JPH02284622A - Separation of useful gas - Google Patents

Separation of useful gas

Info

Publication number
JPH02284622A
JPH02284622A JP1107006A JP10700689A JPH02284622A JP H02284622 A JPH02284622 A JP H02284622A JP 1107006 A JP1107006 A JP 1107006A JP 10700689 A JP10700689 A JP 10700689A JP H02284622 A JPH02284622 A JP H02284622A
Authority
JP
Japan
Prior art keywords
adsorbent
gas
useful gas
useful
adsorption tower
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.)
Pending
Application number
JP1107006A
Other languages
Japanese (ja)
Inventor
Mamoru Inoue
井上 衛
Hisaaki Kamiyama
久朗 神山
Akira Kamimura
彰 上村
Katsushi Kosuge
克志 小菅
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.)
Nippon Steel Corp
Original Assignee
Nippon Steel 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 Nippon Steel Corp filed Critical Nippon Steel Corp
Priority to JP1107006A priority Critical patent/JPH02284622A/en
Publication of JPH02284622A publication Critical patent/JPH02284622A/en
Pending legal-status Critical Current

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  • Carbon And Carbon Compounds (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

PURPOSE:To separate and purify useful gas at a high recovery rate by packing the lower part of an adsorption tower with an adsorbent hardly causing powdering and the upper part with an adsorbent having high adsorbing ability and successively passing the useful gas through the adsorbent in the lower part and the adsorbent in the upper part. CONSTITUTION:When useful gas such as CO is separated from raw gas such as converter gas by a pressure swing adsorption method, the lower part of an adsorption tower 1 is packed with an adsorbent B hardly causing powdering, the upper part with an adsorbent A having high adsorbing ability and the useful gas is successively passed through the adsorbents B, A. These adsorbents may be silica gel or activated carbon supporting copper chloride and the adsorbent hardly causing powdering and the adsorbent having high adsorbing ability are separately produced by regulating calcining temp., etc. The useful gas such as CO can be separated and purified at a high recovery rate.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は圧力スイング吸着法(以T PS醐去と略称す
る)を利用して、CO等の有用ガスを含む原料ガスから
、高純度の有用ガスを分離精製する方法に関するもので
ある。
Detailed Description of the Invention (Field of Industrial Application) The present invention utilizes the pressure swing adsorption method (hereinafter abbreviated as TPS) to obtain high-purity gas from a raw material gas containing useful gases such as CO. The present invention relates to a method for separating and purifying useful gases.

(従来の技術) CDを含む混合ガスからCOの1ノを分離回収する方法
として、深冷分離法、吸収法および吸着法かあることは
周知の通りである。その中でも近年吸着法として、PS
Aによる00分離技術の開発か進められている。
(Prior Art) It is well known that there are cryogenic separation methods, absorption methods, and adsorption methods as methods for separating and recovering CO from a mixed gas containing CD. Among them, in recent years, PS has been used as an adsorption method.
The development of 00 separation technology by A is progressing.

例えばCDの分離回収方法として、特開昭592612
1 ’;’;−公報、同61−122111号公報、同
62119106号公報1同63−7822号公報など
にPSAの操作方法が種々提案されている。
For example, as a method for separating and recovering CDs, JP-A No. 592,612
Various methods of operating the PSA have been proposed in Publication No. 1 ';';-, Publication No. 61-122111, Publication No. 62119106, Publication No. 63-7822, etc.

また、COの選択的吸着剤として、特開昭596941
4号公報、同60−90037号公報、同81−184
31号公報12と種々の製造方法が提案されている。
In addition, as a selective adsorbent for CO, JP-A-596941
Publication No. 4, Publication No. 60-90037, Publication No. 81-184
No. 31 Publication 12 and various manufacturing methods have been proposed.

従来の吸着剤ではCOの選択吸着能が小さいため、2段
のPSA法方式を採用していたが、近年COの選択吸着
能が非常に大きな吸着剤が開発されるようになり、1段
のPSA法で高純度のCOを分離回収することができる
ようにf、/った。
Conventional adsorbents have a small selective adsorption capacity for CO, so a two-stage PSA method has been adopted, but in recent years, adsorbents with a very large selective adsorption capacity for CO have been developed, and a one-stage PSA method has been adopted. The PSA method was used to enable the separation and recovery of highly pure CO.

(発明が解決しようとする課題) しかしながら、高性能のGO吸着剤は比表面積を大きく
するため、粉化しやすいものが多く、吸着塔からキャリ
ーアップして切替え弁や真空ポンプの目詰まりをおこす
心配があった。本発明者らはかかる欠点に鑑み、2種以
上のCO等の有用ガス吸着剤を吸着塔内に最適に充填す
ることによって、上述した粉化問題を解決すると同時に
、高性能の有用ガス分離精製方法を提案するものである
(Problem to be solved by the invention) However, since high-performance GO adsorbents have a large specific surface area, many of them are easily powdered, and there is a risk of carry-up from the adsorption tower and clogging of switching valves and vacuum pumps. was there. In view of these drawbacks, the present inventors solved the above-mentioned pulverization problem by optimally filling an adsorption tower with two or more kinds of useful gas adsorbents such as CO, and at the same time solved the problem of high-performance useful gas separation and purification. This paper proposes a method.

(課題を解決するための手段) 本願発明の要旨は、有用ガスを含む原料ガスより圧力ス
イング吸着法で有用ガスを分離する方法において、吸着
塔の前段に粉化しにくい吸着剤を充填し、次いで吸着塔
の後段に吸着能の大きな吸着剤を充填し、該前段から後
段の吸着剤へ順次有用ガスを通過せしめることを特徴と
する有用ガスの分離方法である。
(Means for Solving the Problems) The gist of the present invention is to provide a method for separating useful gas from a raw material gas containing useful gas by pressure swing adsorption method, in which an adsorbent that is difficult to powder is filled in the front stage of an adsorption tower, and then This method of separating useful gas is characterized in that an adsorbent having a large adsorption capacity is packed in the latter stage of an adsorption tower, and the useful gas is sequentially passed from the former stage to the latter stage adsorbent.

即ち、本発明は粉化しやすいが有用ガスの選択吸着能の
すぐれた吸着剤と、粉化しにくい強固な有用ガス吸着剤
を少なくとも2種類以上同一の吸着塔に最適に充填する
ものである。粉化しにくい強固な吸着剤を吸着塔の前段
に通して流速を抑制し、吸着ガス成分の濃度が低下する
後半即ち、吸着塔の後段に吸着能の大きな吸着剤を配置
することを特徴としている。具体的には、原料ガスを吸
着塔の下部から導入する場合、吸着塔内は減圧状態から
加圧状態に穆行するため、原料ガスは最初大きな流速で
吸着塔内を上昇することになる。吸着剤の粉化は主にこ
の加圧工程に発生するものと考えられる。そこで吸着塔
の下部即ち、前段には粉化しにくい強固な吸着剤を配置
し、原料ガスの流速をまずここで緩和させ、しかる後に
、粉化しやすいが高性能の吸着剤に導入してやる。原料
ガス中の吸着成分は徐々に吸着されて、濃度が低下する
ため、高性能の吸着剤を後段に配置することは回収率を
上げるために有効である。また最後段に前段と同様の強
固な吸着剤を配置してキャリーアップを防止する一方、
パージガスなどの上方からのガス流を緩和する目的でサ
ンドイッチ構造とすることも効果的である。
That is, the present invention optimally fills the same adsorption tower with at least two kinds of adsorbents that are easy to powder but have excellent selective adsorption ability for useful gases and strong useful gas adsorbents that are difficult to powder. A strong adsorbent that is difficult to powder is passed through the first stage of the adsorption tower to suppress the flow rate, and an adsorbent with high adsorption capacity is placed in the latter half of the adsorption tower, where the concentration of adsorbed gas components decreases. . Specifically, when the raw material gas is introduced from the lower part of the adsorption tower, the inside of the adsorption tower moves from a reduced pressure state to a pressurized state, so the raw material gas initially rises inside the adsorption tower at a high flow rate. It is thought that powdering of the adsorbent mainly occurs during this pressurization process. Therefore, a strong adsorbent that is difficult to powder is placed in the lower part of the adsorption tower, that is, in the front stage, and the flow rate of the raw material gas is first relaxed here, and then it is introduced into a high-performance adsorbent that is easy to powder. Since the adsorbed components in the raw material gas are gradually adsorbed and the concentration decreases, placing a high-performance adsorbent in the latter stage is effective in increasing the recovery rate. In addition, a strong adsorbent similar to the previous stage is placed in the last stage to prevent carry-up.
It is also effective to use a sandwich structure for the purpose of alleviating the flow of gas such as purge gas from above.

尚、本発明で述べている粉化しにくい吸着剤とはシャッ
ター試験で得られた粉率が10%以下のものをいうもの
であり、シャッター試験とは1 mm以上の吸着剤10
0g計量し、1mの落下を繰り返した後、1 mm以下
に粉化した割合(粉率)で吸着剤の粉化具合を評価する
ものである。
In addition, the adsorbent that is difficult to powder as described in the present invention is one with a powder ratio of 10% or less obtained in a shutter test, and the shutter test refers to an adsorbent with a particle size of 1 mm or more.
After weighing 0g and repeating a 1m drop, the degree of pulverization of the adsorbent is evaluated based on the ratio of pulverization to 1 mm or less (powder ratio).

次いで後段に用いる吸着剤について述べると、後段に用
いる1及首剤の吸着能は前段に用いる吸着剤の吸着能に
対して20%以上高いものを言う。20%未満では前段
の吸着によって有用ガスの濃度が低下するため、後段で
の吸着が効率よく行なわないためである。
Next, referring to the adsorbent used in the latter stage, the adsorption capacity of the first and second agents used in the latter stage is 20% or more higher than that of the adsorbent used in the former stage. This is because if it is less than 20%, the concentration of useful gas decreases due to the adsorption in the first stage, and therefore the adsorption in the second stage will not be carried out efficiently.

本発明に用いる吸着剤は具体的には例えば活性アルミナ
、シリカゲル、活性炭に塩化銅(I)を担持させたもの
、活性炭に四塩化(I)アルミニウム錯体を担持させた
もの等が有利である。
Specifically, the adsorbent used in the present invention is advantageously, for example, activated alumina, silica gel, activated carbon supported with copper(I) chloride, activated carbon supported with aluminum tetrachloride(I) complex, and the like.

前述した吸着剤を粉化しにくい吸着剤、あるいは吸着能
の大きな吸着剤とするには、吸着剤を製造する際に焼成
温度等を調整して造りわけるものである。
In order to make the above-mentioned adsorbent into an adsorbent that is difficult to powder or has a high adsorption capacity, the calcination temperature and the like are adjusted during the production of the adsorbent.

施  例〕 本発明にもとついて、例えば転炉ガスから高純度の一酸
化炭素を分III精製した実施例について以下に具体的
に説明する。第1図(ア)、m。
EXAMPLE] Based on the present invention, an example in which high purity carbon monoxide was purified from converter gas by fraction III will be specifically described below. Figure 1 (a), m.

(’/)、(1)は吸着剤の充填方法を種々変えた吸着
塔内を模式的に示したもので、2種類の吸着剤(A) 
、 (B)は塩化銅(1)を活性炭に担持させたもので
あり、そのCO吸着性能と強度をそれぞれ表1に示す。
('/), (1) schematically shows the inside of the adsorption tower with various adsorbent filling methods.
, (B) is copper chloride (1) supported on activated carbon, and its CO adsorption performance and strength are shown in Table 1.

〔実 表    1 第1図の(ア)および(イ)は本発明にもとづいて、粉
化しにくい吸着剤(B)を下方に30%充填し、(ア)
ではその上方に吸着剤(A)を、(イ)ではさらに最上
段に10%吸着剤(B)を配置して、上部からのキャリ
ーアウトを防止する充填構造とした。(つ)、(1)は
比較のために、従来通り1種類の吸着剤を充填した例で
ある。表2に各充填による比較例をそれぞh示した。本
発明によれは、吸着剤の粉化トラブルもなく、高純度の
COを高回収率で分離精製することができた。
[Actual Table 1 (A) and (B) in Figure 1 are based on the present invention, with 30% of the adsorbent (B) that is difficult to powder being filled in the lower part, and (A)
In this example, the adsorbent (A) was placed above the adsorbent, and in (a), the 10% adsorbent (B) was further placed on the uppermost stage to form a filling structure to prevent carry-out from the top. For comparison, (1) and (1) are examples in which one type of adsorbent was filled in the conventional manner. Table 2 shows comparative examples with each filling. According to the present invention, highly pure CO could be separated and purified at a high recovery rate without the trouble of pulverization of the adsorbent.

表  2 ある。Table 2 be.

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

第7図(7) 、 (イ)、(つ)、(1)は吸着塔へ
の@着剤の充填方法を模式的に示した図である。 1・・・吸着塔 (発明の効果) 本発明によれは、粉化しやすいが有用ガスの潤沢吸着能
の非常に大きな吸着剤をうまく利用することによって、
高純度のCOガス等の有用ガスを高回収率で分離精製で
きる等顕著な効果が(ア) (イ) 図 (つ)
FIGS. 7(7), (a), (t), and (1) are diagrams schematically showing a method of filling an adsorption tower with an adhesion agent. 1... Adsorption tower (effect of the invention) According to the present invention, by making good use of an adsorbent that is easily powdered but has a very large adsorption capacity for abundant useful gases,
It has remarkable effects such as being able to separate and purify useful gases such as high-purity CO gas with a high recovery rate (A) (B) Figure (T)

Claims (1)

【特許請求の範囲】[Claims] 1 有用ガスを含む原料ガスより圧力スイング吸着法で
有用ガスを分離する方法において、吸着塔の前段に粉化
しにくい吸着剤を充填し、次いで吸着塔の後段に吸着能
の大きな吸着剤を充填し、該前段から後段の吸着剤へ順
次有用ガスを通過せしめることを特徴とする有用ガスの
分離方法
1 In a method of separating useful gases from a raw material gas containing useful gases by pressure swing adsorption, the first stage of the adsorption tower is filled with an adsorbent that is difficult to powder, and then the second stage of the adsorption tower is filled with an adsorbent with a high adsorption capacity. A method for separating useful gas, characterized by passing the useful gas sequentially from the first stage to the second stage adsorbent.
JP1107006A 1989-04-26 1989-04-26 Separation of useful gas Pending JPH02284622A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1107006A JPH02284622A (en) 1989-04-26 1989-04-26 Separation of useful gas

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1107006A JPH02284622A (en) 1989-04-26 1989-04-26 Separation of useful gas

Publications (1)

Publication Number Publication Date
JPH02284622A true JPH02284622A (en) 1990-11-22

Family

ID=14448105

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1107006A Pending JPH02284622A (en) 1989-04-26 1989-04-26 Separation of useful gas

Country Status (1)

Country Link
JP (1) JPH02284622A (en)

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