CN1235666A - 生产加压氮气的方法和设备 - Google Patents

生产加压氮气的方法和设备 Download PDF

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Publication number
CN1235666A
CN1235666A CN97199351A CN97199351A CN1235666A CN 1235666 A CN1235666 A CN 1235666A CN 97199351 A CN97199351 A CN 97199351A CN 97199351 A CN97199351 A CN 97199351A CN 1235666 A CN1235666 A CN 1235666A
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pressure column
lower pressure
nitrogen
liquid
product
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CN97199351A
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霍斯特·科尔迪昂
迪特里希·罗特曼
于尔根·福伊特
克里斯蒂安·孔茨
沃尔夫冈·哈格
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Linde GmbH
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Linde GmbH
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Publication of CN1235666A publication Critical patent/CN1235666A/zh
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
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    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another column
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Abstract

本发明涉及一种在精馏系统中通过低温分馏空气生产压缩氮气的方法和设备,所述系统具有一高压塔(4)和低压塔(5)。所用空气(1,3)引入高压塔(4)中。从高压塔(4)采出含氧液体馏分,并引入到低压塔(5)。在顶部储热器中,至少部分来自低压塔(5)的气体氮(18)通过与蒸发液体(13)间接换热而冷凝。为了以压缩气体(24,24,29)的形式获得来自高压塔的氮气,使用高于低压塔(5)所需操作压力的压力。从低压塔流出的氮(20)在液态暴露在高于低压塔(5)操作压力的压力下。在高压下的液体(22)在蒸发器(23)中通过与热载体(35)间接换热而蒸发,从而生产出压缩氮气(24,25,29)。

Description

生产加压氮气的方法和设备
本发明涉及一种在精馏系统中通过空气低温分馏生产加压氮气的方法，该精馏系统具有一个高压塔(pressure column)和一个低压塔，在该方法中，进料空气进入高压塔，含氧液体馏份从高压塔中采出，并输入到低压塔中，从低压塔中排出的气态氮，在顶部冷凝器通过与蒸发液体间接换热至少部分冷凝，来自低压塔的气态氮作为加压氮气产品，其压力高于低压塔的操作压力。
这一类的方法公开在DE3528374A1中。特别是在低压塔顶部生产的氮气作为压缩产品除去。此外，氮气以气态形式从低压塔采出，在主换热器中以进料空气加热，然后从低压塔的压力压缩到产品压力。
本发明的目的是在高压下以相对低的成本生产氮气。
这一目的是这样实现的：至少一部分在顶部冷凝器的间接换热器中生产的液氮或从低压塔排出的液氮在液态被提高到超过低压塔的压力，并在产品换热器中通过与传热介质间接换热而蒸发，从而作为加压氮气产品被生产出来。产品蒸发器可以设置在一个塔中，也可以设置在塔外。
来自低压塔的氮气产品的压力升高至少部分是在液态下完成的。流体压力的升高可以通过任何已知方法来进行，例如，使用泵，在罐中利用静压势和/或加压蒸发。这意味着在设备成本上比气体压缩机低。另外需要间接换热器，在液体状态下加压的低压塔氮气在该换热器中蒸发。不过，整体上提供了在经济上特别有利的方法。
与直接从高压塔采出加压氮气产品相比，本发明方法的另一优点是产品纯度高。具体地说，在低压塔中，可以实现如氦、氖和/或氢的更易挥发组分的浓缩，这与高压塔的塔顶产品相比是降低了。优选地，在本发明中，低压塔的所有氮气产品都以液态形式从低压塔或其顶部冷凝器中采出。
在根据本发明的方法中，两个塔的操作压力可以是：高压塔为，例如，6-20，优选为7-16巴，低压塔为，例如，3-8，优选为3-6巴。例如，低压塔的顶部冷凝器可以使用来自低压塔的液体作为致冷剂来进行操作，例如，低压塔塔底液体。高压塔的回流通常由冷凝器/蒸发器产生，高压塔顶部和低压塔底部通过冷凝器/蒸发器换热连接。
为了蒸发来自低压塔的在液态下加压的氮，传热介质的选择有两种优选的可能。
第一种选择是：来自高压塔的气体，优选来自高压塔上部或中部的含氮馏分可以作为传热介质。它可以是高压塔的顶部馏分，或者高压塔中间点排出的气体。这一中间点位于高压塔顶下方，多至高压塔内理论板总数的5/6，优选在1/3-5/6处。在产品蒸发器中由间接换热产生的冷凝物至少一部分，优选全部作为回流循环回到高压塔。
另一种选择，或附加的选择是：来自低压塔的气体用作换热介质，以蒸发低压塔的在液态下加压的氮，优选为来自低压塔下部或中部的含氧馏分。它可以是低压塔塔底馏分，或来自低压塔中间点的气体。这一中间点位于低压塔底上方，多至低压塔内理论板总数的5/6，优选在1/3-5/6处。在产品蒸发器中由间接换热产生的冷凝物至少一部分，优选全部作为回流循环回到低压塔。
此外，如果液氮在产品蒸发的间接换热中仅仅部分蒸发，保持为液态的那部分氮返回低压塔也是有利的。在种情况下，产品蒸发器优选作为降膜蒸发器操作。这种类型的蒸发使温差特别小成为可能，从而能得到相应高的蒸发压力，因此，即使用来自高压塔顶部的纯氮作为换热介质，这一压力也仅稍低于(0.3-0.8巴)高压塔内的压力。当保持为液体的那一部分循环时，所用的循环泵是在任何情况下用来增压的泵；低压塔作为一个闪蒸气体分离器。
为了产生致冷量，使过程馏分做功膨胀是很常规的方法。在本发明中，如果用做功膨胀中产生的能量进一步压缩产品蒸发器下游的加压氮气产品是有利的。因此，来自低压塔的加压氮气产品可以低成本地提高到高压塔的压力，并与从高压塔直接排出的氮气产品混合。混合物可以作为产品，或压缩到更高的压力。要进行做功膨胀的过程馏分可以是进料空气的一部分，或来自低压塔顶部冷凝器的蒸发致冷剂，或来自低压塔下部的气体。
通常，在低压塔的顶部冷凝器中，低压塔的塔底液体用作致冷剂以冷凝来自低压塔气态氮。然而，在本发明方法中，如果除加压氮气外，还要生产相对纯的或纯的氧气(纯度高于40摩尔％，特别是高于80摩尔％或高于90摩尔％，优选为99.5-99.999摩尔％)，如果液体馏分－其氧含量在来自高压塔的含氧液体馏分与来自低压塔的塔底液体氧含量之间－用于在顶部冷凝器中冷凝气态氮，则是特别有利的。它可以是来自高压塔本身的含氧液体馏分，或膨胀到约低压塔压力后产生的液体，或在低压塔塔底之上但在含氧液体馏分进料输入点之下采出的液体馏分。在这种方式中，可以从低压塔下部区域以液态和/或气态的形式，准确地说，是在低压塔的超大气压下，采出纯氧产品。与氧产品相比，用于低压塔顶部冷凝器的致冷剂仍然具有较高的氮含量，因此，具有相对低的蒸发温度。
本发明进一步涉及权利要求6-10的设备。
本发明以及本发明的其它细节将在下面参照附图所示的示例性实施方案进行描述，这些附图是：
在以下参照附图对本发明以及本发明的一些细节进行详细描述，这些附图是：
图1显示了本发明方法的第一示例性实施方案及其相应设备，其中产品蒸发器设置在塔外，用来自高压塔的蒸气进行操作，
图2显示了一个改进的示例性实施方案，产品蒸发器用高压塔的中间馏分加热，
图3显示了图1实施方案的另一变形，来自低压塔顶部冷凝器的残余气体做功膨胀，
图4显示了一个实施方案，来自低压塔的气体做功膨胀，
图5显示了一个示例性实施方案，在低压塔中同时生产纯氧，
图6显示了本发明方法的另一示例性实施方案及其相应设备，产品蒸发器设置在塔内，用来自低压塔的蒸气进行操作，
图7显示了一个示例性方案，产品蒸发器设置在塔内，用来自低压塔的蒸气进行操作，
图8和9显示了示例性实施方案，产品蒸发器设置在塔外。
在图1所示方法中，压缩和纯化空气1在主换热器2中冷却，在14巴的压力下输入(3)到高压塔4中。精馏系统还有一个低压塔5，该塔在5巴的压力下操作，经共享冷凝/蒸发器(主冷凝器)6与高压塔换热连接。在从高压塔顶部采出的一部分氮气8在主冷凝器6中液化，经管线9和10作为回流回到高压塔。高压塔的塔底液体11经过低温冷却15、节流(12)后，作为富氧液体馏分进入低压塔5。低压塔5的塔底液体13被低温冷却(14)和膨胀(16)后，引入低压塔5的顶部冷凝器17的蒸发室。在其液化室中，来自低压塔5顶部的气态氮18冷凝；冷凝物19的第一部分作为回流循环回低压塔。
如图1所示，来自顶部冷凝器17的液氮19的另一部分20要么从低压塔采出，或者直接从管线19中分流出来。按照本发明的方法，液氮20在液态下(泵21)加压(如14巴)，并经管线22通过低温冷却器15进入产品蒸发器23。在13.4巴压力下蒸发的氮气24在主换热器2中加热，并作为加压产品25除去。合适的话它可以在气体状态被进一步压缩，且如果需要可以与从高压塔中直接排出的加压氮气27、28混合(29)混合。在这实施方案中，总加压氮气产品29里有约50％是来自低压塔5。
在产品蒸发器23的液化侧，来自高压塔4顶部的气态氮7中一部分35被冷凝。得到的液体36作为附加回流进入高压塔4。在这一实施方案中，产品蒸发器23设计成降膜蒸发器，在其中只发生部分蒸发。保持为液态的氮45循环到低压塔5。
必要时，来自低压塔顶的一部分液氮可以以液体产品30的形式被生产出来。由低压塔的顶部冷凝器17蒸发低压塔5的塔底液体13所产生的不纯氧气31，在换热器14、15和2中加热后作为副产物或作为残余气体除去。例如，它可以用于空气纯化装置的再生。
在图1所示的本发明方法中，一部分空气流32通过做功膨胀33产生致冷量。膨胀空气34引入低压塔5。在膨胀机33中产生的机械能可以用于产品蒸发器23中蒸发的加压氮气产品24的再压缩26，优选通过膨胀机33和压缩机26的直接机械耦合。
图2所示方法不同于这一方法的地方主要是在产品蒸发器中使用了不同的传热介质。在这里，不使用高压塔4的顶部气体7，来自高压塔中间点的气体35′被输入到产品蒸发器23的液化室中。例如，在总共有60块理论塔板的高压塔中，中间点位于高压塔4顶部约20块理论塔板下方。
气体35′仍含有约2摩尔％的氧气，因此，与来自高压塔6(10ppb氧气)顶部的纯氮气相比，具有较高的冷凝温度。产品蒸发器23的蒸发侧的压力也相应较高(为14巴，而不是图1所示情况下的13.4巴)。在间接换热中产生的冷凝物36′被循环到高压塔4，其位置与其组成相对应，特别是在采出点(管线35′或稍高)。
由于在蒸发器23中已由泵21生成的压力较高，因此，在某些情况下，将蒸发的加压氮气24′压缩(图1中的26)到高压塔的压力一这一步骤可以省略，来自低压塔和高压塔的两股氮气产品24′、27′可以在主换热器2(管线29′)上游尽早混合。
如果两塔在相当高的压力下操作(如8-15巴)，所有进料空气3′可以输入到高压塔4。这种类型的方法如图3所示，同样在这里只详细描述与图1所示不同的地方。在此实施方案中高压塔4和低压塔5中的操作压力分别为15巴和5巴。过程的致冷量是由来自低压塔5的顶部冷凝器17的蒸发侧的蒸气31、31′的膨胀做功产生的。如果必要的话，如图1所示，膨胀机33′也可以类似地所氮气产品压缩机26耦合。
图4所示方法也可以在低压下使用(如：高压塔10巴，低压塔3巴)。在这里，膨胀机33″由气体37/38操作，气体是从低压塔5的下部分排出的，特别是直接从塔底上方排出的。这一气体(4.5巴)的压力显著高于顶部冷凝器17蒸发侧的压力(1.25巴)。膨胀机产生的废气39可以在主换热器2的一个单独的通道中加热，并作为副产物排放；如果这一废气在主换热器上游与其它馏分(来自顶部冷凝器17的蒸气31)混合，混合物40在主换热器2中一起加热，则可以不设置这一附加通道，如图4所示。
如果除加压氮气外，还生产纯氧(如99.5摩尔％)，可以使用图5所示方法。这一变形不同于图1所示的地方是：用于低压塔5的顶部冷凝器17的致冷剂13′不是从塔底排出，而是从中间点排出，优选从低压塔5内的液体储存器中排出，该储存器设置在来自高压塔4的含氧液体馏分11的入口下方。在与管线13′连接的液体储存器下方，有约50块理论塔板，通过这些塔板，向下流的液体被富集到所需的氧气纯度。氧气产品可以液态(42)和/或气态(43)排出。必要的话，液体42中的一部分44可以输入到顶部冷凝器17中。如果要求氧气有一定的压力，氧42可以在液态下经已知的内部压缩然后蒸发的方法来升高压力一例如与一部分进料空气相互作用。
图6所示方法与图1所示方法有多处不同。例如，在过程流的低温冷却上不同，其中仅有一个用于这目的的换热器15。低压塔5的塔底产物13中的一部分可以作为液体产品(LOX)被生产出来。在主冷凝器6中液化的氮9中的一部分160可以被低温冷却(15)和节流(161)，并进入低压塔5。高压塔的塔底液体11可以部分(162)进入(163)低压塔顶部冷凝器17的蒸发室。在图6所示实施方案中，来自产品蒸发器23的加压氮气产品24不经再压缩，而是以蒸发压力排出。在这里，是通过残余气体的做功膨胀，并使来自低压塔5的顶部冷凝器17的不纯氧气31中的至少一部分150，在膨胀机133中从换热器2的中间温度做功膨胀产生致冷量。透平废气151在换热器2中再加热，并作为残余气体152除去，或者用于再生进料空气的纯化设备。在膨胀机133中产生的机械能可以供给到再生器中，或用于压缩一个过程馏分，优选直接机械耦合膨胀机133和压缩机，在这里没有示出。
与图1相比，其主要区别在于产品蒸发器23。在液化侧，它是用来自于低压塔的蒸气进行操作的。为了这一目的，在产品蒸发器23的液化侧，低压塔底部上方的一部分气体被冷凝。所得到的液体136返流回低压塔。在这一实施方案中，产品蒸发器23设置在低压塔内。它可以设计成降膜蒸发器，其中仅发生部分蒸发。保持为液态的氮循环到低压塔5。
在图7所示设备中，产品蒸发器23是设立在双塔中，这一点类似于图6。在这里，它位于高压塔4的上部。与图1-5所示方案相类似，产品蒸发器23的液化侧接受来自高压塔4顶部的气态氮7中的一部分35。
在图8中，低温冷却器和产品蒸发器集成在换热器装置223中。在这一实施方案中，高压塔的塔底液体11中的一部分246可以用于高压塔(经阀248)或低压塔(经阀247)顶部的附加冷却。如图1所示，一部分32进料空气通过膨胀做功33产生过程致冷量。
和图8一样，图9的产品蒸发器323构成一个逆流换热器，优选为铝板换热器。然而，与图8不同的是它独立于低温冷却换热器15。
很明显，在这里所示出的本发明的不同变形可以相互结合。在本发明方法每一实施方案以及本发明的设备中，特别是在所有示例性的实施方案中，在精馏系统的塔中，可以使用常规的塔板或规整或乱堆填料作为传质元件。也可以结合起来使用不同类型的传质元件。
示例性的实施方案以及本发明的方法总体上讲特别适合于生产挥发性组分－如氦、氖和/或氢－含量特别低的高纯度氮气。为了这一目的，除了在冷凝器23和17上设置更易挥发组分的排出管线外(图中未示出)，还可以提供其它措施。
首先，在所有示例性实施方案中，输入到泵21中的液氮20可以从低压塔顶部的至少一块理论塔板或实际塔板下方排出，而不是从低压塔顶采出。。例如，在塔顶与改进的液氮20采出点之间，可以有多至10块，优选3-5块理论或实际塔板。即使低压塔中安装了填料，这些塔板也可以按常规精馏塔板设计。
其次，在图6-9所示方法中，可以再作改进，在高压塔4中产生的液氮物流(图6和7中的160)可以作为回流输送(经阀161)低压塔5顶部。这一物流同样可以从中间点采出，即从高压塔4顶部之下的1-10，优选3-5块理论或实际塔板的位置上采出。

Claims (10)

1．一种在精馏系统中通过低温分馏空气生产加压氮气的方法，所述系统具有一高压塔(4)和低压塔(5)，在该方法中，进料空气(1,3；1,3′)进入高压塔(4)，从高压塔(4)采出含氧液体馏分(11)，并输入到低压塔(5)，来自低压塔(5)的气态氮(18)在顶部冷凝器(17)中通过与蒸发液体(13；13′,44)间接换热至少部分冷凝，来自低压塔的氮以气态加压氮产品(24,24′,25,29)的形式被生产出来，其压力高于低压塔(5)的操作压力，其特征在于，在顶部冷凝器(17)中由间接换热产生的液氮或从低压塔排出的液氮(20)中的至少一部分在液态下升压(21)到超过低压塔(5)压力的压力，在产品蒸发器(23)中通过与传热介质(35,35′)间接换热而蒸发，并以加压氮气产品(24,24′,25,29)的形式被生产出来。
2．权利要求1的方法，其特征在于，所用的传热介质是来自高压塔(4)的气体，优选来自高压塔(4)上部或中部的含氮馏分(35,35′)，和/或来自低压(5)的气体，优选来自低压塔(5)的下部或中部的含氧馏分。
3．权利要求1或2的方法，其特征在于，液氮(22)在产品蒸发器(23)的间接换热中仅部分蒸发，保持为液态的那一部分(45)氮被循环到低压塔(5)。
4．权利要求1-3之一所述的方法，其特征在于，过程馏分(32,31′,38)经受做功膨胀(33,33′,33″)，做功膨胀(33,33′,33″)中产生的能量用于进一步压缩(26)产品蒸发器(23)下游的加压氮气产品(24)。
5．权利要求1-4之一所述的方法，其特征在于，液体馏分(13′)－其氧含量在来自高压塔(4)的含氧液体馏分(11)与低压塔(5)的塔底液体(42)的氧含量之间－在顶部冷凝器(17)中被用于冷凝来自低压塔(5)的气态氮(18)。
6．一种在精馏系统中通过低温分馏空气生产加压氮气的设备，所述系统具有一高压塔(4)和低压塔(5)，具有与高压塔(4)连接的空气进料管线(1,3；1,3′)，连接高压塔(4)和低压塔(5)的含氧液体馏分管线(11)，液化侧连接(18)到低压塔(5)上部的顶部冷凝器(17)，以气态加压产品的方式从低压塔(5)采出氮的加压产品管线(24,24′,25,29)，其特征在于，顶部冷凝器(17)的液化侧与低压塔(5)或低压塔(5)上部经液氮管线(20,22)流通连接，液氮管线中有液体增压元件(21)和产品蒸发器(23)，产品蒸发器(23)本身与加压产品管线(24,24′,25,29)连接。
7．权利要求6的设备，其特征在于，产品蒸发器(23)的液化侧连接到(7,8；35′)到高压塔的上部或中部和/或低压塔的下部或中部。
8．权利要求6或7的设备,其特征在于，一条从产品蒸发(23)连接到低压塔(5)的液体返回管线(45)。
9．权利要求6-8之一所述的设备，其特征在于，过程馏分(32,31′,38)的做功膨胀机(33,33′,33″)，膨胀机与压缩机(26)耦合，以进一步压缩产品蒸发器(23)下游的加压氮气产品(24)。
10．权利要求6-9之一所述的设备，其特征在于，致冷剂液体管线(13)，其一端与低压塔(5)的中部或高压塔下部连接，另一端与低压塔(5)的顶部冷凝器(17)的蒸发侧连接。
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CN108207113A (zh) * 2015-02-19 2018-06-26 林德股份公司 获得压缩氮产品的方法及设备
CN107606875A (zh) * 2016-07-12 2018-01-19 林德股份公司 通过低温分离空气产生压缩氮和液氮的方法和设备
TWI737770B (zh) * 2016-07-12 2021-09-01 德商林德股份公司 藉由低溫分離空氣製造加壓氮及液態氮之方法及裝置

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DK0948730T3 (da) 2000-10-16
CA2277838A1 (en) 1998-05-07
WO1998019122A1 (de) 1998-05-07
JP2001509246A (ja) 2001-07-10
PT948730E (pt) 2000-12-29
EP0948730A1 (de) 1999-10-13
EP0948730B1 (de) 2000-08-30
KR20000052974A (ko) 2000-08-25
DE59702301D1 (de) 2000-10-05
DE19735154A1 (de) 1998-05-07
ES2150291T3 (es) 2000-11-16

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