JP3232678B2 - Acetic acid recovery method - Google Patents
Acetic acid recovery methodInfo
- Publication number
- JP3232678B2 JP3232678B2 JP21902392A JP21902392A JP3232678B2 JP 3232678 B2 JP3232678 B2 JP 3232678B2 JP 21902392 A JP21902392 A JP 21902392A JP 21902392 A JP21902392 A JP 21902392A JP 3232678 B2 JP3232678 B2 JP 3232678B2
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- JP
- Japan
- Prior art keywords
- acetic acid
- solvent
- acrylic acid
- distillation column
- water
- 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.)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、プロピレン及び／又は
アクロレインを分子状酸素で接触酸化してアクリル酸を
製造する際に、副生する酢酸を純度良く回収する方法に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for recovering acetic acid by-produced at a high purity when acrylic acid is produced by catalytically oxidizing propylene and / or acrolein with molecular oxygen.
【０００２】[0002]
【従来の技術】プロピレンおよび／またはアクロレイン
を水蒸気の存在下に固体触媒を用いて分子状酸素にて気
相接触酸化することによって得られる反応生成ガスは、
通常、冷却、洗浄されて水溶液として回収される。通
常、この水溶液から溶媒を用いて抽出するか、共沸脱水
することにより水を分離し、得られる粗アクリル酸溶液
を蒸留してアクリル酸を分離、回収している。2. Description of the Related Art A reaction product gas obtained by subjecting propylene and / or acrolein to gas-phase catalytic oxidation with molecular oxygen using a solid catalyst in the presence of steam is as follows:
Usually, it is cooled, washed and recovered as an aqueous solution. Usually, water is separated from the aqueous solution by extraction with a solvent or by azeotropic dehydration, and the resulting crude acrylic acid solution is distilled to separate and recover acrylic acid.
【０００３】反応によってアクリル酸のほかに、アクロ
レイン、酢酸、その他のアルデヒド類等が生成し、これ
らが粗アクリル酸水溶液に含まれる。このうち、アクロ
レインはアクリル酸と沸点差が大きいために簡単に分離
できる。また、その他のアルデヒド類は生成量が極めて
少なく、実用上の問題となることはほとんどない。しか
しながら、酢酸はアクリル酸に対して、酸化触媒や反応
条件によって異なるが、通常、１〜１５ｗｔ％程度副生
し、これを分離、除去することは有効成分の回収および
廃棄物負荷の低減の観点から重要である。[0003] In addition to acrylic acid, acrolein, acetic acid, other aldehydes and the like are produced by the reaction, and these are contained in the crude acrylic acid aqueous solution. Of these, acrolein can be easily separated because of its large boiling point difference from acrylic acid. In addition, the amount of other aldehydes produced is extremely small and hardly causes a practical problem. However, although acetic acid differs from acrylic acid depending on the oxidation catalyst and reaction conditions, it usually produces about 1 to 15 wt% as a by-product. Separation and removal of acetic acid from the viewpoint of recovery of active ingredients and reduction of waste load. Important from.
【０００４】アクリル酸と酢酸を分離する方法として、
蒸留で直接分離する方法（特公昭４９−２４８９８
号）、アクリル酸を安定化させる効果があるといわれる
トルエン、エチルベンゼン、キシレンなどの共沸溶媒を
使用して共沸蒸留する方法（特開昭４９−７２１６号、
特公昭６３−１０６９１号、特開平３−１８１４４０
号、特公昭４１−１１２４７号）が知られている。[0004] As a method for separating acrylic acid and acetic acid,
Direct separation by distillation (JP-B-49-24898)
Azeotropic distillation using an azeotropic solvent such as toluene, ethylbenzene or xylene, which is said to have an effect of stabilizing acrylic acid (JP-A-49-7216,
JP-B-63-10691, JP-A-3-181440
No. JP-B-41-11247) is known.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、蒸留で
直接分離する方法は、アクリル酸と酢酸の沸点差が小さ
いことから、蒸留塔の還流比や段数を大幅に増加させな
ければばらず、更に酢酸分離塔においてアクリル酸の重
合物が蒸留塔内で生成しやすいという問題を有してい
る。従来の共沸蒸留する方法は、酢酸をアクリル酸から
分離することはできるが、酢酸を排水中に捨てることに
なり、排水負荷が大きくなり、また、方法によっては回
収酢酸中にアクリル酸が混入し、純度が低下すると同時
に、アクリル酸がロスしてしまい好ましい方法とは言い
難い。However, in the direct separation method by distillation, since the boiling point difference between acrylic acid and acetic acid is small, the reflux ratio and the number of stages in the distillation column must be greatly increased. There is a problem that a polymer of acrylic acid is easily formed in the distillation column in the separation column. With the conventional azeotropic distillation method, acetic acid can be separated from acrylic acid, but acetic acid is discarded in the wastewater, which increases the drainage load, and depending on the method, acrylic acid is mixed in the recovered acetic acid. However, at the same time as the purity is reduced, acrylic acid is lost, which is not a preferable method.
【０００６】本発明者はかかる問題のない粗アクリル酸
溶液からアクリル酸と酢酸を分離し、精製酢酸を回収す
ることを目的として鋭意検討した結果、粗アクリル酸水
溶液から溶媒を用いて抽出して得られる粗アクリル酸溶
液について、共沸溶媒を用いて第一の蒸留塔で酢酸を留
出させて濃縮した後、第二の蒸留塔で塔頂に実質的にア
クリル酸を留出させずに酢酸と溶媒を留出させ、引続き
第三の蒸留塔で水と共沸させて溶媒を除去することによ
って精製酢酸を回収できることを見出し、本発明に至っ
た。The present inventors have conducted intensive studies for the purpose of separating acrylic acid and acetic acid from a crude acrylic acid solution having no such problems and recovering purified acetic acid. As a result, the crude acrylic acid aqueous solution was extracted with a solvent. About the obtained crude acrylic acid solution, after distilling acetic acid using the azeotropic solvent in the first distillation column and concentrating it, the second distillation column does not substantially distill acrylic acid at the top of the column. The inventors have found that purified acetic acid can be recovered by distilling off acetic acid and the solvent, followed by azeotropic distillation with water in a third distillation column to remove the solvent, and thus have accomplished the present invention.
【０００７】[0007]
【課題を解決するための手段】すなわち本発明は、
（１）プロピレン及び／又はアクロレインを分子状酸素
で接触酸化して生成するガスを冷却及び／又は水に吸収
して得られる粗アクリル水溶液又は該水溶液中のアルデ
ヒド類をストリッピングにより除去した水溶液から溶媒
を用いて抽出して得られる粗アクリル酸溶液及び酢酸と
水のそれぞれと共沸する溶媒を、（２）第一蒸留塔に供
給し、塔頂より供給液に含まれる実質的に全ての水及び
酢酸並びに溶媒及びアクリル酸の一部を留出させ、塔底
液はアクリル酸の回収又は精製工程に供給してアクリル
酸を回収し、（３）第一蒸留塔の留出液を第二蒸留塔に
供給し、塔頂より実質的にアクリル酸を含まない酢酸、
溶媒及び水を留出させ、塔底より残存する酢酸、アクリ
ル酸及び溶媒を取り出して前記第一蒸留塔に循環し、
（４）第二蒸留塔の留出液を第三蒸留塔に供給し、溶媒
を共沸して留去するのに過不足の水を塔頂より加減して
溶媒を留去し、塔底より精製酢酸を取り出すことを特徴
とする酢酸の回収方法である。That is, the present invention provides:
(1) From a crude acrylic aqueous solution obtained by cooling and / or absorbing gas produced by catalytic oxidation of propylene and / or acrolein with molecular oxygen and / or water, or from an aqueous solution from which aldehydes in the aqueous solution have been removed by stripping. A crude acrylic acid solution obtained by extraction with a solvent and a solvent azeotropic with each of acetic acid and water are supplied to (2) the first distillation column, and substantially all of the solvent contained in the supply liquid is supplied from the top of the column. Water and acetic acid and a part of the solvent and acrylic acid are distilled off, and the bottom liquid is supplied to a step of recovering or purifying acrylic acid to recover acrylic acid. Acetic acid that is supplied to the double distillation column and contains substantially no acrylic acid from the top,
Distill the solvent and water, acetic acid, acrylic acid and solvent remaining from the bottom of the column are taken out and circulated to the first distillation column,
(4) The distillate from the second distillation column is supplied to the third distillation column, and the solvent is distilled off by adjusting the amount of excess or deficient water from the top to remove the solvent by azeotropic distillation. This is a method for recovering acetic acid, which comprises extracting more purified acetic acid.
【０００８】プロピレンまたはアクロレインを水蒸気の
存在下に固体触媒を用いて分子状酸素にて気相接触酸化
するとアクリル酸の他に、アクロレイン、酢酸やその他
のアルデヒド類が生成する。通常、反応生成ガスは冷却
及び／または水に吸収して粗アクリル酸水溶液として回
収される。この粗アクリル酸水溶液又は該水溶液中のア
ルデヒド類をストリッピングにより除去した粗アクリル
水溶液から溶媒を用いて抽出して粗アクリル酸溶液を得
る。When propylene or acrolein is oxidized in the gas phase with molecular oxygen using a solid catalyst in the presence of water vapor, acrolein, acetic acid and other aldehydes are produced in addition to acrylic acid. Usually, the reaction product gas is cooled and / or absorbed in water and recovered as a crude acrylic acid aqueous solution. The crude acrylic acid aqueous solution or the crude acrylic aqueous solution from which the aldehydes in the aqueous solution are removed by stripping is extracted with a solvent to obtain a crude acrylic acid solution.
【０００９】抽出溶媒としては、水と共沸する酢酸メチ
ル、酢酸エチル、酢酸プロピル、酢酸イソプロピル、酢
酸イソブチル等のエステル類、メチルエチルケトン、メ
チルイソブチルケトン等のケトン類、水とも酢酸とも共
沸するトルエン、エチルベンゼン、キシレン等の芳香族
炭化水素類及びこれらの混合物が用いられる。Examples of the extraction solvent include esters such as methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate and isobutyl acetate which azeotrope with water, ketones such as methyl ethyl ketone and methyl isobutyl ketone, and toluene which azeotropes with water and acetic acid. And aromatic hydrocarbons such as ethylbenzene and xylene, and mixtures thereof.
【００１０】第一蒸留塔に供給される酢酸と水のそれぞ
れと共沸する溶媒としては、ベンゼン、シクロヘキセ
ン、シクロヘキサン、トルエン、メチルシクロヘキサ
ン、ヘプタン、エチルベンゼン、キシレン、オクタン等
が挙げられる。Examples of the solvent azeotropic with each of acetic acid and water supplied to the first distillation column include benzene, cyclohexene, cyclohexane, toluene, methylcyclohexane, heptane, ethylbenzene, xylene, octane and the like.
【００１１】抽出して得られる粗アクリル酸溶液は、そ
のまま又は蒸留によって溶媒を分離した後に第一蒸留塔
に供給される。第一蒸留塔に供給される共沸溶媒と同じ
溶媒を用いて抽出した場合には粗アクリル酸溶液はその
まま第一蒸留塔に供給してもよいが、通常は溶媒を分離
して第一蒸留塔に供給される。そのまま供給した場合は
水分を含有するが、蒸留によって溶媒を分離した場合に
は、蒸留の際に大部分の水は除去されるので含まれる水
は少量である。The crude acrylic acid solution obtained by the extraction is supplied to the first distillation column as it is or after separating the solvent by distillation. When the extraction is performed using the same solvent as the azeotropic solvent supplied to the first distillation column, the crude acrylic acid solution may be directly supplied to the first distillation column, but usually, the solvent is separated and the first distillation is performed. Feed to tower. When supplied as it is, it contains water, but when the solvent is separated by distillation, most of the water is removed during distillation, so that the amount of water contained is small.
【００１２】以下、本発明の実施態様を示す図１により
説明する。粗アクリル酸溶液がライン４より第一蒸留塔
１に供給される。水と酢酸のそれぞれと共沸する溶媒が
同時に供給される。その量は粗アクリル酸溶液に含まれ
る酢酸と共沸組成量以上である。粗アクリル酸溶液に必
要量以上の共沸溶媒を含む場合は、溶媒を新たに加える
必要はない。FIG. 1 shows an embodiment of the present invention. A crude acrylic acid solution is supplied to the first distillation column 1 from a line 4. A solvent azeotroping with each of water and acetic acid is supplied simultaneously. The amount is not less than the azeotropic composition with acetic acid contained in the crude acrylic acid solution. If the crude acrylic acid solution contains more than the required amount of azeotropic solvent, it is not necessary to add a new solvent.
【００１３】第一蒸留塔１では、留出液を一部還流しな
がら蒸留し、塔頂より供給液に含まれる実質的に全ての
水及び酢酸並びに溶媒及びアクリル酸の一部を留出させ
る。必ずしも全ての酢酸を留出させなくても実施するこ
とは可能であるが、酢酸が塔底液に含まれるとロスにな
るだけでなく、アクリル酸中へ混入するようになり好ま
しくないので、通常、実質的に全量留出させる。アクリ
ル酸および溶媒からなる塔底液はライン６よりアクリル
酸の回収又は精製工程へ供給され、アクリル酸と溶媒を
分離、精製して製品アクリル酸を回収する。なお、塔底
液の一部はアクリル酸抽出工程に循環使用しても良い。In the first distillation column 1, a part of the distillate is distilled while being refluxed, and substantially all of water and acetic acid contained in the feed liquid and a part of the solvent and acrylic acid are distilled from the top of the column. . It is possible to carry out without necessarily distilling out all acetic acid, but if acetic acid is contained in the bottom liquid, it will not only be lost, but it will be mixed into acrylic acid, which is not preferable. , Substantially the entire amount is distilled. The bottom liquid composed of acrylic acid and a solvent is supplied to a process for recovering or purifying acrylic acid from a line 6, and the acrylic acid and the solvent are separated and purified to recover the product acrylic acid. A part of the bottom liquid may be recycled to the acrylic acid extraction step.
【００１４】第一蒸留塔１の留出液はライン５より第二
蒸留塔２に供給し、留出液を一部還流しながら蒸留し、
塔頂より実質的にアクリル酸を含まない酢酸、溶媒及び
水を留出させる。留出液にアクリル酸が含まれるとロス
になるだけでなく、酢酸の純度が下がり好ましくない。
これを避けるために第二蒸留塔２に供給される酢酸の一
部が塔底液に残るようにする。ライン８より残存する酢
酸、アクリル酸及び溶媒を取り出して前記第一蒸留塔に
循環する。The distillate from the first distillation column 1 is supplied to the second distillation column 2 from a line 5, and the distillate is distilled while partially refluxing.
The acetic acid, solvent and water substantially free of acrylic acid are distilled off from the top of the column. When acrylic acid is contained in the distillate, not only loss occurs, but also the purity of acetic acid decreases, which is not preferable.
In order to avoid this, a part of the acetic acid supplied to the second distillation column 2 is left in the bottom liquid. The remaining acetic acid, acrylic acid and solvent are taken out from the line 8 and circulated to the first distillation column.
【００１５】第二蒸留塔２の留出液はライン７より第三
蒸留塔３に供給し、溶媒を共沸して留去するのに不足す
る水をライン９より塔頂に供給して蒸留し、水と溶媒を
留出させ、水は還流し、溶媒は分離してライン１１より
第一蒸留塔１に循環又はアクリル酸の抽出工程に循環す
る。塔底のライン１０より精製酢酸を取り出す。酢酸の
濃度は９５％以上、更には９８％以上にすることが可能
である。溶媒を共沸分離するのに必要量以上の水分を含
む留出液が第二蒸留塔２から供給される場合には留出す
る水の一部をパージする。The distillate from the second distillation column 2 is supplied to a third distillation column 3 through a line 7, and water insufficient for azeotropically distilling off the solvent is supplied from a line 9 to the top of the column to carry out distillation. Then, water and the solvent are distilled off, the water is refluxed, the solvent is separated and circulated from the line 11 to the first distillation column 1 or to the acrylic acid extraction step. The purified acetic acid is taken out from the bottom line 10. The concentration of acetic acid can be 95% or higher, and even 98% or higher. When a distillate containing more water than necessary for azeotropically separating the solvent is supplied from the second distillation column 2, a part of the distilled water is purged.
【００１６】[0016]
【発明の効果】本発明の方法により、プロピレン及び／
又はアクロレインの酸化生成物から効率的にアクリル酸
を含有しない高純度の酢酸を回収することができる。According to the method of the present invention, propylene and / or
Alternatively, high-purity acetic acid containing no acrylic acid can be efficiently recovered from the oxidation product of acrolein.
【００１７】[0017]
【実施例】以下、本発明を実施例で詳細に説明するが、
本発明はこの実施例に限定されない。 実施例１ プロピレンを分子状酸素で接触酸化して生成するガスを
水に吸収して得られる粗アクリル水溶液中のアルデヒド
類をストリッピングにより除去した水溶液から溶媒を用
いて抽出した後に溶媒を蒸留分離して得られたアクリル
酸９２．３ｗｔ％、酢酸７．７ｗｔ％を含む粗アクリル
酸溶液を第一蒸留塔に１．７６ｋｇ／Ｈで供給し、同時
に共沸溶媒としてキシレンを３．９５ｋｇ／Ｈで供給
し、塔頂圧力４０ｍｍＨｇ、塔頂温度４０℃、還流比
０．５で蒸留を行った。 アクリル酸１９．４ｗｔ％、
酢酸６．２ｗｔ％を含むキシレン溶液を留出液として、
アクリル酸２９．５ｗｔ％、酢酸０．１ｗｔ％以下を含
むキシレン溶液を塔底液として得た。Hereinafter, the present invention will be described in detail with reference to Examples.
The present invention is not limited to this embodiment. Example 1 A crude acrylic aqueous solution obtained by absorbing a gas produced by catalytically oxidizing propylene with molecular oxygen into water is extracted with an aqueous solution obtained by stripping aldehydes from a crude acrylic aqueous solution, and then the solvent is separated by distillation. A crude acrylic acid solution containing 92.3 wt% of acrylic acid and 7.7 wt% of acetic acid obtained by the above is supplied to the first distillation column at 1.76 kg / H, and at the same time, 3.95 kg / H of xylene as an azeotropic solvent. And distillation was performed at a top pressure of 40 mmHg, a top temperature of 40 ° C., and a reflux ratio of 0.5. Acrylic acid 19.4 wt%,
A xylene solution containing 6.2% by weight of acetic acid is used as a distillate,
A xylene solution containing 29.5% by weight of acrylic acid and 0.1% by weight or less of acetic acid was obtained as a bottom liquid.
【００１８】第一蒸留塔の留出液を第二蒸留塔へ供給
し、塔頂圧力４０ｍｍＨｇ、塔頂温度４０℃、還流比
６．０で蒸留を行い、酢酸６２．０ｗｔ％、キシレン３
７．８ｗｔ％、アクリル酸３００ｐｐｍ以下の留出液を
得た。塔底からはアクリル酸２０．３ｗｔ％、酢酸２．
８ｗｔ％を含むキシレン溶液が得られ、これは第一蒸留
塔の塔頂へリサイクルした。The distillate from the first distillation column is supplied to the second distillation column, and distillation is performed at a top pressure of 40 mmHg, a top temperature of 40 ° C. and a reflux ratio of 6.0, and 62.0 wt% of acetic acid and xylene 3
A distillate of 7.8 wt% and acrylic acid of 300 ppm or less was obtained. From the bottom of the column, acrylic acid 20.3 wt% and acetic acid 2.
A xylene solution containing 8 wt% was obtained, which was recycled to the top of the first distillation column.
【００１９】第二蒸留塔の留出液を第三蒸留塔へ供給
し、共沸剤として水０．０２ｋｇ／Ｈを塔頂に供給して
塔頂圧力１００ｍｍＨｇで蒸留し、キシレンを留出回収
し、塔底から水１．８ｗｔ％を含む純度９８ｗｔ％以上
の酢酸を０．１１ｋｇ／Ｈで回収した。なお、回収酢酸
中のアクリル酸は０．１ｗｔ％以下であった。The distillate of the second distillation column is supplied to the third distillation column, 0.02 kg / H of water is supplied to the top of the column as an azeotropic agent, and distillation is performed at a top pressure of 100 mmHg to distill and recover xylene. Then, acetic acid having a purity of 98% by weight or more and containing 1.8% by weight of water was recovered from the bottom of the column at 0.11 kg / H. In addition, acrylic acid in the recovered acetic acid was 0.1% by weight or less.
【図１】本発明の実施態様を示す図である。FIG. 1 is a diagram showing an embodiment of the present invention.
１ 第一蒸留塔 ２ 第二蒸留塔 ３ 第三蒸留塔 ４ 第一蒸留塔への供給ライン ５ 第二蒸留塔への供給ライン ６ 第一蒸留塔塔底液の抜き出しライン ７ 第三蒸留塔への供給ライン ８ 第二蒸留塔塔底液の抜き出しライン ９ 水の供給ライン １０ 第三蒸留塔塔底液（精製酢酸）の抜き出しライン １１ 溶媒の取り出しライン DESCRIPTION OF SYMBOLS 1 1st distillation tower 2 2nd distillation tower 3 3rd distillation tower 4 Supply line to 1st distillation tower 5 Supply line to 2nd distillation tower 6 Extraction line of bottom liquid of 1st distillation tower 7 To 3rd distillation tower 8 Line for extracting bottom liquid of second distillation column 9 Line for supplying water 10 Line for extracting bottom liquid (purified acetic acid) of third distillation column 11 Line for extracting solvent
フロントページの続き (56)参考文献 特開 昭56−90034（ＪＰ，Ａ) 特開 平３−181440（ＪＰ，Ａ) 特公 昭41−15569（ＪＰ，Ｂ１) 特公 昭41−11247（ＪＰ，Ｂ１) 特公 昭40−10044（ＪＰ，Ｂ１) 特公 昭43−16965（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.7，ＤＢ名) C07C 51/46 C07C 53/08 C07C 57/05 Continuation of front page (56) References JP-A-56-90034 (JP, A) JP-A-3-181440 (JP, A) JP-B-41-15569 (JP, B1) JP-B-41-11247 (JP) , B1) JP 40-10044 (JP, B1) JP 43-16965 (JP, B1) (58) Fields investigated (Int. Cl. 7 , DB name) C07C 51/46 C07C 53/08 C07C 57/05
Claims (3)
ンを分子状酸素で接触酸化して生成するガスを冷却及び
／又は水に吸収して得られる粗アクリル水溶液又は該水
溶液中のアルデヒド類をストリッピングにより除去した
水溶液から溶媒を用いて抽出して得られる粗アクリル酸
溶液及び酢酸と水のそれぞれと共沸する溶媒を、（２）
第一蒸留塔に供給し、塔頂より供給液に含まれる実質的
に全ての水及び酢酸並びに溶媒及びアクリル酸の一部を
留出させ、塔底液はアクリル酸の回収又は精製工程に供
給してアクリル酸を回収し、（３）第一蒸留塔の留出液
を第二蒸留塔に供給し、塔頂より実質的にアクリル酸を
含まない酢酸、溶媒及び水を留出させ、塔底より残存す
る酢酸、アクリル酸及び溶媒を取り出して前記第一蒸留
塔に循環し、（４）第二蒸留塔の留出液を第三蒸留塔に
供給し、溶媒を共沸して留去するのに過不足の水を塔頂
より加減して溶媒を留去し、塔底より精製酢酸を取り出
すことを特徴とする酢酸の回収方法。1. A method for stripping a crude acrylic aqueous solution obtained by cooling and / or absorbing a gas generated by catalytically oxidizing propylene and / or acrolein with molecular oxygen and / or water, or an aldehyde in the aqueous solution. The crude acrylic acid solution obtained by extracting with a solvent from the aqueous solution removed by the above method and a solvent azeotropic with each of acetic acid and water,
Feed to the first distillation column, distill substantially all of the water and acetic acid contained in the feed liquid and part of the solvent and acrylic acid from the top of the column, and supply the bottom liquid to the acrylic acid recovery or purification process (3) The distillate of the first distillation column is supplied to the second distillation column, and acetic acid, a solvent and water substantially free of acrylic acid are distilled off from the top of the column. The remaining acetic acid, acrylic acid and solvent are taken out from the bottom and circulated to the first distillation column. (4) The distillate from the second distillation column is supplied to the third distillation column, and the solvent is azeotropically distilled off. A method for recovering acetic acid, comprising adjusting the amount of water in excess or deficiency from the top of the column to distill off the solvent, and removing purified acetic acid from the bottom of the column.
ンゼンである請求項１記載の酢酸の回収方法。2. The method for recovering acetic acid according to claim 1, wherein the solvent is toluene, xylene or ethylbenzene.
項１記載の酢酸の回収方法。3. The method for recovering acetic acid according to claim 1, wherein the concentration of the purified acetic acid is 95% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21902392A JP3232678B2 (en) | 1992-08-18 | 1992-08-18 | Acetic acid recovery method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21902392A JP3232678B2 (en) | 1992-08-18 | 1992-08-18 | Acetic acid recovery method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0665139A JPH0665139A (en) | 1994-03-08 |
| JP3232678B2 true JP3232678B2 (en) | 2001-11-26 |
Family
ID=16729046
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21902392A Expired - Fee Related JP3232678B2 (en) | 1992-08-18 | 1992-08-18 | Acetic acid recovery method |
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| Country | Link |
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