CN212842470U - 一种带循环的单塔低温精馏回收氩气*** - Google Patents

一种带循环的单塔低温精馏回收氩气*** Download PDF

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CN212842470U
CN212842470U CN202021278434.5U CN202021278434U CN212842470U CN 212842470 U CN212842470 U CN 212842470U CN 202021278434 U CN202021278434 U CN 202021278434U CN 212842470 U CN212842470 U CN 212842470U
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郝文炳
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Shanghai Lianfeng Gas 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
    • 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
    • F25J3/08Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/02Processes or apparatus using separation by rectification in a single pressure main column system
    • 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
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/40Features relating to the provision of boil-up in the bottom of a column
    • 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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    • 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
    • F25J2200/00Processes or apparatus using separation by rectification
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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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    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/60Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
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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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    • 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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    • 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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    • F25J2250/00Details related to the use of reboiler-condensers
    • F25J2250/02Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
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    • F25J2250/00Details related to the use of reboiler-condensers
    • F25J2250/20Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
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    • F25J2270/00Refrigeration techniques used
    • F25J2270/90External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

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Abstract

本实用新型公开了一种带循环的单塔低温精馏回收氩气***,该***包括氩气压缩机、除一氧化碳器、第一冷却器、除氧器、第二冷却器、氩气预冷机、纯化***、精馏冷箱和氩气循环压缩机;所述精馏冷箱包括换热器、氩塔再沸器、粗液氩节流阀、精氩塔、纯液氩节流阀、氩塔冷凝蒸发器和辅助再沸器。本实用新型利用回收现场会有液氩提供的便利,用液氩提供冷量,不必单独设置膨胀机,净化粗氩气,再利用低温精馏法脱除氮气、氢气,利用循环氩气增强精馏塔效率,提高了氩气的回收率,简化了低温精馏的流程和操作,降低了运行能耗。

Description

一种带循环的单塔低温精馏回收氩气***
技术领域
本实用新型涉及氩气回收技术领域,尤其涉及一种带循环的单塔低温精馏回收氩气***。
背景技术
直拉法是生产单晶硅的主要方法,全球70%~80%的单晶硅通过直拉法生产。最常用的直拉法生产单晶硅工艺是采用即像真空工艺又像流动气氛工艺的减压拉晶工艺;减压工艺是在硅单晶拉制过程中,连续等速地向单晶炉炉膛内通入高纯度氩气,同时真空泵不断地从炉膛向外抽送氩气,保持炉膛内真空度稳定在20托左右,这种工艺既有真空工艺的特点,又有流动气氛工艺的特点。减压拉晶工艺的真空泵一般采用滑阀泵,滑阀泵是用油来保持密封的机械真空泵。氩气携带单晶拉制过程中由于高温而产生的硅氧化物和杂质挥发物,并通过真空泵的抽送排放到大气,回收利用这部分氩气有很大现实意义。
但现有氩气回收纯化的技术中,如专利201210078306.X公开了一种单晶硅生产中氩气回收纯化的方法与装置,其低温精馏部分使用空气循环制冷,能耗高,流程复杂,加入的过量氢气放空,利用率低;专利201410618341.5公开了一种双塔耦合的氩气回收纯化设备及氩气回收纯化方法,用空气压缩,双塔流程,能耗无优势,结构复杂,增加设备投资。
因此,本领域的技术人员致力于开发流程更简洁,操作更方便,氩气回收率更高,能耗更低氩气回收***。
实用新型内容
本实用新型为解决现有氩气回收技术中运动部件多、能耗高、投资大的问题,提供一种带循环的单塔低温精馏回收氩气***。
为实现上述目的,本实用新型采用以下技术方案:
本实用新型提供一种带循环的单塔低温精馏回收氩气***,包括氩气压缩机、除一氧化碳器、第一冷却器、除氧器、第二冷却器、氩气预冷机、纯化***、精馏冷箱和氩气循环压缩机;所述精馏冷箱包括换热器、氩塔再沸器、粗液氩节流阀、精氩塔、纯液氩节流阀、氩塔冷凝蒸发器和辅助再沸器;
管路连接顺序为:
所述氩气压缩机、除一氧化碳器、第一冷却器、除氧器、第二冷却器、氩气预冷机、纯化***依次连接;
所述纯化***的气体出口管路通过所述换热器与所述氩塔再沸器连接,所述氩塔再沸器的冷凝侧管路通过所述粗液氩节流阀与所述精氩塔的中上部连接,所述精氩塔底部液氩管路通过所述纯液氩节流阀与所述氩塔冷凝蒸发器的蒸发侧连接,所述氩塔冷凝蒸发器的蒸发侧氩气出口管路通过所述换热器后分为两路,一路送出所述精馏冷箱,另一路与所述氩气循环压缩机连接;所述氩气循环压缩机的出口管路通过所述换热器、辅助再沸器与所述氩塔冷凝蒸发器的蒸发侧连接;所述精氩塔的塔顶出口管路分为两路,一路通过所述换热器后送出所述精馏冷箱与所述纯化***连接,另一路与所述氩塔冷凝蒸发器的冷凝侧连接。
进一步地,所述辅助再沸器的冷源为所述精氩塔底部的纯液氩,所述辅助再沸器的出口管路与所述精氩塔下部连接。
进一步地,所述辅助再沸器与所述氩塔冷凝蒸发器的连接管路上设有液氩节流阀。
进一步地,所述氩塔冷凝蒸发器的蒸发侧还连接有液氩补充管路。
进一步地,所述第一冷却器与除氧器的连接管路上设有加氢管路。
进一步地,所述精氩塔的塔顶氮气出口管路送出所述精馏冷箱部分的管路上设有氮气补充管路。
本实用新型采用上述技术方案,与现有技术相比,具有如下技术效果:
本实用新型利用回收现场会有液氩提供的便利,用液氩提供冷量,不必单独设置膨胀机,净化粗氩气,再利用低温精馏法脱除氮气、氢气,利用循环氩气增强精馏塔效率,提高了氩气的回收率,简化了低温精馏的流程和操作,降低了运行能耗。
附图说明
图1为本实用新型单塔低温精馏回收氩气***的示意图;
附图标记为:
氩气压缩机1、除一氧化碳器2、第一冷却器3、除氧器4、第二冷却器5、氩气预冷机6、纯化***7、精馏冷箱8、换热器9、氩塔再沸器10、粗液氩节流阀11、精氩塔12、纯液氩节流阀13、液氩补充管路节流阀14、氩塔冷凝蒸发器15、辅助再沸器16、液氩节流阀17、氩气循环压缩机18。
具体实施方式
下面通过具体实施例对本实用新型进行详细和具体的介绍,以使更好的理解本实用新型,但是下述实施例并不限制本实用新型范围。
实施例1
如图1所示,本实施例提供一种带循环的单塔低温精馏回收氩气***,包括氩气压缩机1、除一氧化碳器2、第一冷却器3、除氧器4、第二冷却器5、氩气预冷机6、纯化***7、精馏冷箱8和氩气循环压缩机18;精馏冷箱8包括换热器9、氩塔再沸器10、粗液氩节流阀11、精氩塔12、纯液氩节流阀13、氩塔冷凝蒸发器15和辅助再沸器16;
管路连接顺序为:
氩气压缩机1、除一氧化碳器2、第一冷却器3、除氧器4、第二冷却器5、氩气预冷机7、纯化***7依次连接;
纯化***7的气体出口管路通过换热器9与氩塔再沸器10连接,氩塔再沸器10的冷凝侧管路通过粗液氩节流阀11与精氩塔12的中上部连接,精氩塔12 底部液氩管路通过纯液氩节流阀13与氩塔冷凝蒸发器15的蒸发侧连接,氩塔冷凝蒸发器15的蒸发侧氩气出口管路通过换热器9后分为两路,一路送出精馏冷箱8,另一路与氩气循环压缩机18连接;氩气循环压缩机18的出口管路通过换热器9、辅助再沸器16与氩塔冷凝蒸发器15的蒸发侧连接;精氩塔12的塔顶出口管路分为两路,一路通过换热器9后送出精馏冷箱8与纯化***7连接,另一路与氩塔冷凝蒸发器15的冷凝侧连接。
作为一个优选的实施例,辅助再沸器16的冷源为精氩塔12底部的纯液氩,辅助再沸器16的出口管路与精氩塔12下部连接。
作为一个优选的实施例,辅助再沸器16与氩塔冷凝蒸发器15的连接管路上设有液氩节流阀17。
作为一个优选的实施例,氩塔冷凝蒸发器15的蒸发侧还连接有液氩补充管路。
作为一个优选的实施例,第一冷却器3与除氧器4的连接管路上设有加氢管路。
作为一个优选的实施例,精氩塔12的塔顶氮气出口管路送出精馏冷箱8部分的管路上设有氮气补充管路。
实施例2
采用实施例1提供的***,本实施例提供了一种回收氩气的方法:
需要回收的1890Nm3/h废氩气压力很低,混入空气约5%,首先上述废氩气经过氩气压缩机1加压到1.45MPa(A),经过管路GAr-101进入除一氧化碳器 2,在除一氧化碳器2中装填催化剂,通过催化反应,把一氧化碳催化为二氧化碳,CO出***量<1ppm;去除CO的废氩气出来后经过管路GAr-102进入第一冷却器3冷却至35~40℃,在管路GAr-103中与加入的氢气混合后进入除氧器4,在除氧器中4,氧气与氢气发生反应,生成水并释放热量(视氧气量温度上升会有不同,在O2含量不高于0.4%时,温度会在<100℃);然后通过管路GAr-104高温氩气进入第二冷却器5降温至40℃,通过管路GAr-105进入氩气预冷机6 降温到5~8℃(利于分子筛的吸附),经管路GAr-106进入纯化***7脱除水和二氧化碳,得到的粗氩气主要成为Ar、N2、H2
上述干燥的粗氩气进入精馏冷箱8,首先通过管路GAr-107进入换热器9降温至-154℃后,进入位于精氩塔12底部的氩塔再沸器10,在氩塔再沸器10中,液体测的温度是-156.7℃,经模拟,在GAr-109中94%的气体被液化,出氩塔再沸器10的气液混合流体经粗液氩节流阀11节流降压至0.62MPaA送入精氩塔12 的中上部参与精馏。其中,由于存在压力差,氩塔再沸器10的冷凝侧是1.23MPa (A),-155.5℃;蒸发侧是1MPa(A),-156.7℃,沸点温度会根据压力改变,使再沸器内外侧形成温差1.2℃,从而保证氩塔再沸器10的工作。
上述管路GAr-109进入精氩塔12的流体,其中的气体部分随着塔内气体上升,液体随着塔内液体下降,在上升下降过程中气液发生传热传质过程,液体部分的Ar含量越来越高,在塔底得到纯液氩99.9997%;从精氩塔12底部抽出流路为LAr-201的纯液氩,通过纯液氩节流阀13节流降压送入氩塔冷凝蒸发器15 的蒸发侧;同时,外界补充的液氩60kg/h一并进入氩塔冷凝蒸发器15的蒸发侧,为整个***补充冷量损失。
纯液氩在氩塔冷凝蒸发器15蒸发侧蒸发为氩气,进入换热器9复热回收冷量后,一路送出精馏冷箱8,供给客户,GAr-204是输送管路,在本实施例中压力0.6MPa(G),温度为17℃,流量为1978Nm3/h;
另一路为管路GAr-205中240Nm3/h氩气经循环压缩机18加压后到1.22MPa (A)后,经氩气循环压缩机18自带的冷却器冷却至40℃,经管路GAr-206送入精馏冷箱8内的换热器9冷却至液化温度(-153.6℃),然后进入辅助再沸器 16液化,从管路LAr-202出来时,已经全部液化,LAr-202中的液体经过液氩节流阀17节流后送到氩塔冷凝蒸发器15的蒸发侧,为其提供冷源。其中,辅助再沸器16的冷源来自于精氩塔12底部的纯液氩,被气化后的气体返回到精氩塔 12中,作为上升气体参与精馏。
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 (6)

1.一种带循环的单塔低温精馏回收氩气***,其特征在于,包括氩气压缩机、除一氧化碳器、第一冷却器、除氧器、第二冷却器、氩气预冷机、纯化***、精馏冷箱和氩气循环压缩机;所述精馏冷箱包括换热器、氩塔再沸器、粗液氩节流阀、精氩塔、纯液氩节流阀、氩塔冷凝蒸发器和辅助再沸器;
管路连接顺序为:
所述氩气压缩机、除一氧化碳器、第一冷却器、除氧器、第二冷却器、氩气预冷机、纯化***依次连接;
所述纯化***的气体出口管路通过所述换热器与所述氩塔再沸器连接,所述氩塔再沸器的冷凝侧管路通过所述粗液氩节流阀与所述精氩塔的中上部连接,所述精氩塔底部液氩管路通过所述纯液氩节流阀与所述氩塔冷凝蒸发器的蒸发侧连接,所述氩塔冷凝蒸发器的蒸发侧氩气出口管路通过所述换热器后分为两路,一路送出所述精馏冷箱,另一路与所述氩气循环压缩机连接;所述氩气循环压缩机的出口管路通过所述换热器、辅助再沸器与所述氩塔冷凝蒸发器的蒸发侧连接;所述精氩塔的塔顶出口管路分为两路,一路通过所述换热器后送出所述精馏冷箱与所述纯化***连接,另一路与所述氩塔冷凝蒸发器的冷凝侧连接。
2.根据权利要求1所述的单塔低温精馏回收氩气***,其特征在于,所述辅助再沸器的冷源为所述精氩塔底部的纯液氩,所述辅助再沸器的出口管路与所述精氩塔下部连接。
3.根据权利要求1所述的单塔低温精馏回收氩气***,其特征在于,所述辅助再沸器与所述氩塔冷凝蒸发器的连接管路上设有液氩节流阀。
4.根据权利要求1所述的单塔低温精馏回收氩气***,其特征在于,所述氩塔冷凝蒸发器的蒸发侧还连接有液氩补充管路。
5.根据权利要求1所述的单塔低温精馏回收氩气***,其特征在于,所述第一冷却器与除氧器的连接管路上设有加氢管路。
6.根据权利要求1所述的单塔低温精馏回收氩气***,其特征在于,所述精氩塔的塔顶氮气出口管路送出所述精馏冷箱部分的管路上设有氮气补充管路。
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Publication number Priority date Publication date Assignee Title
CN111637684A (zh) * 2020-07-03 2020-09-08 上海迎飞能源科技有限公司 一种带循环的单塔低温精馏回收氩气***及方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111637684A (zh) * 2020-07-03 2020-09-08 上海迎飞能源科技有限公司 一种带循环的单塔低温精馏回收氩气***及方法

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