CN102721259B - 一种氖氦分离提纯方法 - Google Patents

一种氖氦分离提纯方法 Download PDF

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CN102721259B
CN102721259B CN201210061205.1A CN201210061205A CN102721259B CN 102721259 B CN102721259 B CN 102721259B CN 201210061205 A CN201210061205 A CN 201210061205A CN 102721259 B CN102721259 B CN 102721259B
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CN102721259A (zh
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曹月丛
喻永贵
严寿鹏
俞建
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SHANGHAI QIYUAN GAS DEVELOPMENT Co.,Ltd.
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SHANGHAI QIYUAN AIR SEPARATION TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

本发明提供的一种氖氦分离提纯方法，包括以下将氖氦混合气体进入液氮换热器中冷却至70~85K；进入液氖换热器冷却至25~35K，然后进入气液分离器进行气液分离，分离后的气相为粗氦，液相为粗氖；将所述粗氖经过第二减压阀减压至1.5~2.0bar，进入纯氖塔中分离后，塔底的纯液氖复热气化后加压充瓶；将所述粗氦进入热交换器中冷却至60~70K，并经低温吸附器除去杂质气体后，获得纯氦气，复热后加压充瓶。本发明的氖氦分离提纯方法操作简单、方便，并且安全性高、回收率高、能耗低、易控制、适用于工业大规模化生产需要。

Description

一种氖氦分离提纯方法
技术领域
本发明涉及一种气体分离提纯的方法，尤其涉及一种从含氖氦的混合气体中分离提纯氖气和氦气的方法。
背景技术
氖气与氦气是惰性气体，其在空气中的含量仅为18.18×10-6和5.24×10-6。氖气、氦气在空分设备精馏塔内为不凝气，而以气态聚集在主冷凝器顶部和氮回流液中。不易被分离。
随着科技的发展，氖气和氦气已大量适用于工业的各个领域。氖气多用于充填航标灯、霓虹灯和用作低温实验室的安全致冷剂；氦气用作稀有金属精炼的保护气和配制深水作业、宇航中呼吸用气，用于压力容器、真空系统检漏和制作氦氖激光器，还在原子能、红外线探测、低温电子等方面得到应用。
现有技术中的氖氦混合气的分离提纯技术，早期多采用液氢为冷源。在液氢温度下，将氖氦混合气的温度降低至接近氖的三相点温度，使氖液化。从而达到氖氦分离的目的。但是液氢生产具有复杂性和危险性。
因此，本领域的技术人员致力于开发一种安全方便、回收率高的氖氦分离提纯方法。
发明内容
鉴于上述的现有技术中的问题，本发明所要解决的技术问题是现有的技术安全性低、回收率不高。
本发明提供的一种氖氦分离提纯方法，包括以下步骤：
步骤1，将氖氦混合气体加压到170～200bar，并冷却至90～120K，然后使用液氮将氖氦混合气体冷却至70～85K；
步骤2，将氖氦混合气体进一步冷却至45～55K，并减压至24～30bar，然后用液氖冷却至25～35K，进行气液分离，分离后的气相为粗氦，液相为粗氖；
步骤3，将所述粗氖减压至1.5～2.0bar，精馏制备纯氖；
步骤4，将所述粗氦复热回收冷量后再冷却至60～70K，并经低温吸附除去杂质气体后，获得纯氦气。
在本发明的一个较佳实施方式中，所述步骤1的氖氦混合气体通过以下步骤得到：
步骤1.1，将经过脱氢处理后的粗氖氦混合气增压至25～35bar，通过除水干燥后冷却至80～100K，然后进一步冷却至60～70K，进行气液分离；
步骤1.2，将分离得到的气相经低温吸附除去杂质气体后，获得氖氦混合气体。
本发明的氖氦分离提纯方法操作简单、方便，并且安全性高、回收率高、能耗低、易控制、适用于工业大规模化生产需要。
附图说明
图1是本发明的实施例的装置的结构示意图；
图2是本发明的实施例的包括粗提纯的装置的结构示意图。
具体实施方式
以下将结合附图对本发明做具体阐释。
如图1中所示的本发明的实施例的装置的结构示意图，一种氖氦分离提纯方法，包括以下步骤：
步骤1，将氖氦混合气体经过压缩机9加压到170～200bar，通过第一换热器10冷却至90～120K，再进入液氮换热器11中冷却至70～85K；
步骤2，将通过液氮换热器11后的氖氦混合气经第二换热器12后冷却至45～55K，经过第一减压阀13减压至24～30bar，进入液氖换热器14冷却至25～35K，然后进入气液分离器15进行气液分离，分离后的气相为粗氦，液相为粗氖；
步骤3，将所述粗氖经过第二减压阀16减压至1.5～2.0bar，进入纯氖塔17中分离后，塔底的纯液氖复热气化后加压充瓶；
步骤4，将所述粗氦进入热交换器19中冷却至60～70K，并经低温吸附器20除去杂质气体后，获得纯氦气，复热后加压充瓶。
本发明采用低温高压节流和气液分离使氖与氦分离，之后通过低温精馏获得纯氖，粗氦经过低温吸附除去氖等杂质获得纯氦，并不使用液氢，防止了使用液氢的复杂性和危险性。本发明的氖氦分离提纯方法操作简单、方便，并且安全性高、回收率高、能耗低、易控制、适用于工业大规模化生产需要。
另如图1中所示，在本发明的实施例中，步骤3中的纯液氖可以经液氖换热器14换热使纯液氖汽化，然后分别经过第二换热器12和第一换热器10复热回收冷量后加压充瓶。如此，可充分利用冷量。
优选的，如图1中所示，步骤3中的纯液氖进入液氖换热器前还可以先经过第三减压阀18减压至1.2～1.5bar。
如图2中所示，在本发明的实施例中，还可以包括主换热器3，步骤4中粗氦分别经过第二换热器12和第一换热器10复热回收冷量后进入主换热器3被冷却至80～100K，然后进入热交换器19，进一步冷却至60～70K。如此，可充分利用资源，降低成本。优选的，纯氦气经过主换热器复热后加压充瓶。
如图1中所示，在本发明的实施例中，步骤3中纯氖塔17塔顶的不纯气分别经过第二换热器12和第一换热器10复热后返回步骤1中的氖氦混合气中，重新提纯。如此，循环利用。
此外，如图1中所示，在本发明的实施例中，第一换热器10、液氮换热器11、第二换热器12、第一减压阀13、液氖换热器14、气液分离器15、第二减压16和纯氖塔17置于多层绝热真空容器22中，多层绝热真空容器的真空度为1×10-3～1×10-8Pa。
如图2中所示，在本发明的实施例中，步骤1中的氖氦混合气体可以通过以下步骤得到：
步骤1.1，将经过脱氢处理后的粗氖氦混合气经Ⅰ级压缩机1增压至25～35bar，通过除水干燥器2干燥后通过主换热器3冷却至80～100K，然后进入Ⅰ级热交换器4，进一步冷却至60～70K，进入Ⅰ级气液分离器5进行气液分离；
步骤1.2，将分离得到的气相经Ⅰ级低温吸附器8除去杂质气体后，获得氖氦混合气体。本发明的实施例中采用了低温冷凝法和低温吸附法脱除原料气中的氮和氧等杂质后获得较为纯净的氖氦混合气。
如图2中所示，在本发明的实施例中，Ⅰ级气液分离器5分离得到的液相经过Ⅰ级减压阀6减压至1.2～2.0bar，进入Ⅱ级气液分离器7，Ⅱ级分离的气相经过主换热器3复热后返回步骤1.1中的粗氖氦混合气体中。重新进行提纯，如此，循环利用。
另如图2中所示，在本发明的实施例中，主换热器3、Ⅰ级热交换器4、Ⅰ级气液分离器5、Ⅰ级低温吸附器8、Ⅰ级减压阀6、Ⅱ级气液分离器7置于低温液氮容器21中。低温液氮容器21中盛有液氮，真空度为0.1～0.3bar。其中，Ⅱ级气液分离器7Ⅱ级分离的液相排入到低温液氮容器中的液氮中。
如图1中所示，在本发明的实施例中，采用脱氢后的粗氖氦混合气体(其中，各组分的体积分数为氖46％、氦14.4％、氮37.6％、氧1.5％)为原料气体：
原料气体经Ⅰ级压缩机1增压至33bar，经过除水干燥器2干燥脱除水分后，进入主换热器3中，并被返流的冷气流冷却至95K，再经过Ⅰ级热交换器4冷却至65K，此时原料气中90％以上的氮和氧被冷凝，之后送入Ⅰ级气液分离器5中进行Ⅰ级气液分离，被分离为气相组分和液相组分。
其中，从Ⅰ级气液分离器5分离后的气相组分(其中氖体积分数为75％，氦为23.6％)进入Ⅰ级低温吸附器8后脱除氮和氧等杂质后获得纯净的氖氦混合气，其中氖体积分数为76％，氦为24％。
而从Ⅰ级气液分离器5分离后的液相组分经过Ⅰ级减压阀6节流至1.5bar，并经Ⅱ级气液分离器7进行Ⅱ级分离，被分离为气相组分和液相组分。其中的液相组分排入低温液氮容器21中，气相组分经过主换热器3复热后返回粗氖氦混合气中。
之后，将得到的纯净的氖氦混合气经过主换热器3复热后进入氖氦混合气压缩机9增压至180bar(a)。
将增压后的氖氦混合气首先经过第一换热器10被返流的冷气流冷却至108K，然后进入液氮换热器11被液氮冷却至80K，之后进入第二换热器12被返流冷气流冷却至51K，经过第一减压阀13节流至27bar(a)，进入液氖换热器14与纯液氖换热后冷却至30K，再经过气液分离器15分离为气相组分和液相组分。
经过气液分离器15后得到的液相(氖体积分数为99.2％，氦体积分数为0.8％)经过第二减压阀16节流至1.7bar(a)进入纯氖塔17，在纯氖塔中氖与氦得到完全分离，塔顶得到的气相组分经过第二和第一换热器12和10后返回氖氦混合气中，而塔底得到的液相组分(氖体积分数大于99.995％)经过第三减压阀18节流至1.4bar(a)进入液氖换热器14中换热，然后经过第二和第一换热器12和10后复热，此即为纯氖，可以充入瓶中。
经过气液分离器15得到的气相(氖体积分数为14％，氦体积分数为86％)即为粗氦，粗氦经过第二和第一换热器12和10后复热，回收冷量后进入主换热器3中冷却后，然后经过热交换器19继续冷却至65K，进入低温吸附器20中，脱除氖等杂质后获得纯氦(氦体积分数大于99.999％)，纯氦经过主换热器3复热回收冷量后可以充入瓶中。
另外，如图2中所示，主换热器3、Ⅰ级热交换器4和热交换器19、Ⅰ级气液分离器5和Ⅱ级气液分离器7、Ⅰ级低温吸附器8和低温吸附器20，以及Ⅰ级减压阀6设置在低温液氮容器中21。第一换热器10和第二换热器12、液氮换热器11、液氖换热器14、气液分离器15、纯氖塔17，以及第一减压阀13、第二减压阀16和第三减压阀18设置在多层绝热真空容器22中。
低温液氮容器21中的真空度保持为0.17bar；多层绝热真空容器22中为了保持绝热的效果，采用真空泵19抽真空，真空度为1×10-4Pa。
在本发明的实施例的氖氦分离提纯方法中，可以全程采用分散控制系统(DCS系统)，从而灵活调节运行条件，监控氖氦的浓度，并可根据需要进行设置。
以上对本发明的具体实施例进行了详细描述，但其只是作为范例，本发明并不限制于以上描述的具体实施例。对于本领域技术人员而言，任何对本发明进行的等同修改和替代也都在本发明的范畴之中。因此，在不脱离本发明的精神和范围下所作的均等变换和修改，都应涵盖在本发明的范围内。

Claims (1)

1.一种氖氦分离提纯方法，其特征在于，包括以下步骤：
步骤1，将氖氦混合气体加压到170～200bar，并冷却至90～120K，然后使用液氮将氖氦混合气体冷却至70～85K；
步骤2，将氖氦混合气体进一步冷却至45～55K，并减压至24～30bar，然后用液氖冷却至25～35K，进行气液分离，分离后的气相为粗氦，液相为粗氖；
步骤3，将所述粗氖减压至1.5～2.0bar，精馏制备纯氖；
步骤4，将所述粗氦复热回收热量后再冷却至60～70K，并经低温吸附除去杂质气体后，获得纯氦气；
其中，所述步骤1的氖氦混合气体通过以下步骤得到：
步骤1.1，将经过脱氢处理后的粗氖氦混合气增压至25～35bar，通过除水干燥后冷却至80～100K，然后进一步冷却至60～70K，进行气液分离；
步骤1.2，将分离得到的气相经低温吸附除去杂质气体后，获得氖氦混合气体。
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