JP3563217B2 - Separation and recovery of each component from a mixed solution containing acetone and methylene chloride - Google Patents
Separation and recovery of each component from a mixed solution containing acetone and methylene chloride Download PDFInfo
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- JP3563217B2 JP3563217B2 JP32808796A JP32808796A JP3563217B2 JP 3563217 B2 JP3563217 B2 JP 3563217B2 JP 32808796 A JP32808796 A JP 32808796A JP 32808796 A JP32808796 A JP 32808796A JP 3563217 B2 JP3563217 B2 JP 3563217B2
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- Prior art keywords
- methylene chloride
- acetone
- water
- component
- mixed solution
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Description
【0001】
【発明の属する技術分野】
本発明は、アセトンと塩化メチレンを含有する混合液(以下本混合液という)より、アセトンと塩化メチレンを分離回収し、回収した溶剤を再利用するための回収方法に関するものである。
【0002】
【従来の技術及びその問題点】
数種類の溶剤を含有する混合液から、その溶剤成分を分離して回収する方法として、一般的に蒸留が用いられる。
【0003】
しかし、共沸混合物を形成する溶剤系の場合では、通常の蒸留では分離が不可能となる。アセトンと塩化メチレンの場合においては、質量比でアセトン30、塩化メチレン70、共沸点57.6℃の共沸混合物を形成するため、通常の蒸留では分離が困難で、アセトンと塩化メチレンを含有する廃溶剤をリサイクルすることなく、焼却処分されていた。然るに省資源、省コスト、環境保護の面から、これらの成分を分離回収して再利用することが着目されている。
【0004】
そこで、本発明は、本混合液に第三成分を加えて、アセトンと塩化メチレンを分離回収する方法を提供することを目的とする。
【0005】
【課題を解決するための手段】
一般的に、共沸混合物を形成する溶剤系に第三成分を加えて蒸留することにより、各成分を分離することは、古くから行われているが、共沸混合物を形成する有機溶剤同士の混合系においてはこのような例は少ない。
【0006】
本発明者らは、先に酢酸エチルとアセトニトリル、イソプロパノールとアセトニトリルに第三成分としてノルマルヘキサンを加えて蒸留することにより、各成分を分離回収できることを見出し、特許を出願した(特願平7−333118号)が、この度、アセトンと塩化メチレン混合液では、第三成分として水を用いることにより、各成分を分離回収できることを見出した。
【0007】
すなわち、本発明の特徴の一つとするところは、アセトンと塩化メチレンを含有する混合液に水を加えて蒸留することにより、アセトンと塩化メチレンを分離回収することからなる、アセトンと塩化メチレンを含有する混合液から各成分を分離回収する方法にある。
【0008】
また、本発明の特徴の他の一つとするところは、質量比でアセトン100に対し、5ないし400の塩化メチレンを含有する混合液に水を加えて蒸留することにより、アセトンと塩化メチレンを分離して回収することからなる、アセトンと塩化メチレンを含有する混合液から各成分を分離回収する方法にある。
【0009】
ここに用いる水は、通常の水道水で充分目的を達成できる。
また、質量比でアセトン100に対し、100〜300、望ましくは230前後の塩化メチレンを含有する溶剤混合液に適用すると、経済的に最も有利である。
【0010】
なお、塩化メチレンの割合が増加して、質量比がアセトン100に対し塩化メチレン400以上になると、通常の蒸留でも塩化メチレンの1部が高純度で、例えば、質量比が100:450の場合、450の塩化メチレンの内、約100が分離回収できるが、塩化メチレンが400以下の場合は分離が不可能になる。これに対し、本発明によれば、上記の質量比がいかなる場合においても高純度に分離できる。
【0011】
また、本発明は、上記通常の蒸留では分離回収できない範囲に着目して数値限定したものである。上記の質量比において、本発明においては、塩化メチレンの混合下限は特にないが、強いて言えば、実用上問題のない5〜10、好ましくは5を混合下限としてもよく、本発明では、この数値を限定したものである。
【0012】
ところで、本発明において、加える水の量は、混合液中に存在する塩化メチレンの質量100に対して、5ないし10が望ましい。この水の量が5以下になると、塩化メチレンと水の共沸混合物の生成が不十分となるため、アセトン中に塩化メチレンが残留し、アセトンの純度が低下する。
【0013】
なお、水の量が10を越えると、過剰の水がアセトン中に残留するため、アセトンの脱水の際、不利となるからである。以下に、本発明の詳細を図を用いて説明する。
【0014】
図1は本発明において用いた蒸留装置である。ただし、本発明が本装置を用いるものに限定されるものではない。
図1において、Aは1000mlの蒸留缶であって本混合液が加えられる。水は最初からAに加えておいても良く、又精留途中に精留塔上部の注入口Kから加えても良い。蒸発缶Aはマントルヒーターにより内容物が沸騰するように加熱され、内容物は蒸気となる。Bは内径10mmの精留塔であって、6mm角のマクマホン充填物が充填されている。Aで発生した蒸気は精留塔Bの効果により気液熱交換が繰り返され、共沸点の低い塩化メチレン−水共沸混合物が次第に精留塔Bを上昇し、冷却器Dにより液化し、還流比タイマーによって作動するボール弁Eが開放となる間に、枝管F、冷却管Gを経由して受器Hに貯えられる。
【0015】
その時、塩化メチレンと水の比率は、質量で95対5であり、相互の溶解性が小さいため受器H内で二層に分離する。上層は塩化メチレン数%を含有する水で、第三成分として再利用することができる。注入口Kはこの目的のため使用される。工業的に実施する場合には、この上層はデカンターで分離され、直ちに精留塔に還流され、循環使用される。下層は水約0.1%を含有する塩化メチレンで、脱水剤を用いて脱水することにより、純粋な塩化メチレンを得ることができる。
【0016】
一方、アセトンは次第に精留塔Bを下降し、受器Cに貯えられる。この時若干量の塩化メチレン及び水を伴うが、受器Cをマントルヒーターで加熱することにより、塩化メチレンは再び蒸気となって、精留塔Bに戻るため、受器C中のアセトンは工業的に再利用可能なまでに純度が高められる。ただし、アセトン中に混入する水は、用途に応じて別途蒸留して分離する必要がある。
【0017】
このようにして得られた、アセトン及び塩化メチレンの純度はガスクロマトグラフにより測定された。
ガスクロマトグラフの条件は、下記の通りであった。
【0018】
また、水分はカールフィッシャー水分測定装置(三菱化学製CA−06型)により測定された。
【0019】
【実施例】
〔実施例1〕
アセトン150g、塩化メチレン350g、水35gを蒸発缶Aに入れ、還流比5で精留を行った。受器Hに留出した液の下層部は、無水硫酸ナトリウムを用いて脱水回収した。また、受器Cに蓄えられた水を含有するアセトンを別の精留塔を用いて水分を除去した。本実施例で使用したアセトンは日本石油化学製、塩化メチレンは株式会社トクヤマ製(商品名メタクレン)、水は刈谷市の水道水であった。
【0020】
〔実施例2〕
アセトン150g、塩化メチレン350g、水25gを蒸発缶Aに入れ、実施例1と同一の方法で精留を行った。但し、受器Hに留出した液の上層部は2ml毎に注入口Kから精留塔に戻された。
【0021】
〔実施例3〕
アセトン150g、塩化メチレン350gを蒸発缶Aに入れ、水25gを注入口Kから精留塔に滴加しながら、実施例2と同一の方法で精留を行った。
【0022】
〔実施例4〕
アセトン250g、塩化メチレン250g、水25gを蒸発缶Aに入れ、実施例1と同一の方法で精留を行った。
【0023】
〔比較例5〕
アセトン150g、塩化メチレン350gを蒸発缶Aに入れ、還流比5で精留を行った。
【0024】
〔比較例6〕
アセトン250g、塩化メチレン250gを蒸発缶Aに入れ、還流比5で精留を行った。
【0025】
評価方法として、受器Cに採取され、別途精留により脱水されたアセトン及び受器Hに採取され、無水硫酸ナトリウムにより脱水された塩化メチレンの量、回収率、純度を用いた。
【0026】
実施例、比較例について、評価結果を表1にまとめた。
【0027】
【表1】
【0028】
【発明の効果】
実施例1−4で見られるとおり、本発明の分離回収方法を用いることによりアセトン、塩化メチレンを高収率且つ高純度で回収可能である。従って従来焼却処分されていた溶剤のリサイクルが可能となり、省資源、コスト、環境保護の効果が達成できる。
【図面の簡単な説明】
【図1】本発明の分離回収に用いた蒸留装置を示す図。
【符号の説明】
A…蒸発缶 B…精留塔 C…受器
D…冷却器 E…ボール弁 F…枝管
G…冷却管 H…受器[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for separating and recovering acetone and methylene chloride from a mixed solution containing acetone and methylene chloride (hereinafter referred to as the present mixed solution), and reusing the recovered solvent.
[0002]
[Prior art and its problems]
Distillation is generally used as a method for separating and recovering a solvent component from a mixed solution containing several types of solvents.
[0003]
However, in the case of a solvent system that forms an azeotrope, separation cannot be performed by ordinary distillation. In the case of acetone and methylene chloride, an azeotropic mixture having a mass ratio of acetone 30, methylene chloride 70, and an azeotropic point of 57.6 ° C. is formed, which is difficult to separate by ordinary distillation, and contains acetone and methylene chloride. Waste solvent was incinerated without recycling. However, from the viewpoint of resource saving, cost saving and environmental protection, attention has been paid to separating and recovering these components for reuse.
[0004]
Therefore, an object of the present invention is to provide a method of adding a third component to the present mixed solution to separate and recover acetone and methylene chloride.
[0005]
[Means for Solving the Problems]
In general, it has long been practiced to separate each component by adding a third component to a solvent system forming an azeotrope and distilling the same, but it has been a long time since the organic solvents forming an azeotrope are separated from each other. Such examples are rare in a mixed system.
[0006]
The present inventors have previously found that each component can be separated and recovered by adding normal hexane as a third component to ethyl acetate and acetonitrile, isopropanol and acetonitrile and distilling the same, and have applied for a patent (Japanese Patent Application No. 7-1995). No. 333118) found that each component can be separated and recovered by using water as the third component in a mixed solution of acetone and methylene chloride.
[0007]
That is, where that one of the features of the present invention, by distillation by adding water to the mixed solution containing acetone and methylene chloride, consists of separating and recovering acetone and methylene chloride, containing acetone and methylene chloride from a liquid mixture in a method of separating and recovering each component.
[0008]
Another feature of the present invention is that acetone and methylene chloride are separated by adding water to a mixture containing methylene chloride at a mass ratio of 5 to 400 and distilling water. and consists of recovered, from a mixed solution containing acetone and methylene chloride in the method of the respective components are separated and recovered.
[0009]
As the water used here, ordinary tap water can sufficiently achieve the purpose.
When applied to a solvent mixture containing methylene chloride in a mass ratio of 100 to 300, desirably around 230 with respect to acetone 100, it is most economically advantageous.
[0010]
In addition, when the ratio of methylene chloride increases and the mass ratio becomes 400 or more of methylene chloride with respect to acetone 100, even in ordinary distillation, one part of methylene chloride has high purity. For example, when the mass ratio is 100: 450, Approximately 100 of the 450 methylene chlorides can be separated and recovered, but if the methylene chloride is less than 400, separation becomes impossible. On the other hand, according to the present invention, high-purity separation can be performed regardless of the mass ratio described above.
[0011]
The present invention also Ru der those limited numerical focusing on a range that can not be separated and recovered by the above conventional distillation. In the above SL mass ratio, in the present invention, although mixed lower limit of methylene chloride is not particularly speaking by force, no practical problem 5-10, preferably may be mixed lower limit 5, in the present invention, this The numerical values are limited.
[0012]
By the way, in the present invention, the amount of water to be added is desirably 5 to 10 with respect to the mass 100 of methylene chloride present in the mixture. If the amount of water is 5 or less, the formation of an azeotrope of methylene chloride and water becomes insufficient, so that methylene chloride remains in acetone and the purity of acetone decreases.
[0013]
If the amount of water exceeds 10, excess water remains in acetone, which is disadvantageous in dehydrating acetone. Hereinafter, details of the present invention will be described with reference to the drawings.
[0014]
FIG. 1 shows a distillation apparatus used in the present invention. However, the present invention is not limited to the device using the present device.
In FIG. 1, A is a 1000 ml distillation can to which the mixed liquid is added. Water may be added to A from the beginning, or may be added from the inlet K at the top of the rectification column during rectification. The evaporator A is heated by the mantle heater so that the content boils, and the content becomes steam. B is a rectification column having an inner diameter of 10 mm, which is filled with a 6 mm square packing of McMahon. The vapor generated in A repeats gas-liquid heat exchange by the effect of the rectification column B, and the methylene chloride-water azeotropic mixture having a low azeotropic point gradually rises in the rectification column B, is liquefied by the cooler D, and refluxed. While the ball valve E operated by the ratio timer is opened, it is stored in the receiver H via the branch pipe F and the cooling pipe G.
[0015]
At that time, the ratio of methylene chloride to water is 95: 5 by mass, and the two are separated into two layers in the receiver H because of low mutual solubility. The upper layer is water containing several percent of methylene chloride and can be reused as a third component. Inlet K is used for this purpose. In the case of industrial implementation, this upper layer is separated by a decanter, immediately refluxed to a rectification column and recycled. The lower layer is methylene chloride containing about 0.1% of water, and pure methylene chloride can be obtained by dehydration using a dehydrating agent.
[0016]
On the other hand, acetone gradually goes down the rectification column B and is stored in the receiver C. At this time, a small amount of methylene chloride and water are involved, but by heating the receiver C with a mantle heater, the methylene chloride turns into vapor again and returns to the rectification column B. The purity is increased until it can be reused. However, the water mixed in the acetone needs to be separately distilled and separated according to the use.
[0017]
The purity of the acetone and methylene chloride thus obtained was measured by gas chromatography.
The conditions of the gas chromatograph were as follows.
[0018]
The moisture was measured by a Karl Fischer moisture meter (CA-06, manufactured by Mitsubishi Chemical Corporation).
[0019]
【Example】
[Example 1]
150 g of acetone, 350 g of methylene chloride, and 35 g of water were put into the evaporator A, and rectification was performed at a reflux ratio of 5. The lower layer of the liquid distilled out in the receiver H was dehydrated and recovered using anhydrous sodium sulfate. Further, water containing acetone stored in the receiver C was removed using another rectification column. Acetone used in this example was manufactured by Nippon Petrochemical, methylene chloride was manufactured by Tokuyama Co., Ltd. (trade name: Methecrene), and water was tap water from Kariya city.
[0020]
[Example 2]
150 g of acetone, 350 g of methylene chloride and 25 g of water were put into the evaporator A, and rectification was performed in the same manner as in Example 1. However, the upper layer of the liquid distilled out of the receiver H was returned from the inlet K to the rectification column every 2 ml.
[0021]
[Example 3]
150 g of acetone and 350 g of methylene chloride were placed in the evaporator A, and rectification was performed in the same manner as in Example 2 while 25 g of water was added dropwise from the inlet K to the rectification tower.
[0022]
[Example 4]
250 g of acetone, 250 g of methylene chloride and 25 g of water were put into the evaporator A, and rectification was performed in the same manner as in Example 1.
[0023]
[ Comparative Example 5]
150 g of acetone and 350 g of methylene chloride were put into the evaporator A, and rectification was performed at a reflux ratio of 5.
[0024]
[Comparative Example 6]
250 g of acetone and 250 g of methylene chloride were put into the evaporator A, and rectification was performed at a reflux ratio of 5.
[0025]
As an evaluation method, the amount, recovery rate, and purity of methylene chloride collected in the receiver C and separately dehydrated by rectification and collected in the receiver H and dehydrated with anhydrous sodium sulfate were used.
[0026]
The evaluation results of Examples and Comparative Examples are summarized in Table 1.
[0027]
[Table 1]
[0028]
【The invention's effect】
As seen in Example 1-4, acetone and methylene chloride can be recovered in high yield and high purity by using the separation and recovery method of the present invention. Therefore, it is possible to recycle the solvent which has been conventionally incinerated, thereby achieving the effect of resource saving, cost and environmental protection.
[Brief description of the drawings]
FIG. 1 is a diagram showing a distillation apparatus used for separation and recovery of the present invention.
[Explanation of symbols]
A: evaporator B: rectification column C: receiver D: cooler E: ball valve F: branch pipe G: cooling pipe H: receiver
Claims (1)
質量比でアセトン100に対し、5ないし400の塩化メチレンを含有する混合液に、かかる塩化メチレンの質量100に対して5〜10の割合の水を加えて蒸留することにより、アセトンと塩化メチレンを分離して回収することを特徴とするアセトンと塩化メチレンを含有する混合液から各成分を分離回収する方法。 By distillation by adding water to the mixed solution containing acetone and methylene chloride, in the way you separate and recover acetone and methylene chloride,
To a mixture containing methylene chloride in a mass ratio of 5 to 400 with respect to acetone 100, water is added in a ratio of 5 to 10 with respect to the mass of methylene chloride 100, and the mixture is distilled to obtain acetone and methylene chloride. A method for separating and recovering each component from a mixed solution containing acetone and methylene chloride, which is separated and recovered.
Priority Applications (1)
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JP32808796A JP3563217B2 (en) | 1996-12-09 | 1996-12-09 | Separation and recovery of each component from a mixed solution containing acetone and methylene chloride |
Applications Claiming Priority (1)
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---|---|---|---|
JP32808796A JP3563217B2 (en) | 1996-12-09 | 1996-12-09 | Separation and recovery of each component from a mixed solution containing acetone and methylene chloride |
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JPH10167998A JPH10167998A (en) | 1998-06-23 |
JP3563217B2 true JP3563217B2 (en) | 2004-09-08 |
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Cited By (1)
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KR100879635B1 (en) | 2007-08-27 | 2009-01-21 | 한국화학연구원 | New method for the separation of acetone from waste |
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CN115304451A (en) * | 2022-07-13 | 2022-11-08 | 广药白云山化学制药(珠海)有限公司 | Method for recovering mother liquor of cefathiamidine crude product |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100879635B1 (en) | 2007-08-27 | 2009-01-21 | 한국화학연구원 | New method for the separation of acetone from waste |
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