JPS63192737A - Purification and recovery of methyl ethyl ketone - Google Patents

Purification and recovery of methyl ethyl ketone

Info

Publication number
JPS63192737A
JPS63192737A JP62023583A JP2358387A JPS63192737A JP S63192737 A JPS63192737 A JP S63192737A JP 62023583 A JP62023583 A JP 62023583A JP 2358387 A JP2358387 A JP 2358387A JP S63192737 A JPS63192737 A JP S63192737A
Authority
JP
Japan
Prior art keywords
ethyl ketone
methyl ethyl
mek
water
caustic soda
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
JP62023583A
Other languages
Japanese (ja)
Inventor
Ichiro Watanabe
一郎 渡辺
Shigekazu Hatano
茂和 畑野
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.)
Mitsubishi Heavy Industries Ltd
Original Assignee
Mitsubishi Heavy Industries Ltd
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 Mitsubishi Heavy Industries Ltd filed Critical Mitsubishi Heavy Industries Ltd
Priority to JP62023583A priority Critical patent/JPS63192737A/en
Publication of JPS63192737A publication Critical patent/JPS63192737A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To efficiently purify methyl ethyl ketone, by using caustic soda for extracting and separating water in an zeotropic liquid and a solution of caustic soda containing extracted water for decomposing and removing impurities in purifying and recovering the titled compound in an active carbon adsorption type solvent recovery apparatus. CONSTITUTION:Air containing methyl ethyl ketone (MEK) is fed into an adsorption vessel 2-1 or 2-2 to adsorb the MEK on active carbon 3-1 or 3-2. The MEK adsorbed on the active carbon is desorbed with steam and fed with steam to a flash tank 4. In the tank 4, an aqueous solution of caustic soda from a separator 11 and MEK vapor are subjected to gas-liquid contact to decompose and remove impurities. Vapor from the tank 4 is cooled and condensed in a condenser 5 and separated by specific gravity in a separator 6. The MEK is fed to a distillation column 9 to take out moisture in the MEK together with MEK of azeotropic composition from the column top. The moisture and MEK of azeotropic composition are cooled and condensed in a reflux condenser 10, fed to the separator 11 to extract water with the caustic soda solution and the dehydrated MEK is refluxed to the distillation column 9.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明はメチルエチルケトン含有空気中から活性炭吸着
式溶剤回収装置によりメチルエチルケトンを精製回収す
る方法に関する。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for purifying and recovering methyl ethyl ketone from air containing methyl ethyl ketone using an activated carbon adsorption type solvent recovery device.

〔従来の技術] 活性炭吸着式溶剤回収装置における従来のメチルエチル
ケトン(以下、MKKと記す)精製回収方法上第2図に
よって説明する。
[Prior Art] A conventional method for purifying and recovering methyl ethyl ketone (hereinafter referred to as MKK) using an activated carbon adsorption type solvent recovery device will be explained with reference to FIG.

MKK含有空気(以下、鳳ガスと言う)はガスブロア1
により吸着槽2−1又は2−2に送られ原ガス中のMI
Kは吸着槽2−1又は2−2内の活性炭3−1又は3−
2に吸着捕集される。
MKK-containing air (hereinafter referred to as Otori gas) is supplied by gas blower 1.
MI in the raw gas is sent to adsorption tank 2-1 or 2-2 by
K is activated carbon 3-1 or 3- in adsorption tank 2-1 or 2-2
2 is adsorbed and collected.

活性炭3−1又は3−2のMIIIK吸着量が限界にな
ると原ガスを停止し吸着槽2−1又は2−2に水蒸気上
投入し、活性l1t5−1又は3−2に吸着したM I
n K を脱着させる。脱着したMIK蒸気は水蒸気と
ともに7ラツシユタンク4に流れ、ここで後記のセパレ
ータ6からの排水と気液接触し、排水中に溶解している
MIIiKt−蒸発回収させる。さらにこ\でMIX蒸
気は苛性ソーダと気液接触し、MIK中の不純物である
シア七チルを分解除去する。
When the amount of MIIIK adsorbed on the activated carbon 3-1 or 3-2 reaches its limit, the raw gas is stopped and the MIIIK adsorbed on the activated carbon 5-1 or 3-2.
Detach n K . The desorbed MIK vapor flows together with water vapor into the 7-lush tank 4, where it comes into gas-liquid contact with the waste water from the separator 6, which will be described later, and evaporates and recovers the MIIiKt dissolved in the waste water. Furthermore, the MIX vapor comes into gas-liquid contact with caustic soda to decompose and remove the impurities in MIK, i.e., cyanatyl.

ここでMIK中の不純物であるジアセチル拡Ml!IK
が活性炭3−1又嬬3−2で吸脱着する際、活性炭3−
1又は3−2の触媒作用にょ9MlICの一部が分解し
生成するものである。
Here, diacetyl expansion Ml, which is an impurity in MIK! IK
When adsorbed and desorbed by activated carbon 3-1 or 3-2, activated carbon 3-
A part of 9MlIC is decomposed and produced by the catalytic action of 1 or 3-2.

フラッシュタンク4會出7j M I K蒸気及び水蒸
気はコンデンサ5に流れ凝縮冷却される。この凝縮液は
セパレータ6に流れ、MJCKと水に比重分離する。水
は一部MBKが平衡溶解しているので、前記フラッシュ
メンク4に流しMffiKを回収する。
The flash tank 4 output 7j M I K steam and water vapor flow into the condenser 5 and are condensed and cooled. This condensed liquid flows into the separator 6 and is separated into MJCK and water by specific gravity. Since MBK is partially dissolved in the water in equilibrium, it is poured into the flashmenc 4 to recover MffiK.

Mコに%平衡溶解量の水分を含むため、そのままでは再
利用できないため、次の方法で脱水している。
Since M co contains % equilibrium dissolved amount of water, it cannot be reused as it is, so it is dehydrated using the following method.

セパレータ6から出7j M RKは、フィードポンプ
8により中間メンク7t−経由し蒸留塔9に送る。蒸留
塔?では分離器11に注入され九シクロヘキサンにより
抽出蒸留が行われ、MIK。
7j M RK output from the separator 6 is sent to the distillation column 9 via an intermediate membrane 7t- by a feed pump 8. Distillation tower? Then, it is injected into the separator 11 and subjected to extractive distillation using nine cyclohexane, resulting in MIK.

水、シクロヘキサンの3成分共沸物が蒸留塔々頂から出
てり7ラツクスコンデン?10K15tn、凝縮された
後分離器11に流れる0分組11では液々平衡によシ水
と溶剤CMMK及びシクロヘキサン)に分離する。
A three-component azeotrope of water and cyclohexane comes out from the top of the distillation column, and is it 7 lux condensate? 10K15tn is condensed and then flows into a separator 11 where it is separated into water, solvent CMMK and cyclohexane) by liquid-liquid equilibrium.

このようにシクロヘキサン金注入することによシ、蒸留
塔9及び分離器11間で共沸![及び液々平衡組成の差
にょシ水を糸外へ排出するものである。
By injecting cyclohexane gold in this way, azeotropic distillation occurs between the distillation column 9 and the separator 11! [Due to the difference in liquid-liquid equilibrium composition, water is discharged to the outside of the yarn.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

従来の方法において 1)MIKIC中の水分を除去するために注入するシク
ロへΦサンかMKKに混入し、再利用に問題を生じる場
合かある。
In the conventional method, 1) Φ-san may be mixed into MKK when injected to remove water from MIKIC, causing problems in reuse.

2〕 蒸留塔内が3成分の気液平衡になるため、運転制
御か複雑になる。
2) Since there is a vapor-liquid equilibrium of three components in the distillation column, operation control becomes complicated.

3)蒸留塔内にシクロヘキサンが多量還流するため、蒸
留塔での蒸気消費tか多くなシランユングコストが高く
つく。
3) Since a large amount of cyclohexane is refluxed into the distillation column, the steam consumption in the distillation column is large, resulting in high silane costs.

4)MIK中のジアセチル除去専用に苛性ソーダが必要
である几め、ランニングコストがかかる。
4) Caustic soda is required exclusively for removing diacetyl from MIK, which increases running costs.

5)シクロヘキサンの替わ)にトルエンを注入し水を抽
出除去する方法もあるが、MJlfKとトルエンを分離
する蒸留塔が別に必要になる。
5) There is also a method of injecting toluene into cyclohexane (instead of cyclohexane) to extract and remove water, but this requires a separate distillation column to separate MJlfK and toluene.

〔発明の目的〕[Purpose of the invention]

本発明は従来のMIKの精製回収方法における上述した
不具合を屏消しうるMJelcの精製回収方法上提供し
ようとするものである。゛〔問題点を解決する次めの手
段〕 本発明は、メチルエチルケト7を含有する空気中から活
性炭吸着式溶剤回収装置によ)メチルエチルケトンを回
収する方法において、活性炭に吸着したメチルエチルケ
トンを水蒸気等で脱着し、凝縮回収したメチルエチルケ
トンを蒸留塔に送)、メチルエチルケトン中にf!Is
している水分を共沸蒸留させ、この共沸液に苛性ソーダ
又は苛性ソーダ水g*v注入することによジメチルエチ
ルケトン中に溶解している水分を抽出分離させ、水分を
抽出されたメチルエチルケトンは蒸留塔に還流させ、一
方抽出した水分を含む苛性ソーダ溶液は前記脱着工程で
活性炭から脱着したメチルエチルケトン蒸気と気液接触
させ、メチルエチルケトン中に含まれる不純物を分解除
去することを特徴とするメチルエチルケトンの精製回収
方法である。
The present invention aims to provide a method for purifying and recovering MJelc that can eliminate the above-mentioned problems in conventional methods for purifying and recovering MIK. [Next means for solving the problem] The present invention provides a method for recovering methyl ethyl ketone from air containing methyl ethyl ketone (using an activated carbon adsorption solvent recovery device), in which methyl ethyl ketone adsorbed on activated carbon is desorbed by water vapor or the like. Then, the condensed and collected methyl ethyl ketone is sent to a distillation column), and f! Is
The water dissolved in dimethyl ethyl ketone is extracted and separated by azeotropic distillation of the water dissolved in dimethyl ethyl ketone by injecting g*v of caustic soda or caustic soda water into this azeotropic liquid, and the methyl ethyl ketone from which water has been extracted is passed through a distillation column. A method for purifying and recovering methyl ethyl ketone, characterized in that the extracted caustic soda solution containing water is brought into gas-liquid contact with the methyl ethyl ketone vapor desorbed from the activated carbon in the desorption step, and impurities contained in the methyl ethyl ketone are decomposed and removed. be.

水元明嫁、MIKを蒸留塔に送1ilK中に溶解してい
る水分全共沸蒸留させ、この共沸液(水含有MPIKλ
に笥性ソーダ水溶液t−注入するものである。これは苛
性ンーダの吸水性を利用し、MIK中に溶解している水
分を抽出分離するもので、従来のシクロヘキサノ、トル
エン等の抽出剤よシ効来が高い。
Mizumoto Akiyome sends MIK to a distillation column and azeotropically distills all the water dissolved in ilK, and this azeotropic liquid (water-containing MPIKλ
An aqueous solution of soda is injected into the tank. This extracts and separates water dissolved in MIK by utilizing the water absorbing properties of caustic powder, and is more effective than conventional extractants such as cyclohexano and toluene.

さらに、この苛性ソーダ水溶11MKK中の不純物上分
解除去するのに利用するものである。
Furthermore, it is used to decompose and remove impurities in this aqueous solution of caustic soda 11MKK.

〔実施例〕〔Example〕

本発明によるMIK、Kn製回収方法の一実施態様を第
1図によって説明する。
An embodiment of the method for recovering MIK and Kn products according to the present invention will be explained with reference to FIG.

ここでMMK含有空気(以下、原ガスと言う)はガスブ
ロア1により吸着槽2−1又は2−2に送られ鳳ガス中
のMIKは吸着槽内の活性炭3−1又は3−2に吸着捕
集される。(吸着工程) 活性炭3−1又は3−2のMIX吸着食が限界になると
原ガス七停止し、吸着槽2−1又は2−2に水蒸気を投
入し、活性炭3−1又扛5−2に吸着したMIKt−脱
着させる。(脱着工程) 脱着したMICK蒸気は水蒸気とともに7ラツシユタン
ク4に流れ、仁こで後記のセパレータ6からの排水と気
液接触し、排水中に溶解しているMIKt−蒸発回収さ
せる。さらにMIX蒸気は後記の分離器11からの苛性
ソーダ水溶液と気液接触し、MIK中の不純物であるジ
アセチルを分解除去する。フラッシュタンク4t″出f
t;−M I K蒸気及び水蒸気はコンデンサ5に流れ
凝縮冷却される。この凝縮液はセパレータ6に流れ、M
IKと水に比重分離する。水は一部MBKが平衡溶解し
ているので、前記のとお夛7ラツシユタンク4に流れM
IXを回収する。
Here, MMK-containing air (hereinafter referred to as raw gas) is sent to an adsorption tank 2-1 or 2-2 by a gas blower 1, and MIK in the Otori gas is adsorbed and captured by activated carbon 3-1 or 3-2 in the adsorption tank. collected. (Adsorption process) When the MIX adsorption of activated carbon 3-1 or 3-2 reaches its limit, the raw gas is stopped, water vapor is introduced into adsorption tank 2-1 or 2-2, and activated carbon 3-1 or 5-2 is heated. MIKt adsorbed on - is desorbed. (Desorption step) The desorbed MICK vapor flows together with water vapor into the 7-lush tank 4, where it comes into gas-liquid contact with the waste water from the separator 6, which will be described later, to evaporate and recover MIKt dissolved in the waste water. Further, the MIX vapor comes into gas-liquid contact with an aqueous solution of caustic soda from a separator 11, which will be described later, to decompose and remove diacetyl, which is an impurity in MIK. Flash tank 4t'' output f
t;-M I K vapor and water vapor flow into the condenser 5 and are condensed and cooled. This condensate flows into separator 6 and M
Gravity separation into IK and water. Since some MBK is dissolved in equilibrium in the water, it flows into the above-mentioned 7-lush tank 4.
Collect IX.

MIKも平衡溶解量の水分を含む九め、フィードポンプ
8によシ中関タンク7t−経由して蒸留塔9に送る。蒸
留塔9でMIK中の水分は共沸組成のMJ!lKととも
に蒸留塔々頂から出てリフラックスコンデンサ10に流
れ凝縮された後分離器11に流れる。ここで仁の分離器
11に供給される苛性ソーダ水浴液によ?)、mzxに
#!屏している水分が抽出し苛性ソーダ水浴液に溶解す
る。水が除去され九MIKは蒸留塔9に還流する。脱水
されたMffiKは蒸留塔々底から系外に回収される。
MIK, which also contains an equilibrium dissolved amount of water, is sent to the distillation column 9 by the feed pump 8 via the Nakaseki tank 7t. The water in MIK in distillation column 9 has an azeotropic composition of MJ! It exits from the top of the distillation column together with lK, flows to a reflux condenser 10, is condensed, and then flows to a separator 11. Here, the caustic soda water bath liquid supplied to the separator 11 is used. ), # to mzx! The trapped water is extracted and dissolved in the caustic soda water bath. Water is removed and the 9MIK is refluxed to distillation column 9. The dehydrated MffiK is recovered outside the system from the bottom of the distillation columns.

一方分離器11でMIIIK中の水を溶解した苛性ソー
ダ水溶液はフラッシュタック4に流れ、前記のとおjj
)MJC1C中のジアセチルを分解除去し排水とともに
系外に排出される。
On the other hand, the caustic soda aqueous solution in which the water in MIIIK was dissolved in the separator 11 flows to the flash tack 4 and is
) Diacetyl in MJC1C is decomposed and removed and discharged from the system along with waste water.

〔発明の効果〕〔Effect of the invention〕

1)純度の高いM8区か回収できる。(シクロヘキサン
等の抽出剤の混入がなりh) 2)ランニングコストが少なくなる。(1〜3割程度) 3)他の抽出剤(シクロヘキサン等〕に比べ運転制御か
容易。
1) Highly pure M8 can be recovered. (No contamination with extractants such as cyclohexane.) 2) Running costs are reduced. (approximately 10% to 30%) 3) Easier to control operation compared to other extractants (cyclohexane, etc.).

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

第1図は本発明のMIK精製回収方法の一実施例を説明
する九めの図、第2図は従来法によるMKIm精製回収
方法を説明するための図である。
FIG. 1 is the ninth diagram for explaining an embodiment of the MIK purification and recovery method of the present invention, and FIG. 2 is a diagram for explaining the MKIm purification and recovery method according to the conventional method.

Claims (1)

【特許請求の範囲】[Claims] メチルエチルケトンを含有する空気中から活性炭吸着式
溶剤回収装置によりメチルエチルケトンを回収する方法
において、活性炭に吸着したメチルエチルケトンを水蒸
気等で脱着し、凝縮回収したメチルエチルケトンを蒸留
塔に送りメチルエチルケトン中に溶解している水分を共
沸蒸留させ、この共沸液に苛性ソーダ又は苛性ソーダ水
溶液を注入することによりメチルエチルケトン中に溶解
している水分を抽出分解させ、水分を抽出されたメチル
エチルケトンは蒸留塔に還流させ、一方抽出した水分を
含む苛性ソーダ溶液は前記脱着工程で活性炭から脱着し
たメチルエチルケトン蒸気と気液接触させ、メチルエチ
ルケトン中に含まれる不純物を分解除去することを特徴
とするメチルエチルケトンの精製回収方法。
In a method of recovering methyl ethyl ketone from air containing methyl ethyl ketone using an activated carbon adsorption solvent recovery device, the methyl ethyl ketone adsorbed on the activated carbon is desorbed with water vapor, etc., and the collected methyl ethyl ketone is sent to a distillation column to remove the water dissolved in the methyl ethyl ketone. is subjected to azeotropic distillation, and the water dissolved in methyl ethyl ketone is extracted and decomposed by injecting caustic soda or an aqueous solution of caustic soda into this azeotropic liquid, and the methyl ethyl ketone from which water has been extracted is refluxed to a distillation column. A method for purifying and recovering methyl ethyl ketone, characterized in that the caustic soda solution containing the above is brought into gas-liquid contact with the methyl ethyl ketone vapor desorbed from activated carbon in the desorption step to decompose and remove impurities contained in the methyl ethyl ketone.
JP62023583A 1987-02-05 1987-02-05 Purification and recovery of methyl ethyl ketone Pending JPS63192737A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62023583A JPS63192737A (en) 1987-02-05 1987-02-05 Purification and recovery of methyl ethyl ketone

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62023583A JPS63192737A (en) 1987-02-05 1987-02-05 Purification and recovery of methyl ethyl ketone

Publications (1)

Publication Number Publication Date
JPS63192737A true JPS63192737A (en) 1988-08-10

Family

ID=12114597

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62023583A Pending JPS63192737A (en) 1987-02-05 1987-02-05 Purification and recovery of methyl ethyl ketone

Country Status (1)

Country Link
JP (1) JPS63192737A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102040496A (en) * 2010-12-29 2011-05-04 天津市康科德科技有限公司 Purification method of high-purity organic solvent 4-methyl-2-pentanone
CN102040497A (en) * 2010-12-29 2011-05-04 天津市康科德科技有限公司 Purification method of high-purity organic solvent butanone
JP2019030826A (en) * 2017-08-04 2019-02-28 東洋紡株式会社 Organic solvent recovery system

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102040496A (en) * 2010-12-29 2011-05-04 天津市康科德科技有限公司 Purification method of high-purity organic solvent 4-methyl-2-pentanone
CN102040497A (en) * 2010-12-29 2011-05-04 天津市康科德科技有限公司 Purification method of high-purity organic solvent butanone
JP2019030826A (en) * 2017-08-04 2019-02-28 東洋紡株式会社 Organic solvent recovery system

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