JPH0379048B2 - - Google Patents
Info
- Publication number
- JPH0379048B2 JPH0379048B2 JP58133050A JP13305083A JPH0379048B2 JP H0379048 B2 JPH0379048 B2 JP H0379048B2 JP 58133050 A JP58133050 A JP 58133050A JP 13305083 A JP13305083 A JP 13305083A JP H0379048 B2 JPH0379048 B2 JP H0379048B2
- Authority
- JP
- Japan
- Prior art keywords
- adsorption
- adsorption tower
- pressure
- product
- nitrogen gas
- 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 - Lifetime
Links
- 238000001179 sorption measurement Methods 0.000 claims description 75
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 230000008929 regeneration Effects 0.000 claims description 7
- 238000011069 regeneration method Methods 0.000 claims description 7
- 239000003463 adsorbent Substances 0.000 claims description 6
- 238000010586 diagram Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/04—Purification or separation of nitrogen
- C01B21/0405—Purification or separation processes
- C01B21/0433—Physical processing only
- C01B21/045—Physical processing only by adsorption in solids
Description
この発明はプレツシヤースイング吸着法によつ
て空気から窒素ガスを分離製造する方法に関する
ものである。
従来、カーボンシーブスなどの酸素を吸着する
吸着剤を用いて空気より窒素ガスを製造する、い
わゆるプレツシヤースイング吸着法による窒素ガ
ス製造方法が知られている。このような窒素ガス
製造方法の１つとして、例えば第１図に示した特
公昭56−9442号公報記載の方法がある。原料空気
は管１より圧縮機２に送られ、ここで４Kg／cm2程
度に加圧されたのち、切換弁３ａを経て、切替使
用される２基の吸着塔４ａ，４ｂの一方の吸着塔
４ａに送り込まれる。吸着塔４ａ，４ｂにはカー
ボンシーブスなどの酸素を優先的に吸着する吸着
剤が充填されており、加圧状態で導入された原料
空気中の酸素が吸着され、吸着塔４ａ出口には窒
素を主成分とする製品窒素ガスが得られる。この
製品窒素ガスは管５、弁６ａ、流量調整弁７を経
て、供給先に送られる。（吸着工程）
そして、所定量の酸素を吸着して飽和寸前とな
つた吸着塔４ａは、切換弁３ａの切換によつて原
料空気の導入が停止され、再生工程を終え減圧下
にある他の吸着塔４ｂと管８、弁９を通して連通
される。この操作によつて、吸着塔４ａの上部に
溜つている窒素ガスが吸着塔４ｂに流れ、２つの
吸着塔４ａ，４ｂの内圧が等しくなる。（均圧工
程）
ついで、原料空気は吸着塔４ｂに送られ、製品
窒素ガスが同様に製造される。また、吸着塔４ａ
は真空ポンプ１０に接続されて吸引減圧され、吸
着剤に吸着された酸素が脱着され、吸着剤が再生
される。（再生工程）
以下同様に、この一連操作を吸着塔４ａ，４ｂ
について交互に繰り返すことによつて、製品窒素
ガスが得られる。以上の工程をまとめると第１表
のようになる。
This invention relates to a method for separating and producing nitrogen gas from air by a pressure swing adsorption method. BACKGROUND ART Conventionally, a method for producing nitrogen gas by the so-called pressure swing adsorption method is known, in which nitrogen gas is produced from air using an adsorbent that adsorbs oxygen, such as carbon sieves. One such method for producing nitrogen gas is, for example, the method shown in FIG. 1 and described in Japanese Patent Publication No. 56-9442. The raw air is sent from the pipe 1 to the compressor 2, where it is pressurized to about 4 kg/cm 2 , and then passes through the switching valve 3a to be switched to one of the two adsorption towers 4a and 4b used. It is sent to 4a. The adsorption towers 4a and 4b are filled with an adsorbent such as carbon sieves that preferentially adsorbs oxygen, and oxygen in the feed air introduced under pressure is adsorbed, and nitrogen is released at the outlet of the adsorption tower 4a. Product nitrogen gas, which is the main component, is obtained. This product nitrogen gas is sent to a supply destination via a pipe 5, a valve 6a, and a flow rate adjustment valve 7. (Adsorption step) Then, the adsorption tower 4a, which has adsorbed a predetermined amount of oxygen and is on the verge of saturation, stops introducing feed air by switching the switching valve 3a, and after completing the regeneration step, the adsorption tower 4a, which is almost saturated, It is communicated with the adsorption tower 4b through a pipe 8 and a valve 9. By this operation, the nitrogen gas accumulated in the upper part of the adsorption tower 4a flows to the adsorption tower 4b, and the internal pressures of the two adsorption towers 4a and 4b become equal. (Pressure equalization step) Next, the raw air is sent to the adsorption tower 4b, and product nitrogen gas is produced in the same way. In addition, the adsorption tower 4a
is connected to a vacuum pump 10 to reduce the pressure by suction, oxygen adsorbed by the adsorbent is desorbed, and the adsorbent is regenerated. (Regeneration step) Similarly, this series of operations is performed in the adsorption towers 4a and 4b.
Product nitrogen gas is obtained by repeating the steps alternately. The above steps are summarized in Table 1.
【表】
ところで、上記のような窒素製造方法には下記
のような欠点が指摘されており、その解決が望ま
れている。
すなわち、上記均圧工程で、吸着操作の終了し
た吸着塔を減圧する際、この吸着塔から他方の再
生工程を終えた低圧な吸着塔に向けて放出される
ため、吸着酸素の脱着が起こり、放出ガス中の酸
素含有量が急激に上昇してしまう。そのため、一
方の吸着塔から放出されるガス中の含有酸素が他
方の再生工程を終えた吸着塔内の吸着剤に吸着さ
れ（吸着塔が汚染され）ることになり、高純度の
窒素を得ようとする場合の支障となる。
これに対し、特開昭57−132526号公報には、吸
着塔と製品窒素ガス供給先との間に製品槽を設け
た装置を使い、第２図に示すような連続した工程
によつて高純度な製品窒素ガスを良好な収率で得
るとともに省エネルギー化も実現できるとしてい
る。
上記公報に記載の方法の特徴は、図の工程２ま
たは５にあり、それらの前工程１または４におい
て、破過前（吸着塔から吐出される製品窒素ガス
が未だ所定の製品品位を保つている時点）で、製
品吐出を打切り、引続いて流出するガスを用いて
他の塔の加圧を行なうとしている。
しかし、この方法においては、上記工程２また
は５の後で、吸着終了した方の吸着塔は、吸着圧
を保つたままで、放圧工程（工程３、６）に入る
ことになるため、塔内空隙に存在するガスの回収
を行なうことができず、その結果、製品の回収率
を上げることができないことになる。
この発明は上記事情に鑑みてなされたもので、
プレツシヤースイング吸着法によつて窒素を製造
するに際して、純度を低下させることなく製品窒
素ガスの収量を上げることのできる窒素の製造方
法を提供することを目的とするものである。
以下、この発明を図面を参照して詳しく説明す
る。第３図はこの発明を実施するに好適な装置の
一例を示すもので、第１図に示した装置と共通す
る部分には同一符号を付して説明を簡略化する。
吸着塔４ａに導入された加圧原料空気は、酸素が
吸着除去されて、製品窒素ガスとなり、切換弁６
ａ、管５を経て製品槽１１に送られる。（吸着工
程）。
製品窒素ガス中の酸素濃度が製品濃度よりも増
加した時点で弁６ａが閉じられるとともに弁９，
１２，１３が開けられ、吸着塔４ａ内のガスが真
空再生済みの吸着塔４ｂ下部へ流入させられる。
これと同時に初期において、弁１４が開けられて
製品槽１１から製品窒素ガスが吸着塔４ｂの上部
に供給される。この操作では弁３ａ，９，１２，
１３，１４以外の弁は、閉の状態にある（均圧
（）工程）。
上記吸着塔４ａからの出口酸素がある所定の許
容値に到達したら、弁３ａが閉じられて原料空気
の供給が止められ、弁９，１２，１３を通る管路
を介して吸着塔４ａと吸着塔４ｂとが同圧にされ
る。この時、弁１４は閉の状態にある（均圧
（）工程）。
上記操作で２塔が完全に平衡な圧力にされた
ら、弁１２が閉められるとともに弁１５，１６が
開けられ、真空ポンプ１０により吸着塔４ａが再
生される（再生工程）。
上記（再生工程）において、一方の吸着塔４ｂ
には弁３ｄを介して加圧原料空気が導入され、吸
着塔４ｂは吸着工程になる。この工程が終ると、
弁１６が閉じられるとともに、弁１７，１２，１
５が開かれ、吸着塔４ｂ内のガスが真空再生済み
の吸着塔４ａ下部へ流入され、同時に弁１８を介
して製品槽１１からの製品窒素ガスが吸着塔４ａ
の上部に供給される（均圧（）工程）。
引き続いて、前記均圧（）工程が吸着塔４
ａ，４ｂを位置交換した状態で行なわれ、最後に
弁３ａだけが開状態にされ、原料空気により吸着
塔４ａが吸着圧まで再加圧される（原料加圧工
程）。
この後、前記（吸着工程）に戻り、前記工程が
繰り返され、それによつて高純度な製品窒素ガス
が高回収率で連続して得られる。以上の工程をま
とめると下記第２表および第４図のようになる。[Table] By the way, the following drawbacks have been pointed out in the above-mentioned nitrogen production method, and a solution is desired. That is, when depressurizing the adsorption tower that has completed the adsorption operation in the pressure equalization step, adsorbed oxygen is desorbed because it is released from this adsorption tower to the other low-pressure adsorption tower that has completed the regeneration step. The oxygen content in the emitted gas will rise rapidly. Therefore, the oxygen contained in the gas released from one adsorption tower will be adsorbed by the adsorbent in the other adsorption tower that has completed the regeneration process (the adsorption tower will become contaminated), resulting in highly pure nitrogen being obtained. This will be a hindrance if you try to do so. On the other hand, Japanese Patent Application Laid-Open No. 57-132526 uses a device in which a product tank is installed between an adsorption tower and a product nitrogen gas supply destination, and uses a continuous process as shown in Figure 2 to increase the The company says it will be able to obtain pure nitrogen gas at a good yield and also save energy. The method described in the above publication is characterized by steps 2 or 5 in the figure, and in the preceding step 1 or 4, the process is performed before breakthrough (when the product nitrogen gas discharged from the adsorption tower still maintains a predetermined product quality). At this point, the product discharge will be discontinued and the outflowing gas will be used to pressurize other columns. However, in this method, after the above steps 2 or 5, the adsorption tower that has completed adsorption enters the depressurization step (steps 3 and 6) while maintaining the adsorption pressure. The gas present in the voids cannot be recovered, and as a result, the product recovery rate cannot be increased. This invention was made in view of the above circumstances,
It is an object of the present invention to provide a method for producing nitrogen that can increase the yield of product nitrogen gas without reducing purity when producing nitrogen by a pressure swing adsorption method. Hereinafter, the present invention will be explained in detail with reference to the drawings. FIG. 3 shows an example of a device suitable for carrying out the present invention, and parts common to the device shown in FIG. 1 are given the same reference numerals to simplify the explanation.
The pressurized feed air introduced into the adsorption tower 4a has oxygen adsorbed and removed to become a product nitrogen gas, and the switching valve 6
a. It is sent to the product tank 11 via the pipe 5. (Adsorption process). When the oxygen concentration in the product nitrogen gas increases more than the product concentration, the valve 6a is closed and the valves 9,
12 and 13 are opened, and the gas in the adsorption tower 4a is allowed to flow into the lower part of the adsorption tower 4b which has been vacuum-regenerated.
At the same time, at the beginning, the valve 14 is opened and the product nitrogen gas is supplied from the product tank 11 to the upper part of the adsorption tower 4b. In this operation, valves 3a, 9, 12,
Valves other than 13 and 14 are in a closed state (pressure equalization ( ) step). When the outlet oxygen from the adsorption tower 4a reaches a certain permissible value, the valve 3a is closed and the feed air supply is stopped, and the adsorption tower 4a and adsorption The pressure is the same as that of column 4b. At this time, the valve 14 is in a closed state (pressure equalization ( ) step). When the two towers are brought to a completely balanced pressure by the above operation, valve 12 is closed, valves 15 and 16 are opened, and adsorption tower 4a is regenerated by vacuum pump 10 (regeneration step). In the above (regeneration step), one adsorption tower 4b
Pressurized raw material air is introduced through the valve 3d, and the adsorption tower 4b enters the adsorption process. When this process is finished,
Valve 16 is closed and valves 17, 12, 1
5 is opened, gas in the adsorption tower 4b flows into the lower part of the adsorption tower 4a which has been vacuum regenerated, and at the same time, product nitrogen gas from the product tank 11 flows through the valve 18 into the adsorption tower 4a.
(pressure equalization () process). Subsequently, the pressure equalization () step is carried out in the adsorption tower 4.
This is carried out with the positions of a and 4b exchanged, and finally, only the valve 3a is opened, and the adsorption tower 4a is repressurized to the adsorption pressure by the raw material air (raw material pressurization step). Thereafter, the process returns to the above (adsorption process) and the process is repeated, thereby continuously obtaining a highly purified nitrogen gas product at a high recovery rate. The above steps are summarized as shown in Table 2 and Figure 4 below.
第３図に示したこの発明の実施に好適な装置に
おいて、吸着塔４ａ，４ｂに８Kgのカーボンシー
ブスを充填して種々運転したところ、第３表に示
すような最も望ましい運転条件を得ることができ
た。そして、その運転の結果、99.9％の高純度な
製品窒素ガスが得られた。
When the adsorption towers 4a and 4b were filled with 8 kg of carbon sieves and various operations were carried out in the apparatus shown in FIG. 3 suitable for carrying out the present invention, it was possible to obtain the most desirable operating conditions as shown in Table 3. did it. As a result of this operation, product nitrogen gas with a high purity of 99.9% was obtained.
【表】
以上説明したように、この発明に係るプレツシ
ヤースイング吸着法による窒素製造方法は、吸着
塔と製品窒素ガスの供給先との間に製品槽を設
け、吸着工程を終了した吸着塔に原料空気を供給
して、この吸着塔内の窒素に富むガスを再生済み
の他の吸着塔下部に流入すると同時に、この再生
済みの吸着塔上部に前記製品槽から製品窒素ガス
を供給する均圧（）工程と、この均圧（）工
程終了後に上記吸着工程終了後の上部と前記再生
済みの吸着塔の下部とを連通して両吸着塔を同圧
にする均圧（）工程とから均圧工程を構成した
ものなので、製品窒素ガスの純度を低下させるこ
となく、製品窒素ガスの収量を大幅に増加させる
ことができる。[Table] As explained above, in the nitrogen production method using the pressure swing adsorption method according to the present invention, a product tank is provided between the adsorption tower and the product nitrogen gas supply destination, and the adsorption tower after the adsorption process is At the same time, the nitrogen-rich gas in this adsorption tower flows into the lower part of another regenerated adsorption tower, and at the same time, the product nitrogen gas is supplied from the product tank to the upper part of this regenerated adsorption tower. pressure () step, and after the completion of this pressure equalization () step, a pressure equalization () step in which the upper part after the completion of the adsorption step and the lower part of the regenerated adsorption tower are communicated to make both adsorption towers at the same pressure. Since the pressure equalization process is configured, the yield of the product nitrogen gas can be significantly increased without reducing the purity of the product nitrogen gas.
第１図は従来のプレツシヤースイング吸着法に
よる窒素製造方法の一例に使われていた装置の構
成図、第２図は従来のプレツシヤースイング吸着
法による窒素製造方法の他の例の工程図、第３図
はこの発明を実施するに好適な装置の一例を示す
構成図、第４図はこの発明の窒素製造方法の一例
の工程図である。
２…圧縮機、３ａ，３ｄ，６ａ，６ｂ，９，１
３，１４，１５，１６，１７，１８…切換弁、４
ａ，４ｂ…吸着塔、１０…真空ポンプ、１１…製
品槽。
Figure 1 is a block diagram of an apparatus used in an example of a conventional nitrogen production method using pressure swing adsorption, and Figure 2 is a process diagram of another example of a conventional nitrogen production method using pressure swing adsorption. 3 and 3 are block diagrams showing an example of an apparatus suitable for carrying out the present invention, and FIG. 4 is a process diagram of an example of the nitrogen production method of the present invention. 2...Compressor, 3a, 3d, 6a, 6b, 9, 1
3, 14, 15, 16, 17, 18... switching valve, 4
a, 4b...Adsorption tower, 10...Vacuum pump, 11...Product tank.
Claims (1)
着塔を切換弁により、吸着・均圧・再生・均圧・
吸着の各工程に順次切換えることにより連続的に
空気から製品窒素ガスを製造する方法において、 前記吸着塔と製品窒素ガスの供給先との間に製
品槽を設け、 前記均圧工程を、吸着工程を終了した吸着塔に
原料空気を供給して、この吸着塔より吐出する窒
素に富むガスを再生済みの他の吸着塔下部より流
入すると同時に、この再生済みの吸着塔上部に前
記製品槽から製品窒素ガスを供給する均圧（）
工程と、 前記均圧（）工程終了後に、原料空気の導入
を停止して前記吸着工程終了後の吸着塔の上部と
前記再生済みの吸着塔の下部とを連通して両吸着
塔を同圧にする均圧（）工程とから構成するこ
とを特徴とするプレツシヤースイング吸着法によ
る窒素製造方法。[Claims] 1. A plurality of adsorption towers filled with an adsorbent for adsorbing oxygen are controlled by a switching valve to perform adsorption, pressure equalization, regeneration, pressure equalization, and
In a method for continuously producing product nitrogen gas from air by sequentially switching to each adsorption step, a product tank is provided between the adsorption tower and a supply destination of the product nitrogen gas, and the pressure equalization step is performed as an adsorption step. Feedstock air is supplied to the adsorption tower that has completed the process, and the nitrogen-rich gas discharged from this adsorption tower flows into the lower part of another regenerated adsorption tower, and at the same time, the product from the product tank is transferred to the upper part of the regenerated adsorption tower. Equal pressure to supply nitrogen gas ()
step, and after the pressure equalization step is completed, the introduction of raw air is stopped and the upper part of the adsorption tower after the adsorption step is communicated with the lower part of the regenerated adsorption tower to bring both adsorption towers to the same pressure. A method for producing nitrogen by a pressure swing adsorption method, which is characterized by comprising a pressure equalization step () in which the pressure is equalized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58133050A JPS6027606A (en) | 1983-07-21 | 1983-07-21 | Preparation of nitrogen by pressure swing adsorption method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58133050A JPS6027606A (en) | 1983-07-21 | 1983-07-21 | Preparation of nitrogen by pressure swing adsorption method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6027606A JPS6027606A (en) | 1985-02-12 |
| JPH0379048B2 true JPH0379048B2 (en) | 1991-12-17 |
Family
ID=15095641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58133050A Granted JPS6027606A (en) | 1983-07-21 | 1983-07-21 | Preparation of nitrogen by pressure swing adsorption method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6027606A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2683806B2 (en) * | 1988-03-17 | 1997-12-03 | 住友精化株式会社 | Concentrated oxygen recovery method |
| EP0380723B1 (en) * | 1989-02-01 | 1994-04-06 | Kuraray Chemical Co., Ltd. | Process for separating nitrogen gas by pressure swing adsorption system |
| JP3405565B2 (en) * | 1993-07-23 | 2003-05-12 | 住友精化株式会社 | Gas separation method |
| KR100861550B1 (en) | 2008-06-10 | 2008-10-02 | (주)원하이테크 | Apparatus for generating concentrated gas being capable of controlling concentration of gas by using flow control valve and method of generating concentrated gas by using the same |
| JP6811572B2 (en) * | 2016-09-14 | 2021-01-13 | 株式会社クラレ | Nitrogen gas separation method and nitrogen gas separation device |
-
1983
- 1983-07-21 JP JP58133050A patent/JPS6027606A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6027606A (en) | 1985-02-12 |
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