CN1117697C - 生产超高纯氮的低温系统 - Google Patents

生产超高纯氮的低温系统 Download PDF

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CN1117697C
CN1117697C CN98123488A CN98123488A CN1117697C CN 1117697 C CN1117697 C CN 1117697C CN 98123488 A CN98123488 A CN 98123488A CN 98123488 A CN98123488 A CN 98123488A CN 1117697 C CN1117697 C CN 1117697C
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nitrogen
ultra
hydrogen
high purity
temperature
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CN1216750A (zh
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M·L·马科斯基
小T·J·伯格曼
J·K·霍维尔
小J·P·纳特沃拉
D·R·汤普森
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Praxair Technology Inc
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Praxair Technology Inc
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Abstract

进一步纯化氮气的方法，由此生产基本不含氢、氧和一氧化碳的超高纯氮，其中氮气在温度150k或低于150k的温度下与含金属的吸附剂进行接触。

Description

生产超高纯氮的低温系统
技术领域
本发明一般涉及超高纯氮的生产，更具体地说，涉及使用低温操作法的超高纯氮的生产。
背景技术
电子工业方面氮的使用者典型地需要超高纯氮，这种超高纯氮的任何杂质例如氧、氢和一氧化碳的含量少于1ppb。在由常规低温空气分离装置得到的氮中的这些物质的浓度典型地在约0.5～2ppm的范围内。由于氧的沸点高于氮，所以低温蒸馏几乎完全可除去它。可是，由于一氧化碳的沸点与氮的沸点很接近，氢的沸点又更低，所以存在于送往低温空气分离装置的原料空气中的绝大多数一氧化碳也存在于装置的氮产物中，而氮产物流中的氢浓度约是原料空气中氢浓度的两倍。
典型地是在低温空气分离过程之后使用常规的吸附方法来除去这些杂质。可是，这样的装置是有缺点的，因为进行纯化需要大型的吸附容器。
使用常规室温吸附法来生产超高纯氮的一种替换方法是氢和一氧化碳分别在上游先氧化成水和二氧化碳。然后这些氧化产物在低温空气分离之前在分子筛纯化装置中除去。这种氧化典型地是以催化法进行的。这种氧化方法的主要缺点在于它需要很高的温度，这增加了能量的需求，因而增加了整个方法的费用。另一个缺点在于残留在产物氮气流中的氧必须用另一种方法除去，一般是再使用一个单独的低温蒸馏法，这进一步增加了整个过程的费用。
因此，本发明的目的就是提供一种生产超高纯氮的改进系统。
发明内容
本发明实现了上述的目的和其它的目的，这些目的对于通过阅读本文公开的本领域技术人员是显而易见的，本发明包括：
生产超高纯氮的低温吸附方法，该方法包括使含有一种或多种氢、氧或一氧化碳杂质的氮气在150k或更低的温度下与含金属的吸附剂相接触，和生产基本上不含有氢、氧和一氧化碳的超高纯氮。
本文所用术语“低温吸附”其含意指的是在150k或更低的温度下进行的吸附。
本文所用术语“塔”意指着蒸馏塔或分馏塔或蒸馏区或分馏区，也就是说接触塔或接触区，其中液体和蒸汽相逆流接触以实现液体混合物的分离，例如通过蒸汽相与液相在一系列安装在塔内的竖直分开的塔盘或塔板上和/或在填料构件上进行接触，填料构件可以是结构填料构件和/或随机填料构件。为了进一步讨论蒸馏塔，请参看R.J.Perry和C.H.Chilton编辑的，McGraw-Hill书籍公司纽约发行的化学工程师手册第五版本，第13章，连续蒸馏方法。一个塔可以包括一个塔顶冷凝器，在此冷凝器中蒸汽冷凝为塔的回流液。
蒸汽和液体接触分离法取决于各组分的蒸汽压的差。高蒸汽压(易挥发的或低沸点的)组分将易于在蒸汽相富集，而低蒸汽压(难挥发的或高沸点的)组分将易于在液体相富集。分离方法是部分冷凝，由此可以使用蒸汽混合物的冷却而在蒸汽相富集挥发性组分，和这样难挥发性组分就在液体相富集。精馏或连续蒸馏就是将蒸汽相和液体相逆流处理所获得的连续的部分蒸发和部分冷凝相结合的分离方法。蒸汽相和液体相的逆流接触是绝热的，可以包括两相之间的积分接触或微分接触。使用精馏原理来分离混合物的分离工艺的配置常常可互换地称为精馏塔、蒸馏塔或分馏塔。低温精馏是至少部分地在150k或低于150k的温度下进行的精馏方法。
本文所用术语“间接热交换”其含意指的是将两种流体在它们彼此间没有任何物理接触或相互混合的情况下发生的热交换。
本文所用术语塔的“上部”和“下部”其含意指的是分别位于塔的中点上方和下方的部分。
本文所用术语塔“顶”指的是在塔的内部构件例如塔板或填料上方塔的那一段。
附图说明
图1是本发明优选实施方案的流程图，其中，低温吸附工艺与低温空气分离装置组合成一整体。
图2是本发明另一个优选实施方案的流程图，其中，应用低温吸附工艺来纯化来自贮槽的氮气。
图3是按图2所示的实施方案中再生吸附剂系统的流程图。
具体实施方式
在本发明的方法中，含有ppm量级的一种或多种氢气、氧气或一氧化碳杂质的氮气在150k或低于150k的温度下与吸附剂接触。温度优选地不大于约120k，最优选地温度在80-100k的范围内。吸附剂基本上吸附存在于氮气中的全部的氢、氧和一氧化碳，这导致得到超高纯氮产品，这种超高纯氮基本上不含有氢、氧和一氧化碳。在低温下进行吸附过程可以使低温空气分离系统中产生的氮气从分离系统中排出，和直接进行纯化，而无需在吸附步骤之前进行加热步骤，这样就降低了操作费用。保存在贮槽中的氮气也可以利用本发明的方法进行纯化。在此实施方案中，低温贮槽的氮气在贮存温度或接近于贮存温度的条件下与吸附剂接触，无需进行预热。本发明的低温吸附系统能够使用比利用常规高温装置或室温装置所需要的吸附容器小得多的吸附容器，因此降低了纯化装置的投资费用。
表1列出了在低温下能够有效地吸附氢、氧和一氧化碳的本发明方法的合适的吸附剂，这些吸附剂包括含有镍、铜、钯或铁的吸附剂。优选的吸附剂是含镍吸附剂，最优选的吸附剂是氧化铝载体上的镍(II)的氧化物。吸附剂优选地以吸附剂床的形式装载在对于所需量的吸附剂的合适容量的容器中。
在本发明的优选实施方案中，吸附剂通过在氢气和超高纯氮的气氛中在温度大于120℃，优选地大于200℃的条件下进行加热而再生的。用于吸附剂再生的气氛最优选的组成按超高纯氮中总混合物的体积计，约是1％的氢。氢在吸附剂的表面与一氧化碳和氧反应分别形成甲烷和水。甲烷和水较微弱地与吸附剂键合，因此能够很容易地利用氮气流从吸附剂表面除去。再生是以不同的时间间隔进行的，这取决于吸附剂容器的容量和氢、一氧化碳和/或氧在用作本方法原料的氮气中的浓度。当使用一个或多个容器来生产超高纯氮时，典型情况下可以应用多重容器来使一个或多个容器再生。
图1是流程图，该流程图表示了本发明与低温空气分离装置一体化的低温吸附氮气纯化系统。参照图1，管道1中的原料空气在压缩机2中被压缩，二氧化碳、水和某些烃通过预纯化器3除去。存在于原料空气中的氢和一氧化碳不能被预纯化器除去，因为在压缩机排料条件下，它们不会被预纯化器的分子筛材料所吸附。管道4中的净化空气流然后利用在热交换器5中依靠与回流的间接热交换而冷却到低温。管道6中的冷空气流送入低温精馏塔7，在此精馏塔中原料空气通过低温精馏被分离成氮气和富氧液体。氮气具有相当低的氧浓度，典型情况下小于1ppm。所示出的蒸馏过程是代表能产生具有低浓度氧的氮气的一般蒸馏法。蒸馏法本身并不影响纯化器的设计和构型。因此，与本发明相结合，可以使用任何的方法来生产氮气，只要这种方法可以除氧到很低的含量。如果是用一个不在低温下生产氮的方法，在进行本发明的方法之前，要进行产物流的冷却。超高纯氮可以返回加入蒸馏塔的顶部，以改进蒸馏效率，因而减少了蒸馏塔生产的氮气中的氧含量。
低温氮气离开蒸馏过程，通过管道8、旁路管9和旁路阀V1而到达低温纯化器12或氧分析器10，在进入低温纯化器之前，在氧分析器中测量低温氮气的氧含量，以防止氧含量突增。另一部分氮气30进入顶部冷凝器31，在此冷凝器中，氮气冷凝，作为回流返回塔7。富氧液体从塔7的下部以液流33进入顶部冷凝器31，在此冷凝器中，通过与上述的冷凝氮气进行的间接热交换而被蒸发，此时富氧气体以废物气流34从装置中除去。
图1示出了低温纯化器12。阀(V1-V18)的功能概述以下：V1  旁路9的控制阀。V2  辅助液体管线21。V3  管线11的放空阀。V4  辅助管线21的阀门。V5  从纯化器排出纯化氮产物的阀。V6  管道9或13的清扫阀。V7  用于与再生循环产物流隔离的床12A的隔离阀。V8  用于与再生循环产物流隔离的床12A的隔离阀。V9  用于床12A的再生放空。V10 从床12A到管道22的产品阀。V11 用于与再生循环产物流隔离的床12B的隔离阀。V12 用于与再生循环产物流隔离的床12B的隔离阀。V13 用于床12B的再生放空。V14 床12B到管道22的产品阀。V15 向纯化器提供产物流14的再生循环阀。V16 提供纯氢与产物流15混合的再生循环阀。V17 床12A再生的阀。V18 床12B再生的阀。
使用两台氧分析器重复分析。氮蒸汽流通过管线11进入低温纯化器12，在纯化器12中，除去以1ppb或低于1ppb的浓度而存在的氢、一氧化碳和任何剩余的氧。阀V3是管线11的放空阀。离开纯化器而在管线13中的纯产品物流在热交换器5中加热到室温，然后加以回收。阀V6是管道9或13的清扫阀。
本发明的纯化器12包括两台床12A和12B，两台床含有含金属的吸附剂，例如至少含有5％镍平衡的氧化铝吸附剂材料，优选地含有10-30％镍平衡氧化铝吸附剂材料，最优选地含有20％镍平衡氧化铝吸附剂材料。纯化产物来自床12A或者来自床12B。在每个纯化器床上有一对隔离阀，其作用是将纯化器床与管线11或管线21输送的液流隔开以便再生或可能的停车。12A使用隔离阀V7和V8；12B使用隔离阀V11和V12。当一个床12B吸附时，则一个床12A再生。
实现再生是将来自管线14和阀15的约5％的超高纯氮产物与来自槽27经过阀16和管线15的氢混合，以产生含约1％(体积)氢的混合物，该混合物在加热器16中加热到高于120℃的温度，优选地加热到至少200℃的温度。典型情况下，在将1％氢的混合物引入之前，先将要再生的床加热到至少120℃的温度。热流经过管线17和阀V17而送到纯化器床12A，或经过阀V18而送到12B，加热各自的吸附剂床，释放出任何被吸附的物质。再生废流从12A经过阀9和管线18放空。
再生过程需要不低于120℃的温度，优选地至少200℃，氢与吸附的一氧化碳反应形成甲烷，与氧反应形成水。然后甲烷和水和氢一道很容易解吸。再生循环24小时，在再生期间，两个床换向，用再生床代替吸附床。再生可以每隔24小时或每隔几天进行，这取决于容器的容量。再生流与吸附流成逆流。
也可以使用本发明的低温纯化系统从以液体形态贮存和运输的氮中除去0.5-1ppm的氧和1-2ppm的一氧化碳。当低温精馏装置不工作时，典型地氮以液体形态贮存，以满足使用要求。槽19的备用贮存液体使用蒸发器20加热到室温，经过阀V4，管线21和阀V2到低温纯化器。贮存的液体产物典型地含有很少的氢，因为氢在运输时和在液体贮槽中汽化掉了。而一氧化碳的负荷不论在低温还是在室温下都是相同的，所以它决定了低温吸附器的容器尺寸。因此，低温纯化器的尺寸既可以用于本方法也可以用于液体氮的纯化。
由于纯化器处于低温，当过程氮经过它时，从床12A或床12B离开纯化器的备用氮一开始就是冷的。如果需要加热产物氮，则让产物氮分别经过阀V10或阀V14，和管线22而送往电热乙二醇/水浴23。热流经过管24而送往过滤罐25。经过管线13或24的物流在过滤罐装置25中处理，以便在产物通过管26放出回收之前除去细小颗粒。
此外，在相同质量流速下，在正常操作期间经过纯化器的蒸发的液体氮的体积会大于通过再生器的低温氮的体积。蒸发氮纯化时，通过纯化器的压力损失约是以过程蒸汽观测到的压力损失的四倍。可是，在液体贮槽中得到的压力典型地是相当高的。因此，这种增加了的压力降不会引起问题。
图1实例说明了本发明特别优选的实施方案，在此实施方案中，一部分低温吸附系统产生的超高纯氮经管线28返回到低温精馏塔7的上部，优选地返回到顶部。这种回流操作改进了空气分离装置的效率，降低了低温精馏塔产生的氮气的氧含量。超高纯氮进入顶部冷凝器，用于产生回流。如果需要的话，管线29可以除去顶部冷凝器31的冷凝的氮气，而作为超高纯液体氮回收。
表1包括在87k(-183℃)温度下对已鉴定的低温吸附材料所进行的实验室特性表征工作所得到的数据。选择低温吸附剂材料的准则在于该吸附剂材料以其低温吸附剂中每摩尔金属能吸附最大摩尔数的一氧化碳、氧和氢。由实验工作鉴定的最好的低温度吸附材料是HTC-500TM的Crosfield镍催化剂(由伊利诺斯州·芝加哥Crosfield催化剂商家买到)。
表1
来源/吸附剂 组成   H/M    CO/M    O/M 注解
METADYNE  (Elma，NY) 钨海绵   -   ＜0.01    - ＞700℃下再生
Union Carbide  (Danbury，CT) 9％CuO-Y沸石te   -     0.23    -
Crosfield/HTC-500TM 20％NiO/Al2O3   0.01     0.09    0.02
BASF(Mt.Olive，NJ)/R-3-12TM CuO/ZnO/Al2O3    -   ＜0.01     - 基于40％Cu+的负荷
Union Carbide/OC-112TM 50％CuO；MnO2/SiO2    -   ＜0.01  ＜0.01
Carus (Ottawa，IL)/Carulite-300TM 75％MnO2；15％CuO/Al2O3    -   ＜0.01  ＜0.01 基于75％Mn+3的负荷
Degussa(Tulsa，OK)/E-221TM 0.5％Pd/Al2O3    -     1.1     -
United Catalyst(Louisville，KY)/C12-4-02TM Fe/Al2O3    -   ＜0.01    0.01 基于80％Fe+2的O2负荷
Engelhard (Iselin，NJ)/CR-0211 T 5/32＂TM 18％Cr2O3/Al2O3    -   ＜0.01  ＜0.01
Engelhard/Silica 2351 T1/8＂TM 90％二氧化硅/Al2O3    -     -  ＜0.01
Engelhard/Co-0138 E1/16＂TM 30％Co/二氧化硅    -     0.02  ＜0.01
各种 5A分子筛    -     0.04   -
表1中，H/M，CO/M，O/M分别是原子氢、一氧化碳和氧对给定金属的摩尔比。
在本发明的另一个优选实施方案中，应用独立的低温吸附系统由标准级别的氮例如来自液氮贮槽或液体拖车的氮来生产超高纯氮。图2表示了流程图。使用本发明的低温吸附系统通过低温气相化学吸附来纯化含有浓度为0.1-10ppm到1ppb或更少的氧、氢或一氧化碳中的一种或多种杂质的氮气。
如图2流程图所示，液体氮从槽101取出，流过管线102，通过蒸发器103，或通过走蒸发器旁路的阀104。在任一情况下，蒸发氮都保持在150k的温度或低于150k的温度，优选地80-100k，最优选地保持在约90k的温度。管线105中的氮流以整个产品流作为气体，或作为液体，以1-10加仑/时进入催化床顶部，进行闪蒸。不使用时，闪蒸维持催化床低温制冷。低温高纯氮蒸汽流过催化床106，在此催化床中，至少一种杂质(氧、氢和一氧化碳)经化学吸附而达1ppb或更低。包含催化床的容器107只有一个入口和出口，供流动和/或催化剂处理用。容器应用低温隔热来维持低温。容器是直立的。超高纯氮蒸汽维持在低温，通过管108从此床的底部出口放出。超高纯氮在蒸发器109中加热到室温，利用压力调节器110来调节它的压力，它通过颗粒过滤罐111，以便在回收前消除任何的颗粒物。
优选的镍催化床具有连续纯化低温氮蒸汽达30天而无需再生的能力。此床优选地是够大的，足以纯化来自液体氮贮槽或液体拖车的氮达30天，和可以在较不频繁的再生时间间隔，例如6-12个月下工作。例如，对于一种每小时生产180,000立方英尺(CFH)氮的装置，所需要的催化剂量至少为500磅，但不多于5000磅。
图2所示的低温纯化器不具有经久的再生能力。可使用辅助设备在现场或不在现场进行再生操作使催化剂再生。图3例示了所需要的设备和装置。使经过管线201和阀210的接近室温的约5％的超高纯氮与经过管线202和阀211的氢源物流混合以便在管线203中产生含氮和约1％(体积)氢的再生流，以此实现再生。再生流进入静态混合器204，以保证良好的混合。混合器对于成功地进行此过程并非绝对必要的。再生流然后经过管205，进入加热器206，在加热器中加热到不低于120℃，优选地至少200℃。当热流通过管207排出加热器时，它经过截止阀212，进入催化剂吸附床208，吸附剂床被热流加热，释放出任何被吸附的物质。废再生流通过床和管209放空。
再生过程需要至少120℃的温度，优选地至少200℃，含氢的气流将被吸附的一氧化碳还原为甲烷，将氧还原而形成水。甲烷和水与氢的混合物流然后很容易被解吸。再生循环周期，包括加热和冷却工序，可以从24小时到2周，这取决于容器的容量。再生流与吸附流成逆流。
虽然本发明参照了某些优选的实施方案进行了详细说明，但是本领域技术人员将会认识到，在权利要求的精神和范围内，还可以有本发明的其它实施方案。

Claims (10)

1.生产超高纯氮的低温化学吸附方法，该方法包括在150K或更低的温度下使含有氢、氧或一氧化碳中的一种或多种杂质的氮气与含镍、铜、钯和铁中至少一种的含金属吸附剂相接触，生产氢、氧和一氧化碳的含量少于1ppb的超高纯氮。
2.权利要求1的方法，其中吸附剂含有镍。
3.权利要求2的方法，其中吸附剂是机械载带在含氧化铝基体上的镍(II)氧化物。
4.权利要求1的方法，其中还包括在氢气和超高纯氮的气氛中在不低于120℃的温度下对吸附剂的再生。
5.权利要求4的方法，其中吸附剂与氢和超高纯氮的混合物进行接触而再生。
6.权利要求1的方法，其中氮气取自低温精馏塔。
7.权利要求1的方法，其中氮气取自液氮贮槽。
8.权利要求6的方法，其中一部分超高纯氮引入到低温精馏塔的上部。
9.权利要求8的方法，其中还包括从低温精馏塔回收超高纯氮。
10.权利要求7的方法，其中氮气在与吸附剂接触之前快速挥发。
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