CN1143748A - 监测空气分离设备的操作的方法及装置 - Google Patents

监测空气分离设备的操作的方法及装置 Download PDF

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CN1143748A
CN1143748A CN96102125A CN96102125A CN1143748A CN 1143748 A CN1143748 A CN 1143748A CN 96102125 A CN96102125 A CN 96102125A CN 96102125 A CN96102125 A CN 96102125A CN 1143748 A CN1143748 A CN 1143748A
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B·达尔里迪奥
A·扎科麦特
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

在一种用于监测通过低温精馏分离空气的设备的操作的方法中，检测该设备的蒸发器-冷凝器的蒸浴中的氧化亚氮量的变化。氧化亚氮量可以用红外辐射分析仪测量。

Description

监测空气分离设备的操作的方法及装置
本发明的主题是用于监测通过低温蒸馏分离空气或从空气中分离气体的设备的操作的方法和装置。
在这些空气分离设备中处理的空气含有一些杂质。大多数杂质如烃和氮的氧化物比氧气难挥发并聚集在蒸发器的蒸浴液体中。在单塔的情况下，涉及一种蒸发器一顶部冷凝器，高浓度液体聚集在其中，在双塔的情况下，一般涉及蒸发器-冷凝器，它提供低压塔的氧气和中等压力塔的氮气或者压缩空气或任何其它循环流体(优选在不是中等压力下的氮气)之间的热交换。
溶解度极小(溶解度仅为几ppm)的这些杂质单独或一起存在会产生各种危险，特别是爆炸的危险。从而存在将它们除掉的问题。人们已经使用各种手段来避免在液相或气相中的任何聚集，特别是通过如DE-A-1936049中所述的吸附或者清除蒸发器的蒸浴来阻止其聚集。
安全性要求一方面，防止危险的杂质的聚集，以及另一方面，监测后者的除去是有效的。
到目前为止，人们的注意力一直主要集中在烃上特别是乙炔上。除去装置正在良好地操作的监测是按照烃含量一般通过色谱法(例如用火焰离子化检测法)进行的，但是色谱分析是昂贵的且难以实现。
目前，阻止二氧化碳和水存在于设备的进料空气中是通过在低温分离的上游的吸附来进行的。空气中的一些杂质特别是不饱和烃通过该吸附纯化至少部分受到抑制。其它物料如部分氮的氧化物连续进入冷却单元，所述单元包含一个或多个塔。从而目标在于防止这些杂质在蒸发器的蒸浴中聚集的装置的规模可以减小，但不能省略，这归因于吸附系统的存在，并且需要连续监测为此目的而设置的装置是有效的。
无论设有在低温分离(例如制备液相或气态氧)的上游吸附系统的装置如何操作，蒸发器的蒸浴中的烃含量在大部分时间内是微不足道的并且通常是测不到的，烷烃(甲烷、乙烷、丙烷)除外，但由于预防装置实际上对这些没有危险的污染物质是无效的，分辩它们的含量没有益处。尽管设置好的预防装置是有效的，不检测烃并不要紧，因为它们的设计的限制因素往往是氮的氧化物。另外，它们相对难以测量并且预期使用色谱法分析。从而监测烃并不能够简单而可靠地确认所设置的安全装置在有效地操作。
本发明的目的是制备一种监测空气分离设备的操作的装置，当设置用于防止杂质聚集在蒸发器的蒸浴中的装置操作不好时所述装置容易使用并且有效地检测。
为此，本发明的主题是一种用于监测一种包含一个精馏塔和一个蒸发器-冷凝器的通过低温精馏进行空气分离或从空气中分离气体的设备的操作的方法，其特征在于检测聚集在蒸发器-冷凝器的蒸浴中的氧化亚氮的量的改变。
按照本发明的其它新的特征：
-连续测量液体中氧化亚氮的含量；
-用红外辐射分析仪测量氧化亚氮量；
-测量聚集在蒸发器-冷凝器中的液体中的氧化亚氮量；
-连续检测液体中的氧化亚氮量的变化。
本发明的另一个主题是一种用于监测通过低温精馏进行空气分离的设备的操作的装置，该装置包括用于检测该设备的蒸发器-冷凝器的蒸浴中的氧化亚氮量的变化的装置。
按照其它特征：
-蒸发器-冷凝器设置在双塔的低压塔的罐中；
-用于检测所述变化的装置包括红外辐射分析仪。
本发明的另一主题是使用一种测量空气精馏塔的蒸发器-冷凝器的蒸浴中的氧化亚氮量的分析器。
表示出其特征的是氧化亚氮显示出非常适合作为安全装置的有效操作的指示物。一方面，它在空气中的含量相对恒定在0.3至0.4ppm的数量级。当该设备在稳定的条件下运行时，蒸发器-冷凝器的蒸浴中的氧化亚氮量因而是恒定的，并且只是该设备的液态和气态氧的各自产量的函数。另一方面，氧化亚氮是一种挥发性极小的组分，从而它有聚集在蒸发器的液体中的趋势。从而对于安全性这是不利的。最后，氧化亚氮在液态氧中是相对可溶的，溶解度在90K时为180ppm数量级。从而容易测得的蒸发器的蒸浴中允许的最大氧化亚氮量为在20至30ppm范围内，所述氧化亚氮是在低压塔的罐的液氧中。
这些性质使得液氧浴中的氧化亚氮量或蒸发器的高浓度液体中的氧化亚氮量对设备的操作敏感。特别是，通过几ppm数量级、甚至几+ppm数量级的蒸浴中的量的变化反映出安全清除操作不好(例如是清除管中的阻塞的结果)或者蒸发器的操作不好(蒸发干)，从而很容易测到。所以观察蒸发器的蒸浴中的氧化亚氮量能有效地监测预防装置的操作。
另外，氧化亚氮的分析可以通过红外辐射分析仪进行，该分析仪的使用比色谱法更经济和简单。另外该分析仪能连续分析所述量，这对于色谱法是不可能的。该分析仪可为J-A-04/191654中描述的类型。然而，并不排除使用色谱。
从而通过连续观察蒸发器中的液体中的氧化亚氮量能够代替相同液体中的烃的色谱分析。目标是使得为防止杂质在蒸发器附近聚集而设置的预防装置的令人满意的操作的监测更有效和更经济。
通过利用本发明还可能用液体过滤器来分散，该过滤器设置在常规设备中的蒸发器附近。过滤器如DE-A-19.36.049中所述被用于纯化液态氧或蒸发器的蒸浴中的高浓度液体并必须每周被再生。
使得检测至少氧化亚氮量的变化的成为可能的装置可被用于清洗蒸发器-冷凝器，这使得连续纯化液浴成为可能。另外，该装置可被设置在蒸发器的蒸浴中。
本发明适用于监测包括以“浴”表示的这种蒸发器-冷凝器的设备的方法和适用于监测包括“膜”式蒸发器如在EP-B-130，122中所述的蒸发器的设备的方法。
如果液氧量不够高，蒸发器会操作“至干”，从而氧化亚氮会在蒸发器的氧气通道中结晶。这样，围绕蒸发器的液浴将在氧化亚氮中耗尽而且分析仪将检测氧化亚氮的量的下降。
相反，如果氧化亚氮量增加，这意味着蒸发器的清洗流速太小，这归因于清洗管的堵塞或由于清洗的打开阀未充分打开。
氧化亚氮量的增加还可以归因于空气净化吸附塔的不正常工作，在这些情况下，操作者将调节吸附塔的压力和/或循环时间。

Claims (11)

1.监测通过低温精馏分离空气的设备的操作的方法，所述设备包括一个精馏塔和一个装有液浴的蒸发器-冷凝器，
其特征在于检测聚集在蒸发器-冷凝器中的液体中的氧化亚氮量的变化。
2.按权利要求1的方法，用红外辐射分析仪测量氧化亚氮量。
3.按权利要求1和2的任一个的方法，测量液体中的氧化亚氮量。
4.按权利要求3的方法，连续测量液体中的氧化亚氮量。
5.按前述权利要求之一的方法，其中按照氧化亚氮量的改变，将另外的液体送入蒸发器-冷凝器，增加蒸发器-冷凝器的清洗流速或者调节该设备的空气净化吸附塔的操作。
6.使用分析器测量聚集在空气精馏塔的蒸发器-冷凝器中的液体的氧化亚氮量。
7.用于监测通过低温蒸馏分离空气的设备的操作的装置，包括检测该设备的蒸发器-冷凝器的蒸浴中的氧化亚氮量的变化的装置。
8.按权利要求7的装置，蒸发器-冷凝器设置在双塔的低压塔的罐中。
9.按照权利要求7和8的任一个的装置，其中用于检测所述变化的装置包括红外辐射分析仪。
10.按照权利要求7、8和9之一的装置，其中用于检测所述变化的装置能够测量蒸发器-冷凝器的蒸浴中的氧化亚氮量。
11.空气分离设备，包括按照权利要求7至10之一的装置。
CN96102125A 1995-02-07 1996-02-06 监测空气分离设备的操作的方法及装置 Expired - Fee Related CN1077287C (zh)

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CN100491874C (zh) * 2007-05-24 2009-05-27 武汉钢铁(集团)公司 一种去除大型制氧机中氧化亚氮聚集的方法
TWI699503B (zh) * 2019-06-28 2020-07-21 中國鋼鐵股份有限公司 薄膜式冷凝器液氣比監測系統及監測方法

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JP4624336B2 (ja) * 2006-11-20 2011-02-02 鹿島石油株式会社 深冷分離設備内に蓄積したＮＯｘ化合物の検出方法
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TWI699503B (zh) * 2019-06-28 2020-07-21 中國鋼鐵股份有限公司 薄膜式冷凝器液氣比監測系統及監測方法

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CN1077287C (zh) 2002-01-02
EP0726434A1 (fr) 1996-08-14
EP0726434B1 (fr) 1999-10-27
ZA96938B (en) 1996-07-30
DE69604841D1 (de) 1999-12-02
ES2140038T5 (es) 2004-07-01
JPH08303947A (ja) 1996-11-22
US5629208A (en) 1997-05-13
AU705899B2 (en) 1999-06-03
KR100395315B1 (ko) 2003-11-17
EP0726434B2 (fr) 2003-10-22
DE69604841T3 (de) 2004-07-08
FR2730172A1 (fr) 1996-08-09
ES2140038T3 (es) 2000-02-16
AU4336796A (en) 1996-08-15
CA2168931A1 (fr) 1996-08-08
FR2730172B1 (fr) 1997-03-21
BR9600322A (pt) 1997-12-23
JP2875502B2 (ja) 1999-03-31
CA2168931C (fr) 2007-04-17
KR960030970A (ko) 1996-09-17
DE69604841T2 (de) 2000-05-25

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