JP2017014101A - Method for separating and acquiring oxygen from air by adsorption separation and device therefor - Google Patents

Method for separating and acquiring oxygen from air by adsorption separation and device therefor Download PDF

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Publication number
JP2017014101A
JP2017014101A JP2016134998A JP2016134998A JP2017014101A JP 2017014101 A JP2017014101 A JP 2017014101A JP 2016134998 A JP2016134998 A JP 2016134998A JP 2016134998 A JP2016134998 A JP 2016134998A JP 2017014101 A JP2017014101 A JP 2017014101A
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Prior art keywords
nitrogen
adsorption tower
oxygen
tower
air
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JP6163238B2 (en
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泉 順
Jun Izumi
順 泉
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Adsorption Technology Industries Co Ltd
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Adsorption Technology Industries Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/40Capture or disposal of greenhouse gases of CO2

Abstract

PROBLEM TO BE SOLVED: To provide a method for separating oxygen and nitrogen from the air at a low total oxygen production cost inexpensively maintaining an electric power consumption rate than the conventional oxygen production method.SOLUTION: Provided is a method for separating and acquiring oxygen from the air by adsorption separation includes a series of steps of: a nitrogen adsorption step where air is fed to a nitrogen adsorption tower 4 under the high pressure of the atmospheric pressure or more, nitrogen, moisture, COor the like are removed, the same is stored in a product oxygen tank provided at the back part of the nitrogen adsorption tower 4, and the air enough in oxygen is acquired; a residual oxygen recovery step where, before the reduction of the oxygen concentration, the front part of an auxiliary adsorption tower 13 installed in the back part of the nitrogen adsorption tower 4 and filled with a nitrogen adsorption agent 12 and the back part of the nitrogen adsorption tower 4 are connected, and the oxygen remaining in the back part of the tower is recovered by an auxiliary adsorption tower 13; and a pressure increasing step where, after the completion of the pressure reduction regeneration step of the nitrogen adsorption tower 4, the oxygen recovered by connecting the back part of the nitrogen adsorption tower 4 of the atmospheric pressure and the front part of the auxiliary adsorption tower 13 is fed from the back part of the nitrogen adsorption tower 4, and the pressure of the nitrogen adsorption tower 4 is increased.SELECTED DRAWING: Figure 1

Description

本発明は窒素、水分、CO等を含有する湿り空気からのコンパクトで高効率な酸素と
窒素の分離方法及び装置、特に吸着工程で塔後方に残留した酸素を補助吸着塔に吸着貯蔵
し、次の吸着工程の昇圧工程の昇圧気体として供給して、酸素製造効率を向上させた空気
からの酸素、窒素分離方法及び装置に関する。
The present invention is a compact and highly efficient oxygen and nitrogen separation method and apparatus from humid air containing nitrogen, moisture, CO 2, etc., in particular, adsorbing and storing oxygen remaining behind the tower in the adsorption step in the auxiliary adsorption tower, The present invention relates to a method and an apparatus for separating oxygen and nitrogen from air, which are supplied as a pressurized gas in a boosting process of the next adsorption process and improve oxygen production efficiency.

本発明に関連して現在最もよく使用されている窒素吸着剤を使用した酸素製造装置である
PSA−酸素を引用して背景技術を説明する。
Linde社(現UOP社モレキューラーシブス.デイビジョン)により工業的な製造
の開始された合成ゼオライトは、酸素−窒素2成分系において大きな窒素吸着量と窒素選
択性を有することが示されている。ここで500〜1,000kPaの高圧に空気を圧縮
してCa−A型ゼオライトを窒素吸着剤として充填された吸着塔に導いて空気の中の79
%を占める窒素を吸着して塔頂から93〜95 vol%の酸素を取り出す吸着工程と、吸着
窒素で飽和した吸着塔を大気圧に導いた後、塔頂から製品酸素の一部を流して窒素吸着剤
を再生する工程(向流パージ)から構成される2搭式の酸素製造装置が標準的である。(
高圧吸着−大気圧再生) 2,000mN/h以下の中小容量での酸素製造が可能なこ
とから、操作、保守が容易で、コンパクトなことがユーザに歓迎されて廃水処理、金属精
錬、ごみ焼却炉、医療用等を中心に普及している。PSA−酸素の電力原単位(1m
の酸素製造に必要な消費電力)の低減に着目して、300〜500 kPaの比較的低圧
に吸着圧力を低減し、その替わり50kPa程度の減圧再生を行う加圧吸着−減圧再生が
採用される場合もある。一段の電力原単位の低減のために、大気圧近傍で吸着を行い、再
生は10〜30kPaのかなりの真空で行われる大気圧吸着−減圧再生も採用されており
、これらの操作条件は、初期に開発された高圧吸着−大気圧再生よりも電力原単位低減に
優れている。吸着剤としては当初Caイオン交換A型ゼオライトが主として使用されたが
、サイクルタイムの短縮による装置コンパクト化のためには、吸着速度の大きな吸着剤が
必要なことから、Naイオン交換、Liイオン交換X型ゼオライトが採用されるようにな
っている。
しかし500mN/h以下の酸素製造では、電力原単位の低減は酸素製造のトータル
コストの低減はそれ程有効ではなく、設備費の低減が優先する。
例えば、中容量の酸素製造装置として15mN/hの酸素製造装置を例示すると、高
圧吸着−大気圧再生のPSA−酸素の設備費が700万円程度、電力原単位が1kWh/
N−Oであるので、これを大気圧吸着−真空再生に変更しても、設備費800万円
程度、電力原単位が0.45kWh/mN−Oとなり、電力量単価を20円/kWh
とすると1年間の電力コスト低減は、12万円/年から5.4万円/年の6.6万円/年
にとどまり、100万円の設備費増を吸収できず、大容量酸素製造で強調される電力原単
位の低減が、中小容量酸素製造では有効でないことが示される。
The background art will be described with reference to PSA-oxygen, which is an oxygen production apparatus using the most commonly used nitrogen adsorbent in connection with the present invention.
Synthetic zeolite, which has been industrially produced by Linde (currently UOP Molecular Sieves. Division), has been shown to have large nitrogen adsorption and nitrogen selectivity in an oxygen-nitrogen binary system. . Here, the air is compressed to a high pressure of 500 to 1,000 kPa and led to an adsorption tower packed with Ca-A type zeolite as a nitrogen adsorbent.
% Adsorption of nitrogen from the top of the tower to adsorb 93% to 95 vol% oxygen, and after the adsorption tower saturated with adsorbed nitrogen is introduced to atmospheric pressure, a part of product oxygen is allowed to flow from the top of the tower. A two-column oxygen production apparatus composed of a process of regenerating the nitrogen adsorbent (countercurrent purge) is standard. (
High pressure adsorption-Regeneration at atmospheric pressure) Oxygen production in small and medium capacity of 2,000m 3 N / h or less is possible, so that operation and maintenance are easy and compact are welcomed by users, wastewater treatment, metal refining, It is widely used mainly for garbage incinerators and medical use. Power unit of PSA-oxygen (1m 3 N
Focusing on the reduction of the power consumption required for oxygen production), pressure adsorption-reduced pressure regeneration is adopted in which the adsorption pressure is reduced to a relatively low pressure of 300 to 500 kPa, and instead reduced pressure regeneration of about 50 kPa is adopted. In some cases. In order to reduce the power consumption rate by one stage, adsorption is performed near atmospheric pressure, and regeneration is performed by atmospheric pressure adsorption-regeneration under a considerable vacuum of 10 to 30 kPa. It is superior to the high-pressure adsorption-atmospheric pressure regeneration developed in 1 Initially, Ca ion exchange A-type zeolite was mainly used as the adsorbent, but in order to make the equipment compact by shortening the cycle time, an adsorbent with a high adsorption rate is required, so Na ion exchange, Li ion exchange X-type zeolite has been adopted.
However, in the oxygen production of 500 m 3 N / h or less, the reduction of the power consumption rate is not so effective for the reduction of the total cost of the oxygen production, and the reduction of the equipment cost is given priority.
For example, a 15 m 3 N / h oxygen production apparatus is illustrated as a medium capacity oxygen production apparatus. The equipment cost of high pressure adsorption-atmospheric pressure regeneration PSA-oxygen is about 7 million yen, and the power unit is 1 kWh /
Since it is m 3 N-O 2 , even if it is changed to atmospheric pressure adsorption-vacuum regeneration, the equipment cost is about 8 million yen, the power intensity is 0.45 kWh / m 3 N-O 2 ¥ 20 / kWh
If this is the case, the annual power cost reduction will be 66,000 yen / year, from 120,000 yen / year to 54,000 yen / year. It is shown that the reduction in power intensity emphasized by is not effective in small and medium volume oxygen production.

本発明はこのような従来技術における問題点を解決し、従来の酸素製造法よりも安価で
電力原単位も低値を維持する低トータル酸素製造コストの空気からの酸素、窒素分離方法
及びそのための装置を提供することを目的とする。
The present invention solves such problems in the prior art, and is a method for separating oxygen and nitrogen from air with a low total oxygen production cost that is cheaper than conventional oxygen production methods and maintains a low power consumption rate, and for that purpose An object is to provide an apparatus.

本発明は前記課題を解決する手段として、前方に水分吸着剤を充填し、後方に窒素吸着
剤を充填した窒素吸着塔に、大気圧以上の高圧で湿り空気を供給して、窒素、水分、CO
等を除去して塔後方から酸素を回収して(窒素吸着工程)、酸素濃度が低下する前に、塔
後方に設置した窒素吸着剤を充填した補助吸着塔の前方と窒素吸着塔の後方を連結して、
塔後方に残留する酸素を補助吸着塔に移行し(酸素回収工程)、高圧の窒素吸着塔を塔前
方から系外に開放して、吸着した窒素を放出して大気圧に減圧し(減圧再生工程)、大気
圧の窒素吸着塔の後方と補助吸着塔の前方を連結して回収した酸素を窒素吸着塔の後方か
ら供給して、窒素吸着塔の圧力を上昇し(昇圧工程)、湿り空気を供給する窒素吸着工程
に戻ることを特長とする、高圧窒素吸着−大気圧再生の1塔式圧力スイング−酸素製造方
法および装置を提案する。
As a means for solving the above-mentioned problems, the present invention supplies wet air at a high pressure of atmospheric pressure or higher to a nitrogen adsorption tower filled with a moisture adsorbent in the front and filled with a nitrogen adsorbent in the rear, so that nitrogen, moisture, CO
2 is removed and oxygen is recovered from the rear of the tower (nitrogen adsorption step), before the oxygen concentration decreases, before the auxiliary adsorption tower filled with nitrogen adsorbent installed behind the tower and behind the nitrogen adsorption tower Concatenate
Oxygen remaining behind the tower is transferred to the auxiliary adsorption tower (oxygen recovery process), the high-pressure nitrogen adsorption tower is opened outside the system from the front of the tower, and the adsorbed nitrogen is released to reduce the pressure to atmospheric pressure (reduced pressure regeneration). Process), supplying the recovered oxygen by connecting the back of the nitrogen adsorption tower at the atmospheric pressure and the front of the auxiliary adsorption tower from the back of the nitrogen adsorption tower to increase the pressure of the nitrogen adsorption tower (pressure raising process), and humid air The present invention proposes a high pressure nitrogen adsorption-atmospheric pressure regeneration single tower pressure swing-oxygen production method and apparatus characterized by returning to the nitrogen adsorption step of supplying oxygen.

先述の15mN/hの酸素製造装置で比較すると、従来、高圧吸着−大気圧再生のPS
A−酸素が、空気圧縮機、窒素吸着塔2塔、バルブ8個を基本構造として設備費が700
万円程度、電力原単位が1kWh/mN−O、1年間の消費電力が、電力量単価を2
0円/kWhとすると1年間の電力コストが、12万円/年であるが、本発明では、高圧
吸着−大気圧再生のPSA−酸素が、空気圧縮機、窒素吸着塔1塔、補助吸着塔バルブ4
個を基本構造として設備費が400万円程度に削減され、補助吸着塔による残留酸素の回
収と昇圧工程への供給で、酸素回収率が従来の40%から60%程度に増大するため、電
力原単位が0.8kWh/mN−Oに低減され、1年間の消費電力が、電力量単価を
20円/kWhとすると1年間の電力コストが、9.6万円/年に低減され、コンパクト
で、低設備費、低変動費の空気から酸素と窒素を分離する方法および装置を提供すること
が出来る。
Compared with the above-mentioned 15m 3 N / h oxygen production apparatus, the conventional high pressure adsorption-PS regeneration of atmospheric pressure
A-Oxygen costs 700 units with a basic structure consisting of an air compressor, 2 nitrogen adsorption towers and 8 valves.
About 10,000 yen, the power consumption is 1 kWh / m 3 N-O 2 , and the annual power consumption is 2
If it is 0 yen / kWh, the power cost per year is 120,000 yen / year. In the present invention, PSA-oxygen of high pressure adsorption-regeneration of atmospheric pressure is converted into an air compressor, one nitrogen adsorption tower, auxiliary adsorption. Tower valve 4
Since the equipment cost is reduced to about 4 million yen with the basic structure of the individual, the recovery of residual oxygen by the auxiliary adsorption tower and the supply to the pressurization process will increase the oxygen recovery rate from the conventional 40% to about 60%. When the basic unit is reduced to 0.8 kWh / m 3 N-O 2 and the annual power consumption is 20 yen / kWh, the annual power cost is reduced to 96,000 yen / year. It is possible to provide a method and apparatus for separating oxygen and nitrogen from air that is compact and has low equipment costs and low variable costs.

本発明の方法の一実施態様を実施するフローを示す概略図である。FIG. 2 is a schematic diagram illustrating a flow for carrying out an embodiment of the method of the present invention.

窒素吸着塔に充填する窒素吸着剤としては、Liイオン交換、Naイオン交換、Caイ
オン交換のX型ゼオライトを1種または2種以上使用することが望ましく、補助吸着塔に
充填する窒素吸着剤としても、Liイオン交換、Naイオン交換、Caイオン交換のX型
ゼオライトを1種または2種以上を使用することが望ましい。
As the nitrogen adsorbent packed in the nitrogen adsorption tower, it is desirable to use one or more of Li ion exchange, Na ion exchange, and Ca ion exchange X-type zeolite. However, it is desirable to use one or more X-type zeolites of Li ion exchange, Na ion exchange, and Ca ion exchange.

次に図面を参照して本発明の処理装置を説明する。図1に空気からの本発明の装置を
適用した1塔式圧力スイング法(以下PSA−酸素)フローシートの一例を示す。図1に
おいてPSA−酸素を構成する、(吸着工程)→(残留酸素回収工程)→(減圧再生工程
)→(昇圧工程)の各工程ごとに説明する。
Next, the processing apparatus of the present invention will be described with reference to the drawings. FIG. 1 shows an example of a one-column pressure swing method (hereinafter referred to as PSA-oxygen) flow sheet using the apparatus of the present invention from air. The steps of (adsorption process) → (residual oxygen recovery process) → (reduced pressure regeneration process) → (pressure increase process) constituting PSA-oxygen in FIG. 1 will be described.

(吸着工程)外部空気を流路1から圧縮機2、バルブ3を通じて空気流量1,210リッ
トルN/min、吸着圧力500kPa−absで、吸着塔容量130リットルの窒素吸
着塔4に、吸着時間30秒で供給する。窒素吸着塔4には、前方に水分吸着剤5として比
表面積700m/g以上のシリカゲルをウオッシュコートしたハニカムが、24リット
ル充填されており、後方には窒素吸着塔充填窒素吸着剤6として、1.2mmφのLiイ
オン交換X型ゼオライト(SiO/Al比2.5)が71リットル充填されてい
る。供給された空気の水分が水分吸着剤5で除去され、COおよび窒素が窒素吸着塔充
填窒素吸着剤6で除去されると、窒素吸着塔4の後方から酸素が、酸素濃度90vol%
程度で、未吸着の窒素、アルゴンとともにバルブ7、製品酸素タンク8、バルブ9、流路
10から流過する。
(Adsorption process) External air is passed through the flow path 1 through the compressor 2 and the valve 3 at an air flow rate of 1,210 liters N / min, an adsorption pressure of 500 kPa-abs, and an adsorption time of 30 liters in an adsorption tower capacity of 130 liters. Supply in seconds. The nitrogen adsorption tower 4 is packed with 24 liters of honeycomb, which is washed with silica gel having a specific surface area of 700 m 2 / g or more as a moisture adsorbent 5 in the front, and as the nitrogen adsorption tower-filled nitrogen adsorbent 6 in the rear, It is filled with 71 liters of 1.2 mmφ Li ion exchange X-type zeolite (SiO 2 / Al 2 O 3 ratio 2.5). When water in the supplied air is removed by the moisture adsorbent 5 and CO 2 and nitrogen are removed by the nitrogen adsorbing tower-filled nitrogen adsorbent 6, oxygen is added from the rear of the nitrogen adsorption tower 4 to an oxygen concentration of 90 vol%.
About, it flows through the valve 7, the product oxygen tank 8, the valve 9, and the flow path 10 together with unadsorbed nitrogen and argon.

(残留酸素回収工程)
吸着工程の進行に伴い、窒素吸着塔4の窒素吸着量が増大して流過酸素濃度が低下する。
流過酸素濃度が低下する直前に、圧縮機2を停止して、バルブ3,バルブ7を閉として、
バルブ11を開とすると、窒素吸着塔4の後方に残留する酸素は、バルブ11を通じて補
助吸着塔充填窒素吸着剤12の充填された補助吸着塔13に移行する。補助吸着塔13の
容量としては、30リットルであり、この中に補助吸着塔充填窒素吸着剤12が23リッ
トル充填されている。このため、窒素吸着塔4の圧力は500kPa−absから350
kPa程度に低下し、補助吸着塔13の圧力は300kPa程度に上昇する。補助吸着塔
13に充填される補助吸着塔充填窒素吸着剤12としては、酸素に比べて窒素を選択的に
吸着する、Liイオン交換、Naイオン交換、Caイオン交換のX型ゼオライトを1種ま
たは2種以上使用するのが好ましい。前述の吸着工程での酸素の回収率は40%程度にと
どまり、残る60%の酸素は吸着塔の死容積部および窒素吸着剤への共吸着酸素として残
留しており、酸素の回収はそれ程効率の高いものではない。
ここで補助吸着塔13に窒素吸着塔4後方から高圧気体を移すと、窒素吸着塔4に残留す
る酸素は更に20%程度回収され、全回収率が60%に達する。
なお補助吸着塔13では、補助吸着塔充填窒素吸着剤12への窒素吸着が酸素吸着よりも
選択的なため、補助吸着塔充填窒素吸着剤12には窒素が選択的に吸着され、死容積部の
酸素濃度は上昇する。
これは、後述する昇圧工程での塔後方への高濃度酸素の供給のために非常に重要である。
残留酸素回収工程は、1-5秒程度で完了する。
(Residual oxygen recovery process)
As the adsorption process proceeds, the nitrogen adsorption amount of the nitrogen adsorption tower 4 increases and the flow-over oxygen concentration decreases.
Immediately before the flow-over oxygen concentration decreases, the compressor 2 is stopped and the valves 3 and 7 are closed.
When the valve 11 is opened, oxygen remaining behind the nitrogen adsorption tower 4 is transferred to the auxiliary adsorption tower 13 filled with the auxiliary adsorption tower-filled nitrogen adsorbent 12 through the valve 11. The capacity of the auxiliary adsorption tower 13 is 30 liters, and 23 liters of the auxiliary adsorption tower packed nitrogen adsorbent 12 is filled therein. For this reason, the pressure of the nitrogen adsorption tower 4 is from 500 kPa-abs to 350.
The pressure is reduced to about kPa, and the pressure in the auxiliary adsorption tower 13 is increased to about 300 kPa. As the auxiliary adsorption tower packed nitrogen adsorbent 12 packed in the auxiliary adsorption tower 13, one type of X-type zeolite of Li ion exchange, Na ion exchange, and Ca ion exchange that selectively adsorbs nitrogen compared to oxygen is used. Two or more are preferably used. The recovery rate of oxygen in the aforementioned adsorption process is only about 40%, and the remaining 60% of oxygen remains as co-adsorbed oxygen in the dead volume of the adsorption tower and the nitrogen adsorbent, and the recovery of oxygen is so efficient. Is not expensive.
Here, when the high-pressure gas is transferred from the rear of the nitrogen adsorption tower 4 to the auxiliary adsorption tower 13, about 20% of the oxygen remaining in the nitrogen adsorption tower 4 is further recovered, and the total recovery rate reaches 60%.
In the auxiliary adsorption tower 13, nitrogen adsorption to the auxiliary adsorption tower packed nitrogen adsorbent 12 is more selective than oxygen adsorption. Therefore, nitrogen is selectively adsorbed on the auxiliary adsorption tower filled nitrogen adsorbent 12, and the dead volume portion The oxygen concentration increases.
This is very important for the supply of high-concentration oxygen to the rear of the column in the pressurization step described later.
The residual oxygen recovery process is completed in about 1-5 seconds.

(減圧再生工程)
(残留酸素回収工程)で窒素吸着塔4の圧力は、350kPa−abs程度に低下したの
で、圧縮機2を引き続き停止して、バルブ3,バルブ7,バルブ11を閉として、バルブ
14を開とすると、窒素吸着塔充填窒素吸着剤6から吸着窒素が離脱し、更に向流に流過
する窒素により水分吸着剤5から水分が離脱し、窒素吸着塔充填窒素吸着剤6、水分吸着
剤5は再生され、再び、水分、窒素、COを吸着できるようになる。ここで窒素吸着塔
4の圧力は100kPa−abs(大気圧)に低下する。(減圧再生工程)は、5-10
秒程度で完了する。この間、バルブ7は閉、バルブ9を開としているため、(吸着工程)
で回収された酸素は、製品酸素タンク8に貯蔵されているため、流路10からは全工程で
連続して酸素が流過する。
(Reduced pressure regeneration process)
In the (residual oxygen recovery step), the pressure in the nitrogen adsorption tower 4 has decreased to about 350 kPa-abs. Therefore, the compressor 2 is continuously stopped, the valves 3, 7 and 11 are closed, and the valve 14 is opened. Then, the adsorbed nitrogen is desorbed from the nitrogen adsorbing tower packed nitrogen adsorbent 6, and the water is further desorbed from the water adsorbing agent 5 by the nitrogen flowing in the counterflow. It is regenerated and can again adsorb moisture, nitrogen, and CO 2 . Here, the pressure of the nitrogen adsorption tower 4 is reduced to 100 kPa-abs (atmospheric pressure). (Decompression regeneration step) is 5-10
Complete in seconds. During this time, the valve 7 is closed and the valve 9 is open (adsorption process)
Since the oxygen recovered in the above is stored in the product oxygen tank 8, oxygen flows continuously from the flow path 10 in all steps.

(昇圧工程)
100kPa−abs(大気圧)の窒素吸着塔の後方のバルブ11のみ開とすると(バ
ルブ3,バルブ7,バルブ14を閉とする。)、補助吸着塔13から先ず死容積部の比較
的酸素濃度の高い気体が、窒素吸着塔4後方から窒素吸着塔4に供給され、その後補助吸
着塔充填窒素吸着剤12から吸着された酸素および共吸着窒素が離脱して供給酸素濃度が
上昇するため、窒素吸着塔後方には高濃度の酸素が供給される。このため、窒素吸着塔4
の酸素濃度分布は、吸着工程開始時に塔前方の酸素濃度は低く、塔後方の酸素濃度分布が
高い、効率的な空気からの酸素と窒素分離の可能な状態となっている。窒素吸着塔4の圧
力は100kPa−absから200kPa−absに上昇する。(補助吸着塔13の圧
力は窒素吸着塔4とほぼ同一圧力の、300kPaから200kPaに低下する。)
昇圧工程は、3-5秒程度で完了する。
(昇圧工程)で、(残留酸素回収工程)で補助吸着塔13に回収された残留酸素が昇圧
に使用されているため、1)酸素回収率を向上し、2)窒素吸着塔後方の酸素濃度を高濃
度に維持して酸素/窒素分離効率を向上し、3)円滑な吸着圧力の上昇を同時に達成する
ことが可能である。
(Pressure increase process)
If only the valve 11 behind the nitrogen adsorption tower of 100 kPa-abs (atmospheric pressure) is opened (valve 3, valve 7 and valve 14 are closed), the oxygen concentration in the dead volume portion is first relatively increased from the auxiliary adsorption tower 13. Gas is supplied from the rear of the nitrogen adsorption tower 4 to the nitrogen adsorption tower 4, and then the oxygen adsorbed from the auxiliary adsorption tower packed nitrogen adsorbent 12 and the coadsorbed nitrogen are released to increase the supply oxygen concentration. A high concentration of oxygen is supplied behind the adsorption tower. For this reason, the nitrogen adsorption tower 4
The oxygen concentration distribution in the column is such that the oxygen concentration in the front of the tower is low at the start of the adsorption process and the oxygen concentration distribution in the rear of the tower is high, so that oxygen and nitrogen can be efficiently separated from the air. The pressure in the nitrogen adsorption tower 4 increases from 100 kPa-abs to 200 kPa-abs. (The pressure in the auxiliary adsorption tower 13 decreases from 300 kPa to 200 kPa, which is substantially the same pressure as the nitrogen adsorption tower 4.)
The boosting process is completed in about 3-5 seconds.
Since the residual oxygen recovered in the auxiliary adsorption tower 13 in the (residual oxygen recovery process) is used for pressure increase in (pressure increase process), 1) the oxygen recovery rate is improved, and 2) the oxygen concentration behind the nitrogen adsorption tower Can be maintained at a high concentration to improve the oxygen / nitrogen separation efficiency, and 3) a smooth increase in the adsorption pressure can be achieved simultaneously.

表1に空気からの本発明の装置を適用した1塔式圧力スイング法(以下PSA−酸素)
フローシートの、PSA−酸素を構成する、(吸着工程)→(残留酸素回収工程)→(減
圧再生工程)→(昇圧工程)のバルブの開閉、圧縮機の運転・停止、各工程の標準的な所
要時間を示す、シーケンステーブルを示す。
Table 1 One-column pressure swing method (hereinafter referred to as PSA-oxygen) using the apparatus of the present invention from air
Open / close valves, compressor operation / stop, standard for each process of PSA-oxygen of flow sheet, (adsorption process) → (residual oxygen recovery process) → (reduced pressure regeneration process) → (pressurization process) Shows a sequence table showing the required time.

以下実施例により本発明をさらに具体的に説明する。
本実施例の1塔式PSA−酸素製造装置の仕様を表2に示す。
Hereinafter, the present invention will be described more specifically with reference to examples.
Table 2 shows the specifications of the single-column PSA-oxygen production apparatus of this example.


本装置は、酸素製造量85−170リットルN/分(5−10mN/h)を目標として
製作したもので、窒素吸着塔4には、水分吸着剤ハニカム24リットル、窒素吸着剤とし
て71リットルが、充填されており、補助吸着塔13には、補助吸着塔充填窒素吸着剤1
2が23リットル充填されている。

This apparatus was manufactured with a target of oxygen production of 85-170 liter N / min (5-10 m 3 N / h). The nitrogen adsorption tower 4 has a moisture adsorbent honeycomb of 24 liters and a nitrogen adsorbent of 71. The auxiliary adsorption tower 13 is filled with liters, and the auxiliary adsorption tower-filled nitrogen adsorbent 1
2 is filled with 23 liters.

本装置の操作条件を表3に示す。 Table 3 shows the operating conditions of this apparatus.

本装置は、吸着圧力500kPa−abs、再生終了圧力100kPa−abs、補助吸
着塔13残留酸素回収終了圧力300kPa−abs、補助吸着塔13昇圧終了圧力20
0kPa−abs、1サイクル39秒、窒素吸着剤としては窒素吸着塔4、補助吸着塔1
3ともLiイオン交換X型ゼオライトを使用して操作して、空気からの酸素と窒素の分離
を行い、酸素製造量170リットルN/分(5−10mN/h)、酸素濃度90vol
%の性能が確認されたが、この時の原料空気供給量は、1,210リットルN/分であっ
た。比較対象としては補助吸着塔13を使用せず、残留酸素回収工程、昇圧を省略し、昇
圧については、後流の製品酸素タンク8からの製品酸素を使用した、1塔式PSA−酸素
の酸素製造の空気からの酸素と窒素の分離性能を示す。
窒素吸着塔4の窒素吸着性能が大幅に低下するため酸素製造量は、比較対象では、本発明
の40%程度にとどまり、また供給空気量/製品酸素量比は増大しており、残留酸素回収
工程を付加することで著しく性能向上が改善されることがわかる。
This apparatus has an adsorption pressure of 500 kPa-abs, a regeneration end pressure of 100 kPa-abs, an auxiliary adsorption tower 13 residual oxygen recovery end pressure of 300 kPa-abs, and an auxiliary adsorption tower 13 of a pressure increase end pressure of 20.
0 kPa-abs, 1 cycle 39 seconds, as nitrogen adsorbent, nitrogen adsorption tower 4, auxiliary adsorption tower 1
All three were operated using Li ion-exchanged X-type zeolite to separate oxygen and nitrogen from air, producing oxygen of 170 liters N / min (5-10 m 3 N / h), and oxygen concentration of 90 vol.
% Was confirmed, but the feed rate of raw material air at this time was 1,210 liters N / min. As a comparison object, the auxiliary adsorption tower 13 is not used, the residual oxygen recovery step and the pressure increase are omitted, and for the pressure increase, the product oxygen from the downstream product oxygen tank 8 is used, and the oxygen of one tower PSA-oxygen is used. The separation performance of oxygen and nitrogen from the production air is shown.
Since the nitrogen adsorption performance of the nitrogen adsorption tower 4 is greatly reduced, the amount of oxygen produced is only about 40% of that of the present invention, and the ratio of supply air / product oxygen is increased. It can be seen that the performance improvement is remarkably improved by adding the process.

従来から使用されている窒素吸着剤であるCaイオン交換A型ゼオライトと、本発明の窒
素吸着剤、1)Liイオン交換X型ゼオライト、2)Naイオン交換X型ゼオライト、3
)Caイオン交換X型ゼオライトの酸素/窒素分離性能の比較を表4に示す。
Conventionally used nitrogen adsorbent, Ca ion exchange A-type zeolite, nitrogen adsorbent of the present invention, 1) Li ion exchange X type zeolite, 2) Na ion exchange X type zeolite, 3
Table 4 shows a comparison of oxygen / nitrogen separation performance of Ca ion-exchanged X-type zeolite.

Liイオン交換X型ゼオライトが最も酸素製造量が多く、Caイオン交換X型ゼオライト
、Naイオン交換X型ゼオライトがこれに続く。原料空気量/製品酸素量比は7程度で大
きな差はない。これに対しCaイオン交換A型ゼオライトでは酸素製造量がLiイオン交
換X型ゼオライトの60%程度に低下し、原料空気量/製品酸素量比も8.6と増加し、
その分原料空気圧縮機2は120%大容量のものが必要となる。
Li ion-exchanged X-type zeolite has the largest amount of oxygen production, followed by Ca ion-exchanged X-type zeolite and Na ion-exchanged X-type zeolite. The ratio of the raw material air amount / product oxygen amount is about 7, which is not significantly different. On the other hand, in the Ca ion exchange A type zeolite, the oxygen production amount is reduced to about 60% of the Li ion exchange X type zeolite, and the raw material air amount / product oxygen amount ratio is increased to 8.6,
Accordingly, the raw material air compressor 2 is required to have a capacity of 120%.

本発明の補助吸着塔13から補助吸着塔充填窒素吸着剤12をはずして未充填の状態で実
施例1の操作条件で実施した。補助吸着塔13を使用しない場合、補助吸着塔13から補
助吸着塔充填窒素吸着剤12をはずした残留酸素回収タンクとして使用した本項の実施例
2と、補助吸着塔13に補助吸着塔充填窒素吸着剤12を充填して実施した前項の実施例
1の比較を行った。
The auxiliary adsorption tower packed nitrogen adsorbent 12 was removed from the auxiliary adsorption tower 13 of the present invention, and the unadsorbed state was carried out under the operating conditions of Example 1. When the auxiliary adsorption tower 13 is not used, Example 2 of this section used as a residual oxygen recovery tank in which the auxiliary adsorption tower-packed nitrogen adsorbent 12 is removed from the auxiliary adsorption tower 13, and the auxiliary adsorption tower 13 is filled with the auxiliary adsorption tower-packed nitrogen. A comparison was made with Example 1 in the previous section, which was carried out by filling the adsorbent 12.

実施例2の比較した結果を表5に示す。 Table 5 shows a comparison result of Example 2.

実施例1の補助吸着塔13に補助吸着塔充填窒素吸着剤12を充填して、残留酸素回収工
程、昇圧工程に使用する方法および装置が、酸素製造量が170リットルN/分、原料空
気量/製品酸素量比は7程度で最も高い性能を示すが、本実施例(実施例2)の、補助吸着
塔13に補助吸着塔充填窒素吸着剤12を充填しないが(未充填)、残留酸素タンクとして
、残留酸素回収工程、昇圧工程に使用する方法および装置でも、酸素製造量が150リッ
トルN/分、原料空気量/製品酸素量比は7.2程度にとどまり、従来法に対する新規性
のあることが確認された。
The method and apparatus for filling the auxiliary adsorption tower 13 of Example 1 with the auxiliary adsorption tower-filled nitrogen adsorbent 12 and using it in the residual oxygen recovery step and the pressurization step have an oxygen production amount of 170 liters N / min and a raw material air amount. / The product oxygen amount ratio is about 7 and shows the highest performance. In this example (Example 2), the auxiliary adsorption column 13 is not filled with the nitrogen adsorbent 12 filled with the auxiliary adsorption column (unfilled), but the residual oxygen As a tank, the method and apparatus used for the residual oxygen recovery process and the pressurization process also have an oxygen production amount of 150 liters N / min and a raw material air amount / product oxygen amount ratio of only 7.2. It was confirmed that there was.

本発明は、1−100mN/h程度の中小容量の酸素発生方法および装置に関し、酸素
富化燃焼、環境装置、化学装置に使用する低コスト、コンパクトで高効率な空気からの吸
着法による空気からの酸素と窒素の分離に関する。
The present invention relates to a method and apparatus for generating small and medium volumes of about 1 to 100 m 3 N / h, and is based on a low-cost, compact and highly efficient adsorption method for air used in oxygen-enriched combustion, environmental equipment, and chemical equipment. It relates to the separation of oxygen and nitrogen from the air.

流路―――1
圧縮機―――2
バルブ―――3、7、9、11、14
窒素吸着塔―――4
水分吸着剤―――5
窒素吸着塔充填窒素吸着剤―――6
製品酸素タンク―――8
流路―――10
補助吸着塔充填窒素吸着剤12
補助吸着塔―――13
Channel ---- 1
Compressor--2
Valve-3, 7, 9, 11, 14
Nitrogen adsorption tower--4
Moisture absorbent--5
Nitrogen adsorption tower packed nitrogen adsorbent --- 6
Product oxygen tank-8
Flow path--10
Auxiliary adsorption tower packed nitrogen adsorbent 12
Auxiliary adsorption tower--13

本発明は吸着分離によって空気から酸素を分離して取得する方法およびそのための装置に関し、詳しくは、窒素吸着塔の後方に窒素吸着剤が充填された補助吸着塔を設け、この補助吸着塔を利用する独特の吸着操作によって酸素の製造効率が向上した酸素の取得方法およびそのような方法に用いられるコンパクトな装置に関するThe present invention relates to a method for separating and obtaining oxygen from air by adsorption separation and an apparatus therefor. More specifically, an auxiliary adsorption tower filled with a nitrogen adsorbent is provided behind the nitrogen adsorption tower, and the auxiliary adsorption tower is used. The present invention relates to a method for obtaining oxygen in which the production efficiency of oxygen is improved by a unique adsorption operation, and a compact apparatus used in such a method .

本発明者等吸着分離によって空気から酸素を分離して取得する装置において前記のような補助吸着塔を設けることによって、また、この装置を用いて、下記のような1〜4の一連の工程を1回または繰り返して2回以上遂行することによって上記の課題が解決されることを見出した。
したがって、本発明によれば、
1.前方に水分吸着剤が充填され、それに続いて後方に窒素吸着剤が充填されている窒素吸着塔に圧縮機で大気圧以上の高圧で空気を供給して、空気中の水分を水分吸着剤に吸着させ、それに続いて空気中のCO および窒素を窒素吸着剤に吸着させて、酸素に富む空気を生成させ、これを窒素吸収塔の後方に設けられた製品酸素タンクに貯蔵して、酸素に富む空気を取得する窒素吸着工程、
2.前記窒素吸着塔の窒素吸着剤で窒素が除去された後に窒素吸着塔の後方に残留する空気中の酸素濃度が低下する前に、窒素吸着塔から製品酸素タンクに向かう酸素の流れを止めて、窒素吸着塔の後方から補助吸着塔に向かう流路を開くことによって窒素吸着塔後方に残留する酸素を補助吸着塔に移行させ、この移行した酸素を補助吸着塔で回収する残留酸素回収工程、
3.前記1の窒素吸着工程では閉じていた、窒素吸着塔で吸着されていた窒素、水分およびCO を系外に放出させるために設けられていた流路を開いて、高圧に保たれていた窒素吸着塔を大気圧に減圧することにより、窒素、水分およびCO を大気中に放出させて窒素吸着剤の吸着力を再生させる減圧再生工程、
4.前記2の残留酸素回収工程により補助吸着塔で回収された高圧の酸素を窒素吸着塔の後方からこの窒素吸着塔に供給して窒素吸着塔の圧力を上昇させる昇圧工程、および
からなる一連の工程を1回または繰り返して2回以上遂行することを特徴とする、吸着分離によって空気から酸素を分離して取得する方法、および
前方に水分吸着剤、それに続く後方に窒素吸着剤が充填された窒素吸着塔、窒素吸着塔の後方で流路を介して該窒素吸着塔にそれぞれ連結した製品酸素タンクおよび窒素吸着剤が充填された補助吸着塔、窒素吸着塔に大気圧以上の高圧で空気を供給するための圧縮機、および窒素吸着塔から窒素、水分およびCO を窒素吸着塔外部に放出するために窒素吸着塔の前方に設けられた流路を含む、請求項1又は2に記載の方法に用いられる、吸着分離によって空気から酸素を分離して取得するための装置、
が提供される。
By the present inventors have provided the auxiliary adsorption column, such as in a device for obtaining and separating oxygen from air by adsorption separation, also by using this device, 1-4 a series of steps as described below It has been found that the above-mentioned problems can be solved by performing the above once or repeatedly twice.
Therefore, according to the present invention,
1. Air is supplied to the nitrogen adsorption tower, which is filled with moisture adsorbent in the front and then nitrogen adsorbent in the back, with a compressor at high pressure above atmospheric pressure, and moisture in the air is converted into moisture adsorbent. Next, CO 2 and nitrogen in the air are adsorbed by the nitrogen adsorbent to generate oxygen-enriched air, which is stored in a product oxygen tank provided behind the nitrogen absorption tower, and oxygen Nitrogen adsorption process to acquire rich air,
2. Before the oxygen concentration in the air remaining behind the nitrogen adsorption tower after nitrogen is removed by the nitrogen adsorbent of the nitrogen adsorption tower, the flow of oxygen from the nitrogen adsorption tower to the product oxygen tank is stopped, A residual oxygen recovery step of transferring oxygen remaining behind the nitrogen adsorption tower to the auxiliary adsorption tower by opening a flow path from the rear of the nitrogen adsorption tower to the auxiliary adsorption tower, and recovering the transferred oxygen with the auxiliary adsorption tower,
3. Nitrogen that was kept in a high pressure by opening a channel provided to release nitrogen, moisture, and CO 2 that had been adsorbed in the nitrogen adsorption tower, out of the system , that was closed in the nitrogen adsorption step of 1 above. A reduced pressure regeneration step of regenerating the adsorption power of the nitrogen adsorbent by releasing nitrogen, moisture and CO 2 into the atmosphere by depressurizing the adsorption tower to atmospheric pressure ;
4). A pressure increasing step for increasing the pressure of the nitrogen adsorption tower by supplying high-pressure oxygen recovered by the auxiliary adsorption tower in the second residual oxygen recovery process to the nitrogen adsorption tower from the rear of the nitrogen adsorption tower; and
A method of separating and obtaining oxygen from air by adsorptive separation, characterized in that a series of steps consisting of
A nitrogen adsorbing tower filled with a moisture adsorbent in the front and a nitrogen adsorbent following it, and a product oxygen tank and a nitrogen adsorbent connected to the nitrogen adsorbing tower via a flow path behind the nitrogen adsorbing tower, respectively. The auxiliary adsorption tower, the compressor for supplying air to the nitrogen adsorption tower at a pressure higher than atmospheric pressure, and the front of the nitrogen adsorption tower for releasing nitrogen, moisture and CO 2 from the nitrogen adsorption tower to the outside of the nitrogen adsorption tower A device for separating and obtaining oxygen from air by adsorption separation, which is used in the method according to claim 1, comprising a flow path provided in
Is provided.

実施例1の補助吸着塔13に補助吸着塔充填窒素吸着剤12を充填して、残留酸素回収工程、昇圧工程に使用する方法および装置が、酸素製造量が170リットルN/分、原料空気量/製品酸素量比は7程度で最も高い性能を示すが、本実施例(実施例2)の、補助吸着塔13に補助吸着塔充填窒素吸着剤12を充填しないが(未充填)、残留酸素タンクとして、残留酸素回収工程、昇圧工程に使用する方法および装置でも、酸素製造量が150リットルN/分、原料空気量/製品酸素量比は7.2程度にとどまり、本発明は二つの従来法よりも優れていることが確認された。 The method and apparatus for filling the auxiliary adsorption tower 13 of Example 1 with the auxiliary adsorption tower-filled nitrogen adsorbent 12 and using it in the residual oxygen recovery step and the pressurization step have an oxygen production amount of 170 liters N / min and a raw material air amount. / The product oxygen amount ratio is about 7 and shows the highest performance. In this example (Example 2), the auxiliary adsorption tower 13 is not filled with the nitrogen adsorbent 12 filled with the auxiliary adsorption tower (unfilled), but the residual oxygen as a tank, a residual oxygen recovery process, also a method and apparatus for using the boost process, oxygen production amount is 150 l N / min, the feed air amount / oxygen product amount ratio remains at about 7.2, the present invention is two conventional It was confirmed to be superior to the method .

1、10 流路1, 10 flow path
2 圧縮機2 Compressor
3、7、9、11、14 バルブ3, 7, 9, 11, 14 Valve
4 窒素吸着塔4 Nitrogen adsorption tower
5 水分吸着剤5 Moisture absorbent
6 窒素吸着塔充填窒素吸着剤6 Nitrogen adsorption tower packed nitrogen adsorbent
8 製品酸素タンク8 Product oxygen tank
12 補助吸着塔充填窒素吸着剤12 Auxiliary adsorption tower packed nitrogen adsorbent
13 補助吸着塔13 Auxiliary adsorption tower

Claims (5)

前方に水分吸着剤を充填し、後方に窒素吸着剤を充填した窒素吸着塔に、大気圧以上
の高圧で湿り空気を供給して、窒素、水分、CO等を除去して塔後方から酸素を回収し
て(窒素吸着工程)、酸素濃度が低下する前に、塔後方に設置した窒素吸着剤を充填した補
助吸着塔の前方と窒素吸着塔の後方を連結して、塔後方に残留する酸素を補助吸着塔に移
行し(残留酸素回収工程)、高圧の窒素吸着塔を塔前方から系外に開放して、吸着した窒
素を放出して大気圧に減圧し(減圧再生工程)、大気圧の窒素吸着塔の後方と補助吸着塔
の前方を連結して回収した酸素を窒素吸着塔の後方から供給して、窒素吸着塔の圧力を上
昇し(昇圧工程)、湿り空気を供給する窒素吸着工程に戻ることを特長とする、空気から
の酸素と窒素の分離方法および装置。
Moist air is supplied at a high pressure of atmospheric pressure or higher to a nitrogen adsorption tower filled with a moisture adsorbent in the front and filled with a nitrogen adsorbent in the rear to remove nitrogen, moisture, CO 2 and the like from the rear of the tower. (Nitrogen adsorption step), before the oxygen concentration decreases, connect the front of the auxiliary adsorption tower filled with nitrogen adsorbent installed behind the tower and the rear of the nitrogen adsorption tower, and remain behind the tower Oxygen is transferred to the auxiliary adsorption tower (residual oxygen recovery process), the high-pressure nitrogen adsorption tower is opened out of the system from the front of the tower, the adsorbed nitrogen is released, and the pressure is reduced to atmospheric pressure (decompression regeneration process). Nitrogen is supplied by supplying oxygen from the back of the nitrogen adsorption tower by connecting the back of the nitrogen adsorption tower at the atmospheric pressure and the front of the auxiliary adsorption tower from the rear of the nitrogen adsorption tower to increase the pressure of the nitrogen adsorption tower (pressure increase process) and supply humid air Method and apparatus for separating oxygen and nitrogen from air, characterized by returning to the adsorption process .
請求項1で窒素吸着塔に充填する窒素吸着剤としてLiイオン交換、Naイオン交換、
Caイオン交換のX型ゼオライトを1種または2種以上使用する、空気からの酸素と窒素
の分離方法および装置。
Li ion exchange, Na ion exchange as the nitrogen adsorbent packed in the nitrogen adsorption tower in claim 1,
A method and apparatus for separating oxygen and nitrogen from air, using one or more Ca ion-exchanged X-type zeolites.
請求項1で補助吸着塔に充填する窒素吸着剤としてLiイオン交換、Naイオン交換、
Caイオン交換のX型ゼオライトを1種または2種以上を使用する、空気からの酸素と窒
素の分離方法および装置。
Li ion exchange, Na ion exchange as the nitrogen adsorbent packed in the auxiliary adsorption tower in claim 1,
A method and apparatus for separating oxygen and nitrogen from air, using one or more Ca ion-exchanged X-type zeolites.
請求項1、請求項2、請求項3の工程を窒素吸着塔1搭と補助吸着塔1搭で実施すること
を特長とする、空気からの酸素と窒素の分離方法および装置。
A method and apparatus for separating oxygen and nitrogen from air, characterized in that the steps of claim 1, claim 2 and claim 3 are carried out by one nitrogen adsorption tower and one auxiliary adsorption tower.
請求項1で補助吸着塔に窒素吸着剤を充填しない未充填の気体タンクとして、窒素吸着塔
の吸着工程終了時の窒素吸着塔に残留する酸素を回収し、これを昇圧工程の気体として使
用する空気からの酸素と窒素の分離方法および装置。
As an unfilled gas tank in which the auxiliary adsorption tower is not filled with a nitrogen adsorbent according to claim 1, oxygen remaining in the nitrogen adsorption tower at the end of the adsorption process of the nitrogen adsorption tower is recovered, and this is used as a gas for the pressurization process. Method and apparatus for separating oxygen and nitrogen from air.
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