CN202216490U - 一种高纯液氖提取装置 - Google Patents

一种高纯液氖提取装置 Download PDF

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CN202216490U
CN202216490U CN2011203498468U CN201120349846U CN202216490U CN 202216490 U CN202216490 U CN 202216490U CN 2011203498468 U CN2011203498468 U CN 2011203498468U CN 201120349846 U CN201120349846 U CN 201120349846U CN 202216490 U CN202216490 U CN 202216490U
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heat exchanger
neon
helium
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俞建
曹月丛
严寿鹏
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SHANGHAI QIYUAN AIR SEPARATION TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

本实用新型一种高纯液氖的提取装置，包括提纯高纯液氖的冷凝吸附***以及用于提供冷量的双氦透平膨胀机封闭制冷循环***；所述冷凝吸附***将原料气加压之后冷却，采用低温冷凝法和吸附法脱除原料气中的氮和氧等后获得氖氦混合气，氖氦混合气继续被冷却并采用低温精馏法获得高纯液氖。而所述封闭制冷循环***，采用双氦透平膨胀机实现液氖提取过程中的冷量需求。

Description

一种高纯液氖提取装置
技术领域
本实用新型涉及一种气体分离的装置，具体地说，本实用新型涉及一种由氦氖混合气体中提取高纯液氖的装置。尤其涉及由一种微型高转速气体轴承氦透平膨胀机组成的低压制冷循环，为分离过程提供需要的冷量的装置。
背景技术
氖气，是一种惰性气体，其在空气中含量仅为18.18×10-6。然而随着科技的发展，其已作为重要的能源大量用于工业各个领域。如在电子工业，氖气可用于霓虹灯及高压氖灯、计数管等的填充介质；其可用于激光技术；因液氖具有沸点低等优点，其可作为26~40K之间的低温冷源使用；氖气还可用于高能物理研究。
在氖气的制备工艺中，大多采用空分法制备氖气，其包括先采用粗氖氦塔连续提取少量的粗氖氦混合气。此时粗氖氦混合气中含有氢的体积分数为2～5%；之后，在粗氖氦混合气中加入一定量的氧，使氧与氢完全进行化学反应生成水，进行脱氢处理，而脱氢后的粗氖氦混合气中各组分的体积分数一般为氖51%、氦15%、氮32.5%、氧1.5%。而之后，脱氢后的粗氖氦混合气可用氖氦混合气体压缩机、干燥器，以及冷却器等装置，积累一定数量后集中进行除氮。当除氮设备的温度在65K(用真空泵使液氮的蒸发压力达到0.12bar)和粗氖氦混合气的冷凝压力为30bar时，粗氖氦混合气中的氮和氧被冷凝，未被冷凝的气相中剩余的微量氮和氧在相同温度下进行吸附脱除。这样获得氖体积分数约78%、氦约22%的氖氦混合气体。之后再进行氖氦分离。
在传统的由粗氖氦混合气体分离氖氦的工艺中，包括了精馏塔、气液分离器以及给整个工艺提供冷量的冷凝***。在早期冷凝***中一般以采用液氢为冷源，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。鉴于液氢生产的复杂性和危险性。现代技术是采用带液氮预冷器的氖氦混合气高压(200bar)二次节流制冷使氖液化，从而克服液氢为冷源存在的缺陷。如，美国专利公开号US2010/0221168A1；中国公开号CN101530717A的液氖的提取设备中，均采用液氮冷凝蒸发器给***提供所需的冷量，从而使氖液化。然而这种采用液氮为冷源制备氖气的方法首先需要消耗外界提供的液氮冷量，其次氖氦分离设备属高压设备，给设备的制造和运行带来不安全的隐患。
实用新型内容
本实用新型提供了一种高纯液氖的提取装置，其针对现有的高纯度氖气提取装置中采用液氢或是液氮为冷源的不足，其采用双氦透平膨胀机来实现整个氖气提取过程中低压制冷循环，提供冷量，从而提取高纯度的液氖。
本实用新型高纯液氖的提取装置，通过以下技术方案实现其目的：
一种高纯液氖提取装置，其中，包括冷凝吸附***和封闭制冷循环***；所述冷凝吸附***包括Ⅰ级换热器、Ⅱ级换热器、Ⅰ级气液分离器、Ⅱ级气液分离器、吸附器和精馏塔；
所述Ⅰ级换热器的原料进口与原料气体管道相连接；
所述Ⅰ级换热器的原料出口与Ⅰ级气液分离器原料进口连接、Ⅰ级气液分离器的气体出口与吸附器原料进口连接，吸附器的原料出口与Ⅱ级换热器的原料进口连接、Ⅱ级换热器的原料出口与Ⅱ级气液分离器的原料进口连接、Ⅱ级气液分离器的液体出口与精馏塔的原料进口连接；
所述精馏塔塔釜处设有高纯液氖提取口；
所述封闭制冷循环***包括Ⅰ级氦透平膨胀机和Ⅱ级氦透平膨胀机和氦气循环管道；
所述氦气循环管道包括进气管道和返流管道；所述进气管道经过用于收集压缩氦气的压缩机后依次通过Ⅰ级换热器与Ⅱ级换热器后连接Ⅱ级氦透平膨胀机，并且在Ⅰ级换热器与Ⅱ级换热器之间连接Ⅰ级氦透平膨胀机；所述返流管道由所述Ⅱ级氦透平膨胀机起，通过Ⅱ级换热器与Ⅰ级换热器后返回所述压缩机。
上述的高纯液氖提取装置，其中，所述冷凝吸附***还包括粗氖氦混合气体压缩机和气体干燥器；所述原料气体管道依次通过粗氖氦混合气体压缩机和气体干燥器之后与所述Ⅰ级换热器的原料进口连接。
上述的高纯液氖提取装置，其中，所述精馏塔设有氖气抽取口，所述氖气抽取口与所述粗氖氦混合气体压缩机进口连接。
上述的高纯液氖提取装置，其中，所述冷凝吸附***还包括Ⅲ级气液分离器，所述Ⅲ级分离器原料进口与所述Ⅰ级气液分离器的液体出口连接；且所述Ⅲ级分离器的气体出口与所述粗氖氦混合气体压缩机进口连接。
上述的高纯液氖提取装置，其中，所述Ⅱ级气液分离器与精馏塔之间、和Ⅲ级分离器与所述Ⅰ级气液分离器之间均设有用于调节压力的节流阀。
上述的高纯液氖提取装置，其中，所述Ⅲ级分离器的液体出口通过管道经所述Ⅰ级换热器后排空。
上述的高纯液氖提取装置，其中，所述Ⅰ级换热器、Ⅱ级换热器、Ⅰ级气液分离器、Ⅱ级气液分离器、Ⅲ级分离器、精馏塔和气体吸附器均设置于一个多层绝热真空容器中。
上述的高纯液氖提取装置，其中，所述Ⅱ级气液分离器的气体出口通过所述Ⅱ级换热器、Ⅰ级换热器后与外部氦气收集装置连接。
本实用新型高纯液氖的提取装置中，全程采用分散控制*** (DCS***)，从而实现本实用新型的装置各个部分中组分浓度的监控，以及装置各个部分生产条件的设定调节。
本实用新型和传统技术相比具有以下优点：
1）本实用新型采用双氦透平膨胀机的封闭制冷循环***，为液氖提取过程中提供冷量。
2）采用本实用新型可在提取高纯度液氖的同时，回收粗氦气。
3）本实用新型工艺结构简单，在使用过程中易于操作、控制，适用于高纯度氖气工业大规模化生产需求。
附图说明
图1为本实用新型的结构示意图，
图中，1为粗氖氦混合气压缩机、2为4A分子筛干燥器、3和8均为热交换器、4、6和9均为气液分离器、5和10均为节流阀、7为吸附器、11为精馏塔、13为氦气压缩机、14和15均为氦透平膨胀机、16为真空泵、17为多层绝热真空容器。
具体实施方式
本实用新型一种高纯液氖提取装置，包括提纯高纯液氖的冷凝吸附***以及用于提供冷量的封闭制冷循环***。本实用新型可以脱氢后的氖氦混合气体为原料气体（脱氢后的粗氖氦混合气中各组分的体积分数一般为氖51%、氦15%、氮32.5%、氧1.5%），从中提纯高纯度的液氖。
实施例1：
如图1所示，所述冷凝吸附***包括所述冷凝吸附***还包括粗氖氦混合气体压缩机1、4A分子筛干燥器2、Ⅰ级换热器3、Ⅱ级换热器8、Ⅰ级气液分离器4、Ⅱ级气液分离器9和精馏塔11。在所述气液分离器9和精馏塔11之间设有用于调节液体压力的节流阀10。
所述粗氖氦混合气体压缩机1与外部的原料气体管道连接，用于通入脱氢后的氖氦混合气体，所述粗氖氦气体混合压缩机1依次与所述气体干燥器2以及所述Ⅰ级换热器3的原料进口连接，这样脱氢后氖氦混合气体经所述粗氖氦混合气压缩机1增压至30bar左右，以及4A分子筛干燥器2干燥脱除水分后，沿管线18进入在热交换器3中冷凝至65K左右，此时绝大部分的氮和氧（大约95%以上的氮和氧）被冷凝。
所述Ⅰ级换热器3的原料出口与Ⅰ级气液分离器4原料进口连接，将冷凝后的氧和氮送入所述Ⅰ级气液分离器4中，所述Ⅰ级气液分离器的气体出口与吸附器原料进口连接，吸附器的原料出口与Ⅱ级换热器的原料进口连接；Ⅱ级换热器8的原料出口与Ⅱ级气液分离器9的原料进口连接；Ⅱ级气液分离器9的液体出口再与精馏塔11的原料进口相连接，其中，所述Ⅱ级气液分离器9与所述精馏塔11之间设有节流阀10。而所述Ⅱ级气液分离器9的气体出口通过所述Ⅱ级换热器8、Ⅰ级换热器3后与外部氦气收集装置连接。当由热交换器3中冷凝后的氮气和氧气进入所述Ⅰ级气液分离器4后，被分离成液相和气相组分；气相组分(其中氖体积分数约为76.8%，氦22%)沿管线21进入硅胶吸附器7后得到纯净的氖氦混合气，其氖体积分数为77.7%、氦22.3%。
纯净的氖氦混合气经过气体交换器8被冷却至26K后（其中97%的氖被冷凝），并在所述Ⅱ级气液分离器9中进行Ⅱ级气液分离；得到的液相组分(氖体积分数为98%、氦1.9%)经过节流阀10节流膨胀至1.7bar后进入精馏塔11。而由所述Ⅱ级气液分离器9中得到的气体组分（其中氦气的体积分数达90%左右）经管道22依次通过所述Ⅰ级换热器3、Ⅱ级换热器8后进入氦气收集装置，用于高纯氦气提纯或是另作他用。所述的精馏塔内可为充填瑞士苏尔寿公司制作的DX型实验室不锈钢丝网规整填料，精馏塔再沸器采用调功器控制的电加热进行热量传递，正确控制再沸器的热负荷。
在精馏塔11中氖和氦精馏分离，并由塔底得到高纯度的液氖（氖体积分数大于99.999%），沿管线23排入液氖贮存装置。
所述封闭制冷循环***包括Ⅰ级氦透平膨胀机14和Ⅱ级氦透平膨胀机15以及用于连接各装置的氦气循环管道。所述的氦透平膨胀机的轴承采用气体静动压轴承。氦透平膨胀机采用风机制动，风机的介质为氦气。图中，且两台所述的氦透平膨胀机14和15均采用冷却水装置12，用于实现所述氦透平膨胀机的冷量交换。
所述氦气循环管道包括进气管道和返流管道；所述进气管道一端连接一个用于压缩收集氦气的压缩机13，并由所述压缩机13起，依次通过Ⅰ级换热器3与Ⅱ级换热器8后连接Ⅱ级氦透平膨胀机15，且在Ⅰ级换热器3与Ⅱ级换热器8之间连接Ⅰ级氦透平膨胀机14；而所述返流管道由所述Ⅱ级氦透平膨胀机15起，依次通过Ⅱ级换热器8与Ⅰ级换热器3后返回压缩机13入口，实现氦气循环。工作时，氦气通过进气管道经所述压缩机13压缩至10bar，沿管线24通过热交换器3被冷却至83K左右后进入氦透平膨胀机14，氦气被膨胀至3.5bar、温度降至62K，然后沿管线25进入热交换器8，进行热量交换；之后通入氦透平膨胀机15，氦气膨胀至1.3bar，温度降至24K后，膨胀后的氦气沿管线26再次通入热交换器8和3复热后返回氦压缩机13，进行加压循环使用。
实施例2：
在所述实施例1的基础上，所述冷凝吸附***添加一个Ⅲ级气液分离器6，所述Ⅲ级气液分离器6原料进口与所述Ⅰ级气液分离器4的液体出口连接。其中，由所述所述Ⅰ级气液分离器4分离得到的液相组分可通过阀5节流至1.5bar左右后，进行Ⅲ级气液分离，且将所述Ⅲ级分离器6的气体出口与所述粗氖氦混合气体压缩机1进口连接。气相组分（氖气体积分数约为89%），得到的气相组分并沿管线20返回所述粗氖氦混合气体压缩机1中，循环利用。
而所述Ⅲ级分离器6中得到的液相组分经管道19（氖的体积分数约为0.5%，其余大部分为氮气）进入所述热交换器3复热，进行热量交换达到常温后排入大气。
而所述精馏塔11上还设有氖气抽取口，所述氖气抽取口与所述粗氖氦气体混合压缩机1进口连接，经精馏塔11中得到的气相组分（氖体积分数约为98.9%、氦为1.1%）返回所述粗氖氦混合气体压缩机1中，循环利用。
所述Ⅱ级气液分离器9的气体出口通过所述Ⅱ级换热器8、Ⅰ级换热器3后与外部氦气收集装置连接。分离得到的气相组分(其中氦体积分数约为90%)沿管线22经过换热器3和8复热后收集。其中，氦气的浓度较高，可作为后续氦气提取工艺的原料气体或用于其他，其经济价值较高。
其中，所述Ⅰ级换热器3、Ⅱ级换热器8、Ⅰ级气液分离器4、Ⅱ级气液分离器9、Ⅲ级分离器6、精馏塔11和气体吸附器7以及上述设备间的连接管道等均设置于一个多层绝热真空容器17中。所述的多层绝热真空容器17，真空度要求1×10-4mbar左右，而漏率要求达1×10-7mbar·L/s。这样有效减小工作期间，上述装置与外界的热量交换。
以上对本实用新型的具体实施例进行了详细描述，但其只是作为范例，本实用新型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，任何对本实用新型进行的等同修改和替代也都在本实用新型的范畴之中。因此，在不脱离本实用新型的精神和范围下所作的均等变换和修改，都应涵盖在本实用新型的范围内。

Claims (8)

1.一种高纯液氖提取装置，其特征在于，包括冷凝吸附***和封闭制冷循环***；所述冷凝吸附***包括Ⅰ级换热器、Ⅱ级换热器、Ⅰ级气液分离器、Ⅱ级气液分离器、吸附器和精馏塔；
所述Ⅰ级换热器的原料进口与原料气体管道相连接；
所述Ⅰ级换热器的原料出口与Ⅰ级气液分离器原料进口连接、Ⅰ级气液分离器的气体出口与吸附器原料进口连接，吸附器的原料出口与Ⅱ级换热器的原料进口连接、Ⅱ级换热器的原料出口与Ⅱ级气液分离器的原料进口连接、Ⅱ级气液分离器的液体出口与精馏塔的原料进口连接；
所述精馏塔塔釜处设有高纯液氖提取口；
所述封闭制冷循环***包括Ⅰ级氦透平膨胀机和Ⅱ级氦透平膨胀机和氦气循环管道；
所述氦气循环管道包括进气管道和返流管道；所述进气管道经过用于收集压缩氦气的压缩机后依次通过Ⅰ级换热器与Ⅱ级换热器后连接Ⅱ级氦透平膨胀机，并且在Ⅰ级换热器与Ⅱ级换热器之间连接Ⅰ级氦透平膨胀机；所述返流管道由所述Ⅱ级氦透平膨胀机起，通过Ⅱ级换热器与Ⅰ级换热器后返回所述压缩机。
2.根据权利要求1所述的高纯液氖提取装置，其特征在于，所述冷凝吸附***还包括粗氖氦混合气体压缩机和气体干燥器；所述原料气体管道依次通过粗氖氦混合气体压缩机和气体干燥器之后与所述Ⅰ级换热器的原料进口连接。
3.根据权利要求2所述的高纯液氖提取装置，其特征在于，所述精馏塔设有氖气抽取口，所述氖气抽取口与所述粗氖氦混合气体压缩机进口连接。
4.根据权利要求2所述的高纯液氖提取装置，其特征在于，所述冷凝吸附***还包括Ⅲ级气液分离器，所述Ⅲ级分离器原料进口与所述Ⅰ级气液分离器的液体出口连接；且所述Ⅲ级分离器的气体出口与所述粗氖氦混合气体压缩机进口连接。
5.根据权利要求4所述的高纯液氖提取装置，其特征在于，所述Ⅱ级气液分离器与精馏塔之间、和Ⅲ级分离器与所述Ⅰ级气液分离器之间均设有用于调节压力的节流阀。
6.根据权利要求4所述的高纯液氖提取装置，其特征在于，所述Ⅲ级分离器的液体出口通过管道经所述Ⅰ级换热器后排空。
7.根据权利要求6所述的高纯液氖提取装置，其特征在于，所述Ⅰ级换热器、Ⅱ级换热器、Ⅰ级气液分离器、Ⅱ级气液分离器、Ⅲ级分离器、精馏塔和气体吸附器均设置于一个多层绝热真空容器中。
8.根据权利要求1所述的高纯液氖提取装置，其特征在于，所述Ⅱ级气液分离器的气体出口通过所述Ⅱ级换热器、Ⅰ级换热器后与外部氦气收集装置连接。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105987580A (zh) * 2016-02-03 2016-10-05 安徽万瑞冷电科技有限公司 一种制冷机为冷源的氖氦稀有气体分离精制工艺方法
CN107917578A (zh) * 2017-11-13 2018-04-17 益通天然气股份有限公司 一种混合制冷剂循环液化天然气自净化***
CN108373144A (zh) * 2018-05-24 2018-08-07 浙江智海化工设备工程有限公司 一种粗氖氦精制除氢***
CN109442868A (zh) * 2018-10-26 2019-03-08 中船重工鹏力（南京）超低温技术有限公司 一种去除氧氮分离提纯氖氦的方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105987580A (zh) * 2016-02-03 2016-10-05 安徽万瑞冷电科技有限公司 一种制冷机为冷源的氖氦稀有气体分离精制工艺方法
CN107917578A (zh) * 2017-11-13 2018-04-17 益通天然气股份有限公司 一种混合制冷剂循环液化天然气自净化***
CN107917578B (zh) * 2017-11-13 2019-10-25 益通天然气股份有限公司 一种混合制冷剂循环液化天然气自净化***
CN108373144A (zh) * 2018-05-24 2018-08-07 浙江智海化工设备工程有限公司 一种粗氖氦精制除氢***
CN109442868A (zh) * 2018-10-26 2019-03-08 中船重工鹏力（南京）超低温技术有限公司 一种去除氧氮分离提纯氖氦的方法

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