JPH0225472Y2 - - Google Patents
Info
- Publication number
- JPH0225472Y2 JPH0225472Y2 JP1983077471U JP7747183U JPH0225472Y2 JP H0225472 Y2 JPH0225472 Y2 JP H0225472Y2 JP 1983077471 U JP1983077471 U JP 1983077471U JP 7747183 U JP7747183 U JP 7747183U JP H0225472 Y2 JPH0225472 Y2 JP H0225472Y2
- Authority
- JP
- Japan
- Prior art keywords
- hmpa
- absorption liquid
- water
- absorption
- 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
Links
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 29
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 29
- 238000010521 absorption reaction Methods 0.000 claims description 27
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 16
- 238000003795 desorption Methods 0.000 claims description 11
- 238000011084 recovery Methods 0.000 claims description 9
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 7
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 7
- 229940045803 cuprous chloride Drugs 0.000 claims description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 238000000034 method Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- UCKOCRCUTZRTRW-UHFFFAOYSA-F dialuminum copper octachloride Chemical compound [Al+3].[Al+3].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cu++] UCKOCRCUTZRTRW-UHFFFAOYSA-F 0.000 description 1
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Gas Separation By Absorption (AREA)
- Carbon And Carbon Compounds (AREA)
- Treating Waste Gases (AREA)
Description
【考案の詳細な説明】
本考案は、一酸化炭素（CO）の分離・濃縮装
置に係り、特に吸収液成分を長期間一定にし、安
定に循環使用するに好適なCOの分離・濃縮装置
に関する。[Detailed description of the invention] The present invention relates to a carbon monoxide (CO) separation/concentration device, and particularly to a CO separation/concentration device that is suitable for keeping absorption liquid components constant for a long period of time and for stable circulation. .
化学工業や製鉄工業等において、合成化学原料
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になつている。 In the chemical industry, steel industry, etc., separating, concentrating, and recovering CO from process exhaust gas has become a major technical issue for the production of synthetic chemical raw material gas or for energy conservation.
従来、COを含有するガス源からCOを分離・濃
縮する方法としては、第１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な
る深冷分離法が知られている。後者の方法は、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。 Conventionally, methods for separating and concentrating CO from a gas source containing CO include 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. There is. The latter method consists of a complex cooling and heat recovery system,
Since the operating temperature is low, it is necessary to use expensive equipment materials, and there is also the disadvantage that power consumption is large in order to obtain the low temperature.
一方、吸収法に使用されているCO吸収液とし
ては、従来、アンモニア性第１銅水溶液またはテ
トラクロロアルミン酸銅のトルエン溶液が用いら
れてきた。しかし、前者では溶液単位体積当たり
のCO吸収量が小さいという問題があり、また後
者では水と定量的に反応し劣化するという問題が
あつた。これに対し、本考案者らは、塩化第１銅
（以下CuClと記す）をトリス（ジメチルアミノ）
ホスフインオキシド（別各ヘキサメチルホスホリ
ルトリアミド、以下、HMPAと記す）に溶解せ
しめた吸収液がCO吸収量が高く、水と接触して
も劣化しないことを見出し、該吸収液に適した
COの分離・濃縮装置を考案した（特願昭55−
92607号、実願昭57−87434号）。 On the other hand, as the CO absorption liquid used in the absorption method, an ammoniacal cuprous aqueous solution or a toluene solution of copper tetrachloroaluminate has conventionally been used. However, the former has a problem in that the amount of CO absorbed per unit volume of solution is small, and the latter has a problem in that it reacts quantitatively with water and deteriorates. In contrast, the inventors of the present invention discovered that cuprous chloride (hereinafter referred to as CuCl) was converted into tris(dimethylamino).
It was discovered that an absorption liquid dissolved in phosphine oxide (separately referred to as hexamethylphosphoryl triamide, hereinafter referred to as HMPA) has a high CO absorption amount and does not deteriorate even when it comes in contact with water, and has developed a solution suitable for this absorption liquid.
Devised a device for separating and concentrating CO (patent application 1983-
No. 92607, Utility Application No. 57-87434).
しかし、その後、種々検討したところ、上記の
装置において、水分離器からの回収水中に少量の
HMPAが含まれ、非常に長期間の連続運転に際
しては、吸収液中のHMPAが減少しそれを補給
する必要があるという問題点が明らかになつた。 However, after various studies, we found that in the above equipment, a small amount of water was collected from the water separator.
It has become clear that when the absorption liquid contains HMPA and is operated continuously for a very long period of time, the amount of HMPA in the absorption liquid decreases and it is necessary to replenish it.
本考案の目的は、上記したCuClをHMPAに溶
解せしめ、さらにトルエンで希釈したCO吸収液
（以下、CuCl・HMPA／トルエン液と記す）を
用いたCO分離・濃縮プロセスにおいて、吸収液
成分、特にHMPAを長期間一定に、かつ安定に
循環使用することができるCO分離・濃縮装置を
提供することにある。 The purpose of this invention is to dissolve the above-mentioned CuCl in HMPA and further dilute it with toluene in a CO separation/concentration process using a CO absorption liquid (hereinafter referred to as CuCl/HMPA/toluene liquid). The object of the present invention is to provide a CO separation/concentration device that can constantly and stably circulate and use HMPA over a long period of time.
本考案は、CuCl・HMPA／トルエン液を用い
て低濃度COを含有するガスを処理し、高純度の
COを回収する装置において、CO脱離塔の水分離
装置の後流にHMPA回収装置を設けたことを特
徴とするものである。すなわち、本考案は、CO
を含有するガスを吸収塔に供給し、塩化第１銅と
HMPAを含む吸収液で処理した後、脱離塔で吸
収液からCOを脱離し、さらに脱離ガスを冷却器
および水分離装置で処理して吸収液を回収した
後、脱離塔へ循環させる系統を備えた装置におい
て、水分離装置の後流にHMPA回収装置を設け
たことを特徴とする。 This invention uses a CuCl/HMPA/toluene solution to process gas containing low concentrations of CO, producing high-purity
The apparatus for recovering CO is characterized in that an HMPA recovery apparatus is provided downstream of the water separation apparatus of the CO desorption tower. In other words, the present invention
The gas containing cuprous chloride and
After treatment with an absorption liquid containing HMPA, CO is desorbed from the absorption liquid in a desorption tower, and the desorption gas is further processed in a cooler and water separation device to recover the absorption liquid, which is then circulated to the desorption tower. The apparatus is characterized in that an HMPA recovery device is provided downstream of the water separation device.
以下、本考案を図面によりさらに詳細に説明す
る。第１図は本考案のCO分離・濃縮装置の原理
的な系統図である。図において、COおよびH2O
含有ガスは、原料ガスライン１１から必要に応じ
て前処理装置１で前処理された後、吸収塔２に入
り、吸収塔内の吸収液と接触し、COが吸収され
る。この時、ガス中の一部の水（H2O）は液中
に吸収される。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から大気
中に放出される。一方、COおよびH2Oを吸収し
た液は、COリツチ溶液ライン３１から熱交換器
４を経て脱離塔３に送られ、ここで昇温または減
圧されることによりCOを放散する。脱離塔３か
らの放散ガスライン４１中にはCO以外にH2O、
トルエン、HMPAの蒸気が共存するため、ガス
冷却器５でそれらの蒸気を冷却し、循環ライン７
１をへて水分離装置６へと導き、ここで水が分離
され、HMPAおよびトルエンのみが循環ライン
８１を通じて脱離塔３下部へリサイクルされる。
H2O、HMPAおよびトルエン蒸気を除去された
高濃度COガスはガスライン６１から製品ガスと
して回収される。一方、COを放散した液はリー
ン溶液ライン５１を介して吸収塔２へ戻され、循
環使用される。 Hereinafter, the present invention will be explained in more detail with reference to the drawings. Figure 1 is a basic system diagram of the CO separation/concentration device of the present invention. In the figure, CO and H2O
The contained gas is pretreated in the pretreatment device 1 as necessary from the raw material gas line 11, and then enters the absorption tower 2, contacts the absorption liquid in the absorption tower, and absorbs CO. At this time, some of the water (H 2 O) in the gas is absorbed into the liquid. The absorption tower exhaust gas is discharged into the atmosphere from the exhaust gas line 21 after the entrained components are appropriately removed. On the other hand, the liquid that has absorbed CO and H 2 O is sent from the CO rich solution line 31 to the desorption tower 3 via the heat exchanger 4, where it is heated or depressurized to release CO. In addition to CO, H 2 O,
Since toluene and HMPA vapors coexist, the gas cooler 5 cools these vapors, and the circulation line 7
1 to a water separator 6 where water is separated and only HMPA and toluene are recycled to the lower part of the desorption column 3 through a circulation line 81.
The highly concentrated CO gas from which H 2 O, HMPA and toluene vapor have been removed is recovered from gas line 61 as a product gas. On the other hand, the liquid from which CO has been diffused is returned to the absorption tower 2 via the lean solution line 51 and used for circulation.
ところが、水分離装置６では、トルエンと水の
分離は、これらが溶け合わないことによる比重差
を利用する方法を主に用いているが、さらに詳細
に検討したところ、HMPAがトルエンとH2Oに
相互に分配され、HMPAの一部が系外に除外さ
れるH2O中に溶解し、逸散することが分つた。
ちなみに、トルエン−HMPA−水系における分
配係数は30℃で0.3であつた。このため、本考案
においては、水分離装置６の後流にHMPA回収
装置７を設け、水分離装置６からライン９１を経
て回収された水からさらにHMPAを回収し、こ
れをライン１０１を介して前記循環ライン８１に
戻すようにしている。 However, in the water separation device 6, toluene and water are separated using a method that mainly utilizes the difference in specific gravity due to the fact that they do not dissolve in each other. It was found that a part of HMPA was dissolved in H 2 O, which was excluded from the system, and was dissipated.
Incidentally, the partition coefficient in the toluene-HMPA-water system was 0.3 at 30°C. For this reason, in the present invention, an HMPA recovery device 7 is provided downstream of the water separation device 6, and HMPA is further recovered from the water recovered from the water separation device 6 via the line 91, and this is transferred via the line 101. The water is returned to the circulation line 81.
上記HMPAの回収装置７としては、塩素化炭
化水素を用いる方法（西独特許等1121247号
（1962））、モレキユラーシーブ、活性炭等を用い
た吸着法等を用いたものが例示されるが、水と
HMPAを分離する装置であればどのようなもの
でもよい。 Examples of the HMPA recovery device 7 include a method using chlorinated hydrocarbons (West German Patent No. 1121247 (1962)), a molecular sieve, an adsorption method using activated carbon, etc. water and
Any device that separates HMPA may be used.
上記構成によれば、水分離装置６からの水中に
含まれるHMPAはHMPA回収装置７で回収され
た後、循環ライン１０１および８１をへて脱離塔
３下部へリサイクルされる。一方、分離された
H2Oは排水ライン１１１をへて系外に除去され
る。これにより、HMPAの逸散が事実上なくな
り、長期にわたり吸収液の組成を一定に保ちつ
つ、安定に運転することが可能になる。 According to the above configuration, HMPA contained in the water from the water separation device 6 is recovered by the HMPA recovery device 7 and then recycled to the lower part of the desorption tower 3 through the circulation lines 101 and 81. On the other hand, separated
H 2 O is removed from the system through a drainage line 111. This virtually eliminates the escape of HMPA, making it possible to maintain stable operation while keeping the composition of the absorption liquid constant over a long period of time.
以上、本考案によれば、吸収液中のHMPA濃
度を長期間一定に保ち、安定に効率よくCOを分
離・濃縮することができる。 As described above, according to the present invention, the HMPA concentration in the absorption liquid can be kept constant for a long period of time, and CO can be separated and concentrated stably and efficiently.
第１図は、本考案の一実施例を示すCO分離・
濃縮装置の系統図である。
１……前処理装置、２……吸収塔、３……脱離
塔、５……ガス冷却器、６……水分離装置、７…
…HMPA回収装置、８１……吸収液循環ライン、
９１……水ライン、１０１……回収HMPA循環
ライン。
Figure 1 shows a CO separation system showing one embodiment of the present invention.
It is a system diagram of a concentrator. 1... Pretreatment device, 2... Absorption tower, 3... Desorption tower, 5... Gas cooler, 6... Water separation device, 7...
...HMPA recovery device, 81...Absorption liquid circulation line,
91...Water line, 101...Recovery HMPA circulation line.
Claims (1)
スを吸収塔に供給し、塩化第１銅とトリス（ジメ
チルアミノ）ホスフインオキシドを含む吸収液で
処理した後、脱離塔で吸収液からCOを脱離し、
さらに脱離ガスを冷却器および水分離装置で処理
して吸収液を回収した後、脱離塔へ循環させる系
統を備えた装置において、水分離装置の後流にト
リス（ジメチルアミノ）ホスフインオキシドの回
収装置を設けたことを特徴とするCOの分離・濃
縮装置。 Gas containing carbon monoxide (hereinafter referred to as CO) is supplied to an absorption tower, treated with an absorption liquid containing cuprous chloride and tris(dimethylamino)phosphine oxide, and then removed from the absorption liquid in a desorption tower. desorbs CO,
Furthermore, in an apparatus equipped with a system for treating the desorption gas with a cooler and a water separator to recover an absorption liquid and then circulating it to a desorption tower, tris(dimethylamino)phosphine oxide is added downstream of the water separator. A CO separation/concentration device characterized by being equipped with a recovery device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1983077471U JPS59184921U (en) | 1983-05-25 | 1983-05-25 | Carbon monoxide separation/concentration equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1983077471U JPS59184921U (en) | 1983-05-25 | 1983-05-25 | Carbon monoxide separation/concentration equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59184921U JPS59184921U (en) | 1984-12-08 |
| JPH0225472Y2 true JPH0225472Y2 (en) | 1990-07-12 |
Family
ID=30207498
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1983077471U Granted JPS59184921U (en) | 1983-05-25 | 1983-05-25 | Carbon monoxide separation/concentration equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59184921U (en) |
-
1983
- 1983-05-25 JP JP1983077471U patent/JPS59184921U/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59184921U (en) | 1984-12-08 |
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