颗粒例如FAU结构型如NaX沸石层，除去残留的低浓度的H2O和CO2。注意到吸附剂按照这种方式排列提高了温度作用，即PSA床中温度在脱附期间下降。在其它配置中，仅使用活性化铝从进料空气中除去H2O和CO2。声称这样的配置降低了温度作用。
此外，一些应用要求在低温蒸馏塔中进行处理之前从环境空气中除去H2和CO，生产没有氮、氧、氩和其它空气组分的H2和CO。目前，TSA法不得不用于这样的应用。这导致用于这些方法的预纯化体系的高成本。
发明概述
本发明提供从气体原料流中除去包括H2和CO的气态杂质的方法，该方法包括下列步骤：
a)从气体原料流中除去水；
b)使气体原料流与氧化催化剂接触，使一氧化碳转变为二氧化碳；
c)从气体原料流中除去二氧化碳；
d)使气体原料流与催化剂接触，使氢转变为水；
e)除去由氢转变产生的水。
还可以使用另外的层，除去气体原料流中痕量烃和氮氧化物。较好的气体原料流是空气，空气送入空气分离单元(ASU)中的低温蒸馏单元之前，在变压吸附(PSA)过程中除去杂质。
发明的详细描述
本发明提供一种气体原料流通入空气分离单元的低温蒸馏塔之前除去该气体原料流中气态杂质的方法。该方法包括从原料流气体中除去水、氢、一氧化碳和二氧化碳的变压吸附过程。
该过程包括使含这些杂质的原料流气体通过一个五层床。在第一层，使用常规的水吸附剂来吸附水。在第二层，催化剂使一氧化碳氧化为二氧化碳。在第三层，除去环境的二氧化碳和在第二层产生的二氧化碳。在第四层，催化剂使氢氧化为水，在最后第五层中，第四层产生的水分被吸附。在一个处理区中存在五层，较好的在一个容器中包含三个吸附剂层和两个催化剂层。
第一吸附剂层可以是任何能吸附水的吸附剂，例如活性氧化铝、硅胶或X型沸石如NaX沸石。该层也可以是这些材料的复合物。
包含氧化催化剂的第二层一般是金属氧化物如氧化镍或锰氧化物和铜氧化物的混合物。这种催化剂材料较好的是Hopcalite型催化剂，例如Carulite-300(由Carus Chemical Company制造)。
第三层含有除去二氧化碳的吸附剂，例如活性氧化铝、硅胶或X型沸石如NaX沸石。第三层吸附剂较好的还吸附水，并且可以是一复合材料。第三层的X型沸石材料较好是钠LSX型沸石，它是硅与铝的原子比在0.9-1.1范围的X型沸石材料。
第四层是负载钯或其它贵金属的催化剂，如从Engelhard得到的蛋壳型钯催化剂，但较好的是在疏水性载体上的钯基催化剂，或包含在载体上的助催化剂铂、钯和锡氧化物的催化剂，可以Sofnocat从Molecular Products Co.得到。
第五层除去在第四层中产生的水分。该层可以是吸附水的任何吸附剂如活性氧化铝、硅胶或X型沸石如NaX沸石。该层还可以是这些材料的复合物。
还可以使用任选的第六层和第七层，除去痕量烃和氮氧化物。这些层也可以是复合物层。烃吸附剂通常选自A型和X型沸石以及硅胶。氮氧化物吸附剂通常选自A型、X型或Y型沸石。
本发明的另一个实施方案中，可以不同的顺序实施这些步骤。例如，原料流气体与催化剂接触使氢转变为水的步骤可以在除去气体原料流中二氧化碳的步骤之前进行。从气体原料流中除去二氧化碳的步骤也可以在气体原料流与氧化催化剂接触使一氧化碳转变为二氧化碳之前进行。在这样的步骤顺序下，水也可以被除二氧化碳的吸附剂除去。
本发明的变压吸附法可以在气相变压吸附法采用的常规和已知的压力下实施。这种压力可以在宽范围内变化，但取决于发生吸附的压力以及发生气体脱附的压力。通常，该压力范围从吸附步骤约20巴至吹扫步骤约0.05巴，宜在约10巴至0.15巴范围。更好的在约6巴至1巴范围。此变压吸附法中的温度，在吸附步骤一般在约5-55℃。但是，可以采用高达200℃的温度。
下面，结合具体实施例描述本发明，但是，这些实施例不构成对本发明范围的限制。
实施例
实施例1
在一个床的PSA单元(测得直径为2.14英寸，高91英寸)中进行PSA/PPU试验。在该床中，底部填充67英寸的得自ALcan的AA300的活性氧化铝，12英寸Carulite-300材料，然后是12英寸的Sofnocat催化剂。表1列出试验条件。
                                          表1
进料步骤： 在进料压力为80.5psia，进料温度为25℃，空气流速为3.88scfm下12分钟
排气步骤： 1分钟
吹扫步骤： 9分钟，吹扫气体压力为22.7psia，温度为25℃，吹扫气体氮气流速为3.5scfm
再加压步骤： 2分钟，用来自床顶部的氮气
使用环境空气作为此实施例的进料。用RGA-5CO/H2痕量分析仪测定原料流气体、Carulite层之后的原料流气体以及产品气流中氢和一氧化碳的浓度。表2列出连续循环试验3周后进料步骤中测定的不同气体流中氢和一氧化碳的浓度。
                                       表2
  时间        进料结束        Carulite之后          产品
  H2(ppb)   CO(ppb)   H2(ppb)   CO(ppb)   H2(ppb)   CO(ppb)
  0   207.1   114.9
  3   191.7   0.2   1.0   0.9
  9   208.3   0.4   7.2   0.7
  12   211.9   0.0   10.1   1.3
表2中列出的结果清楚地表明：在试验条件下，一氧化碳被Carulite氧化催化剂完全除去，而氢被Sofnocat氧化催化剂有效除去，从约200ppb降低至约10ppb。
实施例2
重复类似于实施例1中所述的试验，但通过在进料空气中注入2％氢和3.22％一氧化碳，以更高的氢和一氧化碳的空气进料进行试验。此试验的结果列于表3。
                                        表3
    时间        进料结束        Carulite之后          产品
  H2(ppb)   CO(ppb)     H2(ppb)   CO(ppb)   H2(ppb)   CO(ppb)
    0   3120.5   5024.0
    3     350.0   3.6   0.0   2.0
    6     589.6   2.8   0.0   1.8
    9     911.0   1.4   227.8   2.4
    12     2417.3   4.1   546.8   2.6
如表3和实施例2所表明的，空气中全部一氧化碳(约5000ppb)被Carulite氧化催化剂层有效除去。Carulite除去部分氢，再由Sofnocat催化剂进一步除去。在进料步骤结束时产品流中的H2达到546.8ppb。然而，通过在进料步骤时结合Carulite和Sofnocat催化剂，进料空气中95％以上的氢被除去。
参考具体实施方案描述了本发明，本领域技术人员应理解本发明有许多其它形式和变动。所附的权利要求书和本发明覆盖了在本发明精神和范围之内的所有形式和变动。

Claims (12)

1.一种从气体原料流中除去杂质的方法，该方法包括下列步骤：
a)从所述气体原料流中除去水；
b)使气体原料流与氧化催化剂接触，使一氧化碳转变为二氧化碳；
c)从所述气体原料流中除去二氧化碳；
d)使所述气体原料流与氧化催化剂接触，使氢转变为水；
e)从所述气体原料流中除去所述的水。
2.如权利要求1所述的方法，其特征在于所述气体原料流是空气，所述杂质是选自氢、水、一氧化碳和二氧化碳的物质。
3.如权利要求1所述的方法，其特征在于所述方法是变压吸附法。
4.如权利要求1所述的方法，其特征在于所述步骤a)包括使所述气体原料流与除水的吸附剂接触。
5.如权利要求1所述的方法，其特征在于步骤b)的所述氧化催化剂是锰氧化物和铜氧化物的混合物。
6.如权利要求1所述的方法，其特征在于步骤d)的所述氧化催化剂是在疏水性载体上的钯基催化剂。
7.如权利要求1所述的方法，其特征在于步骤c)包括使所述气体原料流与除二氧化碳的吸附剂接触。
8.如权利要求1所述的方法，其特征在于所述方法还包括使所述气体原料流与除去痕量烃和氮氧化物的吸附剂接触。
9.如权利要求1所述的方法，其特征在于所述步骤d)在步骤c)之前进行。
10.如权利要求1所述的方法，其特征在于所述步骤e)包括使所述气体原料流与除去水的吸附剂接触。
11.如权利要求1所述的方法，其特征在于步骤c)在步骤b)之前进行。
12.如权利要求1所述的方法，其特征在于在步骤c)还除去H2O。
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CN114073892A (zh) * 2020-08-19 2022-02-22 普莱克斯技术有限公司 用于进料气体流的预纯化的系统

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