JPH0552468A - Method and device for collecting high purity liquefied nitrogen - Google Patents
Method and device for collecting high purity liquefied nitrogenInfo
- Publication number
- JPH0552468A JPH0552468A JP40603390A JP40603390A JPH0552468A JP H0552468 A JPH0552468 A JP H0552468A JP 40603390 A JP40603390 A JP 40603390A JP 40603390 A JP40603390 A JP 40603390A JP H0552468 A JPH0552468 A JP H0552468A
- Authority
- JP
- Japan
- Prior art keywords
- liquefied nitrogen
- liquefied
- nitrogen
- column
- purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- F25J3/04406—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 using a dual pressure main column system
- F25J3/04412—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 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
-
- 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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
- F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
- F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
-
- 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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
-
- 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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04733—Producing pure argon, e.g. recovered from a crude argon column using a hybrid system, e.g. using adsorption, permeation or catalytic reaction
- F25J3/04739—Producing pure argon, e.g. recovered from a crude argon column using a hybrid system, e.g. using adsorption, permeation or catalytic reaction in combination with an auxiliary pure argon column
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高純度液化窒素の採取
方法及び装置に関し、詳しくは、精留塔及び高純アルゴ
ン塔を備えた空気液化分離装置を用いて高純度液化窒素
を採取する方法及び装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for collecting high-purity liquefied nitrogen, and more specifically, it collects high-purity liquefied nitrogen using an air liquefaction separation apparatus equipped with a rectification column and a high-purity argon column. A method and apparatus.
【０００２】[0002]
【従来の技術】液化窒素を多く使用する半導体工業等の
発展に伴い、従来から液化窒素中に含まれる水素等の低
沸点成分の含有量を、例えば０．１ppm 以下に低減する
空気液化分離装置が各種開発されてきている。これらの
高純度液化窒素採取用の空気液化分離装置は、精留塔に
液化窒素精製用の設備を付加したり、精留塔で液化精留
分離して得た液化窒素を精留塔とは別に設けた精製設備
に導入していた。2. Description of the Related Art With the development of the semiconductor industry that uses a large amount of liquefied nitrogen, an air liquefaction separation apparatus for reducing the content of low-boiling components such as hydrogen contained in liquefied nitrogen to 0.1 ppm or less. Have been developed. These air-liquefaction separation devices for collecting high-purity liquefied nitrogen are equipped with equipment for refining liquefied nitrogen in the rectification tower, and liquefied nitrogen obtained by liquefaction rectification separation in the rectification tower is called a rectification tower. It was installed in a separate refining facility.
【０００３】一方、空気液化分離装置として、高純アル
ゴンを採取する設備を備えたものが知られている。図２
は前記高純アルゴンの採取設備を備えた空気液化分離装
置における窒素採取のための主要な系統を示すもので、
他の系統は省略してある。On the other hand, as an air liquefaction / separation device, there is known one having a facility for collecting high-purity argon. Figure 2
Shows a main system for nitrogen collection in an air liquefaction separation device equipped with the above-mentioned high-purity argon collection facility,
The other lines are omitted.
【０００４】図２において、図示しない前処理設備で圧
縮，精製，冷却されて複精留塔１の下部塔１ａ下部に導
入された原料空気は、該下部塔１ａにおける精留操作に
より塔下部の酸素富化液化空気と塔頂部の窒素ガスとに
分離する。下部塔１ａ下部の酸素富化液化空気は、導管
２から過冷器３，粗アルゴン塔４の凝縮蒸発器４ａを経
て上部塔１ｂに導入される。また、下部塔１ａ頂部の窒
素ガスは、主凝縮器５で液化され、過冷器３で過冷状態
に冷却された後、三つの流れに分岐する。In FIG. 2, raw material air that has been compressed, purified, and cooled by a pretreatment facility (not shown) and introduced into the lower part of the lower column 1a of the double rectification column 1 is rectified in the lower column 1a, and the raw material air Oxygen-enriched liquefied air and nitrogen gas at the top of the column are separated. The oxygen-enriched liquefied air in the lower part of the lower tower 1a is introduced from the conduit 2 into the upper tower 1b through the subcooler 3 and the condensation evaporator 4a of the crude argon tower 4. Further, the nitrogen gas at the top of the lower tower 1a is liquefied in the main condenser 5, cooled in a supercooled state in the subcooler 3, and then branched into three streams.
【０００５】上記液化窒素の第１の流れは導管６，弁６
ａを介して製品液化窒素として採取され、第２の流れは
導管７，弁７ａを介して高純アルゴン塔８の凝縮蒸発器
８ａに導入され、また、第３の流れは導管９，弁９ａを
介して上部塔１ｂ頂部に導入される。The first stream of the liquefied nitrogen is the conduit 6 and the valve 6
The second stream is taken as the product liquefied nitrogen via a, is introduced into the condenser evaporator 8a of the high purity argon column 8 via the conduit 7 and the valve 7a, and the third stream is carried through the conduit 9 and the valve 9a. Is introduced at the top of the upper tower 1b.
【０００６】高純アルゴン塔８の凝縮蒸発器８ａに導入
された液化窒素は、その全量がアルゴンと熱交換して蒸
発し、導管１０から導出される。また、上部塔１ｂ頂部
に導入された液化窒素は上部塔１ｂの還流液となり、該
上部塔１ｂで精留分離した窒素ガスは導管１１に導出さ
れる。The entire amount of liquefied nitrogen introduced into the condenser evaporator 8a of the high purity argon column 8 is heat-exchanged with argon to evaporate and is discharged from the conduit 10. The liquefied nitrogen introduced into the top of the upper tower 1b becomes the reflux liquid of the upper tower 1b, and the nitrogen gas rectified and separated in the upper tower 1b is led to the conduit 11.
【０００７】[0007]
【発明が解決しようとする課題】上記図２に示した窒素
採取系統を有する空気液化分離装置においては、原料空
気中に含まれる水素等の低沸点成分が、窒素と共に下部
塔１ａ頂部に分離し、さらに主凝縮器５で液化される液
化窒素中に濃縮されるため、低沸点成分を含まない高純
度な製品液化窒素を採取することができなかった。In the air liquefaction separation apparatus having the nitrogen collection system shown in FIG. 2, the low boiling point components such as hydrogen contained in the feed air are separated into the top of the lower column 1a together with nitrogen. Further, since it is concentrated in the liquefied nitrogen that is liquefied in the main condenser 5, it is not possible to collect high-purity product liquefied nitrogen that does not contain low boiling point components.
【０００８】従来、このような空気液化分離装置で高純
度窒素を採取する場合には、前述のように、精留塔に液
化窒素精製用の設備、例えば液化窒素を炊き上げるため
の熱交換器，気液分離器及び関連の配管，弁等を追加し
ていたため、大幅な装置の改造が必要であった。Conventionally, when high-purity nitrogen is collected by such an air liquefaction / separation apparatus, as described above, equipment for refining liquefied nitrogen in a rectification tower, for example, a heat exchanger for heating liquefied nitrogen. Since a gas-liquid separator and related pipes and valves were added, it was necessary to remodel the equipment drastically.
【０００９】そこで本発明は、上述の高純アルゴンを採
取する設備を備えた空気液化分離装置において、最小の
設備の変更で容易に高純度液化窒素を採取することがで
きる方法及び装置を提供することを目的としている。Therefore, the present invention provides a method and an apparatus for easily collecting high-purity liquefied nitrogen in the air liquefaction separation apparatus equipped with the above-mentioned equipment for collecting high-purity argon, with a minimum change in equipment. The purpose is to
【００１０】[0010]
【課題を解決するための手段】上記した目的を達成する
ため、本発明の高純度液化窒素の採取方法は、精留塔及
び高純アルゴン塔を備えた空気液化分離装置に原料空気
を導入して液化窒素を採取する方法において、前記精留
塔にて液化精留分離した液化窒素を、前記高純アルゴン
塔の凝縮蒸発器に寒冷源として供給し、該凝縮蒸発器で
前記液化窒素の一部を蒸発させて導出するとともに、未
蒸発の液化窒素を製品として採取することを特徴として
いる。In order to achieve the above-mentioned object, a method for collecting high-purity liquefied nitrogen according to the present invention comprises introducing raw material air into an air liquefaction / separation apparatus equipped with a rectification column and a high-purity argon column. In the method of collecting liquefied nitrogen by liquefaction, the liquefied nitrogen separated by liquefaction and rectification in the rectification tower is supplied to the condensation evaporator of the high-purity argon column as a cold source, and one of the liquefied nitrogen is condensed by the condensation evaporator. It is characterized in that the part is evaporated and led out, and unvaporized liquefied nitrogen is collected as a product.
【００１１】また、本発明の高純度液化窒素の採取装置
は、精留塔及び高純アルゴン塔を備えた空気液化分離装
置からなる液化窒素の採取装置において、前記高純アル
ゴン塔の凝縮蒸発器に、前記精留塔にて液化精留分離し
た液化窒素を導入する液化窒素導入系統と、該凝縮蒸発
器で蒸発したガスを導出するガス導出系統と、該凝縮蒸
発器内の未蒸発の液化窒素を製品として採取する製品液
化窒素採取系統とを設けたことを特徴としている。Further, the high-purity liquefied nitrogen sampling device of the present invention is a liquefied nitrogen sampling device comprising an air liquefaction separation device equipped with a rectification column and a high-purity argon column. , A liquefied nitrogen introduction system for introducing the liquefied nitrogen separated by liquefaction and rectification in the rectification column, a gas derivation system for deriving the gas evaporated in the condensing evaporator, and an unevaporated liquefaction in the condensing evaporator A product liquefied nitrogen sampling system for sampling nitrogen as a product is provided.
【００１２】[0012]
【作 用】上記構成によれば、高純アルゴン塔の凝縮蒸
発器に寒冷源として導入された液化窒素は、その一部が
蒸発する際に、含有する低沸点成分のほとんどを同伴し
て蒸発する。従って、未蒸発の液化窒素中には極微量の
低沸点成分しか残存せず、該未蒸発の液化窒素を採取す
れば、容易に製品高純度液化窒素が得られる。[Operation] According to the above configuration, the liquefied nitrogen introduced as a cold source into the condenser evaporator of the high-purity argon column is vaporized by entraining most of the low-boiling components contained in it when part of it is vaporized. To do. Therefore, only a trace amount of the low boiling point component remains in the non-evaporated liquefied nitrogen, and if the non-evaporated liquefied nitrogen is collected, product high-purity liquefied nitrogen can be easily obtained.
【００１３】また、従来の液化窒素採取装置に比べて、
液化窒素の採取系統を高純アルゴン塔の凝縮蒸発器部分
に接続するだけで良いため、熱交換器，気液分離器等を
付加する必要がない。Further, compared with the conventional liquefied nitrogen sampling device,
Since it is only necessary to connect the liquefied nitrogen sampling system to the condenser evaporator part of the high-purity argon column, it is not necessary to add a heat exchanger, a gas-liquid separator or the like.
【００１４】[0014]
【実施例】以下、本発明の一実施例を図面に基づいて説
明する。図１は、本発明を適用した空気液化分離装置の
一実施例を示す系統図であり、前記図２と同様に、窒素
を採取するための主要な系統のみを示し、他の系統、例
えば酸素採取系統，アルゴン採取系統，排ガス系統等は
省略してある。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a system diagram showing an embodiment of an air liquefaction separation device to which the present invention is applied. As in the case of FIG. 2, only a main system for sampling nitrogen is shown, and another system such as oxygen is shown. The sampling system, argon sampling system, exhaust gas system, etc. are omitted.
【００１５】原料空気は、従来と同様に前処理設備で圧
縮，精製，冷却されて複精留塔２１の下部塔２１ａ下部
に導入され，該下部塔２１ａにおける精留操作により、
塔下部の酸素富化液化空気と塔頂部の窒素ガスとに分離
する。下部塔２１ａ下部の酸素富化液化空気は、導管２
２から過冷器２３，粗アルゴン塔２４の凝縮蒸発器２４
ａを経て上部塔２１ｂに導入される。一方、下部塔２１
ａ頂部の窒素ガスは、主凝縮器２５で液化され、過冷器
２３で過冷状態に冷却された後、二つの流れに分岐す
る。The raw material air is compressed, purified, and cooled in a pretreatment facility in the same manner as in the prior art, and introduced into the lower part of the lower column 21a of the double rectification column 21. By the rectification operation in the lower column 21a,
Separated into oxygen-enriched liquefied air at the bottom of the column and nitrogen gas at the top of the column. The oxygen-enriched liquefied air in the lower part of the lower tower 21a is
2 to supercooler 23, condenser evaporator 24 of crude argon column 24
It is introduced into the upper tower 21b via a. On the other hand, the lower tower 21
The nitrogen gas at the top of a is liquefied in the main condenser 25, cooled to a supercooled state in the subcooler 23, and then branched into two streams.
【００１６】上記液化窒素の第１の流れは、導管２６，
弁２６ａ（液化窒素導入系統）を介して高純アルゴン塔
２７の凝縮蒸発器２７ａに導入され、また、液化窒素の
第２の流れは導管２８，弁２８ａを介して上部塔２１ｂ
の頂部に導入される。高純アルゴン塔２７の凝縮蒸発器
２７ａに導入された液化窒素は、該高純アルゴン塔２７
内のアルゴンガスを凝縮液化させるための寒冷源とな
り、その一部がアルゴンガスとの熱交換により蒸発して
窒素ガスとなり、導管２９（ガス導出系統）から導出さ
れ、弁３０，導管３１，前記過冷器２３を経て製品窒素
ガスとして採取され、あるいは排ガスとして排出され
る。The first stream of liquefied nitrogen is a conduit 26,
It is introduced into the condenser / evaporator 27a of the high purity argon column 27 via the valve 26a (liquefied nitrogen introduction system), and the second stream of liquefied nitrogen is passed through the conduit 28 and the valve 28a to the upper column 21b.
Introduced at the top of. The liquefied nitrogen introduced into the condenser evaporator 27a of the high purity argon column 27 is
It becomes a cold source for condensing and liquefying the argon gas in the inside, and a part of it evaporates by heat exchange with the argon gas to become nitrogen gas, which is led out from the conduit 29 (gas outlet system), and the valve 30, the conduit 31, and the It is taken as product nitrogen gas through the subcooler 23 or discharged as exhaust gas.
【００１７】また、上部塔２１ｂ頂部に還流液として導
入された液化窒素は、前記酸素富化液化空気と共に精留
されて塔底部の酸素と塔頂部の窒素ガスとに分離し、塔
頂部の窒素ガスは、導管３２から導出され、前記導管３
１の窒素ガスに合流する。The liquefied nitrogen introduced into the top of the upper tower 21b as a reflux liquid is rectified together with the oxygen-enriched liquefied air to separate it into oxygen at the bottom of the tower and nitrogen gas at the top of the tower. Gas is drawn from conduit 32, said conduit 3
Combine with 1 nitrogen gas.
【００１８】そして、前記高純アルゴン塔２７の凝縮蒸
発器２７ａにおいては、該凝縮蒸発器２７ａの炊き上げ
効果により、液化窒素中に含まれている水素等の低沸点
成分のほとんどが蒸発し、前記導管２９から窒素ガスと
共に抜き出される。このため、凝縮蒸発器２７ａ中の未
蒸発の液化窒素は、極微量の低沸点成分しか含まない高
純度なものとなる。In the condensation evaporator 27a of the high-purity argon column 27, most of low-boiling components such as hydrogen contained in the liquefied nitrogen are evaporated due to the heating effect of the condensation evaporator 27a. It is withdrawn from the conduit 29 together with nitrogen gas. Therefore, the unvaporized liquefied nitrogen in the condenser-evaporator 27a becomes a high-purity liquid containing only a trace amount of the low boiling point component.
【００１９】このようにして高純度となった液化窒素
は、凝縮蒸発器２７ａに設けられた製品採取用の導管３
３，弁３３ａ（製品液化窒素採取系統）から製品高純度
液化窒素として採取される。従って、従来、過冷器２３
から液化窒素を導出する導管部分で分岐していた製品液
化窒素採取用の導管を、高純アルゴン塔２７の凝縮蒸発
器２７ａ部分に接続するだけで高純度液化窒素を採取す
ることが可能となる。即ち、製品液化窒素採取用の導管
の接続位置を変更するだけで良く、新たな機器や配管系
統を追加しないで高純度な液化窒素を得ることができ
る。The liquefied nitrogen thus highly purified is provided in the condenser / evaporator 27a and is a conduit 3 for collecting products.
3, the high-purity liquefied nitrogen product is sampled from the valve 33a (product liquefied nitrogen sampling system). Therefore, conventionally, the subcooler 23
It is possible to collect high-purity liquefied nitrogen simply by connecting the product liquefied nitrogen collecting conduit that has been branched at the conduit part for discharging liquefied nitrogen from the product to the condensing evaporator 27a part of the high-purity argon column 27. .. That is, it suffices to change the connection position of the conduit for collecting product liquefied nitrogen, and highly purified liquefied nitrogen can be obtained without adding a new device or piping system.
【００２０】ここで、上記実施例装置と従来装置におい
て、得られる製品液化窒素中の低沸点成分（水素）の含
有量を比較した結果を説明する。共通の設定条件は、下
部塔２１ａに導入される原料空気量が２５０００Ｎｍ3
／ｈ，水素含有量が１ppm ，下部塔２１ａの運転圧力が
４．９kg／cm2 Ｇ，過冷器２３出口の液化窒素の流量が
１００００Ｎｍ3 ／ｈ，温度が−１９０℃，高純アルゴ
ン塔２７の運転圧力が０．５kg／cm2 Ｇ，凝縮蒸発器２
７ａの運転圧力が０．９kg／cm2 Ｇで導入する液化窒素
量が６６０Ｎｍ3 ／ｈ，上部塔２１ｂ頂部圧力が０．２
３kg／cm2 Ｇであり、製品液化窒素の採取量は４００Ｎ
ｍ3 ／ｈとした。Here, the results of comparing the contents of the low boiling point component (hydrogen) in the product liquefied nitrogen obtained by the apparatus of the above-mentioned embodiment and the conventional apparatus will be explained. The common setting condition is that the amount of raw material air introduced into the lower tower 21a is 25,000 Nm 3.
/ H, the hydrogen content is 1 ppm, the operating pressure of the lower column 21a is 4.9 kg / cm 2 G, the flow rate of liquefied nitrogen at the outlet of the subcooler 23 is 10000 Nm 3 / h, the temperature is -190 ° C, and the high purity argon column is 27 operating pressure is 0.5 kg / cm 2 G, condensation evaporator 2
The operating pressure of 7a is 0.9 kg / cm 2 G, the amount of liquefied nitrogen introduced is 660 Nm 3 / h, and the top pressure of the upper column 21b is 0.2.
3 kg / cm 2 G, the amount of product liquefied nitrogen collected is 400 N
It was set to m 3 / h.
【００２１】その結果、図１に示す実施例装置から得ら
れた液化窒素中の水素濃度は０．０４３ppm であり、図
２に示す構成の従来装置から得られた、液化窒素中の水
素濃度は２．５ppm であった。また、図２に示す装置構
成において、過冷器３から液化窒素を導出する導管に気
液分離器を設置し、該気液分離器に液化窒素を２．２６
kg／cm2 Ｇに降圧してフラッシュさせ、水素等の低沸点
成分を多く含んでいるフラッシュガス４１１Ｎｍ3 ／ｈ
を抜き出し、低沸点成分が減少した液化窒素９５８９Ｎ
ｍ3 ／ｈを採取した場合は、水素濃度が０．２９ppm に
なった。As a result, the hydrogen concentration in the liquefied nitrogen obtained from the apparatus shown in FIG. 1 was 0.043 ppm, and the hydrogen concentration in the liquefied nitrogen obtained from the conventional apparatus having the configuration shown in FIG. It was 2.5 ppm. Further, in the apparatus configuration shown in FIG. 2, a gas-liquid separator is installed in the conduit for discharging the liquefied nitrogen from the subcooler 3, and the liquefied nitrogen is 2.26 in the gas-liquid separator.
Flash gas 411 Nm 3 / h containing a large amount of low-boiling point components such as hydrogen after reducing the pressure to kg / cm 2 G and flushing
Liquefied nitrogen 9589N with reduced low boiling point components
When m 3 / h was sampled, the hydrogen concentration was 0.29 ppm.
【００２２】上記結果から明らかなように、製品液化窒
素の採取系統を高純アルゴン塔２７の凝縮蒸発器２７ａ
部分に変更するだけで、水素濃度０．１ppm以下の高純
度液化窒素を得ることが可能となり、従来装置を僅かに
変更するだけで高純度液化窒素を採取することができ
る。As is clear from the above results, the product liquefied nitrogen sampling system is connected to the condenser evaporator 27a of the high purity argon column 27.
It is possible to obtain high-purity liquefied nitrogen having a hydrogen concentration of 0.1 ppm or less simply by changing to a part, and it is possible to collect high-purity liquefied nitrogen by slightly changing the conventional apparatus.
【００２３】尚、前記したように、製品液化窒素を採取
する以外の系統は、従来から周知の空気液化分離装置と
同様に構成でき、原料空気量や製品の種類に応じて適宜
最適な装置構成にすることができる。また、液化窒素の
供給系統は、下部塔頂部からのみならず、貯槽に貯留し
てある液化窒素を供給する場合でも良く、さらに、空気
液化分離装置が複数基ある場合に、一つの精留塔から採
取した液化窒素を他の空気液化分離装置の高純アルゴン
塔凝縮蒸発器に導入する場合も本発明の範囲である。As described above, the system other than the one for collecting the product liquefied nitrogen can be constructed in the same manner as the conventionally known air liquefaction separation device, and the optimum device configuration can be selected according to the amount of raw material air and the type of product. Can be The liquefied nitrogen supply system may be used not only from the top of the lower tower but also to supply the liquefied nitrogen stored in the storage tank. Furthermore, when there are multiple air liquefaction separation devices, one rectification tower is used. It is also within the scope of the present invention to introduce the liquefied nitrogen collected from the above into the high-purity argon column condenser evaporator of another air liquefaction separation apparatus.
【００２４】[0024]
【発明の効果】以上説明したように、本発明によれば、
製品液化窒素の採取系統を僅かに変更するだけで高純度
液化窒素を得ることができる。即ち、熱交換器や気液分
離器，配管，弁等の設備，機器を追加することなく最近
の高純度指向に対応できる高純度液化窒素の製造が可能
となった。As described above, according to the present invention,
High-purity liquefied nitrogen can be obtained by only slightly changing the product liquefied nitrogen sampling system. That is, it has become possible to produce high-purity liquefied nitrogen that can be used in recent high-purity orientations without adding equipment and devices such as a heat exchanger, a gas-liquid separator, piping, and valves.
【図１】 本発明の一実施例を示す系統図である。FIG. 1 is a system diagram showing an embodiment of the present invention.
【図２】 従来の空気液化分離装置の一例を示す系統図
である。FIG. 2 is a system diagram showing an example of a conventional air liquefaction separation device.
２１…複精留塔 ２３…過冷器 ２４…粗アルゴン
塔 ２５…主凝縮器 ２７…高純アルゴン塔 ２７ａ…凝縮蒸発器 ３３
…製品採取用の導管21 ... Double rectification tower 23 ... Supercooler 24 ... Crude argon tower 25 ... Main condenser 27 ... Highly pure argon tower 27a ... Condensation evaporator 33
… Conduit for product collection
Claims (2)
液化分離装置に原料空気を導入して液化窒素を採取する
方法において、前記精留塔にて液化精留分離した液化窒
素を、前記高純アルゴン塔の凝縮蒸発器に寒冷源として
供給し、該凝縮蒸発器で前記液化窒素の一部を蒸発させ
て導出するとともに、未蒸発の液化窒素を製品として採
取することを特徴とする高純度液化窒素の採取方法。1. A method for introducing liquefied nitrogen by introducing raw material air into an air liquefaction separation apparatus equipped with a rectification column and a high-purity argon column, wherein liquefied nitrogen liquefied and rectified by the rectification column is separated, It is characterized in that it is supplied as a cold source to the condenser evaporator of the high-purity argon column, a part of the liquefied nitrogen is evaporated and led out in the condenser evaporator, and unvaporized liquefied nitrogen is collected as a product. Method for collecting high-purity liquefied nitrogen.
液化分離装置からなる液化窒素の採取装置において、前
記高純アルゴン塔の凝縮蒸発器に、前記精留塔にて液化
精留分離した液化窒素を導入する液化窒素導入系統と、
該凝縮蒸発器で蒸発したガスを導出するガス導出系統
と、該凝縮蒸発器内の未蒸発の液化窒素を製品として採
取する製品液化窒素採取系統とを設けたことを特徴とす
る高純度液化窒素の採取装置。2. A liquefied nitrogen sampling device comprising an air liquefaction separation device equipped with a rectification column and a high-purity argon column, wherein a liquefaction rectification separation is performed in the condensation evaporator of the high-purity argon column in the rectification column. Liquefied nitrogen introduction system for introducing the liquefied nitrogen
High-purity liquefied nitrogen, which is provided with a gas derivation system for deriving the gas evaporated in the condensation evaporator and a product liquefied nitrogen sampling system for collecting unvaporized liquefied nitrogen in the condensation evaporator as a product. Collecting device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP40603390A JP3072563B2 (en) | 1990-12-25 | 1990-12-25 | Method and apparatus for collecting high-purity liquefied nitrogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP40603390A JP3072563B2 (en) | 1990-12-25 | 1990-12-25 | Method and apparatus for collecting high-purity liquefied nitrogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0552468A true JPH0552468A (en) | 1993-03-02 |
| JP3072563B2 JP3072563B2 (en) | 2000-07-31 |
Family
ID=18515661
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP40603390A Expired - Fee Related JP3072563B2 (en) | 1990-12-25 | 1990-12-25 | Method and apparatus for collecting high-purity liquefied nitrogen |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3072563B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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1990
- 1990-12-25 JP JP40603390A patent/JP3072563B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2023129811A (en) * | 2022-03-07 | 2023-09-20 | レール・リキード－ソシエテ・アノニム・プール・レテュード・エ・レクスプロワタシオン・デ・プロセデ・ジョルジュ・クロード | Air separation apparatus |
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| Publication number | Publication date |
|---|---|
| JP3072563B2 (en) | 2000-07-31 |
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