CN1146544A - 高纯氮气发生器 - Google Patents

高纯氮气发生器 Download PDF

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CN1146544A
CN1146544A CN96110859A CN96110859A CN1146544A CN 1146544 A CN1146544 A CN 1146544A CN 96110859 A CN96110859 A CN 96110859A CN 96110859 A CN96110859 A CN 96110859A CN 1146544 A CN1146544 A CN 1146544A
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liquid nitrogen
pipe
rectifying column
nitrogen
inverted
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山本隆夫
小泉真五
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Teisan KK
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Abstract

高纯氮气发生器,当在液氮贮罐10中产生蒸出气时,该发生器可迅速恢复稳定状态,其中包括一个液氮贮罐10、一个精馏塔7、一个用于将液氮从液氮贮罐供给精馏塔的液氮引入管P15、一个倒U形管P13,该倒U形管的上端设置在所述液氮贮罐10的顶部附近的高度,所述U形管连接到所述液氮贮罐10的底部,所述液氮贮罐10和所述液氮引入管P15借助所述倒U形管相互联接,倒U形管的上端和所述液氮贮罐的顶部借助一管P17相互联接,而且所述管P17上设有一控制阀V3。

Description

高纯氮气发生器
本发明涉及一种利用可装有填料的精馏塔由进料空气产生高纯氮气的装置。
在图2中,表示出一种现有的纯氮气发生器的实例。该装置的主要部分包括一个用于分离和净化作为原料的压缩空气从而得到高纯氮气的填料型精馏塔7,一个用于向填料型精馏塔7提供作为回流液的高纯液氮的液氮贮罐10和一个用于将要被加入填料型精馏塔7中的压缩空气冷却的换热器6,而且该主要部分装在一个真空型隔离容器5中。
至于上述主要部分的附加部分,设有一个包括压缩机1和脱碳酸气和干燥塔4的压缩空气供给系统,一个用于将高纯液氮由液氮贮罐10加到填料型精馏塔7的顶部附近的液氮引入管P15,一个用于绝热膨胀收集在填料型精馏塔7的底部7b的富氧液体以得到极低温空气的膨胀阀V1,一个用于将该极低温空气输送到换热器6作为部分制冷剂的极低温空气管P9,一个用于从填料型精馏塔7的顶部7a取出高纯氮气并将所取出的氮气供给换热器6作为另一部分制冷剂的低温氮气管P8,一个用于将经过换热器6的氮气供给外部的消耗设备的氮气输送管P10,一个用于连接液氮贮罐10的底部与氮气输送管P10的旁通管P14,和一个设在旁通管P14上的为了蒸发由液氮贮罐10引入的液氮的蒸发器11。
另外,  连接液氮贮罐10的顶部与旁通管P14的加压管P22有一个阀V5和蒸发器12,作为加压装置,为了防止液氮贮罐10的压力由于液氮的消耗而降低,还进一步设有连接液压贮罐10与高纯氮气输送管P10的气体释放管P23、P24,它们有一个经过换热器6的中间设置的控制阀6,作为气体释放装置,以防液氮贮罐10的压力变得过大。
在上述装置中,高纯氮气的生产如下进行。
将由液氮贮罐10引入的高纯液氮供给填料型精馏塔7的顶部附近,同时将已经过换热器6被冷却的作为原料的压缩空气加到填料型精馏塔7的底部附近。在填充型精馏塔7内部,压缩空气和液氮相互逆流接触,使得压缩空气中的氧气(在1ata下沸点为-183℃)被选择性地液化而且液氮(在1ata下沸点为-196℃)被蒸发。结果是,富氧的液态空气被收集在填料型精馏塔的底部7b,而且由液氮的蒸发产生的氮气和从压缩空气中分离出的氮气被收集在填料型精馏塔的顶部7a作为高纯氮气。
将被收集在填料型精馏塔的底部7b的富氧液态空气送到膨胀阀V1,在此处它绝热膨胀成极低温空气。
在所述极低温空气经极低温空气管P9送到换热器6作为一部分致冷剂用于冷却压缩空气原料后,将其经管P11释放到大气中。
在分离和纯化后的氮气从填料型精馏塔的顶部7a取出并经低温氮气管P8供给换热器6作为部分致冷剂后,将其经氮气输送管供给外部消耗设备作为高纯氮气产品。
当在液氮贮罐10中由于该装置中的热平衡的不规则而产生蒸出气时,控制阀6会打开使蒸出气经气体释放管P23、P24释放到氮气输送管P10中,因此,液氮贮罐10的内部压力呈稳定状态。
然而,在现有的上述这种高纯氮气发生器中,当蒸出气产生时,经气体释放管P23、P24、换热器6、控制阀V6等流入氮气输送管P10中的氮气量会受到某些限制。从而,液氮贮罐10的压力不能迅速降低,而且高纯液氮会无益地浪费。另外,人们一直希望简化与蒸出气的处理有关的装置,所述装置包括用于蒸出气的系统部件如气体释放管P23、P24和换热器6。
按照本发明,为了解决这些问题,将一个倒U形管连接到所述液氮贮罐的底部,该管上端设置在所述液氮贮罐的顶部附近的高度上,借助所述倒U形管,所述液氮贮罐和所述液氮引入管相互连接,用一个连接管使倒U形管的上端和所述液氮贮罐的顶部相互连接,并且在所述连接管上设置一个控制阀,当所述液氮贮罐的压力超过预定值时,通过打开控制阀将氮气从所述液氮贮罐的顶部引入倒U形管的上端。
这样,能够中断液氮从液氮贮罐向填料型精馏塔的流动,因为液氮在该管中的流动是由虹吸打断的。
本发明的高纯氮气发生器包括:
-一个填料型精馏塔,冷却的压缩空气从其底部附近引入其中,该压缩空气和从其顶部附近引入的液氮相互逆流接触使压缩空气中的氧气液化,所得的空气贮存在底部作为富氧液态空气,而分离出的氮气被收集在顶部;
-一个液氮贮罐,用于贮存液氮;
-一个液氮引入管,用于将液氮从所述液氮贮罐的底部供给所述填料型精馏塔的顶部附近;
-一个换热器,用于使要被加入填料型精馏塔的压缩空气冷却;
-一个膨胀阀,用于使由填料型精馏塔底部取出的所述富氧液态空气绝热膨胀以得到极低温空气;
-一个极低温空气管,用于向所述换热器供给该极低温空气作为致冷剂;和
-一个氮气输送管,用于将所述由填料型精馏塔顶部取出的氮气供给外部消耗设备,其特征在于一个倒U型管连接到所述液氮贮罐底部,该管上端设置在所述液氮贮罐顶部附近高度上,所述液氮贮罐和所述液氮引入管借助所述倒U型管相互连接,该倒U型管的上端和所述液氮贮罐的顶部借助一个管相互连接,而且在所述管上设置一个控制阀,当所述液氮贮罐的压力超过预定值时,控制阀打开以便将氮气从所述液氮贮罐顶部引入该倒U形管的上端。
在图1中,表示涉及本发明高纯氮气发生器的一个实例的流程图。在该图中,标号7表示一个填料型精馏塔(在该实施方案中这是一种规整填料型精馏塔),10表示一个液氮贮罐,P15表示一个液氮引入管,6表示一个换热器,V1表示一个膨胀阀,P9表示一个极低温空气管,P10表示一个液氮输送管,P14表示一个旁通管,P13表示一个倒U型管,P17表示一个用于连接倒U形管的上端与所述液氮贮缸顶部的连接管,V3表示一个控制阀。
借助催化剂塔2和冷却器3使脱碳酸气和干燥塔4与用于提供作为原料的压缩空气的后级空气压缩机1连接,并且借助管P4使用于冷却压缩空气的换热器6与后级脱碳酸气和干燥塔4连接。用于来自换热器6的压缩空气的管P5连接到规整填料型精馏塔7的底部附近。氮气引入管P15连接到规整填料型精馏塔7的顶部附近。该氮气引入管P15和液氮贮罐10的底部借助倒U型管P13相互连接。
规整填料型精馏塔7上设有冷凝器9,规整填料型精馏塔的底部7b与所述冷凝器9的顶部借助于膨胀阀V1相互连接。冷凝器9的顶部和换热器6的(第一)致冷剂供给侧通过极低温空气管P9相互连接。规整填料型精馏塔的顶部7a和换热器6的(第二)致冷剂供给侧通过低温氮气管P8相互连接。所述换热器6、规整填料型精馏塔7、液氮贮罐10和冷凝器9被装在一个真空型隔离容器5中。
氮气输送管P10用于将已经过换热器6的高纯氮气产品供给外部消耗设备。旁通管P14连接到氮气输送管P10上。该旁通管P14借助于倒U形管P13连接液氮贮罐10的底部。在旁通管P14上设有一个用于蒸发液氮的蒸发器11和一个阀V4。
液氮贮罐10的顶部和旁通管P14借助具有设置在其上的阀V5和蒸发器12的加压管P22相互连接。另外,液氮贮罐10的顶部和倒U形管P13的上端借助于连接管P17相互连接。管P17设有阀V3。
下面描述该装置的操作。
在作为原料的空气借助于空气过滤器(未示出)除去灰尘后,将其引入压缩机1并制成压缩空气,压缩空气的压力升至制备氮气所需的压力,例如约8.5ata。然后,将该压缩空气经管P1引入催化剂塔2中。在催化剂塔2中,装有氧化催化剂如钯催化剂,压缩空气中所含的一氧化碳和氢气在高温气氛下借助所述催化剂氧化,分别转化成二氧化碳和水。
然后,压缩空气经管P2进入冷却器3,在压缩空气在此预冷后,将其经管P3加入脱碳酸气和干燥塔4中。该脱碳酸气和干燥塔4装有氧化铝或分子筛,在此除去压缩空气中的二氧化碳和水分。
将已经过脱碳酸气和干燥塔4的压缩空气经管P4引入装在隔离容器(冷箱)5中的换热器6中,并且用致冷剂通过换热将其冷却到接近其沸点(液化点)。来自换热器6的压缩空气的压力变成约8.0ata,且它的温度变成约-165℃。然后,借助管P5将该压缩空气引入规整填料型精馏塔7的底部附近。
在前述压力和温度条件下,一部分压缩空气液化并作为富氧液态空气贮存在于规整填料型精馏塔7的底部7b,而其余部分上升,经过规整填料型精馏塔7成为富氮气体。另一方面,由于将高纯液氮(压力约为8.0ata)作为回流液供给规整填料型精馏塔7的顶部附近,所以,富氮气体通过与在规整填料的倾斜的精馏面上向下流动的回流液体经过逆流气液接触而被冷却,而且通过选择性地液化其氧气成分而被精馏成为高纯氮气,该氮气被收集在规整填料型精馏塔7的顶部7a。
在高纯氮气借助低温氮气管P8被送入换热器6以便被用作使作为原料的压缩空气冷却的一部分致冷剂后,其温度变为常温(在约7.7ata的压力下)。然后,将所得到的常温氮气从氮气输送管P10送到外部消耗设备作为高纯氮气(产品)。
另一方面,贮存在规整填料型精馏塔7的底部7b中的富氧液态空气借助于管P6被送至膨胀阀V1,绝热膨胀(在温度约-190℃)以成为压力约为1.8ata的极低温空气。将该极低温空气借助于管P7送到设置在规整填料型精馏塔7上的冷凝器9。在冷凝器9中,一部分高纯氮气从规整填料型精馏塔的顶部7a被回收以便用极低温空气经过间接换热液化氮气。这样得到的液氮再返回规整填料型精馏塔7的顶部附近并用作一部分回流液体。在来自冷凝器9的极低温空气经极低温空气管P9被送入换热器6以便被用作冷却作为原料的压缩空气的一部分致冷剂后,其温度成为常温。在所得到的常温空气经管P11送入脱碳酸气和干燥塔4以被用作脱碳酸气和干燥塔4的再生气后,将其经管P12排放到大气中。
被用于规整填料型精馏塔7中作为回流液的高纯液氮经倒U形管P13、阀V2和液氮引入管P15从液氮贮罐10的底部被供给规整填料型精馏塔7的顶部附近。
在只供给在规整填料型精馏塔7中分离和提纯的高纯氮气的情况下,当由于需求量增加而导致氮气(产品)供应不足时,打开阀V4,操作蒸发器11。在液氮贮罐10中的液氮经倒U形管P13和旁通管P14被引入蒸发器11中并由于前述操作而蒸发后,将其经阀V4和管P20送入氮气输送管P10中。当液氮贮罐10的压力降低到低于预定压力并且送到规整填料型精馏塔7中的液氮量减少时,打开阀V5并操作蒸发器12。在液氮贮罐10中的液氮经倒U形管P13和旁通管P14引入蒸发器12并由于前述操作蒸发后,它返回液氮贮罐10的顶部,从而恢复液氮贮罐10的压力。
当液氮贮罐10中由于外界传入的热而产生蒸发气并且其压力反常地升至超过预定值(例如约10.9ata)时,打开控制阀V3,从而将蒸发气引到倒U形管P13的上端。由于上述操作,液氮流虹吸破坏并暂时中断。通过重复该现象,液氮贮罐10中的蒸出气被吸收到该罐的液氮中。在液氮贮罐10的压力稳定后关闭控制阀V3,这时,保留在倒U形P13中的蒸出气也被吸收到该管中的液氮中,这样,恢复该管中的液氮流。
由于倒U形管连接到液氮引入管上,所述液氮引入管使液氮贮罐的底部和填料型精馏塔的顶部相互连接,所述倒U形管的上端和所述液氮贮罐的顶部借助一管相互连接,在所述管上设有一控制阀,从而能在液氮贮罐中产生蒸出气时迅速中断液氮由液氮贮罐向填料型精馏塔的流动。由于产生的蒸出气最终被吸收到液氮贮罐的液氮之中,所以能够在不使高纯液氮释放入大气的条件下操作该装置。另外,能够省掉蒸出气的系统部件如气体释放管和换热器,并简化与蒸出气的处理有关的设备。
图1是按照本发明的高纯氮气发生器的一个实施方案的流程图。
图2是现有技术高纯氮气发生器的一个实例的流程图。

Claims (1)

1.一种高纯氮气发生器,包括:
一个精馏塔(7),冷却后的压缩空气由其底部(7b)附近引入其中,该压缩空气和由其顶部附近引入的液氮相互逆流接触,使压缩空气中的氧气液化,所得到的空气贮存在底部作为富氧液体,而分离出的氮气被收集在顶部;
一个液氮贮罐(10),用于贮存液氮;
一个液氮引入管(P15),用于将液氮从所述液氮贮罐的底部供给所述填料型精馏塔的顶部附近;
一个换热器(6),用于使要被加入填料型精馏塔的压缩空气冷却;
一个膨胀阀(V1),用于使由填料型精馏塔底部取出的所述富氧液体绝热膨胀;
一个极低温空气管(P4),用于向所述换热器(6)供给作为致冷剂的极低温空气;和
一个氮气输送管(P10),用于将所述由精馏塔顶部取出的氮气供给外部消耗设备,其特征在于一个倒U形管(P13)连接到所述液氮贮罐的底部,该管的上端设置在所述液氮贮罐的顶部附近的高度上,所述液氮贮罐和所述液氮引入管借助所述倒U形管相互连接,倒U形管的上端和所述液氮贮罐的顶部借助于一个连接管(P17)相互连接,并且在所述连接管上设有一个控制阀(V3),当所述液氮贮罐的压力超过预定值时,控制阀打开以便将氮气从所述液氮贮罐的顶部引入该倒U形管的上端。
CN96110859A 1995-07-26 1996-07-26 高纯氮气发生器 Pending CN1146544A (zh)

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