CN1423108A - 通过低温空气分馏来生产高纯度氮的工艺和设备 - Google Patents

通过低温空气分馏来生产高纯度氮的工艺和设备 Download PDF

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CN1423108A
CN1423108A CN02145709A CN02145709A CN1423108A CN 1423108 A CN1423108 A CN 1423108A CN 02145709 A CN02145709 A CN 02145709A CN 02145709 A CN02145709 A CN 02145709A CN 1423108 A CN1423108 A CN 1423108A
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CN100334412C (zh
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斯特凡·洛赫纳
拉尔夫·施珀雷伊
米夏埃多·劳特尔
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J3/04406Processes 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 using a dual pressure main column system
    • F25J3/04412Processes 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 using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
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    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
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    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04763Start-up or control of the process; Details of the apparatus used
    • F25J3/04769Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854Safety aspects of operation
    • F25J3/0486Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
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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
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/50Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/90Details relating to column internals, e.g. structured packing, gas or liquid distribution
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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
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/42Nitrogen or special cases, e.g. multiple or low purity N2
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

本发明的工艺和设备用来在一种精馏系统中通过低温空气分馏来生产氮,所述精馏系统具有压力塔(4)和低压塔(5)。将压缩空气(1,3)引入到压力塔(4)中。从压力塔(4)中排出含氧液体馏分(11)并且将它输送进低压塔(5)。在质量转移部分(25)上方从低压塔(5)中提取气态氮(18),所述质量转移部分具有至少一块假想或实际板,并且在顶部冷凝器(17)通过与制冷剂(13)进行间接热交换来使所述气态氮至少部分冷凝。在质量转移部分(25)下方从低压塔中排出高纯度氮,从而将它作为氮产品(26,27,30)获取。该工艺和设备具有一种制冷供应系统,制冷流体(31)在其中流动。在质量转移部分(25)上方将来自质量提供系统的至少一部分制冷流体引入低压塔(5)中。

Description

通过低温空气分馏来生产高纯度氮的工艺和设备
技术领域
本发明涉及一种在具有压力塔和低压塔的精馏系统中通过低温空气分馏来生产氮的工艺,其中将工艺压缩空气引进压力塔中,从压力塔中排出含氧液体成分并且将它送进低压塔中,在具有至少一块假想或实际板的质量转移部分上方从低压塔中提取气态氮,并且在顶部冷凝器中通过与制冷剂进行间接热交换来使所述气态氮至少部分冷凝,在质量转移部分下方从低压塔中排出高纯度氮,从而将它获取为氮产品。
背景技术
从EP948730B1和EP955509A1中可以了解这种类型的工艺和相应设备。在这些情况中,在低压塔中可以在高压下获得氮。如果将挡板(“具有至少一块假想或实际板的质量转移部分”)构造进低压塔的上面区域中,则该氮产品可以具有特别高的纯度,并且尤其可以具有非常少量的高挥发性杂质。
发明概述
本发明的目的在于说明一种上述类型的工艺以及在经济上尤为有利的相应设备。
通过以下事实来实现该目的,该工艺具有一种制冷供应系统,制冷流体在其中流动,并且在质量转移部分上方将来自该制冷供应系统的至少一部分制冷流体引进低压塔中。作为可选方案,或者此外,在本发明的范围内还可以将来自制冷供应系统的制冷流体引进压力塔的上面区域中。
在本发明中,制冷流体可以由容易得到的介质形成,将该介质引进低压塔中并且以这种方式作用在低压塔中的质量转移部分中,并且不会损害高纯度氮产品的纯度并且无需使低压塔的操作压力与制冷供应系统的要求匹配。(合适的制冷流体的示例为仍然含有高挥发性杂质的氮)。通过比较,在已知工艺的制冷供应系统中,例如从顶部冷凝器的蒸发空间中提取残余馏分,该残余馏分以做功的方式膨胀成大约为大气压力并且从该工艺中排出。在该情况中,顶部冷凝器的最小操作压力以及因此低压塔的操作压力只由制冷供应系统来确定。在本发明中可以避免这个缺点并且不会降低该产品的纯度。
在本发明中,优选在低压塔的顶部处送入该制冷流体。
在本发明的第一变型中,制冷流体从压力塔中排出,在制冷供应系统中以做功的方式膨胀并且被引进低压塔中。
流体尤其是气体从压力塔压力做功膨胀成低压塔压力将会允许产生特别有利的工艺制冷。这样,可以补偿绝缘和交换损失,并且可以使适当少量的产品液化。在其做功膨胀的上游,制冷流体优选在与将要冷却的工艺流体的直接热交换中受到加热。
质量转移部分由一块或多块精馏板(被称为挡板)形成-为此,以“实际”板数量-或者通过短包装部分(“假想”板数量)来给出该信息。挡板或假想板的数量例如为1-10,优选为2-3。由于在这些挡板下面提取氮产品,所以该氮产品具有非常少量的高挥发性杂质,这些杂质保留在低压塔的顶部中并且从那里与较不纯的氮气流一起被提取出。
制冷流体通常包含比氮更容易挥发的组分。但是,由于送料在所述质量转移部分上方进行,所以这些组分不会进入到在更下方提取的氮产品。
如果从压力塔的上面区域中排出该制冷流体,则是有利的。例如,该制冷流体是由来自该压力塔的富氮气体馏分尤其由该塔的顶部气体形成的。
根据本发明的第二变型,制冷流体是由已经在制冷系统外面生产出的低温液体形成的。
由于将外部液体作为制冷源输送进(液体帮助),所以该工艺具有特别高的灵活性。例如,用于产生制冷的机器例如膨胀式涡轮可以完全或部分除去。该低温液体例如可以通过源于另一个气体分馏设备的液态氮来形成,或者可以使用空气组分的其它混合物。可以通过管路来提供外部流体或者从存储容器中排出。该液体在与外部流体组成相对应的那个位置处输送进。该位置可以是压力塔或低压塔的上面区域。
可以优选在该塔的顶部将低温液体部分或完全引进低压塔。作为可选方案或者此外,可以至少部分地将该低温液体引进压力塔的上面区域。
优选从低压塔的下面区域中将用于顶部冷凝器的制冷剂排出,并且将压力塔的所有富氧产品送进低压塔中。在本发明的范围中,术语“富氧的”指的是其氧含量大于空气中氧含量的任何馏分。
从低压塔中可以提取以气体形式的氮产品。或者,从低压塔中可以提取为液体形式的氮产品,并且该氮产品通过与已经以做功方式膨胀的制冷流体进行间接热交换而蒸发。这两个工艺步骤的组合方案也是可行的。
另外,本发明涉及一种根据权利要求10-12所述的设备。
附图说明
图示出本发明工艺和设备的第一变型;
图2示出本发明工艺和设备的第二变型。
优选实施方案
下面将参照两个示例性实施方案对本发明以及本发明的其它细节进行说明-每个实施方案用于本发明的两个变型的一个(在附图中所示的)。
在图1中所示的示例性实施方案中,在主热交换器2使压缩且净化的气体1冷却并且在9-13巴的压力下将它输送(3)进压力塔4中。精馏系统还具有低压塔5,该塔在2-5巴的压力下工作,并且通过共同的冷凝器-蒸发器(主冷凝器)6与压力塔进行热交换。在压力塔的顶部处已经被排出的一部分氮8在主冷凝器6中被液化,并且通过管道9和10作为回流被部分加入到压力塔中。来自主冷凝器6的液体另一股流体14被过冷(15),并且该液流的第一部分20作为回流被送给低压塔5的顶部。被过冷的氮的第二部分21作为液体产品(PLIN)被排出。在过冷15之后,来自压力塔的底部液体11作为富氧液体馏分被调节(12)进低压塔5中。
同样使低压塔5的底部液体13过冷(15)并且膨胀(16),然后将它引进低压塔5的顶部冷凝器17的蒸发空间中。来自低压塔5的顶部的气态氮18在该冷凝器的液化空间中冷凝;将冷凝物19送回进低压塔中,在那里它被用作附加的回流。从顶部冷凝器17的蒸发空间的下面区域中通过管线22连续地或间歇地提取纯化液体(PURGE)。在顶部冷凝器17中产生出的蒸汽23在热交换器15和2中被温暖到大致室温并且通过管道24排出和/或用作用于未示出的清洗设备(例如分子筛站)的再生气体。通过管道35提取未冷凝的气体尤其含有相对高挥发性的组分的气体。将该气体吹出(36)和/或与蒸汽23混合(37)。
在低压塔5顶部的下方为质量转移部分25,该部分在实施例中由三块实际板(挡板)形成。在该部分下面,通过管道26将气态氮作为高纯度产品排出,并且在热交换器15和2中将它温暖到大约室温。在该示例性实施方案中,在具有后冷却机29的氮压缩机28中将温暖的氮产品27进一步压缩,并且最终通过管道30将它提取出作为最终产品(PGAN)。
通过管道31,从压力塔4中将一部分气态顶部氮提取作为制冷流体,在主热交换器2中将它温暖到中间温度,并且通过管道32输送给膨胀机33,该膨胀机例如设计用作发生器蜗轮。将已经以做功的方式膨胀成大约低压塔压力的制冷流体34输送到低压塔的顶部上,即在挡板25上方送进。这些工艺步骤和/或用于这些步骤的设备部件形成根据本发明第一变型的“制冷供应系统”。
作为可选方案或者另外,根据本发明第一变型,可以将作为制冷流体的氮压缩成大于在“制冷供应系统”中的压力塔压力,然后可以以做功方式膨胀并且被送进压力塔中(优选在顶部处)(在该图中未示出)。
在涡轮33出故障的情况中,通过将来自精馏系统外面的低温液体(38)送进该精馏系统的其中一个塔中(“液体帮助”),从而可以使该设备在紧急模式中操作,如在图2实施例中所描述的一样。与在后面的专利申请不一样,低温液体不必在精馏系统外面已经生产出;而是,在紧急操作中也可以使用在该设备的正常操作期间生产出的并且存储在存储容器中的液体(例如液态氮)。
在图1中所示的示例性实施方案可以以这样一种方式改进,从而在低压塔中生产出气态和/或液态氧产品。为此,在过冷15之后,只有部分来自压力塔的底部液体11被调节进低压塔5中作为含氧液体馏分;另一部分在阀门12的上游分出来并且流进顶部冷凝器17的蒸发空间。从而就完全或部分不需要要从低压塔将底部液体输送16进该蒸发空间。从低压塔5的底部区域提取以气体和/或液体形式的氧产品。
在图2中所示的示例性实施方案中,压缩并且干净的空气1在主热交换器2中被冷却并且在9-10巴的压力下被送给(3)压力塔4。另外,精馏系统具有低压塔5,该塔在2-3巴的压力下工作并且通过共同的冷凝器-蒸发器(主冷凝器)6与压力塔进行热交换。在压力塔的顶部处被排出的氮8在主冷凝器6中液化并且通过管道9和10作为回流被加入到压力塔中。来自主冷凝器6的液体9的另一部分15被过冷(15),并且其第一部分20作为回流被部分输送给低压塔5的顶部。被过冷的氮的第二部分21作为液态产品PLIN被提取。在过冷15之后,来自压力塔的底部液体11被调节(12)进低压塔5中作为含氧液体馏分。
同样使来自低压塔5的底部液体13过冷(15)并且膨胀(16),然后将它输送进低压塔5的顶部冷凝器17的蒸发空间中。来自低压塔5的顶部的气态氮18收缩进入该冷凝器的液化空间;将冷凝物19输送回低压塔中,在那里它被用作附加的回流。从顶部冷凝器17的蒸发空间的下面区域中通过管道22连续地或间歇地提取纯化液体(PURGE)。在顶部冷凝器17中产生的蒸汽23在热交换器15和2中被温暖到室温并且通过管道24排出和/或用作未示出的清洗装置(例如分子筛站)的再生气体。未冷凝的气体尤其是含有挥发性相对较高的组分的气体通过管道35提取。该气体被吹出(36)和/或与蒸汽23混合(37)。
在低压塔5的顶部下面具有质量转移部分25,该部分在该实施例中是由三块实际板(挡板)形成。在该部分下面,气态氮作为高纯度产品通过管道26被排出并且在热交换器15和2中被加热到大约室温。在该示例性实施方案中,温暖的氮产品27在具有后冷却器29的氮压缩机28中受到进一步压缩并且最终通过管道30作为最终产品(PGAN)被提取。
通过管道38将还没有在精馏系统的一个塔4、5中产生的液态氮输送给低压塔的顶部-即在挡板25的上方。在该实施例中,例如通过罐车从由外部源装满的存储容器39中排出该低温液体。这些工艺步骤和/或用来实施这些步骤的设备部件形成根据本发明的第二变型的“制冷供应系统”。
作为可选方案或者另外,在根据本发明第二变型的“制冷供应系统”中,来自存储容器39的液态氮可以作为制冷流体输送进压力塔中(优选在顶部)(在图中未示出)。
在图2中所示的示例性实施方案可以以这样的方式进行改变,从而在低压塔中产生出气态和/或液态氧产品。为此,在过冷15之后,压力塔的底部液体11只有一部分被调节进低压塔5中作为含氧液态馏分;另一部分在阀门12上游分出去并且流进顶部冷凝器17的蒸发空间中。可以完全或部分不需要从低压塔中将底部液体输送16进该蒸发空间中。从低压塔5的底部区域中提取以气态和/或液态形式的氧产品。

Claims (12)

1.一种用于在精馏系统中通过低温空气分馏来生产高纯度氮的工艺,所述精馏系统具有压力塔(4)以及低压塔(5),其中将工艺压缩空气(1,3)引入压力塔(4)中,从该压力塔(4)中排出含氧液体馏分(11)并且将它输送进低压塔(5)中,在具有至少一块假想或实际板的质量转移部分上方从低压塔(5)中提取气态氮(18),并且在顶部冷凝器(17)中通过与制冷剂(12)进行间接热交换来使所述气态氮至少部分冷凝,并且在质量转移部分(25)下方从低压塔(5)中排出高纯度氮(26、27、30),其特征在于,该工艺具有一种制冷供应系统,其中制冷流体(31、32、34;38)流动,并且在质量转移部分(25)上方将来自制冷供应系统的至少部分制冷流体引入(34;38)进低压塔(5)或者进入压力塔(4)的上面区域。
2.如权利要求1所述的工艺,其特征在于,所述制冷流体从压力塔(4)被排出,在制冷供应系统中以做功的方式膨胀(33),并且被引进(34)低压塔(5)中。
3.如权利要求2所述的工艺,其特征在于,从压力塔(4)的上面区域中排出所述制冷流体(31)。
4.如权利要求1-3所述的工艺,其特征在于,通过已经在精馏系统外面产生的低温液体(38)来形成制冷流体。
5.如权利要求4所述的工艺,其特征在于,将所述低温液体局部或完全引入低压塔(5)中。
6.如权利要求1-5所述的工艺,其特征在于,从低压塔(5)的下面区域中排出用于顶部冷凝器(17)的制冷剂(13)。
7.如权利要求1-6中任一所述的工艺,其特征在于,将压力塔(4)的所有富氧产品(11)送进(12)低压塔(5)中。
8.如权利要求1-7中任一所述的工艺,其特征在于,从低压塔(5)中提取至少部分为气体形式的氮产品(26)。
9.如权利要求1-8中任一所述的工艺,其特征在于,从低压塔中提取至少部分为液体形式的氮产品,并且通过与已经以做功方式膨胀的制冷流体进行间接热交换使之蒸发。
10.一种用于在精馏系统中通过低温空气分馏来生产氮的设备,所述精馏系统具有压力塔(4)和低压塔(5),该设备具有:导入进压力塔(4)中的压缩空气管道(1,3);用于含氧液体馏分的管道(11),该管道从压力塔(4)中导入进低压塔(5)中;顶部冷凝器(17),其液化侧在质量转移部分(25)上方与低压塔(5)的区域连接,所述质量转移部分具有至少一块假想或实际板;以及用于排出高纯度氮的氮产品管道(26,27,30),该管道在质量转移部分(25)的下面与低压塔(5)相连,其特征在于,该设备包括一种制冷供应系统,该系统具有制冷流体管道(31,32,34;38),该管道在质量转移部分(25)上方与低压塔(5)连接。
11.如权利要求10所述的设备,其特征在于,所述制冷供应系统具有膨胀机(33),其入口与压力塔(4)连接(11,32),而出口与制冷流体管道(31,32,34;38)连接(34)。
12.如权利要求10或11所述的设备,其特征在于,所述制冷流体管道设计成为一种液体管道(38),用来送入已经在精馏系统外面生产出的低温液体。
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