JPS6155034B2 - - Google Patents
Info
- Publication number
- JPS6155034B2 JPS6155034B2 JP53130562A JP13056278A JPS6155034B2 JP S6155034 B2 JPS6155034 B2 JP S6155034B2 JP 53130562 A JP53130562 A JP 53130562A JP 13056278 A JP13056278 A JP 13056278A JP S6155034 B2 JPS6155034 B2 JP S6155034B2
- Authority
- JP
- Japan
- Prior art keywords
- column
- argon
- purity
- crude argon
- crude
- 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.)
- Expired
Links
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 302
- 229910052786 argon Inorganic materials 0.000 claims description 153
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 60
- 239000007789 gas Substances 0.000 claims description 45
- 229910052757 nitrogen Inorganic materials 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 5
- 230000003247 decreasing effect Effects 0.000 claims description 4
- 230000007423 decrease Effects 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 238000007664 blowing Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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
- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
- F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
- F25J3/048—Argon recovery
-
- 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
-
- 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
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)
Description
【発明の詳細な説明】
本発明は、液化精留法による空気分離装置にお
いて、酸素およびアルゴン採取が組合されたプラ
ントの粗アルゴン塔の自動運転法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for automatically operating a crude argon column in a plant with combined oxygen and argon extraction in an air separation apparatus using a liquefaction rectification process.
新製鋼法、特殊溶接、半導体工業用としてのア
ルゴンの需要が増加している昨今、アルゴンの経
済的価値が重要視されている。アルゴンは周知の
如く液化精留法により製造されているが、以下に
一例として、従来技術による全低圧式空気分離装
置での粗アルゴン塔の運転方法を、第１図に示す
系統図に基づいて説明する。 Recently, the economic value of argon has become important as the demand for argon for new steel manufacturing methods, special welding, and the semiconductor industry is increasing. As is well known, argon is produced by the liquefaction rectification method, and below, as an example, we will explain how to operate a crude argon column in a total low-pressure air separation device based on the system diagram shown in Figure 1. explain.
第１図は、主精留塔および粗アルゴン塔回りの
系統図であり、粗アルゴン塔コンデンサーには、
ハンプソン式熱交換器を採用した場合である。 Figure 1 is a system diagram around the main rectification column and crude argon column.
This is the case when a Hampson heat exchanger is used.
粗アルゴン塔２０のフイードガスは、精留塔上
塔下部２８のサイドカツト段より管路２１を経て
粗アルゴン塔２０下部へ送入され、粗アルゴン２
０塔内を上昇し、塔頂の粗アルゴン塔コンデンサ
ー２６で、管路２４を経て供給された液体空気と
熱交換して液化した下降液と、棚段２７上で気液
接触して精留分離され、塔頂に行くにしたがつて
アルゴン純度が高くなり、例えば塔頂より純度98
％Arの製品粗アルゴンとして管路２５より導出
される。 The feed gas in the crude argon column 20 is sent from the side cut stage of the upper column lower part 28 of the rectification column to the lower part of the crude argon column 20 via the pipe 21, and the feed gas is fed into the lower part of the crude argon column 20.
The descending liquid rises in the 0 column and is liquefied by heat exchange with the liquid air supplied through the pipe 24 in the crude argon column condenser 26 at the top of the column, and is brought into gas-liquid contact on the tray 27 to be rectified. Argon is separated, and the purity of argon increases as it goes to the top of the column, for example, purity 98
%Ar product is led out from pipe 25 as crude argon.
一方、粗アルゴン塔２０下部からは酵素分に富
んだ液が抽出され、管路２２を経て精留塔上塔下
部２８へと戻される系統となつている。従来の粗
アルゴン塔２０の運転管理方法は、次の２通りで
ある。(1)粗アルゴン塔２０へのフイードガス中の
アルゴン純度を一定に保つように管理する方法。
この場合、製品アルゴンガスの純度は管路２５の
点で、粗アルゴン塔２０へのフイードガス中のア
ルゴン純度は管路２１の点で、粗アルゴン塔２０
からの戻り液純度は管路２２の点で、それぞれ分
析している。(2)粗アルゴン塔２０の中間部のアル
ゴン純度を一定値以上に保つように管理する方
法。すなわち、アルゴン純度変化の大きい粗アル
ゴン塔２０中間部のガス相あるいは液相部より、
分析用の混合ガス（Ar−O2−N2）を分析用ノズル
より抽出して、アルゴン分析計でアルゴン純度を
分析管理することによつて、管理頂製品粗アルゴ
ン純度に常に規定値内に保つように、粗アルゴン
塔２０へのフイードガス量ならびにフイードガス
中のアルゴン純度および、製品アルゴン量の調整
を遠隔操作で行なう方法。 On the other hand, a liquid rich in enzymes is extracted from the lower part of the crude argon column 20 and is returned to the lower part 28 of the upper column of the rectification column via a pipe 22. There are two conventional operational management methods for the crude argon column 20 as follows. (1) A method of managing the argon purity in the feed gas to the crude argon column 20 to keep it constant.
In this case, the purity of the product argon gas is at the point of line 25, and the purity of argon in the feed gas to the crude argon column 20 is at the point of line 21, and the purity of the argon in the feed gas to the crude argon column 20 is
The purity of the return liquid from each line is analyzed at the point of line 22. (2) A method of managing the argon purity in the middle part of the crude argon column 20 to keep it above a certain value. That is, from the gas phase or liquid phase in the middle part of the crude argon column 20 where the argon purity changes greatly,
By extracting the mixed gas for analysis (Ar-O 2 -N 2 ) from the analysis nozzle and controlling the argon purity with an argon analyzer, the crude argon purity of the controlled product is always within the specified value. A method of remotely controlling the amount of feed gas to the crude argon column 20, the purity of argon in the feed gas, and the amount of product argon so as to maintain the same level of purity.
前記の如き２通りの運転方法には下記のような
問題点がある。前者、すなわち、粗アルゴン塔へ
のフイードガス中のアルゴン純度を一定に保つよ
うな運転方法においては、粗アルゴン塔内部の純
度変化に対しては敏感でないため、例えば粗アル
ゴン塔へのフイードガス量およびアルゴン純度を
一定に保つていても、塔頂抜出し製品粗アルゴン
量の増減により、製品粗アルゴン純度は変化する
ので、この変化が粗アルゴン塔内の純度変化をき
たし、粗アルゴン塔戻り液の純度変化となつて現
われ、主精留塔上下部の純度変化となり、最終的
に粗アルゴン塔へのフイードガス中のアルゴン純
度の変化となつて現われるのは長時間を経てから
である。したがつて、粗アルゴン塔へのフイード
ガス純度は一定でも、塔頂製品アルゴン純度は低
下しているという事態も起り得るわけである。ま
た、フイードアルゴン純度が例えば若干低下して
いる傾向の時でも、粗アルゴン塔内の純度分布が
変化して、塔頂製品粗アルゴン純度が低下し始め
る迄は時間遅れが存在するので、塔頂製品粗アル
ゴン純度が低下傾向となつてはじめて、純度回復
処置を実施せざるを得ないこととなり、その結
果、製品粗アルゴン純度を乱して、規定純度内に
回復させるために、一定の時間製品粗アルゴン採
取量を減量しなければならないことになり、極め
て不経済である。加うるに粗アルゴン塔へのフイ
ードガス純度で運転管理しているため、サイドカ
ツト段のアルゴン純度の分析のみでは、運転管理
が困難であるという問題がある。粗アルゴン塔へ
のフイードガス組成と、主精留塔のサイドカツト
段のガス組成とは全く等しいものであるが、周知
の通り主精留塔上塔内各部のアルゴン純度分布
は、第２図で見るようにピークを持つており、同
一アルゴン純度Ａでも２点あり、異なるのはアル
ゴン成分外の窒素純度Ｂならびに酸素純度Ｃであ
る。また、窒素ならびに酸素の純度分布も第２図
に示しているが、第２図でわかるように、アルゴ
ン純度Ａがピークの時には窒素純度Ｂは高くなつ
ており、ピーク値の少し下では、窒素純度Ｂはピ
ーク値の窒素純度Ｂよりも一桁低い値となつてい
る。粗アルゴン塔へのフイードガス中に窒素が混
入した場合、塔頂コンデンサーの液体空気との熱
交換では凝縮しないために、粗アルゴン塔のコン
デンサーおよび塔頂部に次第に蓄積されていき、
本来の液体空気とアルゴンの温度差を小さくして
いくので、コンデンサーの熱交換性能が低下す
る。このため、一般的には、粗アルゴン塔へのフ
イードガス中のアルゴン純度は、アルゴンのピー
ク値よりも若干低い純度で、すなわち、窒素純度
が低い状態で運転するのが良いとされているが、
前記の通り同一アルゴン純度でも２点あるので、
アルゴン純度の他に窒素純度も正確に把握してお
かないと、現在運転しているサイドカツト段の分
布位置が明確にならず、運転操作を誤ることがあ
る。 The two operating methods described above have the following problems. In the former method, that is, the argon purity in the feed gas to the crude argon column is kept constant, it is not sensitive to purity changes inside the crude argon column. Even if the purity is kept constant, the product crude argon purity will change due to an increase or decrease in the amount of product crude argon extracted from the top of the column. This change will cause a change in the purity in the crude argon column, and a change in the purity of the crude argon column return liquid. This appears as a change in the purity of the upper and lower portions of the main rectification column, and finally appears as a change in the argon purity in the feed gas to the crude argon column after a long period of time. Therefore, even if the purity of the feed gas to the crude argon column is constant, a situation may occur in which the purity of the argon product at the top of the column is decreasing. Furthermore, even when the feed argon purity tends to decrease slightly, for example, there is a time lag until the purity distribution in the crude argon column changes and the crude argon purity of the column top product starts to decrease. Only when the crude argon purity of the top product starts to decrease does it become necessary to carry out purity recovery measures. The amount of crude argon extracted as a product must be reduced, which is extremely uneconomical. In addition, since the operation is controlled by the purity of the feed gas to the crude argon column, there is a problem in that it is difficult to control the operation only by analyzing the argon purity of the side cut stage. The feed gas composition to the crude argon column and the gas composition in the side cut stage of the main rectification column are exactly the same, but as is well known, the argon purity distribution in each part of the upper column of the main rectification column can be seen in Figure 2. There are two peaks even for the same argon purity A, and the difference is in nitrogen purity B and oxygen purity C, which are other than the argon component. Figure 2 also shows the purity distribution of nitrogen and oxygen. As can be seen in Figure 2, when argon purity A is at its peak, nitrogen purity B is high, and slightly below the peak value, nitrogen purity is high. Purity B is an order of magnitude lower than the peak nitrogen purity B. If nitrogen is mixed into the feed gas to the crude argon column, it will not condense through heat exchange with the liquid air in the top condenser, so it will gradually accumulate in the condenser and top of the crude argon column.
As the temperature difference between the original liquid air and argon is reduced, the heat exchange performance of the condenser decreases. For this reason, it is generally said that it is best to operate with the purity of argon in the feed gas to the crude argon column being slightly lower than the peak value of argon, that is, with the purity of nitrogen being low.
As mentioned above, there are two points for the same argon purity, so
If the nitrogen purity is not accurately known in addition to the argon purity, the distribution position of the side cut stage currently in operation will not be clear, which may lead to incorrect operation.
後者、すなわち粗アルゴン塔中間部のアルゴン
純度一定値以上に保つような運転方法には次に述
べる問題点がある。すなわち、粗アルゴン塔への
フイードガス中の窒素純度を分析しないで、粗ア
ルゴン塔中間部のアルゴン純度のみを分析してい
るので、フイードガス中に多量の窒素が混入した
場合に、運転操作を誤ることが起り得る。第２図
において、アルゴン純度がピーク値の状態で粗ア
ルゴン塔へフイードガスを送入したとすると、窒
素も多量に混入しており、窒素が多量に混入した
時の粗アルゴン塔内のアルゴン純度分布は、運転
条件により多少変動はあるが、粗アルゴン塔の中
間部ないしは中間部より若干上部でアルゴン純度
がピークになり、これより上部にいくにしたがつ
て、アルゴン純度は低下する分布となる。これは
窒素の影響である。しかるに、粗アルゴン塔中間
部におけるアルゴン純度が時間とともに増加して
いく傾向なので、塔頂製品粗アルゴン純度も規定
値内を保ち続けるかというと、上記の理由で必ず
しもそうでは無い場合もある。 The latter method of operation, in which the argon purity in the intermediate portion of the crude argon column is maintained above a certain value, has the following problems. In other words, only the argon purity in the middle part of the crude argon column is analyzed without analyzing the nitrogen purity in the feed gas flowing into the crude argon column, so if a large amount of nitrogen is mixed into the feed gas, it is possible to make a mistake in operation. can occur. In Figure 2, if the feed gas is fed into the crude argon column when the argon purity is at its peak value, a large amount of nitrogen is also mixed in, and the argon purity distribution in the crude argon column when a large amount of nitrogen is mixed in. Although there is some variation depending on the operating conditions, the argon purity peaks at the middle or slightly above the middle of the crude argon column, and the argon purity decreases as it goes higher. This is the effect of nitrogen. However, since the argon purity in the middle part of the crude argon column tends to increase over time, the crude argon purity of the column top product may not always remain within the specified value for the reasons mentioned above.
次に、前者ならびに後者に共通した問題点は、
粗アルゴン塔の運転が自動化されていないため、
フイードガス量、コンデンサーへの液体空気送入
量、製品酸素量、製品アルゴン抜出量等の調整が
繁雑で時間を要すため、運転員の人件費等が増大
するという点である。 Next, the problems common to the former and the latter are:
Since the operation of the crude argon tower is not automated,
Adjustments to the amount of feed gas, the amount of liquid air fed into the condenser, the amount of product oxygen, the amount of product argon extracted, etc. are complicated and time consuming, which increases personnel costs for operators.
本発明は、液化精留法により製品アルゴン（ガ
スおよび液）を製造する空気分離装置の粗アルゴ
ン塔の運転方法に関するもので、製品粗アルゴン
純度を規定値に保つために繁雑な調整を必要とし
ない自動運転法を提供するものである。 The present invention relates to a method for operating a crude argon column in an air separation device that produces product argon (gas and liquid) by a liquefaction rectification method, and requires complicated adjustments to maintain product crude argon purity at a specified value. It provides an automatic driving method that does not require automatic driving.
以下、本発明を実施した装置の一例を図面によ
り詳細に説明する。第３図は本発明を適用した主
精留塔および粗アルゴン塔回りの系統図である。 Hereinafter, an example of an apparatus implementing the present invention will be explained in detail with reference to the drawings. FIG. 3 is a system diagram around the main rectification column and crude argon column to which the present invention is applied.
粗アルゴン塔２０のフイードガスは、精留塔上
塔下部２８のサイドカツト段より管路２１を経て
粗アルゴン塔２０下部へ送入されるが、管路２１
に設置された分析用ノズルより抽出したフイード
ガスの一部は、記録調節分析計３２に導かれ、例
えばMax.2％程度からppmオーダの窒素純度に分
析される。そして、製品粗アルゴン抜出量と製品
粗アルゴン純度を規定値に保つために、必要な窒
素純度以下になるように、可逆式熱交換器３３出
口の管路３４に設置された製品酸素量調節弁３５
へ記録調節分析計３２より電気信号を送り、これ
を自動的に開閉させて製品酸素抜出量を調整す
る。 The feed gas in the crude argon column 20 is sent from the side cut stage of the upper column lower part 28 of the rectification column to the lower part of the crude argon column 20 via the pipe 21.
A part of the feed gas extracted from the analysis nozzle installed in the feed gas is guided to the recording control analyzer 32, where it is analyzed to have a nitrogen purity ranging from about 2% maximum to ppm order, for example. In order to maintain the product crude argon withdrawal amount and the product crude argon purity at specified values, the product oxygen amount is adjusted using a product oxygen amount installed in the pipe line 34 at the outlet of the reversible heat exchanger 33 so that the nitrogen purity is below the required nitrogen purity. valve 35
An electric signal is sent from the recording control analyzer 32 to the device to automatically open and close it to adjust the amount of oxygen extracted from the product.
また、管路２１にはフイードガス中のアルゴン
純度を分析する記録分析計４０とフイードガス量
を計測する指示調節流量計３９とが設置されてお
り、記録分析計４０で分析したアルゴン純度と指
示調節流量計３９にて計測したフイードガス流量
とをガスケード制御にて演算して、粗アルゴン塔
２０へフイードされる正味のアルゴン量を算出
し、これに見合つた量の液体空気を粗アルゴン塔
２０のコンデンサー２６へ供給するため、管路４
１に設置されている液体空気吹込調節弁４２を自
動的に開閉させる電気信号を送つて、コンデンサ
ー２６の熱交換性能を安定させながら、粗アルゴ
ン塔２０へのフイードガス量を一定に保つ。 Further, a recording analyzer 40 for analyzing the argon purity in the feed gas and an indication adjustment flow meter 39 for measuring the amount of feed gas are installed in the pipe line 21, and the argon purity analyzed by the recording analyzer 40 and the indication adjustment flow rate are installed in the pipe line 21. The net amount of argon to be fed to the crude argon column 20 is calculated by calculating the feed gas flow rate measured at the total 39 using gascade control, and the amount of liquid air commensurate with this amount is transferred to the condenser 26 of the crude argon column 20. Conduit 4 to supply
An electrical signal is sent to automatically open and close a liquid air blow control valve 42 installed in the argon column 1, thereby stabilizing the heat exchange performance of the condenser 26 and keeping the feed gas amount to the crude argon column 20 constant.
粗アルゴン塔２０下部より送入されたフイード
ガスは、粗アルゴン塔２０内を上昇し、塔頂の粗
アルゴン塔コンデンサー２６で、管路２４を経て
供給された液体空気と熱交換して液化した下降液
と、棚段２７上で気液接触し精留分離されて、塔
頂に行くにしたがつてアルゴン純度が高くなり、
例えば塔頂より純度98％Arの製品粗アルゴンと
して管路２５より導出される。製品粗アルゴン純
度を規定値に保つためにアルゴン純度変化の大き
い粗アルゴン塔２０中間部のガス相あるいは液相
部に、少くとも１個以上の分析ノズルを設置し、
Ar−O2−N2の混合ガスを抽出して記録調節分析
計３０に導き、管路２５に設置した製品粗アルゴ
ン抜出弁３１と組合せて、粗アルゴン塔２０内の
アルゴン純度変化に対応して製品粗アルゴン抜出
弁３１を自動的に開閉させて製品粗アルゴン抜出
量を増減させる。 The feed gas fed from the lower part of the crude argon column 20 rises in the crude argon column 20, exchanges heat with the liquid air supplied through the pipe 24 at the crude argon column condenser 26 at the top of the column, and liquefies the feed gas. The argon is brought into contact with the liquid on the tray 27 and separated by rectification, and the purity of argon increases as it reaches the top of the column.
For example, crude argon product with a purity of 98% Ar is discharged from the top of the column through a pipe 25. In order to maintain the product crude argon purity at a specified value, at least one or more analysis nozzles are installed in the gas phase or liquid phase in the middle of the crude argon column 20 where the argon purity changes greatly,
The mixed gas of Ar-O 2 -N 2 is extracted and guided to the recording control analyzer 30, and in combination with the product crude argon extraction valve 31 installed in the pipe line 25, it responds to changes in argon purity in the crude argon column 20. Then, the product crude argon extraction valve 31 is automatically opened and closed to increase or decrease the product crude argon extraction amount.
更に、粗アルゴン塔コンデンサー２６の熱交換
性能を効果的にするため、粗アルゴン塔コンデン
サー２６に設置した分析ノズルより、分析用混合
ガスを抽出して記録調節分析計３６に導き、窒素
純度を分析し、分析した窒素純度に対応させて、
粗アルゴン塔コンデンサー２６より窒素成分をブ
ローする管路３７に設置した窒素ブロー弁３８を
自動的に開閉させて、粗アルゴン塔コンデンサー
２６の熱交換に悪影響を与えない窒素純度に保
つ。 Furthermore, in order to make the heat exchange performance of the crude argon column condenser 26 effective, a mixed gas for analysis is extracted from an analysis nozzle installed in the crude argon column condenser 26 and guided to a recording control analyzer 36 to analyze the nitrogen purity. Then, depending on the analyzed nitrogen purity,
A nitrogen blow valve 38 installed in a pipe 37 for blowing nitrogen components from the crude argon column condenser 26 is automatically opened and closed to maintain nitrogen purity at a level that does not adversely affect heat exchange in the crude argon column condenser 26.
一方、粗アルゴン塔２０下部からは酸素分に富
んだ液が抽出され、管路２２を経て精留塔上塔下
部２８へと戻される。 On the other hand, an oxygen-rich liquid is extracted from the lower part of the crude argon column 20 and is returned to the lower part 28 of the upper column of the rectification column via the pipe 22.
以上述べたように本発明によれば、粗アルゴン
塔へのフイードガス量、粗アルゴン塔コンデンサ
ーへの液体空気流入量、粗アルゴン塔塔頂部から
の放出窒素量、製品酸素抜出量、製品粗アルゴン
抜出量等、人手による繁雑な調整を必要とせず、
粗アルゴン塔を常時最適状態で自動運転すること
ができる。 As described above, according to the present invention, the amount of feed gas to the crude argon column, the amount of liquid air flowing into the crude argon column condenser, the amount of nitrogen released from the top of the crude argon column, the amount of product oxygen extracted, and the amount of product crude argon There is no need for complicated manual adjustments such as the extraction amount,
The crude argon column can be automatically operated in an optimal state at all times.
第１図は全低圧式空気分離装置における粗アル
ゴン塔の従来技術による運転方法の一例を示す主
精留塔および粗アルゴン塔回りの系統図、第２図
は主精留塔上塔内のアルゴン、酸素、窒素純度分
布図、第３図は本発明を実施した装置の一例を示
す主精留塔および粗アルゴン塔回りの系統図であ
る。
２０……粗アルゴン塔、２１，２２，２４，２
５，３４，３７，４１……管路、２６……粗アル
ゴン塔コンデンサー、２７……棚段、２８……精
留塔上塔下部、３０，３２，３６……記録調節分
析計、３１……製品粗アルゴン抜出弁、３３……
可逆式熱交換器、３５……製品酸素調節弁、３８
……窒素ブロー弁、３９……指示調節流量計、４
０……記録分析計、４２……液体空気吹込調節
弁。
Figure 1 is a system diagram of the main rectification column and crude argon column showing an example of a conventional operating method for the crude argon column in a total low-pressure air separation device. , oxygen, and nitrogen purity distribution diagrams. FIG. 3 is a system diagram around a main rectification column and a crude argon column showing an example of an apparatus in which the present invention is implemented. 20... Crude argon column, 21, 22, 24, 2
5, 34, 37, 41... Pipe line, 26... Crude argon column condenser, 27... Shelf, 28... Rectification column upper and lower column, 30, 32, 36... Recording control analyzer, 31... ...Product crude argon extraction valve, 33...
Reversible heat exchanger, 35...Product oxygen control valve, 38
...Nitrogen blow valve, 39...Indication adjustment flow meter, 4
0... Recording analyzer, 42... Liquid air blowing control valve.
Claims (1)
ガスを粗アルゴン塔下部に供給し、粗アルゴン塔
上部より製品粗アルゴンを抜出するようにした粗
アルゴン塔において、粗アルゴン塔中間部より混
合ガスを押出してアルゴン純度を分析し、粗アル
ゴン塔内のアルゴン純度変化に対応して製品粗ア
ルゴン純度を規定値内に保つように製品粗アルゴ
ン抜出量を増減し、精留塔上塔より粗アルゴン塔
へ供給するアルゴン含有ガス中の窒素純度を分析
し、供給ガス中の窒素純度に対応して粗アルゴン
塔への供給ガス中の窒素純度を規定値内に保つよ
うに精留塔上塔下部からの製品酸素抜出量を増減
し、粗アルゴン塔塔頂コンデンサーより混合ガス
を抽出して窒素純度を分析し、粗アルゴン塔塔頂
コンデンサー内に蓄積される窒素純度に対応して
粗アルゴン塔塔頂コンデンサー内の窒素純度を規
定値以下に保つように粗アルゴン塔塔頂部からの
放出窒素量を増減し、精留塔上塔より粗アルゴン
塔へ供給するアルゴン含有ガスの流量を測定する
と同時に供給ガス中のアルゴン純度を分析し、前
記供給ガス流量とアルゴン純度とをカスケード制
御により演算して粗アルゴン塔へ供給される正味
アルゴン量を算出し、粗アルゴン塔への供給アル
ゴン量に見合つた量の液体空気を粗アルゴン塔塔
頂コンデンサー内へ供給するようにしたことを特
徴とする粗アルゴン塔の自動運転法。1. In the crude argon column, in which argon-containing gas is supplied from the upper column of the rectification column of the air separation device to the lower part of the crude argon column, and product crude argon is extracted from the upper part of the crude argon column, mixing is carried out from the middle part of the crude argon column. The argon purity is analyzed by extruding the gas, and in response to changes in argon purity in the crude argon column, the amount of crude argon extracted from the product is increased or decreased in order to keep the product crude argon purity within the specified value, and the product is extracted from the upper column of the rectification column. The nitrogen purity in the argon-containing gas supplied to the crude argon column is analyzed, and the nitrogen purity in the gas supplied to the crude argon column is maintained within the specified value in accordance with the nitrogen purity in the supplied gas. The amount of product oxygen removed from the bottom of the column is increased or decreased, the mixed gas is extracted from the crude argon column top condenser and the nitrogen purity is analyzed, and the crude The amount of nitrogen released from the top of the crude argon column is increased or decreased to keep the nitrogen purity in the argon column top condenser below the specified value, and the flow rate of argon-containing gas supplied from the upper column of the rectification column to the crude argon column is measured. At the same time, the argon purity in the supply gas is analyzed, and the supply gas flow rate and argon purity are calculated by cascade control to calculate the net amount of argon to be supplied to the crude argon column. A method for automatically operating a crude argon column, characterized in that a proportionate amount of liquid air is supplied into a crude argon column top condenser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13056278A JPS5560164A (en) | 1978-10-25 | 1978-10-25 | Method of automatically operating coarse argon tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13056278A JPS5560164A (en) | 1978-10-25 | 1978-10-25 | Method of automatically operating coarse argon tower |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5560164A JPS5560164A (en) | 1980-05-07 |
| JPS6155034B2 true JPS6155034B2 (en) | 1986-11-26 |
Family
ID=15037212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13056278A Granted JPS5560164A (en) | 1978-10-25 | 1978-10-25 | Method of automatically operating coarse argon tower |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5560164A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63263381A (en) * | 1987-04-20 | 1988-10-31 | 住友金属工業株式会社 | Method of controlling concentration of nitrogen in raw material argon |
| US4784677A (en) * | 1987-07-16 | 1988-11-15 | The Boc Group, Inc. | Process and apparatus for controlling argon column feedstreams |
| US7204101B2 (en) * | 2003-10-06 | 2007-04-17 | Air Liquide Large Industries U.S. Lp | Methods and systems for optimizing argon recovery in an air separation unit |
| FR2951532A1 (en) * | 2009-10-15 | 2011-04-22 | Air Liquide | Method for separating argon enriched flow from air, involves measuring oxygen content at point in head and/or point under head of column, and regulating flow of impure argon based on oxygen content at point in head and/or point below head |
| FR3108970B1 (en) | 2020-04-02 | 2022-10-28 | Air Liquide | Method for starting an argon separation column of an air separation device by cryogenic distillation and unit for carrying out the method |
-
1978
- 1978-10-25 JP JP13056278A patent/JPS5560164A/en active Granted
Non-Patent Citations (1)
| Title |
|---|
| THERMODYNAMICBASES OF THE SEPARATION OF AIR DIAGRAMS CHPTER4 * |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5560164A (en) | 1980-05-07 |
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