CN1646869A - 用于通过低温空气分离获取氩的方法 - Google Patents
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Abstract
本发明涉及一种用于通过低温分离空气获取氩的方法。精馏***(2,4)具有至少一个空气分离塔(4),它被一个在塔纵向方向上延伸的隔离壁(5)分成一个第一分段和一个第二分段(6,7)。含有氧和氩的流体(3)被输入到第一分段(6)中。从第二分段(7)中获取氩浓度在15%到50%之间的含有氧和氩的流体(13)。
Description
本发明涉及一种用于通过在一个精馏***中低温分离空气来获取氩的方法,该精馏***具有三个串联安置的精馏段,其中,第一和第二以及第二和第三精馏段分别在气体方面和液体方面相互连接,并且,第二精馏段具有两个分段,它们在气体方面和液体方面不相互连接并且被并列地流过,其中,向两个分段中的第一分段内输入含有氧和氩的流体,从两个分段中的第二分段中提取含有氧和氩的流体。
氩的沸点位于氧和氮的沸点之间。在传统的采用两级精馏低温分离空气时,氩在低压塔的中间区域内富集。为了获取氩,从该区域中提取通常主要由氧和氩组成的气态馏分。该含有约10%氩的浓缩馏分被输入所谓的粗氩塔,在其中进行氧和氩的精馏分离。在粗氩塔顶部可提取出氩,在其液池里积聚了主要含氧的液体,这些液体回流到低压塔内。
在实际中常常要求氩纯度在95%以上。但在已知方法中向粗氩塔输入只含有约10%氩的流体。为了能够将它浓缩到所要求的高的氩纯度并且在粗氩塔顶部提取出所希望的产品量,必须将大量的蒸汽输入粗氩塔并且在它里面精馏。粗氩塔的横截面必须选择得相应大,因此会产生很大的投资费用。
特别是从获取碳氢化合物的技术领域中已经知道,使用所谓的隔离壁塔用于分离三元混合物。在一个隔离壁塔中,塔的一部分被一个在塔纵向方向上安置的壁分成两个分段。在该隔离壁的上面和下面,这两个分段分别在流动方面连接。在采用适当的操作方法时,流入到隔离壁一侧的分段内的三组分混合物在一个唯一的塔里被分离成三种馏分。最容易沸腾的组分可以在隔离壁塔的顶部获取,中等沸腾的组分在与输入侧相反的隔离壁另一侧获取,最难沸腾的组分从液池获取。与没有隔离壁的塔相比,借助隔离壁塔能够使侧提取口上的中等沸腾组分达到较高的浓度。
迄今为止在低温空气分离中几乎没有采用隔离壁塔,因为它难以调节。在EP 0 638 778 B1中介绍了一种在隔离壁塔内低温分离空气的方法。低压塔在其中间区域内被一个隔离壁分开。在隔离壁的一侧输入来自压力塔的液池液体,而在隔离壁的另一侧抽出含氩的流体。为了改善该方法的调节,在隔离壁的输入液池液体的一侧取出废流体。工艺参数这样选择,使得获取的含氩流体具有最低70%的氩浓度。
当要求产品的氩浓度在70%范围内时,采用EP 0 638 778 B1中介绍的方法可减少粗氩塔内的理论塔板数并且节省建筑高度。但如果要求例如95%以上的高氩浓度,则将从低压塔提出并输送给粗氩塔的流体浓缩到70%以上氩的优点就变得越来越小。这是由于,为了达到高的氩浓度,粗氩塔内必须有多个理论塔板用于从氩中去除最终百分比含量的氧。也就是说,在纯度要求高时,输入粗氩塔内的流体的初始浓度只起微小作用。
因此,本发明的任务是,提供一种用于通过低温空气分离来获取氩的改进方法。
按照本发明,该任务通过开头所述类型的方法解决,其中,从第二分段中获取的流体中的氩浓度在15%到50%之间,优选在15%到40%之间,特别优选在20%到35%之间。
本发明基于这样的知识:在预先规定氩产品的量和纯度时,提高输入粗氩塔内的流体中的氩的初始浓度随之带来输送的蒸汽量减少。就粗氩塔横截面相应减小并且能够节省费用而言,这是有利的。
但空气分离塔的侧提取口上的氩浓度提高使得空气分离塔的结构复杂和调节费事。此外要注意,在产品要求高时在空气分离塔的侧提取口上浓缩氩浓度的优点越来越小,因为如上面所介绍的,在这种情况下,粗氩塔内的理论塔板数主要取决于要达到的最终浓度,不取决于初始浓度。
现在研究表明,为了达到正常功能必须输入粗氩塔中的最小蒸汽量起先随着氩浓度的增加下降,但是,从氩浓度为50%起保持相同。也就是说,侧提取口上进一步氩浓缩达到50%以上时不能继续减少输入粗氩塔内的蒸汽量,因此没有可能继续减小粗氩塔的横截面。只保留了在输入粗氩塔内的混合物中氩浓度较高的优点。但由于在要求氩纯度高时粗氩塔内的理论塔板数基本不取决于初始浓度,所以继续提高从空气分离塔获取的流体内的氩浓度不再有意义。在本发明范围内,对这个事实进行了详细研究并且确定,在从第二分段获取的流体内氩纯度在15%到50%之间是特别有利的。
在实际中表明,当从第二分段获取的流体中的氩浓度在15%和40%之间、优选在20%和35%之间时,该方法是特别有利的。
在使用隔离壁塔时本发明是特别有利的。在这种情况下,精馏***具有至少一个空气分离塔,它具有三个串联安置的精馏段,其中,分别彼此相邻的精馏段在气体方面和液体方面相互连接。中间的精馏段具有一个隔离壁,该隔离壁将精馏段分成两个分段。在第二精馏段内通过该隔离壁来阻止两个分段之间的气体交换和液体交换。但两个分段与位于上面的和位于下面的精馏段在流动方面连接。
代替隔离壁塔,也可以通过两个相互平行安置的塔来分成两个被平行流过的分段。从一个第一空气分离塔的一个中间部位上提取出液体并输送给一个第二塔。气体从第一空气分离塔的一个第二中间部位上引出并进入第二塔内。在第二塔的顶部上产生的气体和来自第二塔的液池的液体最好在这两个中间部位上回流到第一空气分离塔中。在这个结构中,两个在流动方面分开的分段不是通过一个隔离壁、而是通过两个并联的塔来实现。
从第二分段提取出的流体最好被输入一个粗氩塔中,该流体根据结构或是从空气分离塔中取出、或是从第二塔中取出。积聚在那里的、主要含氧的液池液体最好回流到第二分段内,也就是说,回流到那个从中也提取含氩馏分的分段内。
本发明优选适用于具有一个压力塔和一个低压塔的精馏***,其中,隔离壁安置在低压塔内,并且,来自压力塔的富氧流体,特别是液池液体,被输入第一分段中。
特别是当要在粗氩塔内获取纯度在95%以上、优选98%以上的高纯度氩和/或氧含量低于100ppm、优选低于10ppm的氩时,本发明方法表明具有优点。如果在粗氩塔内使用100个以上、优选在150到200个之间的理论塔板,则本发明特别有利。在这些情况下,粗氩塔的结构高度总是由高的最终纯度所要求的理论塔板数来决定。但是,与没有隔离壁塔的传统方法相比,粗氩塔的直径可以明显减小。
最好在空气分离塔内填入用于精馏的填料。在此有利的是,这些填料安置在多个上下叠置的区域内,即所谓的床内,其中,要精馏的液体和/或要精馏的气体被收集在每两个床之间并且被重新分布到下一个填料床上。如果代替填料使用其他内装件或者装置用于在空气分离塔内精馏,同样合适的是,在空气分离塔内相隔一定间距设置收集器和/或分布器,以便能够抵制塔内的分布不匀。
位于空气分离塔内的两个被隔开的区域之间的隔离壁最好分别在一个填料床的上端部上或下端上终止,或者在使用其他内装件时在相应区域的上端部上或下端部上终止,该区域被一个收集器/分布器与相邻区域分隔开。因为在两个塔区域的接合处总要安置收集器/分布器,所以在引入隔离壁时不必设置另外的收集器/分布器。只有直接安置在隔离壁上方的收集器/分布器必须被改装,使得它以希望的方式将液体分布到两个被隔离壁相互隔开的分段上。如果代替隔离壁塔使用一个平行于第一空气分离塔安置的第二塔,与此相应。
在此证明特别有利的是,空气分离塔、特别是双塔设备中的低压塔被分成四个区域,在使用填料的情况下被分成四个填料床,并且,隔离壁设置在第二和第三区域的高度上。
在第一和第二分段中最好装入对上升的气体作用相同压力降的传质元件。
下面借助在附图中示出的实施例详细介绍本发明以及本发明的其他细节。图中示出:
图1 用于实施本发明方法的一个装置,
图2 本发明的另一个实施形式,
图3 输入粗氩塔内的单位蒸汽量与其氩浓度的依赖关系,
图4 氩产量与输入粗氩塔内的蒸汽中的氩浓度的依赖关系。
在图1中示出一个可获取氩的低温空气分离设备的精馏部分。输入空气1在相应净化和冷却之后被导入压力塔2中。积聚在压力塔2的液池内的富氧液体通过管道3被输入到低压塔4中。
低压塔4构成为隔离壁塔。在低压塔4内设置了填料作为精馏元件,它们安置在多个上下叠置的床19、20、21、22上,这些床分别具有大约6米的高度。在每两个床之间设置了用于收集和分布低压塔4内向下流动的液体的收集器/分布器23、24、25、26、27。
在低压塔4的中间区域内这样安置了一个隔离壁5,使得低压塔4被分成两个分段6、7。在此,隔离壁5在两个中间填料床20和21的总长度上延伸。在该区域内不能在两个被隔开的分段6、7之间发生气体交换和液体交换。
相反,在被隔开的分段6、7的下面和上面的床19和22在低压塔4的整个横截面上延伸,致使在两个分段6、7中被分开的上升的及下降的气体流及液体流又汇聚在一起。
在被隔开的分段6内通过管道3将液池液体从压力塔2输入到低压塔4中。为此可以通过管道12将透平机空气导入低压塔4内。在低压塔4的顶部上可以通过管道8获取气态的氮产品。此外,在被隔开的分段6、7的上方设置了一个用于不纯氮的提取口9。通过管道10和11可以从低压塔4的液池获取气态的或者液态的氧产品。
在两个分段6和7内装入了具有相同比表面积的填料。这样,在低压塔内上升的蒸汽在两个分段6、7内遭受相同的压力损失。向下流动的液体借助于分布器24、25被分布到两个分段6、7上。尤其是在两个分段6、7上提供给相同的液体量。但是,为了将方法优化,在分段6和7内设置不同的液体通过能力是完全有意义的。使上升的蒸汽根据相反流动的液体量和填料床20、21内的压力损失分布到两个分段6、7上当然是有利的。
从分段7中提取主要含有氩和氧的、氩浓度为35%的流体13并且输送到一个设置有填料的粗氩塔14内。在粗氩塔14内精馏该氧-氩混合物。在粗氩塔14的顶部,所产生的氩在一个顶部冷凝器15中冷凝,一部分作为剩余氧含量低于10ppm的产品16被获取,一部分17作为回流液体又被送回到粗氩塔14上。液态氧积聚在粗氩塔14的液池内,通过管道18回流到低压塔4的被隔开的分段7中。
在低压塔4内通过隔离壁5将来自压力塔2的液池液体3和透平机空气12与氩提取口13分隔开。采用这种方式,在氩提取口13内产生的氩浓度比在没有隔离壁的塔内明显更高。
在图2中示出了本发明的一个实施形式,在这个实施形式中,设置了一个平行的旁塔30来代替隔离壁5。在两个附图中相同的元件用相同的标记标明。
在这种情况下,低压塔4没有隔离壁。从精馏段22流下来的液体借助于分布器24被分布到构成第一分段的床20、21上。第二分段通过该旁塔30实现。从填料床22流下来的液体的一部分通过管道31从低压塔4中排出并被输送到旁塔30的顶部上。在旁塔30的顶部上产生的气体通过管道32在填料床21上方回流到低压塔4内。相应地,借助管道33将液体从旁塔30输送到低压塔4内以及借助管道34将气体从低压塔4输送到旁塔30内。
在图1和图2所示实施形式中工艺方法是相同的,其中只是在图2中低压塔4的精馏段20、21代表第一分段6,旁塔30代表第二分段7。相应地,流体3、12被输入到低压塔4内,而含氩的流体13被从旁塔30中提取出。
在本发明范围内,根据蒸汽的氩浓度通过模拟来确定输入粗氩塔14内的单位蒸汽量,也就是说与氩产品量有关的蒸汽量。在图3中示出了求出的依赖关系。在此,以氩产品纯度为98.5%和氩产量恒定、也就是说氩产品与输入空气中的氩量的比例不变为出发点。
实的曲线示出了在无限理论塔板数时的理论最低蒸汽量。虚的曲线示出了针对理论塔板数为50计算的曲线走向。两个曲线具有基本相同的走向。然而,从针对有限塔板数的曲线中得知,在这种情况下与理论曲线相比必须输入多出约30%至40%的蒸汽量。
两个曲线表明,起先随着氩浓度提高必须将越来越少的蒸汽输入粗氩塔14中,以便得到所要求纯度和量的氩。但是,这些曲线在氩浓度为约50%时分别与一个下极限值接近。在氩浓度更高时可期待的是,要输入的蒸汽量没有或者只稍微还继续下降。
当供应给粗氩塔14的流体中的氩浓度提高时,蒸汽量降低,因此,粗氩塔的直径可以相应地较小。然而看到的是,蒸汽量的减少只到氩浓度为约50%时为止。相反,当氩浓度提高到50%以上时,在已有条件下不能继续减少蒸汽量,这样就不能继续减小粗氩塔的横截面。然而,随着浓度提高而出现的低压塔调节费用却明显增加。
在希望的产品纯度为98.5%时,粗氩塔14内的理论塔板数也不会通过提高要输入的蒸汽13中的氩浓度而大大降低,因为在产品纯度高时塔板数由所要达到的最终浓度决定,而不是由初始浓度决定。
按照本发明,低压塔4这样工作,使得侧提取口13中的氩浓度达到45%。在这个浓度时,输入到粗氩塔4内的蒸汽量降到最低并且粗氩塔14的直径与蒸汽量相应地减小。
在图4中示出了依赖于输入粗氩塔内的蒸汽中的氩浓度的氩产量。实的曲线给出了针对一个短隔离壁计算的值,虚的曲线给出了针对一个长隔离壁计算的值。其中,低压塔内的塔板数保持不变。
从实的曲线中看到,在输入蒸汽中的氩浓度处于10%到25%之间的范围内时氩产量保持基本不变。该曲线在25%时中断,因为随着隔离壁长度增大不能达到更高的氩浓度。虚曲线的计算以隔离壁较长为基础,在此,也是在氩浓度为30%以上至90%的较高范围内确定基本恒定的氩产量。因此,提高氩浓度不会对产量产生不利影响。
Claims (13)
1、用于通过在一个精馏***中低温分离空气获取氩的方法,该精馏***具有三个串联安置的精馏段,其中,第一与第二精馏段以及第二与第三精馏段分别在气体方面和液体方面相互连接,其中,第二精馏段具有两个分段,它们在气体方面和液体方面不相互连接并且被并列地流过,其中,向这两个分段中的第一分段内输入含有氧和氩的流体,从这两个分段中的第二分段中提取含有氧和氩的流体,其特征为,从第二分段(7,30)中提取的流体(13)中的氩浓度在15%到50%之间,优选在15%到40%之间,特别优选在20%到35%之间。
2、按照权利要求1所述的方法,其特征为,该精馏***具有至少一个空气分离塔(4),它有三个串联安置的精馏段(19,20,21,22),其中,第二精馏段(20,21)具有一个在塔纵向方向上延伸的隔离壁(5),通过此,空气分离塔(4)在隔离壁(5)的高度上被分成一个第一分段(6)和一个第二分段(7)。
3、按照权利要求1所述的方法,其特征为,该精馏***具有至少一个第一空气分离塔(4)和一个第二塔(30),它们在上端部上和下端部上在气体方面和液体方面与第一空气分离塔(4)的中间部位连接,其中,位于第一空气分离塔的这些中间部位之间的段(20,21)和第二塔(30)构成所述两个分段。
4、按照权利要求3所述的方法,其特征为,从第二塔(30)中提取出含有氧和氩的流体(13)。
5、按照权利要求1至4之一所述的方法,其特征为,从第二分段(7,30)中取出的流体(13)被输送给一个粗氩塔(14)。
6、按照权利要求5所述的方法,其特征为,来自该粗氩塔(14)的液池液体返回到第二分段(7,30)中。
7、按照权利要求5或6所述的方法,其特征为,在粗氩塔(14)中获取纯度在95%以上、优选98%以上的氩。
8、按照权利要求5至7之一所述的方法,其特征为,在粗氩塔(14)中获取氧含量低于10ppm的氩。
9、按照权利要求5至8之一所述的方法,其特征为,粗氩塔(14)具有100个以上、优选150至200个理论塔板。
10、按照权利要求1至9之一所述的方法,其特征为,在精馏段(19,20,21,22)内至少部分地装入用于精馏的填料。
11、按照权利要求10所述的方法,其特征为,含有氧和氩的流体分别在两个精馏段之间被收集和/或分布(23,24,25,26,27)。
12、按照权利要求1至9之一所述的方法,其特征为,在精馏***内呈气态上升的、含有氧和氩的流体在第一和第二分段(6,7)内遭受同样的压力损失。
13、按照权利要求1至12之一所述的方法,其特征为,该精馏***具有一个压力塔(2)和一个低压塔(4),其中,隔离壁(5)安置在低压塔(4)内,并且,来自压力塔(2)的富氧的流体(3)被输入第一分段(6)中。
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CN103748427A (zh) * | 2011-08-25 | 2014-04-23 | 林德股份公司 | 用于低温分馏流体混合物的方法和设备 |
CN106468498A (zh) * | 2015-08-20 | 2017-03-01 | 林德股份公司 | 用于通过低温分馏空气来制备氧气的蒸馏塔***和装置 |
CN112955707A (zh) * | 2018-10-23 | 2021-06-11 | 林德有限责任公司 | 用于低温分离空气的方法和设备 |
CN114923313A (zh) * | 2022-05-17 | 2022-08-19 | 陕西聚能新创煤化科技有限公司 | 粗氩精制液氩***及其精制工艺 |
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PL2822683T3 (pl) | 2012-03-06 | 2016-11-30 | Wypełnienie konstrukcyjne | |
KR102089407B1 (ko) * | 2013-07-18 | 2020-03-16 | 주식회사 엘지화학 | 증류 장치 |
JP6204231B2 (ja) * | 2014-03-11 | 2017-09-27 | 大陽日酸株式会社 | 空気液化分離装置及び方法 |
WO2023140986A1 (en) | 2022-01-19 | 2023-07-27 | Exxonmobil Chemical Patents Inc. | Compositions containing tri-cyclopentadiene and processes for making same |
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US5339648A (en) * | 1993-08-05 | 1994-08-23 | Praxair Technology, Inc. | Distillation system with partitioned column |
US5755933A (en) * | 1995-07-24 | 1998-05-26 | The M. W. Kellogg Company | Partitioned distillation column |
US5970742A (en) * | 1998-04-08 | 1999-10-26 | Air Products And Chemicals, Inc. | Distillation schemes for multicomponent separations |
EP0952415A1 (fr) * | 1998-04-21 | 1999-10-27 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Procédé et installation de distillation d'air avec production variable d'argon |
US5946942A (en) * | 1998-08-05 | 1999-09-07 | Praxair Technology, Inc. | Annular column for cryogenic rectification |
US6138474A (en) * | 1999-01-29 | 2000-10-31 | Air Products And Chemicals, Inc. | Argon production control through argon inventory manipulation |
US6250106B1 (en) * | 1999-12-13 | 2001-06-26 | Air Products And Chemicals, Inc. | Process for separation of multicomponent fluids using a multizone distallation column |
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FR2831953B1 (fr) * | 2001-11-05 | 2004-09-24 | Air Liquide | Procede de distillation d'air avec production d'argon et installation de distillation d'air correspondante |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103748427A (zh) * | 2011-08-25 | 2014-04-23 | 林德股份公司 | 用于低温分馏流体混合物的方法和设备 |
CN103748427B (zh) * | 2011-08-25 | 2015-12-23 | 林德股份公司 | 用于低温分馏流体混合物的方法和设备 |
CN106468498A (zh) * | 2015-08-20 | 2017-03-01 | 林德股份公司 | 用于通过低温分馏空气来制备氧气的蒸馏塔***和装置 |
CN106468498B (zh) * | 2015-08-20 | 2020-09-22 | 林德股份公司 | 用于通过低温分馏空气来制备氧气的蒸馏塔***和装置 |
CN112955707A (zh) * | 2018-10-23 | 2021-06-11 | 林德有限责任公司 | 用于低温分离空气的方法和设备 |
CN112955707B (zh) * | 2018-10-23 | 2023-01-24 | 林德有限责任公司 | 用于低温分离空气的方法和设备 |
CN114923313A (zh) * | 2022-05-17 | 2022-08-19 | 陕西聚能新创煤化科技有限公司 | 粗氩精制液氩***及其精制工艺 |
CN114923313B (zh) * | 2022-05-17 | 2024-02-09 | 陕西聚能新创煤化科技有限公司 | 粗氩精制液氩***及其精制工艺 |
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WO2003087686A1 (de) | 2003-10-23 |
RU2004133324A (ru) | 2006-01-27 |
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