JPS58219914A - Preparation of carbon monoxide absorbing liquid - Google Patents
Preparation of carbon monoxide absorbing liquidInfo
- Publication number
- JPS58219914A JPS58219914A JP57100657A JP10065782A JPS58219914A JP S58219914 A JPS58219914 A JP S58219914A JP 57100657 A JP57100657 A JP 57100657A JP 10065782 A JP10065782 A JP 10065782A JP S58219914 A JPS58219914 A JP S58219914A
- Authority
- JP
- Japan
- Prior art keywords
- dimethylamino
- tris
- carbon monoxide
- phosphine oxide
- absorbing liquid
- 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.)
- Granted
Links
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Gas Separation By Absorption (AREA)
- Carbon And Carbon Compounds (AREA)
- Treating Waste Gases (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、−酸化炭素（以下ＣＯと記す）の吸収液に係
り、特にＣＯを含有する各種ガス源からＣＯ分離、濃縮
して回収するための安定な吸収液の調製法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an absorption liquid for -carbon oxide (hereinafter referred to as CO), and in particular to a stable absorption liquid for separating, concentrating and recovering CO from various gas sources containing CO. Regarding preparation method.
化学工業や製鉄工業等において１合成化学用原料ガスの
製造あるいは省エネルギのために１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
的課題になっている。BACKGROUND ART In the chemical industry, iron and steel industry, etc., it has become a major technical issue to separate, concentrate and recover CO from process exhaust gas, for example, in order to produce raw material gas for synthetic chemistry or to save energy.
ＣＯを含有するガス源からＣＯを分離、濃縮しうる方法
には、現在、第一銅塩の溶液等の吸収液を使用する吸収
法、およびそれとは原理的に異る深冷分離法が知られて
いる。後者の深冷分離法は、複雑な溶却、熱回収シ具・
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
を得名ために、動力消費量が大きくなるという欠点があ
る。Currently, there are two known methods for separating and concentrating CO from a CO-containing gas source: an absorption method that uses an absorption liquid such as a cuprous salt solution, and a cryogenic separation method that is fundamentally different from that method. It is being The latter cryogenic separation method requires complex melting, heat recovery equipment and
Since the operating temperature is low, it is necessary to use expensive equipment materials, and the low temperature also has the disadvantage of increasing power consumption.
一方、吸収法に使用されるＣＯ吸収液とじては、従来、
アンモニア性第一銅水溶液または。On the other hand, the CO absorption liquid used in the absorption method has conventionally been
Ammoniacal cuprous solution or.
塩酸性第一銅塩水溶液が用いられてきた。しかし、いず
れも水溶液単位体積あたりのＣＯ吸収量が小さいという
問題があった。これに対し本発明者らは、塩化第一銅（
以下ＣｕＱｔと記す）をトリスジメチルアミンホスフィ
ンオキシト（以下ＨＭＰＡと記す）に溶解せしめた。Ｃ
Ｏ吸収量の高い吸収液を開発した（特願昭５５−９２／
Ａ７号厄この吸収液は単位体積あたりのＣＯ吸収量が水
溶液系のものに較べて非常に高く、実際のプＪセスの適
用時には１種々の利点がある。Aqueous hydrochloric cuprous salt solutions have been used. However, both methods have a problem in that the amount of CO absorbed per unit volume of aqueous solution is small. In contrast, the present inventors discovered cuprous chloride (
CuQt) was dissolved in trisdimethylaminephosphine oxide (hereinafter referred to as HMPA). C
Developed an absorbing liquid with high O absorption capacity (Patent application 1982-1992/
This No. A7 absorption liquid has a much higher CO absorption amount per unit volume than an aqueous solution, and has various advantages when used in actual processes.
しかし、上記吸収液はＣＯ以外忙水分を吸収するという
性質があり、このだめ原料ガス中に通常含まれる水分が
操作中に吸収液中に混入してくることは避けられない。However, the absorption liquid has the property of absorbing moisture other than CO, and it is inevitable that the moisture normally contained in the raw material gas will be mixed into the absorption liquid during operation.
ところで、吸収液法におけるＣＯ分離・濃縮プロセスで
は、一般に、低温でのＣＯ吸収、およびＣＯを吸収した
液゛を加熱することによるＣＯの放散というサイクルが
繰り返し行われるが、前述の吸収液に水分が混入すると
、放散塔またはリボイラ等で加熱される際９次式に従っ
て塩化第一銅の加水分解が生じ、それに伴いＯｕ＋０が
沈殿し、液中のＣＯ吸収に有効な一価の銅の濃度が低下
する。このことは吸収液のｃ’ｏ吸収吸収能カが経済的
に低下すると七を意味する。By the way, in the CO separation/concentration process using the absorption liquid method, a cycle of CO absorption at low temperatures and CO dissipation by heating the CO-absorbed liquid is generally repeated. If chloride is mixed in, cuprous chloride will be hydrolyzed according to the 9th order formula when heated in a stripping tower or reboiler, etc., and Ou+0 will precipitate as a result, and the concentration of monovalent copper, which is effective for CO absorption in the liquid, will decrease. descend. This means that the c'o absorption capacity of the absorbing liquid is economically reduced.
２ Ｃ！ｕ Ｇｌ＋ Ｈ２０４：！ ０ｕｌｌＯ↓＋２
ｗａｔ本発明の目的は、上記先願技術を改善し、吸収
液中に水分が混入しても吸収性能の低下を生じないｇｏ
吸収液を提供するにある。2C! u Gl+ H204:! 0ullO↓+2
An object of the present invention is to improve the prior art described above, and to provide a method that does not cause a decrease in absorption performance even when water is mixed into the absorption liquid.
Provides an absorbent solution.
本発明は、（塩化第一銅とトリス（ジメチルアミノンホ
スフィンオキシトおよび有機溶媒を含む一酸化炭素吸収
液を調製するに際し、トリス（ジメチルアミノ）ホスフ
ィンオキシト中の不純物であるジメチルアミンを除去す
ることを特徴とする一酸化炭素吸収液の調製法。）、で
ある。The present invention involves removing dimethylamine, which is an impurity in tris(dimethylamino)phosphine oxide, when preparing a carbon monoxide absorption solution containing cuprous chloride, tris(dimethylamino)phosphine oxide, and an organic solvent. A method for preparing a carbon monoxide absorption liquid characterized by:
上記目的を達盛スるため９本発明においては。In order to achieve the above object, the present invention has the following features.
吸収液の一組成をなすトリス（ジメチルアミノ）ホスフ
ィンオキシト中にしばしば含まれるジメチルアミンを除
去して、吸収液を調製することを特徴とするものである
。This method is characterized in that the absorption liquid is prepared by removing dimethylamine, which is often contained in tris(dimethylamino)phosphine oxide, which is a component of the absorption liquid.
即ち、市販のトリス（ジメチルアミノ）ホスフィンオキ
シト中には、不純物としてジメチルアミンが含まれるが
９発明者らは、前記の塩化第一銅の加水分解反応が、ジ
メチルアミンの存在下で加速されることを見出し０本発
明を達成するに到った。That is, although commercially available tris(dimethylamino)phosphine oxide contains dimethylamine as an impurity,9 the inventors found that the hydrolysis reaction of cuprous chloride was accelerated in the presence of dimethylamine. The present invention was achieved based on this discovery.
なお、ジメチルアミノの除去法として、例えばトリス（
ジメチルアミノ）ホスフィンオキシト中に鄭ガスを吹込
み、揮発性のジメチルアミノを弾数させても良い０ま九
、ジメチルアミンは、アルカリ性であり、フリーの状態
でトリス（ジメチルアミノ）ホスフィンオキシト中に微
量存在すると、蟲腋するホスフィンオキシトはＰＨ５以
上を示す。（ＰＨはトリス（ジメチルアξ〕）ホスフィ
ンオキシト１ｆを１００９ Ｏ１８０に投入し画定した
。）
以下１本発明を試験例及び実施例をもって説明する。・
試験例１
役付試験管に市販のトリス（ジメチルアンノンホスフィ
ンオキシドを１５０ｓ−採取し、これＫＯｕａｔを７５
ｍｍｏｌ溶解せしめ九のち、トルエンで５０−に希釈
した。この液を２本ａｌａｌｌＬ、１本目にはＨ畠０を
０．５ ｓｇ ＠加し、他の１本には、ジメチルアミン
のν、５ｖｐｏ１７ Ｌ溶液を０．８７ ｍ （ジメチ
ルアミノ８．５ ｖｓｇＩＱｔｓ ｕｓ ｏ Ｕ−５ｓ
ｍｇ ）添加し、そレ−ｔ’ｊＬｔ−９０００で５０分
間加熱して、生成したＯｕｉ Ｏを定量した。In addition, as a method for removing dimethylamino, for example, Tris (
It is also possible to blow gas into the dimethylamino)phosphine oxide to make volatile dimethylamino a number of particles.Dimethylamine is alkaline, and in its free state, tris(dimethylamino)phosphine oxyto When present in trace amounts, phosphine oxyto exhibits a pH of 5 or higher. (PH was determined by adding tris(dimethylaξ)phosphine oxide 1f to 1009 O180.) The present invention will be explained below with reference to test examples and examples.・Test Example 1 Commercially available tris (dimethylannonphosphine oxide) was collected in a test tube for 150 s, and KOuat was 75 s.
After 9 mmol was dissolved, it was diluted to 50 mmol with toluene. Add 0.5 sg of this solution to the first bottle, and add 0.87 m of dimethylamine ν, 5vpo17L solution to the other bottle (dimethylamino 8.5 vsgIQts). us o U-5s
mg) was added and heated for 50 minutes using Solet-t'jLt-9000, and the produced Oui O was quantified.
その結果、励０のみを添加し丸ものでは２．５−のＯｕ
ｔ Ｏが生成したのみであったが、ジメチルアミ′ン水
Ｓ痕を添加し友ものにおいては、約６倍の１５−一のｃ
ｕｔ ｏが生成した０これにより、０ｕａＬの加水分解
反応が、ジメチルアミンにより加速されることが明らか
になった。なお、ジメチルアミンは。As a result, only 0 excitation was added, and in the round one, 2.5-Ou
Only tO was produced, but in the case where dimethylamine water S traces were added, the amount of 15-1 was about 6 times as large.
This revealed that the hydrolysis reaction of 0uaL was accelerated by dimethylamine. In addition, dimethylamine.
吸収液のＰＭを上昇させ反応を促進してｉるものと考え
られる。It is thought that this increases the PM of the absorption liquid and promotes the reaction.
実施例１
市販のトリス（ジメチルアミノ）ホスフィンオキシトに
乾燥した塩化水素ガスを０−２５ ｓｆｗＡｄ。Example 1 Dry hydrogen chloride gas was added to commercially available tris(dimethylamino)phosphine oxide at 0-25 sfwAd.
の割合で吹込んだところ、６０分後に先にのべた測定方
法によるＰＨが６に低下した。（吹込前のｐＨｄ１２）
このトリス（ジメチルアミノ）ホスフィンオキシトを用
いて、試験例１と同じ組成の吸収液を調製し、試験例１
と同じくＨ２Ｏを０．５ｙ添加し、９０°Ｃで６０時間
加熱したが、沈殿の生成は全く認められず本発明の有効
性が確認できた。When the mixture was injected at a ratio of 1, the pH decreased to 6 after 60 minutes according to the measurement method described above. (pHd12 before blowing)
Using this tris(dimethylamino)phosphine oxide, an absorption liquid having the same composition as in Test Example 1 was prepared, and
Similarly, 0.5y of H2O was added and heated at 90°C for 60 hours, but no precipitation was observed, confirming the effectiveness of the present invention.
実施例２
栓付試験管に、実施列１と同様に処理したトリス（ジメ
チルアミノ）ホスフィンオキシトｔ−２００ｍｍＱｌ採
取し、これに０ｕＧ４を１００ ｍｍｏｌ溶解せしめた
のち、トルエンで５０−に希釈し、さらにＨ２Ｏを０．
５ｍ／ｉ加したのち、９０°Ｃで６０時間加熱したが、
沈殿の生成は全く認められなかった。この結果、液中の
Ｃ！ｕｏｔ濃度が高くても９本発明は有効であることが
認められる。Example 2 200 mmQl of tris(dimethylamino)phosphine oxytane treated in the same manner as in Example 1 was collected in a stoppered test tube, and 100 mmol of 0uG4 was dissolved therein, and then diluted to 50% with toluene. Furthermore, add 0.0% H2O.
After heating at 90°C for 60 hours,
No formation of precipitate was observed. As a result, C! It is recognized that the present invention is effective even when the uot concentration is high.
実施例６
実施例１において、塩化水素ガスに替えて、乾燥窒素ガ
スを１１ ／ｍｌｎの割合で、トリス（ジメチルアミノ
）ホスフィンオキシトに＝吹込んだところ、２０時間後
にＰＨが６に低下した。このトリス（ジメチルアミノ）
ホスフィンオキシトを用いて実施例１と同様の検討を行
ったが、この場合においても、 （ｕ２０の生成は全く
認められなかった。低沸点（ｂ、９７°Ｃ／ ７６０
ｎｒｎＮｌ ）のジメチルアミンが乾燥窒素によシ揮散
除去されたためであり、ジメチルアミンの除去が、液の
安定性を左右していることを示している。Example 6 In Example 1, instead of hydrogen chloride gas, dry nitrogen gas was blown into tris(dimethylamino)phosphine oxide at a rate of 11/ml, and the pH decreased to 6 after 20 hours. . This tris(dimethylamino)
The same study as in Example 1 was conducted using phosphine oxide, but in this case as well, no formation of U20 was observed.Low boiling point (b, 97°C/760
This is because dimethylamine (nrnNl) was removed by volatilization with dry nitrogen, indicating that the removal of dimethylamine affects the stability of the liquid.
以上９本発明によれば、塩化第一銅とトリス（ジメチル
アミノ）ホスフィンオキシトおよび有機溶媒からなる吸
収液の調製時に、トリス（ジメチルアミノ）ホスフィン
オキシト中のジメチルアミンを除去することによシ、水
が混入しても容易に分解せず、高温で安定でかつ高性能
のＣＯ吸収液とすることができる。According to the present invention, the dimethylamine in tris(dimethylamino)phosphine oxide is removed during the preparation of an absorption liquid consisting of cuprous chloride, tris(dimethylamino)phosphine oxide, and an organic solvent. Moreover, even if water is mixed in, it does not easily decompose, and it is possible to obtain a CO absorption liquid that is stable at high temperatures and has high performance.
Claims (3)
ィンオキシトおよび有機溶媒を含む一酸化炭素吸収液を
調製するに際し、トリス（ジメチルアミノ）ホスフィン
オキシト中の不純物であるジメチルアミンを除去するこ
とを特徴とする一酸化炭素吸収液の調製法。(1) When preparing a carbon monoxide absorption solution containing cuprous chloride and tris(dimethylamino) phosphine oxide and an organic solvent, remove dimethylamine, an impurity in tris(dimethylamino)phosphine oxide. A method for preparing a carbon monoxide absorbing liquid, characterized by:
ト中の不純物ジメチルアミノを塩化水素ガスで中和除去
することを特徴とする特許請求の範囲第１項記載の一酸
化炭素吸収液の調製法。(2)) A method for preparing a carbon monoxide absorption liquid according to claim 1, characterized in that impurity dimethylamino in lith(dimethylamino)phosphine oxide is neutralized and removed with hydrogen chloride gas.
ト中の不純物ジメチルアミンを乾燥窒素ガスを吹き込み
発散除去することを特徴とする特許請求の範囲第１項記
載の一酸化炭素吸収液の調製法。(3) A method for preparing a carbon monoxide absorption liquid according to claim 1, characterized in that the impurity dimethylamine in tris(dimethylamino)phosphine oxide is removed by blowing dry nitrogen gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57100657A JPS58219914A (en) | 1982-06-14 | 1982-06-14 | Preparation of carbon monoxide absorbing liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57100657A JPS58219914A (en) | 1982-06-14 | 1982-06-14 | Preparation of carbon monoxide absorbing liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58219914A true JPS58219914A (en) | 1983-12-21 |
| JPH0262293B2 JPH0262293B2 (en) | 1990-12-25 |
Family
ID=14279875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57100657A Granted JPS58219914A (en) | 1982-06-14 | 1982-06-14 | Preparation of carbon monoxide absorbing liquid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58219914A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0310064A2 (en) * | 1987-09-30 | 1989-04-05 | Babcock-Hitachi Kabushiki Kaisha | CO-absorbing solution, process for absorbing and recovering CO |
| JP2011037774A (en) * | 2009-08-12 | 2011-02-24 | Toei Corp | Process for producing methylenebisbenzotriazolyl(hydroxyalkyl)phenol compound |
-
1982
- 1982-06-14 JP JP57100657A patent/JPS58219914A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0310064A2 (en) * | 1987-09-30 | 1989-04-05 | Babcock-Hitachi Kabushiki Kaisha | CO-absorbing solution, process for absorbing and recovering CO |
| US4950462A (en) * | 1987-09-30 | 1990-08-21 | Babcock-Hitachi Kabushiki Kaisha | Process for absorbing CO |
| JP2011037774A (en) * | 2009-08-12 | 2011-02-24 | Toei Corp | Process for producing methylenebisbenzotriazolyl(hydroxyalkyl)phenol compound |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0262293B2 (en) | 1990-12-25 |
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