JPH11270965A - Air liquefaction separation device and operation method thereof - Google Patents

Air liquefaction separation device and operation method thereof

Info

Publication number
JPH11270965A
JPH11270965A JP7269298A JP7269298A JPH11270965A JP H11270965 A JPH11270965 A JP H11270965A JP 7269298 A JP7269298 A JP 7269298A JP 7269298 A JP7269298 A JP 7269298A JP H11270965 A JPH11270965 A JP H11270965A
Authority
JP
Japan
Prior art keywords
liquid
reflux liquid
flow rate
reflux
column
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
Application number
JP7269298A
Other languages
Japanese (ja)
Other versions
JP4104726B2 (en
Inventor
Yoshiyuki Masui
義行 桝井
Shigeru Yuzawa
茂 湯沢
Koichi Okamoto
孝一 岡本
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Japan Oxygen Co Ltd
Taiyo Nippon Sanso Corp
Original Assignee
Japan Oxygen Co Ltd
Nippon Sanso Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Japan Oxygen Co Ltd, Nippon Sanso Corp filed Critical Japan Oxygen Co Ltd
Priority to JP7269298A priority Critical patent/JP4104726B2/en
Publication of JPH11270965A publication Critical patent/JPH11270965A/en
Application granted granted Critical
Publication of JP4104726B2 publication Critical patent/JP4104726B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • 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
    • 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
    • F25J3/04642Recovering noble gases from air
    • F25J3/04648Recovering noble gases from air argon
    • F25J3/04654Producing crude argon in a crude argon column
    • F25J3/04666Producing 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
    • F25J3/04672Producing 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
    • F25J3/04678Producing 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • 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
    • 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
    • F25J3/04406Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • 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
    • 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
    • F25J3/04472Processes 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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages
    • F25J3/04478Processes 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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for controlling purposes, e.g. start-up or back-up procedures
    • F25J3/04484Processes 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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for controlling purposes, e.g. start-up or back-up procedures for purity control during steady state operation
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • 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
    • 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
    • F25J3/04793Rectification, e.g. columns; Reboiler-condenser
    • F25J3/048Argon recovery
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • 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
    • F25J2290/00Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62Details of storing a fluid in a tank

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

(57)【要約】 【課題】 増減量操作時の粗アルゴン塔内で生じる還流
比のアンバランスを緩和することにより、製品ガスの純
度変動を最小に抑えながら迅速に増減量操作を行う。 【解決手段】 粗アルゴン塔7に、アルゴン凝縮器5で
生成した還流液を貯溜する液溜6を付設し、該液溜に、
粗アルゴン塔7の還流液を抜出して導く還流液導入径路
71と、液溜6に貯溜された還流液を粗アルゴン塔7に
供給する還流液供給径路72とを設けるとともに、供給
還流液量を調節するための調節弁21Vを設けた。
(57) [Summary] [PROBLEMS] To reduce or reduce the imbalance in the reflux ratio generated in a crude argon column during the operation of increasing and decreasing the amount of gas, thereby quickly performing the operation of increasing and decreasing the amount of purity of the product gas while minimizing the fluctuation. SOLUTION: A crude argon column 7 is provided with a liquid reservoir 6 for storing a reflux liquid generated by an argon condenser 5, and the liquid reservoir is
A reflux liquid introduction path 71 for extracting and guiding the reflux liquid of the crude argon tower 7 and a reflux liquid supply path 72 for supplying the reflux liquid stored in the liquid reservoir 6 to the crude argon tower 7 are provided. A control valve 21V for adjustment was provided.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、空気液化分離装置
及びその運転方法に関し、詳しくは、低温で空気を液化
精留することにより、少なくともアルゴン(粗アルゴン
を含む)を製品として採取する空気液化分離装置であっ
て、製品需要の大幅な変動に迅速に対応することができ
る空気液化分離装置及びその運転方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an air liquefaction / separation apparatus and an operation method thereof, and more particularly, to air liquefaction in which at least argon (including crude argon) is collected as a product by liquefying and rectifying air at a low temperature. The present invention relates to an air liquefaction separation apparatus capable of quickly responding to a large fluctuation in product demand and a method of operating the same.

【0002】[0002]

【従来の技術】酸素,窒素,アルゴンといった工業ガス
の多消費ユーザーである製鉄所や化学工場等において
は、ガスの大幅な需要変動が頻繁に繰り返されることが
多い。これに対応するため、これらの工業ガスの製造設
備である空気液化分離装置には、製品量の大幅な増減に
迅速に対応できる能力が求められている。
2. Description of the Related Art In steel mills and chemical factories, etc., who are consumers of industrial gases such as oxygen, nitrogen, and argon, large demand fluctuations of the gas are frequently repeated. In order to cope with this, an air liquefaction / separation apparatus, which is a facility for producing these industrial gases, is required to have an ability to quickly respond to a large increase or decrease in the amount of products.

【0003】例えば、空気液化分離装置にガスホルダー
や液化ガス貯槽のようなバックアップ設備を付設して製
品ガスを貯留し、需要増大時には、前記バックアップ設
備から製品ガスを補給し、需要減少時には、余剰の製品
ガスをバックアップ設備に貯留するようにしている。し
かし、製品ガスの大幅需要変動に対応するためには、大
型のバックアップ設備を必要とし、需要減少時にバック
アップ設備の貯留能力を超えた場合には、装置のターン
ダウンや製品ガスの放風を行わなければならなかった。
For example, a backup device such as a gas holder or a liquefied gas storage tank is attached to an air liquefaction / separation device to store product gas, and when demand increases, product gas is supplied from the backup device. Product gas is stored in a backup facility. However, large backup equipment is required to cope with large fluctuations in product gas demand, and if the storage capacity of the backup equipment is exceeded when demand decreases, equipment is turned down and product gas is blown off. I had to.

【0004】また、前記ガスホルダー方式においては、
需要増の際にも製品ガスの供給圧力を確保するため、製
品圧縮機の吐出圧力を製品の送ガスに必要な圧力よりも
遥かに高い圧力に設定して運転するため、動力の無駄が
大きいという問題点がある。一方、製品ガスを液化して
貯留する方式では、製品ガスを液化する際に多大な動力
を要するという問題がある。さらに、製品ガスの放風
は、過剰な生産を意味し、明らかに無駄な動力を消費し
ていることになる。
[0004] In the gas holder system,
In order to secure the supply pressure of the product gas even when the demand increases, the operation is performed by setting the discharge pressure of the product compressor to a pressure much higher than the pressure required for the product gas supply, so there is a large waste of power. There is a problem. On the other hand, the method of liquefying and storing the product gas has a problem that a large amount of power is required for liquefying the product gas. Furthermore, the blowing of product gas means excessive production, which obviously consumes wasted power.

【0005】[0005]

【発明が解決しようとする課題】したがって、空気液化
分離装置自身の能力として、需要の増減量に合わせて製
品ガスの生産量を迅速に増減量できることが要求される
が、製品ガスの生産量を急激に増減量すると、製品純度
が変動する不都合がある。
Therefore, the capability of the air liquefaction / separation apparatus itself is required to be able to rapidly increase or decrease the production amount of product gas in accordance with the increase or decrease in demand. If the amount is rapidly increased or decreased, there is a disadvantage that the purity of the product fluctuates.

【0006】すなわち、蒸留塔の増減量操作を行う場
合、上昇ガスの流量変化は、遅れが殆ど無いのに対し、
還流液の流量は、時間的な遅れを伴って変化するため、
蒸留塔の負荷を変更する場合には、還流液量を上昇ガス
量より早く変化させるように制御系を設定するなどして
このアンバランスを緩和し、製品純度の変動を抑えるよ
うにしている。
That is, when the amount of increase or decrease of the distillation column is performed, the change in the flow rate of the ascending gas has almost no delay.
Since the flow rate of the reflux liquid changes with time delay,
When the load of the distillation column is changed, a control system is set so that the amount of the reflux liquid is changed earlier than the amount of the ascending gas.

【0007】しかし、製品ガスとしてアルゴンを生産す
る装置に設けられた粗アルゴン塔においては、上昇ガス
の流量と還流液の流量とが、塔頂部に設けた粗アルゴン
凝縮器で一意的に制御されているため、液量の変更とガ
ス量の変更とに時間差を設けることができず、例えば、
原料空気量比で毎分3%といった迅速な操業変更を行う
と、製品アルゴンの純度が損なわれたり、純度が大きく
変動したりするため、粗アルゴン塔の操業変更を迅速に
行うことはできなかった。特に、規則充填物を使用した
粗アルゴン塔は、棚段式のものに比べてより顕著に純度
変動等を生じるため、増減量操作の迅速化にとって大き
な制限となっている。
However, in a crude argon column provided in an apparatus for producing argon as a product gas, the flow rate of the rising gas and the flow rate of the reflux liquid are uniquely controlled by a crude argon condenser provided at the top of the column. Therefore, it is not possible to provide a time difference between the change of the liquid amount and the change of the gas amount, for example,
If a rapid operation change such as 3% per minute in the raw material air ratio is performed, the purity of the product argon is impaired or the purity fluctuates greatly, so that the operation change of the crude argon column cannot be quickly performed. Was. In particular, a crude argon column using an ordered packing causes a remarkable fluctuation in purity or the like as compared with a tray-type column, and this is a great limitation for speeding up the operation of increasing or decreasing the amount.

【0008】そこで本発明は、増減量操作時の粗アルゴ
ン塔内で生じる還流比のアンバランスを緩和することに
より、製品アルゴンをはじめとする各種製品ガスの純度
変動を最小に抑えながら迅速に増減量操作を行うことが
できる空気液化分離装置及びその運転方法を提供するこ
とを目的としている。
[0008] Accordingly, the present invention reduces the unbalance of the reflux ratio generated in the crude argon column during the operation of increasing or decreasing the amount, thereby rapidly changing the purity of various product gases including the product argon while minimizing the fluctuation. An object of the present invention is to provide an air liquefaction / separation apparatus capable of performing a volume operation and a method of operating the same.

【0009】[0009]

【課題を解決するための手段】上記目的を達成するた
め、本発明の空気液化分離装置及びその運転方法は、下
部塔,上部塔及び主凝縮蒸発器を有する複精留塔と、液
化空気を液化寒冷源とするアルゴン凝縮器を塔頂部に有
する粗アルゴン塔とを備え、圧縮,精製,冷却した原料
空気を液化精留することにより、製品として少なくとも
アルゴンを採取する空気液化分離装置において、前記粗
アルゴン塔に、該粗アルゴン塔の還流液を貯溜する液溜
を付設し、該液溜に前記粗アルゴン塔の還流液を導く還
流液導入径路と、該液溜に貯溜された還流液を前記粗ア
ルゴン塔に供給する還流液供給径路とを設けるととも
に、前記還流液導入径路及び還流液供給径路の少なくと
もいずれか一方に、該経路を流れる還流液の流量を調節
する流量調節手段を備えたことを特徴としている。
In order to achieve the above object, the present invention provides an air liquefaction / separation apparatus and a method for operating the same, comprising: a double rectification column having a lower tower, an upper tower and a main condensing evaporator; A crude argon column having an argon condenser as a liquefaction cold source at the top of the column, wherein the compressed, purified, and cooled raw material air is liquefied and rectified to obtain at least argon as a product in the air liquefaction separation device. The crude argon column is provided with a liquid reservoir for storing the reflux liquid of the crude argon column, and a reflux liquid introduction path for guiding the reflux liquid of the crude argon column to the liquid reservoir, and a reflux liquid stored in the liquid reservoir. A reflux liquid supply path for supplying the crude argon column is provided, and at least one of the reflux liquid introduction path and the reflux liquid supply path is provided with a flow control means for controlling a flow rate of the reflux liquid flowing through the path. It is characterized in that was.

【0010】さらに、本発明の空気液化分離装置は、前
記還流液供給径路に流量検出手段と流量制御手段とを備
えたことを特徴とし、前記液溜に液面検出手段を設ける
とともに、前記還流液導入径路又は前記還流液供給径路
に前記液面検出手段からの信号によって液溜の液面を制
御する液面制御手段とを備えたことを特徴とし、前記液
溜を、前記アルゴン凝縮器と前記粗アルゴン塔の頂部と
を連結する液化アルゴン径路の途中に設けたことを特徴
としている。
Further, the air liquefaction / separation apparatus of the present invention is characterized in that a flow rate detecting means and a flow rate controlling means are provided in the reflux liquid supply path. Liquid level control means for controlling the liquid level of the liquid reservoir by a signal from the liquid level detection means in the liquid introduction path or the reflux liquid supply path, characterized in that the liquid reservoir, the argon condenser and It is characterized in that it is provided in the middle of a liquefied argon path connecting the top of the crude argon column.

【0011】また、本発明の空気液化分離装置の運転方
法は、上記構成の空気液化分離装置の運転方法であっ
て、前記粗アルゴン塔の還流液の少なくとも一部を前記
液溜に貯溜し、該貯溜された還流液を、装置の運転状態
に応じた流量で前記粗アルゴン塔に供給することを特徴
としている。さらに、本発明の空気液化分離装置の運転
方法は、装置が一定の状態で運転されているときの前記
還流液の流量は、前記液溜から粗アルゴン塔に供給する
還流液の流量が一定になるように行うか、あるいは、前
記液溜の液面が一定になるように制御することを特徴と
し、装置が増量運転又は減量運転に移行する際における
前記還流液の流量の増減速度は、前記アルゴン凝縮器の
寒冷源となる液化空気の流量の増減速度よりも早くする
ことを特徴としている。
The method for operating an air liquefaction / separation apparatus according to the present invention is the method for operating an air liquefaction / separation apparatus having the above structure, wherein at least a part of the reflux liquid of the crude argon column is stored in the liquid storage, The stored reflux liquid is supplied to the crude argon column at a flow rate according to the operation state of the apparatus. Further, in the method for operating the air liquefaction / separation apparatus of the present invention, the flow rate of the reflux liquid when the apparatus is operated in a constant state is such that the flow rate of the reflux liquid supplied to the crude argon column from the liquid reservoir is constant. Or so that the liquid level of the liquid reservoir is controlled to be constant, the rate of increase or decrease of the flow rate of the reflux liquid when the apparatus shifts to the increasing operation or the decreasing operation, It is characterized in that the flow rate of the liquefied air serving as a cold source of the argon condenser is increased or decreased more rapidly.

【0012】[0012]

【発明の実施の形態】図1は、本発明の空気液化分離装
置の一形態例を示す系統図である。この空気液化分離装
置は、製品として粗アルゴンガス(RAr),酸素ガス
(GO),窒素ガス(GN)を生産するものであっ
て、下部塔1,上部塔2及び主凝縮蒸発器3を有する複
精留塔4と、アルゴン凝縮器5及び液溜6を有する粗ア
ルゴン塔7と、各種ガスや液を熱交換させるための主熱
交換器8及び過冷器9と、装置を所定の運転状態に制御
するための各種制御手段とにより形成されている。
FIG. 1 is a system diagram showing an embodiment of an air liquefaction / separation apparatus according to the present invention. This air liquefaction / separation apparatus produces crude argon gas (RAr), oxygen gas (GO 2 ), and nitrogen gas (GN 2 ) as products, and comprises a lower tower 1, an upper tower 2 and a main condensing evaporator 3 A double rectification column 4 having a gas turbine, a crude argon column 7 having an argon condenser 5 and a liquid reservoir 6, a main heat exchanger 8 and a supercooler 9 for exchanging heat of various gases and liquids, and a predetermined device And various control means for controlling the operation state.

【0013】図示しない圧縮機で所定圧力に圧縮され、
精製設備で精製された原料空気(AIR)は、流量指示
調節計(FIC)11により制御される調節弁11Vを
通って主熱交換器8に流入し、複精留塔4等から導出さ
れた各種低温ガスと熱交換を行って所定温度に冷却され
た後、経路51を通って前記下部塔1の下部に導入され
る。
Compressed by a compressor (not shown) to a predetermined pressure,
The raw material air (AIR) purified by the purification equipment flows into the main heat exchanger 8 through a control valve 11V controlled by a flow rate controller (FIC) 11, and is extracted from the double rectification column 4 and the like. After being cooled to a predetermined temperature by performing heat exchange with various low-temperature gases, it is introduced into the lower part of the lower tower 1 through a path 51.

【0014】下部塔1に導入された原料空気は、塔内で
の精留操作によって塔頂部の窒素ガスと塔底部の酸素富
化液化空気とに分離する。塔頂部の窒素ガスは、経路5
2を経て前記主凝縮蒸発器3に導入され、上部塔底部の
液化酸素と熱交換を行って液化し、その一部が経路53
に分岐する他は、経路54を経て下部塔1の頂部に戻さ
れ、下部塔1の還流液となる。一方、前記経路53に分
岐した液化窒素は、過冷器9で冷却された後、流量調節
計(FC)12で調節される調節弁12Vを通り、経路
55から上部塔2の頂部に導入されて上部塔2の還流液
となる。
The feed air introduced into the lower tower 1 is separated into a nitrogen gas at the top of the tower and an oxygen-enriched liquefied air at the bottom of the tower by a rectification operation in the tower. The nitrogen gas at the top of the tower
2 and is introduced into the main condensing evaporator 3 and liquefied by heat exchange with liquefied oxygen at the bottom of the upper column.
Is returned to the top of the lower tower 1 via a path 54 and becomes the reflux liquid of the lower tower 1. On the other hand, the liquefied nitrogen branched to the path 53 is cooled by the subcooler 9, passes through a control valve 12 V controlled by a flow controller (FC) 12, and is introduced into the top of the upper tower 2 from a path 55. To become the reflux liquid of the upper tower 2.

【0015】また、下部塔底部の酸素富化液化空気は、
経路56に抜出されて過冷器9で冷却され、下部塔底部
の酸素富化液化空気量(液面高さ)を検出する液面調節
計(LC)13により制御される調節弁13Vを通り、
経路57を通って上部塔2の中段に導入される。さら
に、下部塔1の下段からは、塔内を流下する還流液の一
部である液化空気が経路58に抜出され、過冷器9で冷
却された後、流量指示調節計(FIC)14により制御
される調節弁14Vを通り、前記アルゴン凝縮器5に寒
冷源として導入される。アルゴン凝縮器5でアルゴンを
凝縮させることにより気化した液化空気(空気)は、経
路59を経て上部塔2の中段部に導入される。
The oxygen-enriched liquefied air at the bottom of the lower column is
A control valve 13V controlled by a liquid level controller (LC) 13 for extracting the oxygen-enriched liquefied air amount (liquid level) at the bottom of the lower tower is extracted from the passage 56 and cooled by the supercooler 9. Street,
It is introduced into the middle stage of the upper tower 2 through a path 57. Further, from the lower stage of the lower tower 1, liquefied air, which is a part of the reflux liquid flowing down in the tower, is extracted to a passage 58 and cooled by the subcooler 9, and then the flow rate indicating controller (FIC) 14 Is introduced into the argon condenser 5 as a cold source through a control valve 14V controlled by The liquefied air (air) vaporized by condensing the argon in the argon condenser 5 is introduced into the middle part of the upper tower 2 via the path 59.

【0016】上部塔2に導入された前記経路55からの
液化窒素、前記経路57からの酸素富化液化空気及び経
路59からの空気(気化した液化空気)は、上部塔2で
の精留操作により、塔頂部の窒素ガスと、塔底部の液化
酸素とに分離する。
The liquefied nitrogen introduced into the upper tower 2 from the passage 55, the oxygen-enriched liquefied air from the passage 57, and the air (vaporized liquefied air) from the passage 59 are rectified by the upper tower 2. This separates into nitrogen gas at the top of the column and liquefied oxygen at the bottom of the column.

【0017】塔頂部の窒素ガスは、経路60に抜出さ
れ、過冷器9の寒冷源となった後、主熱交換器8で原料
空気を冷却することにより昇温し、流量調節計(FC)
15により制御される調節弁15Vを通って経路61か
ら製品窒素ガス(GN)として採取される。
The nitrogen gas at the top of the tower is extracted to a passage 60 and becomes a cold source of the subcooler 9. Then, the temperature of the raw material air is increased by cooling the raw air in the main heat exchanger 8, and a flow controller ( FC)
The gas is collected as product nitrogen gas (GN 2 ) from the path 61 through a control valve 15V controlled by the control valve 15.

【0018】また、塔底部の液化酸素は、主凝縮蒸発器
3で前記窒素ガスと熱交換を行うことにより蒸発して酸
素ガスとなり、一部が経路62に抜出され、残部は上部
塔2の上昇ガスとなる。経路62に抜出された酸素ガス
は、主熱交換器8で昇温した後、流量指示調節計(FI
C)16により制御される調節弁16Vを通って経路6
3から製品酸素ガス(GO)として採取される。塔底
部の液化酸素の一部は、経路64に抜出され、過冷器9
を経た後、上部塔底部の液化酸素量(液面高さ)を検出
する液面調節計(LC)17により制御される調節弁1
7Vを通り、経路65から製品液化酸素(LO)ある
いは液化酸素中への炭化水素の濃縮を防止するための保
安液化酸素として抜出される。
The liquefied oxygen at the bottom of the tower is evaporated by performing heat exchange with the nitrogen gas in the main condensing evaporator 3 to become oxygen gas. Gas. After the oxygen gas extracted to the passage 62 is heated in the main heat exchanger 8, the flow rate indicating controller (FI)
C) Path 6 through a control valve 16V controlled by 16
3 is collected as product oxygen gas (GO 2 ). A part of the liquefied oxygen at the bottom of the tower is withdrawn to the passage 64 and
, A control valve 1 controlled by a liquid level controller (LC) 17 for detecting the amount of liquid oxygen (liquid level) at the bottom of the upper tower.
After passing through 7 V, it is withdrawn from the passage 65 as product liquefied oxygen (LO 2 ) or as safe liquefied oxygen to prevent the concentration of hydrocarbons in the liquefied oxygen.

【0019】さらに、上部塔2の中段上部からは、不純
窒素ガスが経路66に抜出され、過冷器9及び主熱交換
器8を経た後、上部塔2の塔頂部の圧力を検出する圧力
調節計(PC)18により制御される調節弁18Vを通
って経路67から廃窒素ガス(RN)として導出され
る。
Further, from the upper middle part of the upper tower 2, the impure nitrogen gas is extracted to the path 66, passes through the subcooler 9 and the main heat exchanger 8, and detects the pressure at the top of the upper tower 2. It is discharged as waste nitrogen gas (RN 2 ) from a passage 67 through a control valve 18V controlled by a pressure controller (PC) 18.

【0020】そして、上部塔1の中段部からは、アルゴ
ンを採取するための原料ガスとなるフィードアルゴンが
経路68に抜出され、流量計(FI)19で流量を検出
されながら粗アルゴン塔7の下部に導入され、粗アルゴ
ン塔7の上昇ガスとなる。粗アルゴン塔7での精留によ
って塔頂部に発生した粗アルゴンガスは、経路69を経
てアルゴン凝縮器5に導入され、前記液化空気との熱交
換によって大部分が液化し、該アルゴン凝縮器5と粗ア
ルゴン塔7の頂部とを連結する液化アルゴン径路70を
形成する還流液導入径路71,前記液溜6,還流液供給
径路72,調節弁21Vを経て粗アルゴン塔7の塔頂部
に導入され、粗アルゴン塔7の還流液となる。この還流
液量を調節する流量調節手段である調節弁21Vは、液
溜6内の液面高さを検出する液面検出手段である液面調
節計(LC)20及び還流液供給径路72を流れる還流
液の流量を検出する流量検出手段である流量指示調節計
(FIC)21によって制御される。また、粗アルゴン
塔7の底部に流下した還流液(酸素富化液)は、経路7
3によって上部塔2に戻される。採取される粗アルゴン
ガス(RAr)は、液溜6の上部から経路74に抜出さ
れ、主熱交換器8で昇温した後、流量指示調節計(FI
C)22により制御される調節弁22Vを通って経路7
5から取出される。
Then, from the middle part of the upper tower 1, feed argon as a raw material gas for collecting argon is extracted to a passage 68, and the flow rate is detected by a flow meter (FI) 19 while the crude argon tower 7 is detected. And becomes a rising gas of the crude argon column 7. The crude argon gas generated at the top of the column by the rectification in the crude argon column 7 is introduced into the argon condenser 5 through a path 69, and is mostly liquefied by heat exchange with the liquefied air. The liquid is introduced into the top of the crude argon column 7 through a reflux liquid introduction path 71 forming a liquefied argon path 70 connecting the top of the crude argon tower 7, the liquid reservoir 6, the reflux liquid supply path 72, and the control valve 21 V. , And becomes a reflux liquid of the crude argon tower 7. The control valve 21V, which is a flow rate adjusting means for adjusting the amount of the reflux liquid, is connected to a liquid level controller (LC) 20, which is a liquid level detecting means for detecting the liquid level in the liquid reservoir 6, and the reflux liquid supply path 72. It is controlled by a flow rate controller (FIC) 21 which is a flow rate detecting means for detecting the flow rate of the flowing reflux liquid. Further, the reflux liquid (oxygen-enriched liquid) flowing down to the bottom of the crude argon column 7 is supplied to the passage 7.
It is returned to the upper tower 2 by 3. The sampled crude argon gas (RAr) is extracted from the upper part of the liquid reservoir 6 to the path 74, and after the temperature is raised in the main heat exchanger 8, the flow rate indicating controller (FI)
C) Path 7 through control valve 22V controlled by 22
Taken out of 5.

【0021】このように、液化アルゴン径路70の途中
に液溜6を設けるとともに、該液溜6から粗アルゴン塔
7に供給する還流液量を制御する流量指示調節計21及
び調節弁21Vを設けたことにより、粗アルゴン塔7の
還流液量を、装置の運転状態に応じて任意に設定するこ
とができる。すなわち、装置の増減量操作における還流
液の変化量を上昇ガスの変化量に先行させて変化させる
ことが可能となるので、塔内での精留操作を適正な状態
に保つことができ、粗アルゴンの純度変動を低減でき
る。さらに、粗アルゴン塔7の運転状態によって影響を
受ける上部塔2等も適正な運転状態に保つことができる
ので、製品酸素ガス等の純度変動も低減でき、各製品ガ
スの純度が、設定された純度以下に低下することがなく
なる。
As described above, the liquid reservoir 6 is provided in the middle of the liquefied argon path 70, and the flow rate indicating controller 21 and the control valve 21V for controlling the amount of reflux liquid supplied from the liquid reservoir 6 to the crude argon column 7 are provided. Accordingly, the amount of the reflux liquid in the crude argon column 7 can be arbitrarily set according to the operation state of the apparatus. That is, since the amount of change in the reflux liquid in the operation of increasing or decreasing the amount of the apparatus can be changed prior to the amount of change in the rising gas, the rectification operation in the column can be maintained in an appropriate state, and Variations in argon purity can be reduced. Furthermore, since the upper tower 2 and the like, which are affected by the operation state of the crude argon column 7, can also be kept in an appropriate operation state, fluctuations in purity of product oxygen gas and the like can be reduced, and the purity of each product gas is set. It does not decrease below the purity.

【0022】このように形成した空気液化分離装置にお
いて、製品ガスの生産量を増減する場合は、あらかじめ
設定されたプログラムに応じて各調節計が各調節弁の開
度を制御し、各経路を流れる気液の流量を増減すること
により行われる。
In the air liquefaction / separation apparatus thus formed, when the production amount of the product gas is increased or decreased, each controller controls the opening of each control valve according to a preset program, and controls each path. This is performed by increasing or decreasing the flow rate of flowing gas-liquid.

【0023】例えば、100%負荷の運転状態から70
%負荷の状態に減量する際には、原料空気供給ラインの
流量指示調節計11によって調節弁11Vが絞られ、原
料空気供給量が所定の減速度で70%に減らされるとと
もに、所定のタイミングで各調節計及び調節弁が作動
し、各部の気液の流量を、最終的に70%負荷の状態に
応じた流量に変更する。なお、70%負荷のときの各部
の流量は、単純に70%になるわけではなく、各製品ガ
スの純度が所定純度を保てるように適当な流量に調節さ
れる。
For example, from an operation state of 100% load, 70
When the amount is reduced to the% load state, the control valve 11V is throttled by the flow rate indicator controller 11 of the raw air supply line, the raw air supply amount is reduced to 70% at a predetermined deceleration, and at a predetermined timing. Each controller and control valve are operated, and the flow rate of gas and liquid in each section is finally changed to a flow rate corresponding to a 70% load condition. In addition, the flow rate of each part at the time of a 70% load is not simply 70%, but is adjusted to an appropriate flow rate so that the purity of each product gas can maintain a predetermined purity.

【0024】表1は、100%負荷における原料空気量
が100000Nm/hで、純度保証値99.6vo
l%以上の製品酸素ガスの採取量が21000Nm
h、純度97vol%以上の粗アルゴンガスの採取量が
870Nm/hであって、70%負荷における原料空
気量が70000Nm/hで、製品酸素ガスの採取量
が14680Nm/h、粗アルゴンガスの採取量が5
20Nm/hに、それぞれ設定した装置において、各
負荷で安定した状態で運転しているときの主要部の流量
[Nm/h]と純度(ガス組成)[vol%]とを示
すものである。
Table 1 shows that the raw material air amount at 100% load is 100,000 Nm 3 / h, and the purity guarantee value is 99.6 vo.
1% or more of product oxygen gas is collected at 21,000 Nm 3 /
h, the collection amount of crude argon gas having a purity of 97 vol% or more is 870 Nm 3 / h, the raw material air amount at 70% load is 70000 Nm 3 / h, the collection amount of product oxygen gas is 14680 Nm 3 / h, Gas collection volume is 5
To 20 nm 3 / h, in the apparatus set respectively, shows a flow of a main part [Nm 3 / h] and a purity (gas composition) [vol%] of when operating in a stable state in each load is there.

【表1】 [Table 1]

【0025】このような設定における装置において、液
溜6や調節弁21V等を設けた場合(本実施例)と、液
溜等を設けない場合(従来例)とを比較した。なお、本
実施例における増量運転時及び減量運転時の各気液の流
量変化量は、液溜6から粗アルゴン塔7に供給する還流
液の変化量のみを毎分2%に設定し、これ以外は全て毎
分1%で変化させた(廃窒素ガスは圧力が一定になるよ
うに制御)。一方、液溜や調節弁が無い従来例における
粗アルゴン塔7の還流液量は、アルゴン凝縮器5に導入
される液化空気量に依存しており、還流液量の直接的な
制御は行っていない(他は全て毎分1%)。
In the apparatus in such a setting, the case where the liquid reservoir 6, the control valve 21V and the like are provided (this embodiment) and the case where no liquid reservoir and the like are provided (conventional example) were compared. In the present embodiment, the amount of change in the flow rate of each gas and liquid during the increase operation and the decrease operation is set to 2% per minute only for the change amount of the reflux liquid supplied from the liquid reservoir 6 to the crude argon column 7. Other than the above, all were changed at 1% per minute (the pressure of the waste nitrogen gas was controlled to be constant). On the other hand, the amount of reflux liquid in the crude argon column 7 in the conventional example having no liquid reservoir or control valve depends on the amount of liquefied air introduced into the argon condenser 5, and the amount of reflux liquid is directly controlled. No (all others 1% per minute).

【0026】まず、70%負荷から100%負荷に増量
運転を行う場合、上部塔1から経路68を経て粗アルゴ
ン塔7に供給されるフィードアルゴン中のアルゴン濃度
は、本実施例では、増量開始後約40分で極小値約6v
ol%になり、以後漸増して所定の9.43vol%に
到達したのに対し、従来例では、約40分後に極小値約
5vol%になった。
First, when the increasing operation is performed from the 70% load to the 100% load, the argon concentration in the feed argon supplied from the upper tower 1 to the crude argon tower 7 via the path 68 is determined in the present embodiment. After about 40 minutes, the minimum value is about 6v
ol%, and thereafter gradually increased to a predetermined 9.43 vol%, whereas in the conventional example, the minimum value was about 5 vol% after about 40 minutes.

【0027】経路75から採取される粗アルゴン中の酸
素濃度は、本実施例では、増量開始後約6時間で極大値
約2.2vol%になり、以後非常にゆっくりと減少し
ていったのに対し、従来例では、約4時間後に極大値約
5vol%になった。また、粗アルゴン中の窒素濃度
は、本実施例では、増量開始後約30分で極大値約0.
6vol%になり、すぐに元に戻ったが、従来例では、
増量開始後約2時間からゆっくりと変化した。
In the present embodiment, the oxygen concentration in the crude argon collected from the passage 75 reaches a maximum value of about 2.2 vol% in about 6 hours after the start of the increase, and then decreases very slowly. On the other hand, in the conventional example, the maximum value was about 5 vol% after about 4 hours. In the present embodiment, the nitrogen concentration in the crude argon reaches a maximum value of about 0.3 in about 30 minutes after the start of the increase.
It became 6 vol% and returned immediately, but in the conventional example,
It slowly changed from about 2 hours after the start of the dose increase.

【0028】経路63から採取される製品酸素ガスの純
度は、本実施例では、増量開始後約2時間で極大値約9
9.83vol%になり、従来例では、約2時間後に極
大値約99.85vol%になり、両者共、以後漸減し
ていった。
In the present embodiment, the purity of the product oxygen gas collected from the passage 63 reaches a maximum value of about 9 at about 2 hours after the start of the increase.
In the conventional example, the maximum value was about 99.85 vol% after about 2 hours, and both gradually decreased thereafter.

【0029】次に、100%負荷から70%負荷に減量
運転を行う場合、前記フィードアルゴン中のアルゴン濃
度は、本実施例では、減量開始後約30分で極小値約6
vol%になり、全体としてみるとほとんど変動しなか
ったのに対し、従来例では、約40分後に極大値約20
vol%になり、以後2時間程度で所定値に戻った。
Next, when performing a weight reduction operation from a 100% load to a 70% load, in this embodiment, the argon concentration in the feed argon is set to a minimum value of about 6 minutes in about 30 minutes after the start of the weight reduction.
vol.%, and hardly fluctuated as a whole, whereas the conventional example had a maximum value of about 20 after about 40 minutes.
vol%, and returned to a predetermined value in about 2 hours thereafter.

【0030】前記粗アルゴン中の酸素濃度は、本実施例
ではほとんど変動しなかったのに対し、従来例では、約
80分後に極小値約0.7vol%になり、以後漸増し
ていった。
The oxygen concentration in the crude argon hardly fluctuated in this embodiment, whereas in the conventional example, it reached a minimum value of about 0.7 vol% after about 80 minutes, and gradually increased thereafter.

【0031】前記製品酸素ガスの純度は、本実施例で
は、減量開始後約60分で極大値約99.8vol%に
なるが、全体としてみるとほとんど変動しなかったのに
対し、従来例では、約100分後に、保証値を下回る極
小値約99vol%になり、以後漸増していった。
In the present embodiment, the purity of the product oxygen gas reaches a maximum value of about 99.8 vol% in about 60 minutes after the start of the weight reduction, but it hardly fluctuates as a whole. After about 100 minutes, the minimum value was below the guaranteed value, about 99 vol%, and gradually increased thereafter.

【0032】上述の増量運転及び減量運転の状況をみる
と、従来例は、増量時に粗アルゴン中の酸素濃度が大き
く上昇し、減量時に製品酸素ガスの純度が大きく低下し
ている。これらの数値は、いずれも許容値や保証値を満
足できるものではなく、流量の変動速度を毎分1%より
もかなり低く設定しなければならないことがわかる。一
方、本実施例では、これらの濃度変動が抑制されてお
り、許容値や保証値を十分に満足する数値となってい
る。
Looking at the situation of the above-mentioned increase operation and decrease operation, in the conventional example, the oxygen concentration in the crude argon greatly increases when increasing the amount, and the purity of the product oxygen gas decreases greatly when decreasing the amount. It is understood that none of these numerical values can satisfy the permissible value or the guaranteed value, and it is necessary to set the fluctuation rate of the flow rate to be much lower than 1% per minute. On the other hand, in the present embodiment, these density fluctuations are suppressed, and the numerical values sufficiently satisfy the allowable value and the guaranteed value.

【0033】また、粗アルゴン塔7の還流液の変化速度
を、他の変化速度より早く、特に、アルゴン凝縮器5に
寒冷源として導入される液化空気の変化速度より早く設
定することにより、還流液量の変化を上昇ガス量の変化
に対応させることができるので、上述の濃度変動抑制効
果が得られるだけでなく、従来に比べて全体の流量増減
速度を高く設定することが可能となるので、増減量操作
を迅速に行うことができる。
By setting the rate of change of the reflux liquid in the crude argon column 7 faster than the other rates of change, in particular, faster than the rate of change of the liquefied air introduced as a cold source into the argon condenser 5, Since the change in the liquid amount can be made to correspond to the change in the rising gas amount, not only the above-described effect of suppressing the concentration fluctuation can be obtained, but also the overall flow rate increasing / decreasing speed can be set higher than in the past. In addition, the operation of increasing or decreasing the amount can be performed quickly.

【0034】なお、定常運転時における粗アルゴン塔7
の還流液量は、流量指示調節計21によって還流液供給
径路72の流量を一定に保つようにしてしてもよく、液
面調節計20によって液溜6内の液面を一定に保つよう
にしてもよい。
The crude argon column 7 during steady operation
The amount of the reflux liquid may be controlled such that the flow rate of the reflux liquid supply path 72 is kept constant by the flow rate controller 21, and the liquid level in the liquid reservoir 6 is kept constant by the liquid level controller 20. You may.

【0035】また、図1に想像線で示すように、還流液
導入径路71と還流液供給径路72とを接続し、液溜6
をバイパスする経路76及び弁76Vを設け、この経路
76に一定量の還流液を流し、残部を流量調節用として
液溜6を通すようにしても同様の効果が得られる。この
場合は、液溜6等を小型化することができる。
As shown by the imaginary line in FIG. 1, the reflux liquid introduction path 71 and the reflux liquid supply path 72 are connected to
A similar effect can be obtained by providing a path 76 and a valve 76V for bypassing the flow path, allowing a fixed amount of reflux liquid to flow through this path 76, and passing the remainder through the liquid reservoir 6 for flow rate adjustment. In this case, the size of the liquid reservoir 6 and the like can be reduced.

【0036】図2は、本発明の空気液化分離装置の他の
形態例を示す系統図である。この空気液化分離装置は、
粗アルゴン塔30を上下2層構造とし、上層の精留段3
1の下方に、塔内を流下する還流液の少なくとも一部を
抜取って液溜32に導く還流液導入経路33を接続し、
下層の精留段34の上方に、液溜32内の還流液を塔内
に供給する還流液供給経路35を接続するとともに、該
還流液供給経路35に、液溜33内の液面高さを検出す
る液面調節計(LC)36及び還流液供給径路35を流
れる還流液の流量を検出する流量指示調節計(FIC)
37によって制御される調節弁37Vを設けたものであ
る。
FIG. 2 is a system diagram showing another embodiment of the air liquefaction / separation apparatus of the present invention. This air liquefaction separation device
The crude argon tower 30 has an upper and lower two-layer structure, and an upper rectification stage 3
A reflux liquid introduction path 33 for extracting at least a part of the reflux liquid flowing down in the column and leading the liquid to the liquid reservoir 32 is connected below 1
A reflux liquid supply path 35 for supplying the reflux liquid in the liquid reservoir 32 into the tower is connected above the lower rectification stage 34, and the liquid level in the liquid reservoir 33 is connected to the reflux liquid supply path 35. Level controller (LC) 36 for detecting the flow rate and a flow rate indicating controller (FIC) for detecting the flow rate of the reflux liquid flowing through the reflux liquid supply path 35.
A control valve 37V controlled by 37 is provided.

【0037】本形態例は、粗アルゴン塔30を流下する
還流液の一部又は全部を、還流液導入経路33により塔
外に抜出して液溜32に貯留し、所定量の還流液を、還
流液供給径路35により液溜32から粗アルゴン塔30
に供給するようにしたものであって、下層の精留段34
における還流液量を任意に設定できるように形成したも
のである。
In this embodiment, part or all of the reflux liquid flowing down the crude argon column 30 is drawn out of the tower through a reflux liquid introduction path 33 and stored in a liquid reservoir 32, and a predetermined amount of the reflux liquid is refluxed. The liquid supply path 35 separates the crude argon tower 30 from the liquid reservoir 32.
And the lower rectification stage 34
Is formed so that the amount of the reflux liquid in can be arbitrarily set.

【0038】したがって、本形態例においても、粗アル
ゴン塔全体の還流液量の調節はできないものの、下層の
精留段34を流下する還流液量を、装置の運転状態に応
じて適切に調節することができるので、前記形態例と略
同様の濃度変動抑制や増減量運転操作の迅速化を図るこ
とができる。
Therefore, in this embodiment as well, although the amount of reflux liquid in the entire crude argon column cannot be adjusted, the amount of reflux liquid flowing down the lower rectification stage 34 is appropriately adjusted according to the operation state of the apparatus. Therefore, it is possible to suppress the concentration fluctuation and to speed up the increase / decrease amount driving operation in substantially the same manner as in the embodiment.

【0039】また、本形態例では、還流液導入経路33
の抜取り量を一定とし、還流液供給径路35に調節弁3
7Vを設けて粗アルゴン塔30への還流液供給量を調節
するように形成したが、還流液供給径路35に調節弁を
設けず、還流液導入経路33に調節弁を設け、粗アルゴ
ン塔30の中間から抜取る還流液量を調節するように形
成しても、下層の精留段34における還流液の量を任意
に調節することができる。
In this embodiment, the reflux liquid introduction path 33
And the control valve 3 is connected to the reflux liquid supply path 35.
7 V was provided to adjust the supply amount of the reflux liquid to the crude argon column 30. However, a control valve was not provided in the reflux liquid supply path 35, and a control valve was provided in the reflux liquid introduction path 33. Even if it is formed so as to adjust the amount of reflux liquid withdrawn from the middle of the above, the amount of reflux liquid in the lower rectification stage 34 can be arbitrarily adjusted.

【0040】なお、本形態例は、粗アルゴン塔30及び
その周辺の構成、粗アルゴンを採取する前記経路74
が、粗アルゴン塔30の頂部とアルゴン凝縮器5とを接
続するガス経路38から分岐する点を除いては、図1に
示した前記形態例と同一に形成しているので、前記形態
例における構成要素と同一の構成要素には同一符号を付
して詳細な説明は省略する。
In this embodiment, the configuration of the crude argon column 30 and its surroundings, and the route 74 for collecting the crude argon are described.
However, except that it is branched from the gas path 38 connecting the top of the crude argon column 30 and the argon condenser 5, it is formed in the same manner as the embodiment shown in FIG. The same components as those of the first embodiment are denoted by the same reference numerals, and the detailed description is omitted.

【0041】また、規則充填物を使用した充填塔を粗ア
ルゴン塔30に使用する際には、上下の充填物の間に設
けられている液体捕集分配装置における液体捕集部を液
溜として利用し、液体捕集部と液体分配部と間や、液体
分配部に適宜な流量制御手段を設けるようにしてもよ
く、あるいは、液体捕集部で捕集した還流液を外部の液
溜に抜出し、外部の液溜から液体分配部に還流液を供給
するように形成するとともに、抜出し部や供給部の適当
な位置で流量制御を行うようにしてもよい。さらに、図
1の構成と図2の構成とを併用してもよい。
When a packed column using the structured packing is used for the crude argon column 30, the liquid collecting section in the liquid collecting and distributing device provided between the upper and lower packings is used as a liquid reservoir. Utilization may be provided between the liquid collecting part and the liquid distributing part, or in the liquid distributing part, with an appropriate flow rate control means, or the reflux liquid collected by the liquid collecting part may be stored in an external liquid reservoir. Withdrawing and supplying the reflux liquid from the external liquid reservoir to the liquid distribution unit may be performed, and the flow rate may be controlled at an appropriate position of the extraction unit or the supply unit. Further, the configuration of FIG. 1 and the configuration of FIG. 2 may be used together.

【0042】[0042]

【発明の効果】以上説明したように、本発明は、原料ガ
ス(フィードアルゴン)が下部から供給され、上部に還
流液を生成する凝縮器を備えた粗アルゴン塔に液溜等を
付設して還流液の流量を調節できるようにしたので、粗
アルゴン塔内の上昇ガス量と還流液量とを別々に独立し
て操作することができ、装置の運転状態に応じて最適な
還流液量に設定することができる。例えば、減量操作時
には粗アルゴン塔へ供給する還流液を減量し、逆に増量
操作時には粗アルゴン塔に供給する還流液の流量を迅速
に増量させることができるため、粗アルゴン塔内の上昇
ガスと還流液との増減速度のアンバランスを緩和させる
ことができ、製品純度の変動幅を小さく抑えることがで
きるとともに、増減量操作を迅速に行うことができる。
As described above, according to the present invention, a raw gas (feed argon) is supplied from below, and a liquid reservoir or the like is attached to a crude argon column provided with a condenser for generating a reflux liquid on the upper part. Since the flow rate of the reflux liquid can be adjusted, the amount of the rising gas in the crude argon column and the amount of the reflux liquid can be separately and independently operated, and the optimum reflux liquid amount can be adjusted according to the operation state of the apparatus. Can be set. For example, the amount of the reflux liquid supplied to the crude argon column is reduced during the volume reduction operation, and the flow rate of the reflux liquid supplied to the crude argon column can be rapidly increased during the volume increase operation. The imbalance in the rate of increase and decrease with the reflux liquid can be relaxed, the fluctuation range of the product purity can be reduced, and the operation of increasing and decreasing can be performed quickly.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 本発明の空気液化分離装置の一形態例を示す
系統図である。
FIG. 1 is a system diagram showing one embodiment of an air liquefaction / separation apparatus of the present invention.

【図2】 同じく他の形態例を示す系統図である。FIG. 2 is a system diagram showing another embodiment.

【符号の説明】[Explanation of symbols]

1…下部塔、2…上部塔、3…主凝縮蒸発器、4…複精
留塔、5…アルゴン凝縮器、6…液溜、7…粗アルゴン
塔、8…主熱交換器、9…過冷器、11V〜22V…調
節弁、70…液化アルゴン径路、71…還流液導入径
路、72…還流液供給径路、FIC…流量指示調節計、
LC…液面計
DESCRIPTION OF SYMBOLS 1 ... Lower tower, 2 ... Upper tower, 3 ... Main condensation evaporator, 4 ... Double rectification tower, 5 ... Argon condenser, 6 ... Liquid reservoir, 7 ... Crude argon tower, 8 ... Main heat exchanger, 9 ... Subcooler, 11 V to 22 V: control valve, 70: liquefied argon path, 71: reflux liquid introduction path, 72: reflux liquid supply path, FIC: flow rate indicating controller,
LC: Liquid level gauge

Claims (7)

【特許請求の範囲】[Claims] 【請求項1】 下部塔,上部塔及び主凝縮蒸発器を有す
る複精留塔と、液化空気を液化寒冷源とするアルゴン凝
縮器を塔頂部に有する粗アルゴン塔とを備え、圧縮,精
製,冷却した原料空気を液化精留することにより、製品
として少なくともアルゴンを採取する空気液化分離装置
において、前記粗アルゴン塔に、該粗アルゴン塔の還流
液を貯溜する液溜を付設し、該液溜に前記粗アルゴン塔
の還流液を導く還流液導入径路と、該液溜に貯溜された
還流液を前記粗アルゴン塔に供給する還流液供給径路と
を設けるとともに、前記還流液導入径路及び還流液供給
径路の少なくともいずれか一方に、該経路を流れる還流
液の流量を調節する流量調節手段を備えたことを特徴と
する空気液化分離装置。
1. A double rectification column having a lower column, an upper column, and a main condensation evaporator, and a crude argon column having an argon condenser having a liquefied air as a liquefaction cold source at the top of the column. In the air liquefaction / separation apparatus for collecting at least argon as a product by liquefying and cooling the cooled raw material air, the crude argon column is provided with a liquid reservoir for storing a reflux liquid of the crude argon column. A reflux liquid introduction path for guiding the reflux liquid of the crude argon column and a reflux liquid supply path for supplying the reflux liquid stored in the liquid reservoir to the crude argon tower, and the reflux liquid introduction path and the reflux liquid. An air liquefaction / separation apparatus characterized in that at least one of the supply paths is provided with a flow rate adjusting means for adjusting the flow rate of the reflux liquid flowing through the path.
【請求項2】 前記還流液供給径路に、流量検出手段と
流量制御手段とを備えたことを特徴とする請求項1記載
の空気液化分離装置。
2. The air liquefaction / separation apparatus according to claim 1, wherein a flow rate detecting means and a flow rate controlling means are provided in the reflux liquid supply path.
【請求項3】 前記液溜に、液面検出手段を設けるとと
もに、前記還流液導入径路又は前記還流液供給径路に、
前記液面検出手段からの信号によって液溜の液面を制御
する液面制御手段とを備えたことを特徴とする請求項1
記載の空気液化分離装置。
3. A liquid level detecting means is provided in the liquid reservoir, and the liquid supply path or the liquid supply path is
2. A liquid level control means for controlling a liquid level in a liquid reservoir in accordance with a signal from said liquid level detection means.
An air liquefaction separation device as described.
【請求項4】 前記液溜は、前記アルゴン凝縮器と前記
粗アルゴン塔の頂部とを連結する液化アルゴン径路の途
中に設けられていることを特徴とする請求項1記載の空
気液化分離装置。
4. The air liquefaction / separation apparatus according to claim 1, wherein the liquid reservoir is provided in the middle of a liquefied argon path connecting the argon condenser and the top of the crude argon column.
【請求項5】 請求項1乃至5のいずれかに記載の空気
液化分離装置の運転方法であって、前記粗アルゴン塔の
還流液の少なくとも一部を前記液溜に貯溜し、該貯溜さ
れた還流液を、装置の運転状態に応じた流量で前記粗ア
ルゴン塔に供給することを特徴とする空気液化分離装置
の運転方法。
5. The method for operating an air liquefaction / separation apparatus according to claim 1, wherein at least a part of the reflux liquid of the crude argon column is stored in the liquid reservoir. A method for operating an air liquefaction / separation apparatus, wherein a reflux liquid is supplied to the crude argon column at a flow rate according to the operation state of the apparatus.
【請求項6】 装置が一定の状態で運転されているとき
の前記還流液の流量は、前記液溜から粗アルゴン塔に供
給する還流液の流量が一定になるように行うか、あるい
は、前記液溜の液面が一定になるように制御することを
特徴とする請求項5記載の空気液化分離装置の運転方
法。
6. The flow rate of the reflux liquid when the apparatus is operated in a constant state is such that the flow rate of the reflux liquid supplied from the liquid reservoir to the crude argon column is constant, or The method according to claim 5, wherein the liquid level of the liquid reservoir is controlled to be constant.
【請求項7】 装置が増量運転又は減量運転に移行する
際における前記還流液の流量の増減速度は、前記アルゴ
ン凝縮器の寒冷源となる液化空気の流量の増減速度より
も早くすることを特徴とする請求項5記載の空気液化分
離装置の運転方法。
7. The method according to claim 1, wherein the rate of change of the flow rate of the reflux liquid when the apparatus shifts to the increase operation or the decrease operation is faster than the change rate of the flow rate of the liquefied air serving as a cold source of the argon condenser. The method for operating an air liquefaction / separation apparatus according to claim 5, wherein
JP7269298A 1998-03-20 1998-03-20 Operation method of air liquefaction separator Expired - Fee Related JP4104726B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7269298A JP4104726B2 (en) 1998-03-20 1998-03-20 Operation method of air liquefaction separator

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7269298A JP4104726B2 (en) 1998-03-20 1998-03-20 Operation method of air liquefaction separator

Publications (2)

Publication Number Publication Date
JPH11270965A true JPH11270965A (en) 1999-10-05
JP4104726B2 JP4104726B2 (en) 2008-06-18

Family

ID=13496684

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7269298A Expired - Fee Related JP4104726B2 (en) 1998-03-20 1998-03-20 Operation method of air liquefaction separator

Country Status (1)

Country Link
JP (1) JP4104726B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3604994A1 (en) * 2018-08-01 2020-02-05 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and device for producing argon by cryogenic distillation of air

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3604994A1 (en) * 2018-08-01 2020-02-05 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and device for producing argon by cryogenic distillation of air
FR3084736A1 (en) * 2018-08-01 2020-02-07 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude PROCESS AND APPARATUS FOR THE PRODUCTION OF ARGON BY CRYOGENIC AIR DISTILLATION
CN110793271A (en) * 2018-08-01 2020-02-14 乔治洛德方法研究和开发液化空气有限公司 Method and apparatus for producing argon by cryogenic distillation of air
US11441840B2 (en) 2018-08-01 2022-09-13 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and plant for the production of argon by cryogenic distillation of air

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