CN101218479B - 用于制备粗制氖气的方法和设备 - Google Patents

用于制备粗制氖气的方法和设备 Download PDF

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CN101218479B
CN101218479B CN200680011525.9A CN200680011525A CN101218479B CN 101218479 B CN101218479 B CN 101218479B CN 200680011525 A CN200680011525 A CN 200680011525A CN 101218479 B CN101218479 B CN 101218479B
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J·A·韦伯
N·M·普罗塞尔
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Abstract

低温精馏系统，采用了相分离器(30)和双柱空气分离设备，其中所述相分离器可以包括一个或多个塔盘(32)，其中一些储存液体经过过冷和相分离以制备粗制氖气(5)，残余液体(34)用于回流到所述双柱设备的低压柱(21)。

Description

用于制备粗制氖气的方法和设备
技术领域
本发明一般涉及空气的低温精馏，更特别地，涉及空气的低温精馏以制备氖。
背景技术
氖是空气中以大约18份/百万(ppm)的低浓度存在的有价惰性气体。氖可用作灯泡和发光信号管中的填充气体。另外，由于氖光可以穿透其它光不能穿透的雾，所以氖被用于飞机航标中。可以改进氖回收的系统将会是相当期望的。
发明内容
本发明的一个方面是：
用于制备粗制氖的方法，包括：
(A)通过在高压柱中进行低温蒸馏分离原料空气，以制备含有氖的储存蒸气(shelf vapor)，使至少部分所述含有氖的储存蒸气冷凝以制备含有氖的液体；
(B)使所述含氖液体过冷，将所得流体通过分离器，在所述分离器内将所述流体分离成含有氖的蒸气和残余液体；和
(C)使残余液体由所述分离器通入低压柱，回收含氖蒸气作为产物粗制氖气。
本发明的另一方面是：
用于制备粗制氖的装置，包括：
(A)高压柱、具有重沸器/冷凝器的低压柱、和用于将原料空气通入所述高压柱的设备；
(B)过冷器、分离器、用于将含氖流体从所述高压柱通入所述重沸器/冷凝器、从所述重沸器/冷凝器通入所述过冷器、和从所述过冷器通入分离器的设备；和
(C)用于将液体从所述分离器通入所述低压柱的设备，和用于从所述分离器回收蒸气作为产物粗制氖气的设备。
本文所用的术语“原料空气”是指主要包含氧气和氮气同时也含有氖气的混合物，比如环境空气。
本文所用的术语“柱”是指蒸馏或分馏柱或者区，即，接触柱或者区，其中液体和蒸气相逆流接触以实现流体混合物的分离，比如通过在安装在柱中的一系列垂直分开的塔盘或塔板上、和/或在填充元件比如结构化填充物或者无序填充物上使蒸气和液相接触。有关对蒸馏柱的进一步讨论，请参见R.H.Perry和C.H.Chilton编辑的ChemicalEngineer’s Handbook，第五版，McGraw-Hill Book Company，New York，第13节，The Continuous Distillation Process。
蒸气和液体的接触分离过程取决于组分的蒸气压差。蒸气压高的(或者挥发性强或者沸点低的)组分往往富集在蒸气相中，而蒸气压低的(或者挥发性低或者沸点高的)组分往往富集在液相中。部分冷凝是分离过程，由此蒸气混合物的冷却可以用来使挥发性组分富集在蒸气相中，因而挥发性低的组分富集在液相中。精馏或者连续蒸馏是将连续部分汽化和冷凝结合在一起的分离过程，如同对蒸气和液相进行逆流处理所实现的那样。蒸气和液相的逆流接触通常是绝热的，可以包括在所述相之间的积分性接触(逐步的)或者差分性接触(连续的)。采用精馏原理分离混合物的分离过程装置通常可以和术语精馏柱、蒸馏柱或者分馏柱互换使用。低温精馏是至少部分在150K或者以下的温度进行的精馏过程。
本文所用术语“间接换热”是指使两种流体处于换热关系，但流体互相没有任何物理接触或者混合。
本文所用术语“重沸器”和“重沸器/冷凝器”是指由液体生成柱或者分离器蒸气的换热设备。
本文所用术语“过冷”和“过冷器”分别表示用于将液体冷却至比该液体在现有压力下的饱和温度低的温度的方法和装置。
本文所用术语“上部分”和“下部分”是指柱的分别在其中点之上和之下的那些区段。
本文所用术语“粗制氖气”是指氖气浓度为400ppm-10000ppm的流体。
本文所用术语“塔盘”是指蒸气-液体接触台阶。
本文所用术语“相分离器”是指其中进料被分成各个蒸气和液体级分的容器。通常，容器具有足够的横截面积以使蒸气和液体通过重力分离。
附图说明
图1是本发明的低温精馏系统的一个优选实施方案的简化示意图，其中分离器包括至少一个塔盘。
图2是本发明的低温精馏系统的另一优选实施方案的简化示意图，其中分离器是相分离器。
图3是本发明的低温精馏系统的另一优选实施方案的简化示意图，其中部分含氖液体绕过过冷器。
图4是本发明的另一优选实施方案的示意图，其中液态进料空气被闪蒸，蒸气作为粗制氖气的一部分被回收，残余液体通入低压柱。
发明详述
结合附图具体描述本发明。现在参见图1，原料空气1被通入高压柱20，所述高压柱的操作压力通常为60-220磅每平方英寸绝对压力(psia)。在图1所示的本发明实施方案中，原料空气1是气态料流，料流11中的液体原料空气也被送入系统。料流11分成料流12和料流6，其中料流12通过阀门13作为料流14进入高压柱20，料流6通过阀门15作为料流16进入低压柱21。
在高压柱20内，原料空气通过低温精馏分离成富氧液体和富氮蒸气。富氧液体在料流3中从柱20的下部分抽取，通过换热器17而冷却以形成料流18，通过阀门19作为料流22进入到低压柱21中。从高压柱20的上部分在料流23中抽取含有30-70ppm氖气的富氮蒸气或者储存蒸气，并通入到重沸器/冷凝器24中，在此处通过和低压柱底部液体的间接换热而冷凝。该含氖液体在料流25中从重沸器/冷凝器24中抽取。料流25的一部分26以回流形式返回到高压柱20的上部分。来自重沸器/冷凝器24的另一部分含氖流体在料流27中被通入过冷器28。
在过冷器28内，含氖液体通过和来自低压柱的氮气料流间接换热而过冷，所得的流体作为料流2中的过冷含氖液体从过冷器28中抽取。料流2通过阀门29，然后在料流31中进入分离器30。
在图1所示的本发明实施方案中，分离器30包含至少一个塔盘30。也就是说，在图1所示的本发明实施方案中，分离器30是小型精馏柱。分离器30还包含重沸器33，所述重沸器33通过在料流4中通到该重沸器33的部分储存蒸气进行驱动。在分离器30内，含氖液体分离成含氖蒸气和残余液体。残余液体在料流34中从分离器30通入到低压柱21的上部分。由于用粗制氖气去除了大多数轻质组分，所以该液体形成了含有极低浓度轻质组分的高纯氮产物。含氖蒸气在料流5中从分离器30中回收，作为产物粗制氖气。通常，该粗制氖气被送入氖精炼厂，用于制备高纯氖气或者精炼氖气。料流4中的含氖储存蒸气在重沸器33中冷凝，然后在料流35中从重沸器33中送出。优选，如图1所示，料流35通入料流27，然后通入过冷器28，最后进入分离器30，用于随后回收该流体中的氖气，作为料流5中的部分粗制氖气。
低压柱21在比高压柱20的压力低的压力下操作，通常压力为16-75psia。在低压柱21内，被通入该柱的各种流体通过低温精馏分离成富氧液体和富氮蒸气。富氧液体在料流36中从柱21的下部分抽取，用于作为产物氧回收，所述产物氧的氧浓度为至少90摩尔％。如果需要，如图1所示，富氧液体在作为高压液体和/或气体氧回收之前，可以通过泵37升高压力。富氮蒸气在料流9中从柱21的上部分抽取，通过过冷器28和换热器17而得以加热，并作为氮浓度为至少99.9摩尔％的产物氮38被回收。为了控制产物纯度，在料流9的抽取水平面的下方从柱21抽取含氮废物料流39，通过过冷器28和换热器17而得以加热，并在料流40中从该系统中排出。
图2举例描述了本发明的另一个实施方案，其中分离器是相分离器。对于共有要素而言，图2中的附图标记和图1中的附图标记相同，这些共有要素不再进行详细描述。在图2所示的本发明的实施方案中相分离器50不包含重沸器，因而相分离基本上完全是源于通过阀门29的闪蒸以及在该相分离器内的重力分离。但是，相分离器50可以包含重沸器，在这种情况下，采用图1所示的料流4和35的流体流也会被用于图2所示的本发明实施方案中。
对于共有要素而言，图3所示本发明实施方案中的附图标记和图2中的附图标记相同，这些共有要素不再详细进行描述。现在参见图3，料流27的一部分60并不过冷，而是通过阀门61并且作为料流62和闪蒸料流31合并。这样增加了在相分离器50中制备的蒸气量，因此提高了对挥发性更强的氖气的回收，所述氖气优先富集在蒸气中而不是在残余液体中，所述残余液体从分离器通入低压柱。
对于共有要素而言，图4所示本发明实施方案中的附图标记和图2中的附图标记相同，这些共有要素不再详细进行描述。现在参见图4，通过阀门15闪蒸的液态空气料流6在料流16中通入原料空气相分离器45。来自原料空气相分离器45的蒸气在料流46中通入粗制氖料流5，以形成部分粗制氖产物。来自原料空气相分离器45的液体在料流47中通入低压柱21。本发明的这个实施方案不仅仅用于提高对氖的回收，而且提高了氮产物的纯度，这是因为轻质杂质在料流46中从系统中排出了，否则它们会存在于氮产物中。
对图1所示的本发明实施方案进行了计算机模拟，结果示于表1中。这些结果用于示例目的，并不旨在限制。料流的编号和图1的相对应。
表1
Figure G2006800115259D00061
虽然已经参考一些优选实施方案对本发明进行了详细描述，但是本领域技术人员会认识到，在权利要求的精神和范围内还有本发明的其它实施方案。

Claims (12)

1.用于制备粗制氖气的方法，包括：
(A)通过在高压柱中进行低温精馏分离原料空气，以制备含有氖的储存蒸气，使至少部分所述含有氖的储存蒸气冷凝以制备含有氖的液体；
(B)使所述含氖液体过冷，将所得流体通入分离器，在所述分离器内将所述流体分离成含有氖的蒸气和残余液体；和
(C)使残余液体由所述分离器通入低压柱，回收含氖蒸气作为产物粗制氖气。
2.权利要求1的方法，其中所述分离器包含至少一个塔盘。
3.权利要求1的方法，其中所述分离器包含重沸器，和其中含氖的储存蒸气通入到重沸器。
4.权利要求1的方法，其中所述含氖液体的一部分没有经过过冷就被通入分离器。
5.权利要求1的方法，进一步包括将液态原料空气通入低压柱。
6.权利要求1的方法，进一步包括部分蒸发液体原料空气料流，将部分蒸发的液体原料空气料流加入原料空气相分离器，将残余液体通入低压柱，和回收所得的蒸气作为产物粗制氖气的一部分。
7.用于制备粗制氖气的装置，包括：
(A)高压柱、具有重沸器/冷凝器的低压柱、和用于分别将气态原料空气料流和液体原料空气料流通入所述高压柱的设备；
(B)过冷器、分离器、用于将含氖流体从所述高压柱通入所述重沸器/冷凝器、从所述重沸器/冷凝器通入所述过冷器、和从所述过冷器通入分离器的设备；和
(C)用于将液体从所述分离器通入所述低压柱的设备，和用于从所述分离器回收蒸气作为产物粗制氖气的设备。
8.权利要求7的装置，其中所述分离器包含至少一个塔盘。
9.权利要求7的装置，其中所述分离器包含重沸器，并进一步包含用于将流体从高压柱通入重沸器的设备。
10.权利要求9的装置，进一步包括用于将流体从重沸器通入过冷器的设备。
11.权利要求7的装置，进一步包括用于将流体从重沸器/冷凝器通入分离器的设备，其中所述流体不通过过冷器。
12.权利要求7的装置，进一步包括原料空气相分离器、用于将部分蒸发的原料空气通入原料空气相分离器的设备、用于将液体从原料空气相分离器通入低压柱的设备、和用于将蒸气从原料空气相分离器通入产物粗制氖气的设备，所述部分蒸发的原料空气来源于液体原料空气料流。
CN200680011525.9A 2005-02-18 2006-02-08 用于制备粗制氖气的方法和设备 Expired - Fee Related CN101218479B (zh)

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