CN108302899A - 一种利用液化空气提取贫氪氙产品的空分***及方法 - Google Patents

一种利用液化空气提取贫氪氙产品的空分***及方法 Download PDF

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CN108302899A
CN108302899A CN201810271057.3A CN201810271057A CN108302899A CN 108302899 A CN108302899 A CN 108302899A CN 201810271057 A CN201810271057 A CN 201810271057A CN 108302899 A CN108302899 A CN 108302899A
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tower
poor krypton
krypton xenon
xenon
air
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沈浩
张敏
李楠
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ZHEJIANG XINRUI AIR SEPARATION EQUIPMENT CO Ltd
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
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    • F25J3/04048Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
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    • F25J3/02Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
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    • F25J3/04642Recovering noble gases from air
    • F25J3/04648Recovering noble gases from air argon
    • F25J3/04654Producing crude argon in a crude argon column
    • F25J3/04666Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642Recovering noble gases from air
    • F25J3/04745Krypton and/or Xenon
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00Processes characterised by the type or other details of the feed stream
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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Abstract

一种利用液化空气提取贫氪氙产品的空分***,它包括一主要由上塔和下塔通过中间主冷凝蒸发器构成的空分精馏塔,下塔引出液化空气用管路分别接入上塔和粗氩塔上部相接的粗氩冷凝器,粗氩冷凝器中引出液化空气接入贫氪氙塔,经过所述固定于贫氪氙塔底部相接的贫氪氙塔蒸发器的冷却之后,从底部引出提取的贫氪氙液,贫氪氙塔的顶部引出氪氙成分的饱和态空气用管路连接并送入上塔;所述的方法包括:a、从粗氩冷凝器引出的液化空气通过1号管路作为原料液进入贫氪氙塔顶部精馏,在贫氪氙塔蒸发器中通过2号管路取出贫氪氙液产品,在贫氪氙塔顶部通过3号管路取出空气进入上塔中部参与精馏;b、气液临界点的空气大部分通过4号管路进入下塔参与精馏,另外一小部分通过5号管路进入贫氪氙塔蒸发器吸收腔做吸收冷量,液化后的液化空气通过6号管路降压后输入上塔中部参与精馏。

Description

一种利用液化空气提取贫氪氙产品的空分***及方法
技术领域
本发明涉及的是一种利用液化空气提取贫氪氙产品的空分***及方法,属于能源、化工领域的低温空气分离技术。
背景技术
稀有气体一般是指氩、氖、氦、氪、氙五种气体。除了氦主要由天然气提取外,空气是这些稀有气体的主要来源。随着国民经济的发展,稀有气体的应有越来越广泛,需求也越来越大,从空气中回收稀有气体显露出极高的经济价值。
目前贫氪氙液的提取主要通过大型空分中所带的氪氙粗制装置实现。这种制取方法必须在空分上塔低部或者粗氩冷凝器顶部安装一段精馏塔板,如若建设初期没安装这段塔板则不能够通过这种方法制取贫氪氙液,如图1所示;而且在上塔加装的这段塔板上气液比和上塔其他部分相比有很大差别,稍有设计偏差和操作偏差容易造成整个空分工况的不稳定。因此,设计操作难度高,投资大,产量受空分规模的限制,难适应现代化企业对氪氙越来越大的需求。
发明内容
本发明的目的在于克服现有技术存在的不足,而提供一种可在不增加空分塔板的前提下提取贫氪氙液,既适用于新上空分装置建设、也适用于原有未带氪氙粗制装置空分改造,具备投资及占用空间都比较小且适用性强的利用液化空气提取贫氪氙产品的空分***及方法。
本发明的目的是通过如下技术方案来完成的,一种利用液化空气提取贫氪氙产品的空分***,它包括一主要由上塔和下塔通过中间主冷凝蒸发器构成的空分精馏塔,所述空分精馏塔下塔引出液化空气用管路分别接入上塔和粗氩塔上部相接的粗氩冷凝器,所述的粗氩冷凝器中引出液化空气接入贫氪氙塔,经过所述固定于贫氪氙塔底部相接的贫氪氙塔蒸发器的冷却之后,从底部引出提取的贫氪氙液,贫氪氙塔的顶部引出氪氙成分的饱和态空气用管路连接并送入上塔。
作为优选:所述的贫氪氙塔蒸发器的吸收腔输入接口连接从空分输入的中压气液临界点的空气或从外界输入的中压氮气,所述的贫氪氙塔蒸发器的吸收腔输出接口接出液化空气输入上塔或连接液氮管线。
一种利用所述空分***提取贫氪氙产品的方法,所述的方法包括:
a、从粗氩冷凝器引出的液化空气通过1号管路作为原料液进入贫氪氙塔顶部精馏,在贫氪氙塔蒸发器中通过2号管路取出贫氪氙液产品,在贫氪氙塔顶部通过3号管路取出空气进入上塔中部参与精馏;
b、气液临界点的空气大部分通过4号管路进入下塔参与精馏,另外一小部分通过5号管路进入贫氪氙塔蒸发器吸收腔做吸收冷量,液化后的液化空气通过6号管路降压后输入上塔中部参与精馏。
作为优选:所述的贫氪氙塔和贫氪氙塔蒸发器从上到下依次布置,贫氪氙塔蒸发器内空气的液化温度高于液化空气的蒸发温度,通过控制空气和液化空气的压力实现;
所述的贫氪氙塔为一种精馏塔,精馏元件采用填料加分布器或采用筛板结构或采用填料加筛板的组合塔结构;所述的贫氪氙塔蒸发器采用板翅式换热器或管式换热器结构;所述的所有管路均分别安装有调节管路内介质压力的常规结构控制阀门。
本发明的有益效果是:
首先,本方法能从空分粗氩冷凝器产生的液化空气中提取贫氪氙液,无需对空分主流路进行更改,可用于新建空分项目也可应用于原有空分改造,应用范围广而且投资小,流程效率高,大大降低了贫氪氙气的生产门槛;
其次,贫氪氙气产量高,整套空分中氙的提取率达70%左右,贫氪氙塔中氙提取率达98%左右。
第三,具有低温精馏方法的一切优点,而无技术背景所述的原方法的局限。
附图说明
图1是现有技术的不提取贫氪氙的空分流程示意图。
其中:C1为下塔,C2为上塔,C3为粗氩塔,K1为主冷凝蒸发器,K2为粗氩冷凝器,E1为过冷器。
图2是本发明所述空分液化空气中提取贫氪氙的流程图。
其中:C1为下塔,C2为上塔,C3为粗氩塔,C4为贫氪氙塔,K1为主冷凝蒸发器,K2为粗氩冷凝器,K4为贫氪氙塔蒸发器,G1为主冷凝蒸发器吸收腔,G2为贫氪氙塔冷凝器吸收腔,G4为贫氪氙塔蒸发器吸收腔,E1为过冷器。
具体实施方式
下面将结合附图对本发明作详细的介绍:图2所示,本发明所述的一种用液化空气提取贫氪氙产品的空分***,它包括一主要由上塔C2和下塔C1通过中间主冷凝蒸发器K1构成的空分精馏塔,所述空分精馏塔下塔C1引出液化空气用管路分别接入上塔C2和粗氩塔C3上部相接的粗氩冷凝器K2,所述的粗氩冷凝器K2中引出液化空气接入贫氪氙塔C4,经过所述固定于贫氪氙塔C4底部相接的贫氪氙塔蒸发器K4的冷却之后,从底部引出提取的贫氪氙液,贫氪氙塔C4的顶部引出氪氙成分的饱和态空气用管路连接并送入上塔C2。
图中所示,所述的贫氪氙塔蒸发器K4的吸收腔G2输入接口连接从空分输入的中压气液临界点的空气或从外界输入的中压氮气,所述的贫氪氙塔蒸发器K4的吸收腔G2输出接口接出液化空气输入上塔C2或连接液氮管线。
一种利用所述空分***提取贫氪氙产品的方法,所述的方法包括:
a、从粗氩冷凝器K2引出的液化空气通过1号管路作为原料液进入贫氪氙塔C4顶部精馏,在贫氪氙塔蒸发器K4中通过2号管路取出贫氪氙液产品,在贫氪氙塔C4顶部通过3号管路取出空气进入上塔C2中部参与精馏;
b、气液临界点的空气大部分通过4号管路进入下塔参与精馏,另外一小部分通过5号管路进入G4贫氪氙塔蒸发器吸收腔做吸收冷量,液化后的液化空气通过6号管路降压后输入上塔中部参与精馏。
本发明所述的贫氪氙塔C4和贫氪氙塔蒸发器K4从上到下依次布置,贫氪氙塔蒸发器内空气的液化温度高于液化空气的蒸发温度,通过控制空气和液化空气的压力实现;
所述的贫氪氙塔C4为一种精馏塔,精馏元件采用填料+分布器或采用筛板结构或采用填料加筛板的组合塔结构;所述的贫氪氙塔蒸发器K4采用板翅式换热器或管式换热器结构;所述的所有管路均分别安装有调节管路内介质压力的常规结构控制阀门。
实施例:空气中的氪含量为1.14ppm,氙含量为0.086ppm。在空分下塔实现氧氮分离的过程中,空气中微量的氪氙都浓缩在液化空气中进入空分上塔和粗氩冷凝器,然后随氧气和液氧产品输出***,加入贫氪氙塔后,使粗氩冷凝器产生的液化空气先经过贫氪氙塔精馏提取其中的氪氙成分,再将取出了氪氙组分的饱和态空气送入上塔继续参加精馏。
2、通过控制输入贫氪氙塔内的液化空气压力以及输入贫氪氙塔蒸发器的中压气液临界点的空气(或氮气)压力,保证两种物流存在温差(例如:液化空气压力为0.25MPa(A)时,蒸发温度为-176.7℃;中压空气为0.562MPa(A)时,冷凝温度为-173.4℃,两者存在温差3.3℃)。这样,中压空气(或氮气)的冷凝和液氮的蒸发可同时进行。
3、在贫氪氙塔中,上升蒸发气与下流冷凝液产生热交换,不断的热交换使底部液体中的氪氙浓缩,从而得到氙总含量为200ppm左右的贫氪氙液。
本发明具有以下特点:
1、从液化空气中分离出产品贫氪氙液:空分下塔氧氮分离中,氪氙为重组分存在于液化空气中,本发明用粗氩冷凝器产生的液化空气作为原料,将原料中的氪氙与氧氮组分进行分离。
2、具有充足的热源:如前所述,贫氪氙塔的热源可采用来自原空分内的流路,分别被冷凝后再次进入原空分参与精馏,其冷源的量不受约束,能够充分满足贫氪氙塔的精馏需要,从而提高贫氪氙塔的贫氪氙提取率。

Claims (4)

1.一种利用液化空气提取贫氪氙产品的空分***,它包括一主要由上塔(C2)和下塔(C1)通过中间主冷凝蒸发器(K1)构成的空分精馏塔,所述空分精馏塔下塔(C1)引出液化空气用管路分别接入上塔(C2)和粗氩塔(C3)上部相接的粗氩冷凝器(K2),其特征在于所述的粗氩冷凝器(K2)中引出液化空气接入贫氪氙塔(C4),经过所述固定于贫氪氙塔(C4)底部相接的贫氪氙塔蒸发器(K4)的冷却之后,从底部引出提取的贫氪氙液,贫氪氙塔(C4)的顶部引出氪氙成分的饱和态空气用管路连接并送入上塔(C2)。
2.根据权利要求1所述的利用液化空气提取贫氪氙产品的空分***,其特征在于所述的贫氪氙塔蒸发器(K4)的吸收腔(G4)输入接口连接从空分输入的中压气液临界点的空气或从外界输入的中压氮气,所述的贫氪氙塔蒸发器(K4)的吸收腔(G4)输出接口接出液化空气输入上塔(C2)或连接液氮管线。
3.一种利用权利要求1或2所述空分***提取贫氪氙产品的方法,其特征在于所述的方法包括:
a、从粗氩冷凝器(K2)引出的液化空气通过1号管路作为原料液进入贫氪氙塔(C4)顶部精馏,在贫氪氙塔蒸发器(K4)中通过2号管路取出贫氪氙液产品,在贫氪氙塔(C4)顶部通过3号管路取出空气进入上塔(C2)中部参与精馏;
b、气液临界点的空气大部分通过4号管路进入下塔(C1)参与精馏,另外一小部分通过5号管路进入贫氪氙塔蒸发器(G4)吸收腔做吸收冷量,液化后的液化空气通过6号管路降压后输入上塔(C2)中部参与精馏。
4.根据权利要求3所述的利用空分***提取贫氪氙产品的方法,其特征在于所述的贫氪氙塔(C4)和贫氪氙塔蒸发器(K4)从上到下依次布置,贫氪氙塔蒸发器(K4)内空气的液化温度高于液化空气的蒸发温度,通过控制空气和液化空气的压力实现;
所述的贫氪氙塔(C4)为一种精馏塔,精馏元件采用填料+分布器或采用筛板结构或采用填料加筛板的组合塔结构;所述的贫氪氙塔蒸发器(K4)采用板翅式换热器或管式换热器结构;所述的所有管路均分别安装有调节管路内介质压力的常规结构控制阀门。
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