CN108955086A - 用于净化气体混合物的装置和方法 - Google Patents

用于净化气体混合物的装置和方法 Download PDF

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CN108955086A
CN108955086A CN201810488237.7A CN201810488237A CN108955086A CN 108955086 A CN108955086 A CN 108955086A CN 201810488237 A CN201810488237 A CN 201810488237A CN 108955086 A CN108955086 A CN 108955086A
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mixture
neon
unit
temperature
cryogenic
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CN108955086B (zh
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P·巴嘉奥克斯
C·布维耶
F·迪朗
M·斯塔普福林
G·齐克
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

本发明涉及用于净化气体混合物的装置，用于从包含氖气的混合物生产浓缩气体尤其是氖气，包括容纳包括依次串联布置的以下单元的低温净化回路的冷箱：至少一个低温吸附净化单元，用于通过在65‑100K温度尤其是65K下的低温吸附来净化混合物；用于将混合物冷却至25‑65K的冷却单元；和用于对混合物进行低温蒸馏以在低温蒸馏单元的出口处生产浓缩液体的低温蒸馏单元，其中冷却单元包括通过热交换器从混合物提取热能的至少一个低温制冷机。本发明还涉及用于净化包含氖气的气体混合物以生产富氖气体的方法。

Description

用于净化气体混合物的装置和方法
技术领域
本发明涉及用于净化气体混合物的方法和装置。
本发明特别地涉及净化气体混合物以获得纯的或几乎纯的气体，例如氖气。
本发明更加特别地涉及用于净化气体混合物的装置，以从包含氖的混合物中生产浓缩的气体，尤其是氖气。所述装置包括容纳有低温净化回路的冷箱，所述低温净化回路包括串联布置的以下单元：至少一个低温吸附净化单元，所述至少一个低温吸附净化单元用于通过低温吸附来净化混合物，所述低温吸附在65K与100K之间的温度特别是65K的温度下进行；之后的冷却单元，所述冷却单元用于将所述混合物冷却至25K与65K之间的温度；以及之后的低温蒸馏单元，所述低温蒸馏单元用于对所述混合物进行低温蒸馏以在所述低温蒸馏单元的出口处生产浓缩液体。
背景技术
氖气是在电子器件中广泛使用的稀有气体。
特别是对于这些应用来说，这一气体必须被净化到相当高的纯度水平(在处理结束时杂质需为几ppm的数量级)。
为获得浓缩气体，存在几种净化思路。
然而，已知的方法无法容易地协调纯度、对不纯气体的净化能力(针对过程入口处的各种各样的成分)以及能源性能之间的要求。
已知的用于净化氖气的方法通常使用联接至低温蒸馏装置的低温净化装置。
文献DE102010042247描述了使用氦气闭环(逆布雷顿循环：膜压缩和两个串联的涡轮机)来冷却混合物到26K的温度以及冷凝氖气，以从氦气中重力分离。在下游，净化是使用低温蒸馏来完成的。
根据其它已知的方案，净化是通过压缩和膨胀的依次运行而获得的。对于这种类型的方法，纯度不可能达到ppm的数量级，只能得到百分之一的数量级。事实上，除非使用了(有效的)最终蒸馏塔，否则杂质氦仍然溶解在液态氖中。
发明内容
本发明的一个目标是克服前文描述的在先技术中的一些或全部缺陷。
为了这一目标，根据本发明并且遵从之前存在的通常定义的方法，主要特征在于：用于将混合物冷却至25K-65K之间温度的单元，该单元包括至少一个低温冷却器，所述至少一个低温冷却器通过热交换器从混合物抽取热功率/量。
在低温蒸馏之前使用低温冷却器类型的冷源——被称作“低温制冷机”(cryocooler)——使得极为有效地完善气体的净化成为可能。
事实上，这一冷源是本地的/局部的。“本地的/局部的冷源(Local cold source)”指代的是并非分阶段的/非分级式的制冷系统。冷能在给定的温度下在该系统的一端产生，这不同于制冷循环——制冷循环在不同的对应温度、在多个单独的阶段(不同的端)产生冷能。
可对温度进行精细控制。如果有必要的话，这允许最为接近待冷凝气体的三相点，因此能大幅减少液相杂质。
此外，本发明的实施例可包括以下特征中的一个或多个：
-所述至少一个低温制冷机包括吉福特-麦克马洪型低温制冷机、脉冲气体管、斯特林型低温制冷机、逆巴顿循环型/逆布雷顿循环型型低温制冷机和焦耳-汤姆逊型低温制冷机中的至少一者；
-冷却单元包括多个串联的低温制冷机，以及接收流体混合物并与所述串联的低温制冷机的冷面进行热交换的至少一个热交换器；
-装置在冷箱中包括位于低温吸附净化单元的上游的以下至少一者：用于冷却混合物的第一低温交换器，其配置为冷却混合物至65K-110K之间的温度，优选为等于80K的温度；与输送混合物的管线进行热交换的至少一个液氮浴；
低温吸附净化单元包括至少两个吸附器，其并联布置并浸入65K液氮浴中，并交替运行(吸附阶段/再生阶段)；
-低温蒸馏单元是用于分离氖和氦的塔；
-装置包括用于在低温蒸馏单元的出口处回收液化的浓缩气体的管线，回收管线与位于冷箱中的至少一个用于冷却混合物的单元进行热交换；
-用于回收液化的浓缩气体的管线与以下的至少一者进行热交换：液氮浴，其与低温吸附净化单元上游的用于输送混合物的管线进行热交换；交换器，用于冷却位于低温制冷机上游的混合物；
-该装置包括，在冷箱的上游的以下至少一者：用于提取包含在混合物中的至少部分的氢气的单元；用于提取包含在混合物中的至少部分的水和/或二氧化碳的干燥器；
-用于提取包含在混合物中的至少部分的氢气的单元包括催化反应器，其配置为用于通过与氧气反应而将混合物中的氢气转化为水，
-干燥器包括至少一份优选两份吸附剂，用于交替工作进行水和二氧化碳的捕获。
本发明还涉及用于净化包含氖气的气体混合物以生产富氖气体的方法，所述方法使用根据上文或下文中的任意一个特征的净化装置进行，所述方法包括：通过低温吸附来净化混合物的步骤，该步骤使用低温吸附净化单元，在63.5K-80K之间的温度进行低温吸附以从混合物中除去至少部分的氮气、氧气、一氧化碳和氩气；然后是使用低温制冷机来冷却混合物的步骤，将混合物冷却至25-65K之间的温度并接近氖的三相点，以冷凝氖气；然后是低温蒸馏混合物的步骤，在低温蒸馏单元中进行以在低温蒸馏单元的出口处产生所述的富氖液体。
根据其它特别的特征：
-待净化的气体混合物包括：氖气，体积百分比15-65％；氦气，体积百分比3-20％；氢气，体积百分比0.2-4％；氮气，体积百分比20-60％；并且生产获得的所述浓缩气体包括体积百分比85-100％的氖气；
-在装置的入口处的氖气体积流量和在装置的出口处的氖气体积流量的比例(或产出)大于85％，优选为85-98％。
本发明还可涉及包括上文或下文给出的特征的任意组合的任何替代设备或方法。
附图说明
在参考图1阅读以下说明后，其它的特别的特征和优点会更加明显。图1示出了示意性的部分视图，该图示出了根据本发明的装置的可行的示例的结构和操作的示例。
具体实施方式
图1示出了用于净化气体混合物的装置1，其包括净化回路，净化回路的入口2供应有包含氖气、氦气和存在于空气中的气体类型的杂质的待净化气体。
例如，气体混合物或者原料气体由氮气、氖气、氦气、氢气、一氧化碳和可能的微量的其它气体(氩气、氧气、二氧化碳等)组成。
例如，待净化的气体混合物包括体积百分比为15-60％的氖气、体积百分比为3-20％的氦气、体积百分比为0.2-4％的氢气、以及体积百分比20-60％的氮气。
例如，在设备入口处，混合物的压强/压力可以是大约1.5巴(bar)，温度是大约5-35℃。
优选地，该装置用于生产浓缩的氖气，其体积百分比为85-100％，尤其是高于99％，例如是至少99.999％。
在入口的下游，该装置1可包括压缩机3，压缩机3可选地带有用于将压缩气体冷却至室温的系统(为简明起见未示出)。
在压缩机3的下游，该装置优选地包括用于提取包含在混合物中的至少部分的氢气的单元4。
例如，单元4通过将氧气受控地注入催化剂床(例如铝加上氧化钯涂层的类型)中或催化剂床的上游来对压缩后的原料气体进行“热”净化以去除杂质氢气和一氧化碳。放热的化学反应导致水和二氧化碳的形成。可通过液化作用(参见用于化合物水(the compoundH2O)的水分离罐6)和分子筛(例如，13X型、氧化铝或硅胶)的吸附而从原料混合物中去除这些化合物。
为了这一目的，在单元4的下游和水分离罐6的上游，气体可在交换器5中被冷却。
在水分离罐6的下游，该装置优选地包括干燥器7，用于去除包含在混合物中的至少部分的水蒸气和/或二氧化碳。例如，水和二氧化碳可以在多个分子筛塔中被除去，所述多个分子筛塔交替运行(一个处于吸附阶段，同时另一个处于再生阶段，例如使用热氮气的流或一些其它惰性气体的流进行)。
在干燥器7的下游，混合物进入(例如真空隔离的)冷箱19，在冷箱19中混合物在第一低温冷却交换器8中被冷却。第一低温冷却交换器8例如是板式逆流交换器，其配置为将混合物冷却至65K-110K之间的温度，例如80K。
在下游，混合物在一个或两个液氮浴9、10(例如，通过与输送混合物的、尤其为管式的热交换器进行热交换)中被冷却。第一液氮浴9例如维持在大气压力和饱和状态，而第二液氮浴10例如维持在低于大气压的压力(例如0.18bar的临界压力)和65K的温度下。
在下游，分离罐11回收主要由氮组成的液相。然后该液体可被再循环至两个浴9、10中的至少一个，以便通过将低温流体整合在单元的热平衡中来利用该低温流体。
然后气相在用于通过低温吸附来进行净化的净化单元12中被净化。单元12包括例如交替运作(吸附/再生)的两份分子筛来捕获氮气、氧气和氩气。
在单元12的下游，混合物主要由氦气和氖气组成。
主要由氦气和氖气组成的混合物可在交换器13中被冷却至例如为大约35K的温度。这一交换器13例如是逆流管式的，其与净化后的氖交换热量(如下将要详述的)。这一热交换器可例如具有多个内管，在壳体中输送例如待加热的净化后的氖。
在下游，通过冷却单元14将混合物冷却至例如约25K。冷却单元14包括至少一个带有例如经由热交换器从混合物中提取热量的冷头的低温制冷机。
“低温制冷机”指代的是用于在恒定的温度下、非分级的制冷机器，例如吉福特-麦克马洪型低温制冷机、脉冲气体管、斯特林型低温制冷机或焦耳-汤姆逊型低温制冷机。
因此，所述“低温制冷机”并不是如上引用的文献中的(例如使用氦气的)冷却回路。
例如，冷却单元14包括串联的一个或多个低温制冷机和一个或多个接收流体混合物并与所述串联的低温制冷机的冷头进行热交换的热交换器(例如由铜或铝制成)。
冷却的混合物进入相分离罐15。液氖被回收作为至少一个低温蒸馏塔16的进料。
被回收的气体混合物可用于冷却例如蒸馏塔16的隔热部件/隔热罩。可在相分离罐15和蒸馏塔16之间设置膨胀阀(未图示)来将压力降低至例如1.5bar，并促进氦气-氖气分离。
蒸馏塔16可不带有冷凝器。在塔顶部的气体(例如一半是氖气，一半是氦气)可以可选地被循环至在装置1的入口2处的压缩机3。
例如，氖气/氦气混合物的分离(在相分离器15的出口处大约1体积百分比的氦气)可在充有填料(规整或者散装)的蒸馏塔16中完成。具有加热器的蒸馏器可使在液体提取部离开低温蒸馏塔16的氦气少于3ppmv。
因此，可以液相回收净化后的氖。这种冷的液氖可被安排与位于低温吸附净化单元12和低温冷却单元14之间的冷却交换器13进行热交换。
冷的液氖之后可与两个氮浴中的至少一个(例如氮浴9)进行热交换，并且然后与第一低温冷却交换器8进行热交换。
在冷箱的出口18处，浓缩的氖可被加热至室温，并且然后例如在高压缸中被压缩。
因此，本装置以使氖气和氦气与其它其余成分(氮气、空气中的微量气体)分离为目标而对原料气体进行低温净化。通过例如液体冷凝(在77K，然后在65K)以及随后通过低温吸附(例如在65K)而从原料混合物中分离氮气。用于进行这些分离和用于冷却原料混合物的冷源可以是大气压或高于大气压的饱和状态下的液氮，和/或低于大气压的饱和状态下的液氮。使用一个或多个低温冷却器(其可以是吉福特-麦克马洪型、脉冲管等)来将吸附阶段之后保留的氦气和氖气冷却至接近25K的温度(该温度接近纯物质Ne的三相点)。在此温度下，很大比例的氖将被液化，并且能被从氦气更多的气相中分离。然而，富氖液相将需要进行蒸馏以使氖与溶解在氖中的残留氦(大约1体积百分比)分离。
本装置使氖的纯度达到很高(杂质少于10ppmv)成为可能。
如图中用虚线所示的那样，可经由至少一个供应管线20而将冷却流体(液氮源，例如在冷箱之外)供应至氮浴9、10中的至少一个。此外，可设置管线21以用于从氮浴9,10中的至少一个中回收蒸发的气体。这些回收管线21可用于与第一低温冷却交换器8进行热交换。然后，在回收管线21中流动的流体可被收集至冷箱的出口。
根据一个可行的变型，冷却单元14可包括用于制冷的装置或由其组成，该用于制冷的装置根据克劳德循环(基于氖和/或氢的闭合循环，其最冷的部分是由给定压力下的流体的液化作用的温度施加的)。常规而言，克劳德循环包括进行与膨胀系统(尤其是利用焦耳-汤姆逊效应的阀)相关联的一个或多个逆布雷顿循环的流体，该膨胀系统将该流体膨胀至达到目标低温。通过所述膨胀获得的冷端构成本地的/局部的冷源。
根据另一个可行的变型(进行结合或作为替代)，用于提取氢气的单元4可被去掉，并且安装可以是用于净化氢气，即用于生产不含杂质如氦气、氮气和氩气的氢气。

Claims (13)

1.用于净化气体混合物的装置，该装置用于从包含氖气的混合物生产浓缩气体，尤其是氖气，所述装置包括容纳有低温净化回路的冷箱(19)，所述低温净化回路包括依次串联布置的以下单元：
至少一个低温吸附净化单元(12)，所述至少一个低温吸附净化单元(12)用于通过低温吸附来净化混合物，所述低温吸附在65K与100K之间的温度、尤其是65K的温度下进行；
冷却单元(14)，所述冷却单元用于将所述混合物冷却至25K与65K之间的温度；以及
低温蒸馏单元(16)，所述低温蒸馏单元(16)用于对所述混合物进行低温蒸馏以在所述低温蒸馏单元(16)的出口处生产浓缩液体，
其特征在于，用于将混合物冷却至25K与65K之间的温度的所述冷却单元(14)包括非分级式制冷系统和通过热交换器从所述混合物提取热量的至少一个低温制冷机，所述至少一个低温制冷机包括吉福特-麦克马洪型低温制冷机、脉冲气体管、斯特林型低温制冷机中的至少一者。
2.根据权利要求1所述的装置，其特征在于，所述冷却单元(14)包括多个串联的低温制冷机和至少一个热交换器，所述至少一个热交换器用于接收流体混合物并与所述串联的低温制冷机的冷面进行热交换。
3.根据权利要求1或2所述的装置，其特征在于，在所述冷箱(19)中包括位于所述低温吸附净化单元(12)的上游的以下至少一者：用于冷却所述混合物的第一低温交换器(8)，所述第一低温交换器配置为将所述混合物冷却至65K与110K之间的温度，优选为80K的温度；与输送所述混合物的管线进行热交换的至少一个液氮浴(9、10)。
4.根据权利要求1-3中任一项所述的装置，其特征在于，所述低温吸附净化单元(12)包括并联布置的至少两个吸附器，所述至少两个吸附器浸在65K的液氮浴中并且交替运行(吸附阶段/再生阶段)。
5.根据权利要求1-4中任一项所述的装置，其特征在于，所述低温蒸馏单元(16)是用于分离氖和氦的塔。
6.根据权利要求1-5中任一项所述的装置，其特征在于，所述装置包括用于在所述低温蒸馏单元(16)的出口处回收液化的浓缩气体的回收管线(17)，所述回收管线(17)与位于所述冷箱(19)中的至少一个用于冷却混合物的单元(8、9、13)进行热交换。
7.根据权利要求6所述的装置，其特征在于，所述回收液化的浓缩气体的回收管线(17)与以下的至少一者进行热交换：液氮浴(9)，所述液氮浴(9)与在所述低温吸附净化单元(12)的上游输送混合物的管线进行热交换；交换器(13)，所述交换器用于冷却位于低温制冷机(14)上游的混合物。
8.根据权利要求1-7中任一项所述的装置，其特征在于，包括位于所述冷箱(19)的上游的以下至少一者：用于提取包含在所述混合物中的至少部分的氢气的单元(4)；用于提取包含在所述混合物中的至少部分的水和/或二氧化碳的干燥器(7)。
9.根据权利要求8所述的装置，其特征在于，所述用于提取包含在所述混合物中的至少部分的氢气的单元(4)包括催化反应器，所述催化反应器配置为用于通过与氧气反应而将所述混合物中的氢气转化为水。
10.根据权利要求8或9所述的装置，其特征在于，所述干燥器(7)包括用于交替工作以捕获水和二氧化碳的至少一份、优选两份吸附剂。
11.用于净化包含氖气的气体混合物以生产富氖气体的方法，所述方法使用根据权利要求1-10中任一项所述的净化装置进行，所述方法包括以下步骤：
通过低温吸附来净化混合物，所述低温吸附通过低温吸附净化单元(12)而在63.5K与80K之间的温度下进行以从所述混合物中除去至少部分的氮气、氧气、一氧化碳和氩气；
通过低温制冷机将所述混合物冷却至25K与65K之间的温度并接近氖的三相点，以使氖气冷凝；以及
在低温蒸馏单元(16)中对所述混合物进行低温蒸馏，以在所述低温蒸馏单元(16)的出口处产生氖浓缩液。
12.根据权利要求11所述的方法，其特征在于，待净化的气体混合物包括按体积计占比以下的物质：15％-65％的氖气；3％-20％的氦气；0.2％-4％的氢气；20％-60％的氮气；并且生产得到的浓缩气体包含按体积计占比85％-100％的氖气。
13.根据权利要求11或12所述的方法，其特征在于，在所述装置的入口处的氖气的体积流量和在装置的出口处的氖气的体积流量的比例大于85％，优选在85％与98％之间。
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