JPH0121087B2 - - Google Patents
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- JPH0121087B2 JPH0121087B2 JP55118266A JP11826680A JPH0121087B2 JP H0121087 B2 JPH0121087 B2 JP H0121087B2 JP 55118266 A JP55118266 A JP 55118266A JP 11826680 A JP11826680 A JP 11826680A JP H0121087 B2 JPH0121087 B2 JP H0121087B2
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- absorption liquid
- absorption
- carbon monoxide
- oxygen
- liquid
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Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、一酸化炭素（CO）吸収液の再生方
法に係り、特にCOの吸収液を再生して循環使用
する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for regenerating a carbon monoxide (CO) absorbent, and particularly to a method for regenerating and recycling a CO absorbent.
化学工業や製鉄工業等において、合成化学用原
料ガスの製造または省エネルギのために、例えば
プロセス排ガスからCOを分離、濃縮して回収す
ることが大きな技術的課題となつている。
In the chemical industry, iron and steel industry, etc., separating, concentrating, and recovering CO from process exhaust gas has become a major technical issue, for example, in order to produce raw material gas for synthetic chemicals or to save energy.
COを含有するガス源からCOを分離、濃縮する
方法には、現在、第１銅塩の溶液塔の吸収液を使
用する吸収液法、およびそれとは原理的にことな
る深冷離法が知られている。後者の深冷分離法
は、複雑な冷却、熱回収システムから構成されて
おり、操作温度が低温であるため、装置材料とし
て高価なものを使用する必要があり、また低温を
得るために、動力消費量が大きくなるという欠点
がある。 Currently known methods for separating and concentrating CO from a gas source containing CO include the absorption liquid method, which uses an absorption liquid from a cuprous salt solution column, and the cryogenic separation method, which is fundamentally different from the absorption liquid method. It is being The latter cryogenic separation method consists of a complex cooling and heat recovery system, and because the operating temperature is low, it is necessary to use expensive equipment materials. The disadvantage is that the amount of consumption increases.
一方、吸収液法に使用されるCO吸収液として
は、従来、アンモニア性第１銅水溶液または塩酸
性第１銅塩水溶液が用いられている。これらの吸
収液においては、CO吸収に直接関与する一価の
銅を溶液中に可溶可させるために、クロロ錯体ま
たはアンミン錯体を形成させているものと考えら
れる。ところで、吸収液法によるCO分離、濃縮
プロセスの基本をなすCO吸収反応は、溶液中に
存在する一価の銅にCOが配位することにより起
きる。一方、COを含有する各種ガス源には、CO
が通常10〜30容量％含まれるが、その他に0.1〜
0.5容量％の酸素（O2）が含まれることが多い。
このようなガスを対象としてCOの分離、濃縮を
行うと、通常、吸収液はCOとともにO2をも吸収
し、この際、一般的には液中の一価の銅はO2に
より二価の銅へ酸化される。しかるに、生成した
二価の銅へはCOは配位しないため、吸収液のCO
吸収能力は低下し、連続運転が困難になるという
問題点がある。 On the other hand, as the CO absorption liquid used in the absorption liquid method, an ammoniacal cuprous aqueous solution or a hydrochloric acid cuprous salt aqueous solution has conventionally been used. In these absorption liquids, it is thought that a chloro complex or an ammine complex is formed in order to make monovalent copper, which is directly involved in CO absorption, soluble in the solution. By the way, the CO absorption reaction, which is the basis of the CO separation and concentration process using the absorption liquid method, occurs when CO coordinates with monovalent copper present in the solution. On the other hand, various gas sources containing CO include
Usually contains 10 to 30% by volume, but in addition 0.1 to 30% by volume.
Often contains 0.5% by volume of oxygen (O 2 ).
When separating and concentrating CO from such gases, the absorption liquid usually absorbs O 2 as well as CO, and at this time, monovalent copper in the liquid is generally converted into divalent copper by O 2 . is oxidized to copper. However, since CO does not coordinate with the generated divalent copper, the CO of the absorption liquid
The problem is that the absorption capacity decreases, making continuous operation difficult.
本発明の目的は、上記従来技術の欠点をなく
し、O2によつてCO吸収能力が低下したCO吸収
液を効率よく再生することができるCO吸収液の
再生方法を提供することにある。
An object of the present invention is to provide a method for regenerating a CO absorption liquid that eliminates the drawbacks of the above-mentioned conventional techniques and is capable of efficiently regenerating a CO absorption liquid whose CO absorption capacity has been reduced by O 2 .
本発明は、一酸化炭素と酸素を含むガスを、一
価の銅とリンの酸素酸誘導体を含む吸収液に接触
させて一酸化炭素を吸収させる際に、前記酸素に
よつて一酸化炭素吸収能力が低下した吸収液を、
一酸化炭素の共存下で60〜150℃に加熱すること
を特徴とする。
The present invention enables carbon monoxide to be absorbed by the oxygen when a gas containing carbon monoxide and oxygen is brought into contact with an absorption liquid containing monovalent copper and an oxyacid derivative of phosphorus to absorb carbon monoxide. absorbing liquid whose capacity has decreased,
It is characterized by heating to 60-150℃ in the coexistence of carbon monoxide.
本発明に用いられる一価の銅とリンの酸素酸誘
導体を含む吸収液は、本発明者らが提案した特許
第1436953号に詳細に記載されており、一価の銅
としては塩化第１銅が好ましく用いられ、またリ
ンの酸素酸誘導体としては、例えばリン酸エステ
ル、ホスフインオキシド類等が用いられる。 The absorption liquid containing monovalent copper and an oxyacid derivative of phosphorus used in the present invention is described in detail in Patent No. 1436953 proposed by the present inventors, and the monovalent copper is cuprous chloride. is preferably used, and as the oxygen acid derivative of phosphorus, for example, phosphoric acid esters, phosphine oxides, etc. are used.
塩化第１銅と、リンの酸素酸誘導体としてトリ
スジメチルアミノホスフインオキシドとを含む吸
収液を用いた場合、吸収液は、COとともにO2を
吸収し、一価の銅と酸素との錯体または二価の銅
を生成すると考えられる。前者の一価の銅（Cu
(1)）と酸素（O2）との錯体は、トリスジメチル
アミノホスフインオキシドをＬで表せば、次式の
反応によつて生成し、
2L・Cu(1)＋O2→（Ｌ・Cu(1)）2・O2
この吸収液は、COの共存下に60〜150℃、好ま
しくは80〜150℃に加熱することによつて溶液中
の一酸化炭素錯体（Ｌ・Cu(1)・CO）と以下の反
応を起こし、再生されると推察される。 When an absorption liquid containing cuprous chloride and trisdimethylaminophosphine oxide as an oxygen acid derivative of phosphorus is used, the absorption liquid absorbs O 2 together with CO and forms a complex of monovalent copper and oxygen or It is thought to produce divalent copper. The former monovalent copper (Cu
(1)) and oxygen (O 2 ), if trisdimethylaminophosphine oxide is represented by L, it is generated by the reaction of the following formula: 2L・Cu(1)+O 2 →(L・Cu (1)) 2・O 2 This absorption liquid is heated to 60 to 150℃, preferably 80 to 150℃ in the presence of CO to remove the carbon monoxide complex (L・Cu(1)・CO) It is assumed that the following reaction occurs and is regenerated.
2L・Cu(1)・CO＋（Ｌ・Cu(1)）2・O2→2CO2＋
3L・Cu(1)
この反応は両者が錯体として活性化しているた
め容易に進行し、従つて吸収液が容易に再生され
る。また二価の銅が生成している場合には、加熱
により吸収液中の二価の銅は一価の銅に還元され
て再生される。これらの吸収液は再び循環使用す
ることができる。 2L・Cu(1)・CO+(L・Cu(1)) 2・O 2 →2CO 2 +
3L・Cu(1) This reaction progresses easily because both are activated as a complex, and the absorption liquid is therefore easily regenerated. In addition, if divalent copper is generated, the divalent copper in the absorption liquid is reduced to monovalent copper and regenerated by heating. These absorbents can be recycled again.
以下、本発明による一酸化炭素吸収液の再生方
法を図面により詳細に説明する。 Hereinafter, the method for regenerating a carbon monoxide absorption liquid according to the present invention will be explained in detail with reference to the drawings.
第１図は、本発明を用いたCO分離、濃縮プロ
セスの原理的なフローシートである。図におい
て、CO含有ガスは、必要に応じて前処理装置１
で前処理され、原料ガスライン１１を通じ吸収塔
２に入り、吸収塔２内の吸収液と接触し、COが
吸収される。この際、CO含有ガス中にO2が存在
すると吸収液中の例えば一価の銅は、酸素錯体を
生成するか、またはO2により二価の銅に酸化さ
れ、CO吸収能力が低下する。なお、吸収塔排ガ
スは、飛沫同伴成分を適宜除去されたのち、排ガ
スライン２１を通じ大気中に放出される。一方、
COを吸収した液は熱交換器４を経て還元塔５に
送られる。還元塔において吸収液は60℃〜150℃
に保たれ、必要に応じてCOガスライン５１から
COが吹き込まれる。この操作により吸収液中の
Cu(1)とO2との錯体はCu(1)錯体に還元されるか、
または二価の銅は一価の銅へ還元される。還元塔
５を出た吸収液は分離塔３に送られ、さらに昇温
または減圧されることにより、COを放散する。
分離塔３からの排ガスは高濃度のCOを含有する
が、飛沫同伴成分を除去した後、ガスライン４１
をへて製品ガスとなる。COを分離した液はライ
ン６１から吸収塔２にもどり循環使用される。 FIG. 1 is a basic flow sheet of the CO separation and concentration process using the present invention. In the figure, the CO-containing gas is supplied to the pretreatment device 1 as necessary.
It enters the absorption tower 2 through the raw material gas line 11, comes into contact with the absorption liquid in the absorption tower 2, and absorbs CO. At this time, if O 2 is present in the CO-containing gas, for example, monovalent copper in the absorption liquid will generate an oxygen complex or be oxidized to divalent copper by O 2 , reducing the CO absorption capacity. Note that the absorption tower exhaust gas is discharged into the atmosphere through the exhaust gas line 21 after the entrained components are appropriately removed. on the other hand,
The liquid that has absorbed CO is sent to the reduction tower 5 via the heat exchanger 4. In the reduction tower, the temperature of the absorption liquid is 60°C to 150°C.
from the CO gas line 51 as needed.
CO is injected. By this operation, the amount of
Is the complex between Cu(1) and O 2 reduced to Cu(1) complex?
Or divalent copper is reduced to monovalent copper. The absorption liquid leaving the reduction tower 5 is sent to the separation tower 3, where the temperature is further increased or the pressure is reduced, thereby dissipating CO.
The exhaust gas from the separation tower 3 contains a high concentration of CO, but after removing the entrained components, it is passed through the gas line 41.
It becomes a product gas. The liquid from which CO has been separated is returned to the absorption tower 2 through line 61 and is used for circulation.
上記プロセスにおいて、吸収液を再生する際の
操作条件は、吸収液中のCu(1)とO2錯体または二
価の銅の濃度、すなわちCO含有ガス中のO2濃度
により変化することができる。通常、還元温度は
高い方が、反応速度が早くなるので好ましいが、
60℃以上、特に80℃以上にすることが望ましい。
一方、吸収液を再生するためには、COが吸収液
中に共存している必要がある。吸収液の温度が
150℃以上になると、COは、溶液中にもはや存在
し得なくなる。以上の点から還元塔５における吸
収液の温度は60〜150℃、好ましくは80℃〜150℃
の範囲である。 In the above process, the operating conditions for regenerating the absorption liquid can be changed depending on the concentration of Cu(1) and O 2 complex or divalent copper in the absorption liquid, that is, the O 2 concentration in the CO-containing gas. . Generally, a higher reduction temperature is preferable because the reaction rate becomes faster.
It is desirable that the temperature be 60°C or higher, especially 80°C or higher.
On the other hand, in order to regenerate the absorption liquid, CO must coexist in the absorption liquid. The temperature of the absorption liquid
Above 150°C, CO can no longer exist in solution. From the above points, the temperature of the absorption liquid in the reduction tower 5 is 60 to 150°C, preferably 80 to 150°C.
is within the range of
さらに、還元塔５における操作圧力は、常圧20
Kg／cm2Ｇの範囲が好ましい。操作圧力を高くする
ことにより、吸収液中のCO濃度が増加し、の結
果、再生速度が早くなる。 Furthermore, the operating pressure in the reduction tower 5 is normal pressure 20
A range of Kg/cm 2 G is preferred. By increasing the operating pressure, the CO concentration in the absorbent increases, resulting in a faster regeneration rate.
以下、本発明を実施例によりさらに具体的に説
明する。
EXAMPLES Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例 １
窒素雰囲気下で、容積100mlの円筒状ガラス容
器に、塩化第１銅（CuCl）9.90ｇ（0.1モル）お
よびトリス（ジメチルアミノ）ホスフインオキシ
ドを50ml添加した後30℃に保つた（この溶液中の
CuCl濃度は２モル／である）。これに、O22％、
N298％（容量％）なる組成のガスを常圧下、
200Nml／minの割合で17.5分吹きこみ、吸収液の
酸素吸収を行つた。その結果、溶液中に0.25モ
ル／の二価の銅、または0.0625モル／の二価
の銅に相当する酸素錯体が生成した。なお、一価
の銅の濃度は1.75モル／であつた。Example 1 Under a nitrogen atmosphere, 9.90 g (0.1 mol) of cuprous chloride (CuCl) and 50 ml of tris(dimethylamino)phosphine oxide were added to a cylindrical glass container with a volume of 100 ml, and the container was kept at 30°C ( in this solution
CuCl concentration is 2 mol/). Add to this 2 % O2,
A gas with a composition of 98% N 2 (volume %) was added under normal pressure.
Oxygen was absorbed by the absorption liquid by blowing at a rate of 200Nml/min for 17.5 minutes. As a result, an oxygen complex corresponding to 0.25 mole/divalent copper or 0.0625 mole/divalent copper was generated in the solution. Note that the concentration of monovalent copper was 1.75 mol/.
この溶液中にCO50％、N250％からなるガスを
常圧で、200Nml／minnの割合で吹き込みつつ90
℃に昇温し、１時間放置した。その結果、吸収液
中の二価の銅の濃度は0.05モル／（二価の銅に
相当する酸素錯体としては0.0125モル／）に低
下しており、トリス（ジメチルアミソ）ホスフイ
ンオキシド中で吸収液が再生されることが示され
た。 A gas consisting of 50% CO and 50% N2 was blown into this solution at a rate of 200Nml/min at normal pressure for 90 minutes.
The temperature was raised to ℃ and left for 1 hour. As a result, the concentration of divalent copper in the absorption liquid was reduced to 0.05 mol/(0.0125 mol/as an oxygen complex equivalent to divalent copper), and It was shown that the liquid was regenerated.
実施例 ２
実施例１と同様な方法で、1.9モル／の一価
の銅および0.1モル／の二価の銅（酸素錯体と
して0.025モル／）を含むトリス（ジメチルア
ミノ）ホスフオンオキシド溶液50mlを、容積100
mlの円筒状ガラス容器中で調整した。この吸収液
に実施例１と同様の条件でCO含有ガスを吹き込
み還元処理を行つた。その結果、吸収液中には二
価の銅または酸素錯体は全く存在せず、2.0モ
ル／の一価の銅が存在していた。Example 2 In the same manner as in Example 1, 50 ml of a tris(dimethylamino)phosphone oxide solution containing 1.9 mol/monovalent copper and 0.1 mol/divalent copper (0.025 mol/as an oxygen complex) was added. , volume 100
ml in a cylindrical glass container. A CO-containing gas was blown into this absorption liquid under the same conditions as in Example 1 to perform a reduction treatment. As a result, there was no divalent copper or oxygen complex present in the absorption liquid, and 2.0 mol/monovalent copper was present.
実施例 ３
実施例１と同様の方法で、２モル／のuClを
含むトリス（ジメチルアミノ）ホスフインオキシ
ド溶液を調整し、30℃、CO分圧0.2atmにおける
CO平衡吸収量を求めたところ、吸収液１ml当た
り22.3mlのCOを吸収した。Example 3 A tris(dimethylamino)phosphine oxide solution containing 2 mol/uCl was prepared in the same manner as in Example 1, and the solution was prepared at 30°C and a CO partial pressure of 0.2 atm.
When the equilibrium CO absorption amount was determined, 22.3 ml of CO was absorbed per 1 ml of absorption liquid.
一方、実施例２で示した、酸素吸収処理した吸
収液の30℃、CO分圧0.2atmにおけるCO平衡吸収
量を求めたところ、吸収液１ml当たり19.0mlであ
り、酸素吸収処理前のものに比べCO吸収能力が
低下していた。 On the other hand, as shown in Example 2, when the equilibrium CO absorption amount at 30°C and CO partial pressure 0.2 atm of the absorbent treated with oxygen absorption treatment was determined, it was 19.0 ml per 1 ml of the absorbent, and it was found that Compared to this, the CO absorption capacity was decreased.
さらに、実施例２と同様な方法で還元処理した
吸収液について、30℃、CO分圧0.2atmにおける
CO平衡吸収量を求めたところ、吸収液１ml当た
り22.3mlのCOを吸収した。 Furthermore, regarding the absorption liquid reduced in the same manner as in Example 2, at 30°C and CO partial pressure 0.2atm,
When the equilibrium CO absorption amount was determined, 22.3 ml of CO was absorbed per 1 ml of absorption liquid.
以上の結果より、塩化第１銅をトリス（ジメチ
ルアミノ）ホスフインオキシドに溶解せしめた
CO吸収液は、O2によりCO吸収性能が低下する
が、液を高温に保ち還元処理することにより再生
され、CO吸収能力が回復することが明らかにな
つた。 Based on the above results, cuprous chloride was dissolved in tris(dimethylamino)phosphine oxide.
It has been revealed that the CO absorption performance of the CO absorption liquid decreases due to O 2 , but by keeping the liquid at a high temperature and subjecting it to reduction treatment, it can be regenerated and the CO absorption capacity can be restored.
実施例 ４
実施例１と同様な方法で、２モル／のCuCl
を含むトリス（ジメチルアミノ）ホスフインオキ
シド溶液50mlを調整した。この溶液を30℃に保ち
つつ、CO20％、O20.1％、N279.9％（容量％）か
らなる組成のガスを常圧下、200Nml／minの割
合で35分間吹き込んだ。その結果、吸収液１ml当
たり20.5mlのCO吸収したが、同時に0.06モル／
の二価の銅（酸素錯体として0.015モル／）が
生成した。Example 4 In the same manner as in Example 1, 2 mol/CuCl
50 ml of tris(dimethylamino)phosphine oxide solution was prepared. While maintaining this solution at 30° C., a gas having a composition of 20% CO, 0.1% O 2 , and 79.9% N 2 (volume %) was blown into the solution at a rate of 200 Nml/min for 35 minutes under normal pressure. As a result, 20.5 ml of CO was absorbed per ml of absorption liquid, but at the same time 0.06 mol/ml of CO was absorbed.
of divalent copper (0.015 mol/oxygen complex) was produced.
その後、窒素ガスを200Nml／minの割合で吹
き込みつつ吸収液を90℃に保ち、COを分離した。
その結果、35分間で20.5mlのCOが回収されたが、
吸収液中には二価の銅（または酸素錯体）は全く
存在せず、2.0mol／の一価の銅が存在してい
た。 Thereafter, the absorption liquid was maintained at 90°C while blowing nitrogen gas at a rate of 200 Nml/min to separate CO.
As a result, 20.5ml of CO was recovered in 35 minutes, but
There was no divalent copper (or oxygen complex) in the absorption liquid, and 2.0 mol/monovalent copper was present.
このことは、CO分離、濃縮の対象となるガス
源中のCO、O2濃度により条件が大きく異なるも
のの、CO分離塔において充分な滞留時間をとれ
ば、特別に再生装置（還元塔）を設けなくても、
分離塔内で同時に吸収液を再生することが可能で
あることを示している。第２図は、還元塔を設け
ない場合のCO分離、濃縮プロセスのフローシー
トであり、第１図の場合に比べ、分離塔３の滞留
時間を長くするように下部の容量を大きくしたも
のである。 Although the conditions for this vary greatly depending on the CO and O 2 concentrations in the gas source to be separated and concentrated, if sufficient residence time is allowed in the CO separation tower, a special regeneration device (reduction tower) can be installed. Even without,
This shows that it is possible to simultaneously regenerate the absorption liquid within the separation column. Figure 2 is a flow sheet for the CO separation and concentration process without a reduction tower, and compared to the case in Figure 1, the lower capacity of the separation tower 3 is increased to lengthen the residence time. be.
本発明によれば、COおよびO2を含有するガス
源から、吸収液の劣化を抑制しつつ、またO2を
吸収してCO旧主性能が低下した吸収液を、連続
的に再生して循環使用することができるなど、優
れた効果が達成される。
According to the present invention, while suppressing the deterioration of the absorption liquid from a gas source containing CO and O 2 , the absorption liquid whose CO main performance has deteriorated due to absorption of O 2 is continuously regenerated. Excellent effects such as being able to be used repeatedly are achieved.
第１図および第２図は、それぞれ本発明のCO
分離、濃縮プロセスの実施例を示すフローシート
である。
２……吸収塔、３……分離塔、５……還元塔、
１１……ガス供給ライン。
Figures 1 and 2 show the CO of the present invention, respectively.
1 is a flow sheet showing an example of a separation and concentration process. 2...Absorption tower, 3...Separation tower, 5...Reduction tower,
11...Gas supply line.
Claims (1)
リンの酸素酸誘導体を含む吸収液に接触させて一
酸化炭素を吸収させる際に、前記酸素によつて一
酸化炭素吸収能力が低下した吸収液を、一酸化炭
素の共存下で60〜150℃に加熱することを特徴と
する一酸化炭素吸収液の再生方法。 ２ 特許請求の範囲第１項において、前記再生さ
れた吸収液を循環使用することを特徴とする一酸
化炭素吸収液の再生方法。[Claims] 1. When a gas containing carbon monoxide and oxygen is brought into contact with an absorption liquid containing monovalent copper and an oxyacid derivative of phosphorus to absorb carbon monoxide, the carbon monoxide is absorbed by the oxygen. A method for regenerating a carbon monoxide absorbing liquid, which comprises heating an absorbing liquid whose carbon oxide absorption capacity has decreased to 60 to 150°C in the coexistence of carbon monoxide. 2. A method for regenerating a carbon monoxide absorbing liquid according to claim 1, characterized in that the regenerated absorbing liquid is recycled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55118266A JPS5742521A (en) | 1980-08-29 | 1980-08-29 | Method for separation and concentration of carbon monoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55118266A JPS5742521A (en) | 1980-08-29 | 1980-08-29 | Method for separation and concentration of carbon monoxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5742521A JPS5742521A (en) | 1982-03-10 |
| JPH0121087B2 true JPH0121087B2 (en) | 1989-04-19 |
Family
ID=14732373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP55118266A Granted JPS5742521A (en) | 1980-08-29 | 1980-08-29 | Method for separation and concentration of carbon monoxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5742521A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD260042A1 (en) * | 1987-04-24 | 1988-09-14 | Nagema Veb K | DEVICE FOR HOLDING AND WRAPPING OF BONBONS |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4019879A (en) * | 1975-09-26 | 1977-04-26 | Union Carbide Corporation | Selective adsorption of carbon monoxide from gas streams |
-
1980
- 1980-08-29 JP JP55118266A patent/JPS5742521A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5742521A (en) | 1982-03-10 |
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