JPH1025272A - Purification of acetonitrile - Google Patents
Purification of acetonitrileInfo
- Publication number
- JPH1025272A JPH1025272A JP17911096A JP17911096A JPH1025272A JP H1025272 A JPH1025272 A JP H1025272A JP 17911096 A JP17911096 A JP 17911096A JP 17911096 A JP17911096 A JP 17911096A JP H1025272 A JPH1025272 A JP H1025272A
- Authority
- JP
- Japan
- Prior art keywords
- acetonitrile
- oxazole
- water
- evaporator
- rectification
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、粗製アセトニトリ
ル中に含まれるオキサゾールを除去して、精製アセトニ
トリルを連続的に得る方法に関するものである。TECHNICAL FIELD The present invention relates to a method for continuously obtaining purified acetonitrile by removing oxazole contained in crude acetonitrile.
【０００２】[0002]
【従来の技術】プロピレン又はイソブチレンと酸素とア
ンモニアの気相接触反応によりアクリロニトリル又はメ
タクリロニトリルを製造する方法が知られている。この
方法において得られる反応生成物中にはアクリロニトリ
ル又はメタクリロニトリルの他に、副生したアセトニト
リル及び少量のオキサゾールが含まれている。このよう
なアクリロニトリルからアセトニトリルやオキサゾール
を分離するには、通常水による抽出精留が行われ、この
際副生物として、アセトニトリルとオキサゾールを含む
水溶液が得られる。この副生アセトニトリルを工業原料
として使用するためには、その中のオキサゾールを除去
しなければならないが、オキサゾールの沸点がアセトニ
トリルに近接しているため精留によってこれを完全に除
去することは非常に困難である。2. Description of the Related Art A method for producing acrylonitrile or methacrylonitrile by a gas-phase catalytic reaction between propylene or isobutylene, oxygen and ammonia is known. The reaction product obtained by this method contains acetonitrile by-produced and a small amount of oxazole in addition to acrylonitrile or methacrylonitrile. In order to separate acetonitrile and oxazole from such acrylonitrile, extraction and rectification with water is usually performed. At this time, an aqueous solution containing acetonitrile and oxazole is obtained as a by-product. In order to use this by-product acetonitrile as an industrial raw material, it is necessary to remove oxazole therein, but since the boiling point of oxazole is close to acetonitrile, it is very difficult to completely remove it by rectification. Have difficulty.
【０００３】従来、この副生アセトニトリル中のオキサ
ゾールを除去する方法としては、特定の無機塩を加えて
オキサゾール無機塩錯化合物を形成させ沈殿除去する方
法（英国特許第１、１５６、７１３号明細書）が知られ
ている。この方法は特殊な薬品を使用しなければなら
ず、また生成した沈殿の分離操作が厄介であるなどの欠
点がある。Conventionally, as a method for removing oxazole in a by-product acetonitrile, there is known a method of adding a specific inorganic salt to form an oxazole inorganic salt complex compound and removing it by precipitation (UK Patent No. 1,156,713). )It has been known. This method has drawbacks in that a special chemical must be used and the operation of separating the formed precipitate is troublesome.
【０００４】他方において、水、シアン化水素、アクリ
ロニトリル、アセトン及び高沸点ニトリルなどの不純物
を含む粗製アセトニトリルにベンゼンを加えて精留する
ことにより精製する方法（特公昭４５−３６４９０号公
報）も知られている。この方法は系外への逸散によるベ
ンゼンの消費、脱シアン化水素のため水酸化アルカリや
硫酸第一鉄などの薬品を使用する必要があり、使用した
薬品の分離工程が複雑であることなどの理由により、工
業的方法として充分満足できるものとは言えない。更
に、薬品の添加なしに粗製アセトニトリルを水０．５〜
５重量％の存在下精留塔で抽出精留することによりオキ
サゾールを他の低沸不純分と共に分離除去する方法（特
開昭５５−１４３９５０号公報）が知られている。[0004] On the other hand, a method of purifying crude acetonitrile containing impurities such as water, hydrogen cyanide, acrylonitrile, acetone and high-boiling nitrile by adding benzene thereto and rectifying the same (Japanese Patent Publication No. 45-36490) is also known. I have. This method consumes benzene due to escape from the system and requires the use of chemicals such as alkali hydroxide and ferrous sulfate for hydrogen cyanide, which makes the separation process of the used chemicals complicated. Therefore, it cannot be said that the method is sufficiently satisfactory as an industrial method. Further, the crude acetonitrile was added to water 0.5 to
A method is known in which oxazole is separated and removed together with other low-boiling impurities by extraction and rectification in a rectification column in the presence of 5% by weight (JP-A-55-143950).
【０００５】しかしながら、特開昭５５−１４３９５０
号公報に示される方法は、精留塔で粗製アセトニトリル
を水により抽出精留してオキサゾールを分離除去する際
に、酢酸塩およびアクリル酸塩などの沈殿物が生成し精
留塔の多孔板および塔底リボイラーを閉塞させる問題が
あった。その結果、精留塔を一旦停止して水洗浄する必
要があり、連続的に精留できないので、工業的に有利な
方法では無かった。However, Japanese Patent Application Laid-Open No. 55-143950
The method disclosed in the publication, when separating and removing oxazole by extracting and rectifying crude acetonitrile with water in a rectification tower, precipitates such as acetates and acrylates are generated, and a perforated plate of the rectification tower and There was a problem of blocking the bottom reboiler. As a result, it is necessary to temporarily stop the rectification column and wash it with water, so that rectification cannot be performed continuously, and this is not an industrially advantageous method.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、オキサゾー
ル、水、酢酸塩およびアクリル酸塩を含有する粗製アセ
トニトリルからのアセトニトリルの精製方法において、
精留塔を一旦停止して、生成した沈殿の分離操作をする
ことなく、連続的に精留できるアセトニトリルの精製方
法を提供するものである。The present invention relates to a process for purifying acetonitrile from crude acetonitrile containing oxazole, water, acetate and acrylate.
An object of the present invention is to provide a method for purifying acetonitrile that can be continuously rectified without temporarily stopping a rectification column and performing an operation of separating a generated precipitate.
【０００７】[0007]
【課題を解決するための手段】本発明は、オキサゾー
ル、水、酢酸塩およびアクリル酸塩を含有する粗製アセ
トニトリルをあらかじめ蒸発缶に供給し、該粗製アセト
ニトリル中を濃縮し、残存するアセトニトリルと共に酢
酸塩およびアクリル酸塩を蒸発装置の下部より除去し、
一方該蒸発缶上部よりオキサゾール、水を含有する１次
精製アセトニトリルを精留塔へ供給し連続精留を行い、
塔頂よりオキサゾールを水及び少量のアセトニトリルと
共に共沸混合物として濃縮分離し、塔下部より精製アセ
トニトリルを回収することを特徴とするアセトニトリル
の精製方法である。According to the present invention, a crude acetonitrile containing oxazole, water, acetate and acrylate is supplied to an evaporator in advance, the crude acetonitrile is concentrated, and the acetate is removed together with the remaining acetonitrile. And acrylate are removed from the lower part of the evaporator,
Meanwhile, oxazole and primary purified acetonitrile containing water are supplied to the rectification column from the upper part of the evaporator to perform continuous rectification,
A method for purifying acetonitrile, comprising concentrating and separating oxazole together with water and a small amount of acetonitrile as an azeotrope from the top of the tower, and recovering purified acetonitrile from the bottom of the tower.
【０００８】本発明の方法により、オキサゾールを他の
低沸不純分と共に非常に効率的に分離除去でき、精留塔
内に沈殿物を生成させること無く長期に渡ってアセトニ
トリルを連続的に精製することができる。含有する水の
量がアセトニトリル及びオキサゾールをそれぞれ水との
共沸組成にするに充分な量であることが好ましい。According to the method of the present invention, oxazole can be separated and removed very efficiently together with other low-boiling impurities, and acetonitrile can be continuously purified over a long period of time without forming a precipitate in a rectification column. be able to. It is preferable that the amount of water contained is sufficient to make each of acetonitrile and oxazole have an azeotropic composition with water.
【０００９】以下、本発明を詳細に説明する。通常アン
モキシデーション工程から副生される粗製アセトニトリ
ルは濃度５〜３０重量％であり、不純物として水４５〜
９５重量％、シアン化水素０．５〜５重量％、オキサゾ
ール０．５〜１０重量％、アクリロニトリル０．０１〜
０．５重量％、及び１〜２重量％のプロピオニトリル等
を含んでいる。粗製アセトニトリル精製においては、通
常先ずアルカリ処理によりシアン化水素および水分を除
去して、アセトニトリルの濃縮が行われる。濃縮後のア
セトニトリル中の水分は５〜２０重量％である。ここで
アルカリは一般式ＭＯＨで表され、Ｍはアルカリ金属、
すなわち、リチウム、ナトリウム、カリウム、ルビジウ
ム、セシウム、フランシウムおよびアンモニウム基であ
る。この際、アセトニトリルの加水分解により酢酸塩が
生成し、またアクリロニトリルの加水分解よりアクリル
酸塩が生成する。これら酢酸塩及びアクリル酸塩は水溶
性であるが、アセトニトリルに溶解しない。次に、粗製
アセトニトリル中のオキサゾールを分離除去するため
に、精留塔でアセトニトリルを水により抽出精留が行わ
れる。この際、粗製アセトニトリルの水分は塔頂よりオ
キサゾール及び少量のアセトニトリルと共に混合物とし
て濃縮分離されることにより、水分中に溶解していた酢
酸塩及びアクリル酸塩はアセトニトリル中に析出し、沈
殿物として精留塔の多孔板及び塔底リボイラーを閉塞さ
せる問題が生じる。Hereinafter, the present invention will be described in detail. Usually, crude acetonitrile by-produced from the ammoxidation process has a concentration of 5 to 30% by weight, and water 45 to
95% by weight, hydrogen cyanide 0.5-5% by weight, oxazole 0.5-10% by weight, acrylonitrile 0.01-
0.5% by weight and 1-2% by weight of propionitrile and the like. In the purification of crude acetonitrile, hydrogen cyanide and moisture are firstly removed by alkali treatment, and then acetonitrile is concentrated. The water content in the acetonitrile after concentration is 5 to 20% by weight. Here, the alkali is represented by the general formula MOH, M is an alkali metal,
That is, lithium, sodium, potassium, rubidium, cesium, francium and ammonium groups. At this time, acetate is generated by hydrolysis of acetonitrile, and acrylate is generated by hydrolysis of acrylonitrile. These acetates and acrylates are water soluble, but do not dissolve in acetonitrile. Next, in order to separate and remove oxazole in the crude acetonitrile, acetonitrile is extracted and rectified with water in a rectification column. At this time, the water content of the crude acetonitrile is concentrated and separated as a mixture with oxazole and a small amount of acetonitrile from the top of the column, so that the acetate and acrylate dissolved in the water precipitate in the acetonitrile and are purified as a precipitate. There is a problem that the perforated plate and the bottom reboiler of the distillation tower are closed.
【００１０】本発明においては、粗製アセトニトリルを
水の存在下に抽出精留する前にあらかじめ粗製アセトニ
トリル中の酢酸塩及びアクリル酸塩を蒸発装置により濃
縮した少量のアセトニトリルと共に分離除去した後、粗
製アセトニトリル中のオキサゾールを水による抽出精留
により分離除去する。本発明の蒸発缶は、通常用いられ
ているものが使用される。蒸発条件としては、蒸発缶内
温度の範囲は１ａｔｍにおけるアセトニトリルの沸点以
上〜酢酸の沸点以下、すなわち８１〜１１８℃、蒸発缶
圧力は温度に対応するアセトニトリルの蒸気圧、すなわ
ち１．０〜２．８ｋｇ／ｃｍ2Ｇの範囲で選択される。In the present invention, before the crude acetonitrile is extracted and rectified in the presence of water, acetate and acrylate in the crude acetonitrile are separated and removed together with a small amount of acetonitrile concentrated by an evaporator, and then the crude acetonitrile is removed. The oxazole therein is separated and removed by extraction and rectification with water. As the evaporator of the present invention, a commonly used evaporator is used. As the evaporation conditions, the temperature in the evaporator is in the range from the boiling point of acetonitrile at 1 atm to the boiling point of acetic acid, that is, 81 to 118 ° C., and the evaporator pressure is the vapor pressure of acetonitrile corresponding to the temperature, ie, 1.0 to 2. It is selected in the range of 8 kg / cm 2 G.
【００１１】本発明においてオキサゾールの分離除去は
精留塔の中間部に粗製アセトニトリルと水を液状態或い
はガス状態で連続的に供給し、塔頂よりオキサゾールを
水５〜４０重量％及び少量のアセトニトリルと共に混合
物として濃縮分離し、塔下部よりオキサゾールを含まな
いアセトニトリルを回収する。すなわち、このような条
件下ではアセトニトリルとオキサゾールの比揮発度は非
常に大きくなり従来通常の精留法では完全に分離できな
かったアセトニトリルとオキサゾールの精留分離が可能
となるのである。精留塔への供給は精留分離のための蒸
気削減を図るためにはガス状が好ましい。水の含有量は
０．５〜５重量％が好ましいが、精留分離のための蒸気
節減及びアセトニトリルの回収率の向上を図るためには
１〜３重量％の範囲がより好ましい。In the present invention, separation and removal of oxazole are carried out by continuously supplying crude acetonitrile and water in a liquid state or a gas state to an intermediate portion of a rectification column, and converting oxazole from the top of the column with 5 to 40% by weight of water and a small amount of acetonitrile. And the mixture is concentrated and separated as a mixture, and acetonitrile containing no oxazole is recovered from the lower part of the column. That is, under such conditions, the specific volatility of acetonitrile and oxazole becomes very large, and the rectification and separation of acetonitrile and oxazole, which could not be completely separated by the conventional rectification method, becomes possible. The supply to the rectification column is preferably gaseous in order to reduce the vapor for rectification separation. The water content is preferably 0.5 to 5% by weight, but is more preferably in the range of 1 to 3% by weight in order to save steam for rectification and improve the recovery of acetonitrile.
【００１２】本発明で用いる精留塔としては、通常２０
〜６０段の多孔板式精留塔が用いられる。精留条件とし
ては、塔底圧力０．２〜０．３ｋｇ／ｃｍ2Ｇ、塔底温
度８０〜９５℃、塔頂圧力０．０１〜０．１５ｋｇ／ｃ
ｍ2Ｇ、塔頂温度７０〜８５℃の範囲で選択される。塔
頂より連続的に留分を排出させ、最下段より１／２〜３
／４、好ましくは２／３の段の位置に原料を供給し、か
つ塔底部よりアセトニトリルを抜き出しながら精留を継
続すれば、低沸不純分は塔頂部から蒸気として除かれ、
塔底部より精製アセトニトリルが９０重量％以上の高い
回収率で回収される。The rectification column used in the present invention is usually 20
A perforated plate rectification column having up to 60 stages is used. The rectification conditions include a bottom pressure of 0.2 to 0.3 kg / cm 2 G, a bottom temperature of 80 to 95 ° C., and a top pressure of 0.01 to 0.15 kg / c.
m 2 G, and the tower top temperature is selected in the range of 70 to 85 ° C. Distillate is continuously discharged from the top of the column, and 1/2 to 3 from the bottom
If the raw material is supplied to the position of 段, preferably ２, and rectification is continued while extracting acetonitrile from the bottom of the column, low-boiling impurities are removed as vapor from the top of the column,
Purified acetonitrile is recovered from the bottom of the column at a high recovery rate of 90% by weight or more.
【００１３】次に添付図面に従って、本発明方法の好適
な実施態様を説明する。図１は本発明方法の１例を示す
説明図であり、１は通常の蒸発缶で、粗製アセトニトリ
ル原料は供給口３より供給され、一次精製アセトニトリ
ルは取り出し口５より抜き出される。この蒸発缶は缶底
部の水蒸気導入口６から吹き込まれるスチームにより缶
内温度８１〜１１８℃好ましくは８１〜８７℃に保持さ
れている。高沸不純物である酢酸アルカリ塩及びアクリ
ル酸アルカリ塩は、缶底部の排出口４より連続的に排出
される。アセトニトリル及び低沸不純物は取り出し口５
より抜き出され、シーブトレーを有する通常の精留塔１
の下部より２／３の位置に設けられた供給口７より供給
され、アセトニトリルは塔底部取り出し口８より抜きだ
される。この蒸発塔は塔底部の水蒸気導入口９から吹き
込まれるスチームにより塔底温度８５〜９０℃好ましく
は８７〜８９℃、塔頂部７５〜８０℃にに保持されてい
る。低沸不純物は塔頂部の排出口１０より連続的に排出
され、還流受槽１１を経て一部は導管１２により精留塔
２内に還流され、残りは排出管１３により系外へ出され
る。Next, a preferred embodiment of the method of the present invention will be described with reference to the accompanying drawings. FIG. 1 is an explanatory view showing an example of the method of the present invention, wherein 1 is an ordinary evaporator, in which a crude acetonitrile raw material is supplied from a supply port 3 and primary purified acetonitrile is withdrawn from a discharge port 5. The temperature of the evaporator is kept at 81 to 118 ° C, preferably 81 to 87 ° C, by steam blown from a steam inlet 6 at the bottom of the can. Alkali acetate and alkali acrylate, which are high-boiling impurities, are continuously discharged from the outlet 4 at the bottom of the can. Acetonitrile and low boiling impurities are taken out from outlet 5
Ordinary rectification column 1 with a sieve tray
The acetonitrile is supplied from a supply port 7 provided at a position 2/3 below the bottom of the column, and acetonitrile is extracted from a bottom port 8. The temperature of the evaporating tower is maintained at 85 to 90 ° C., preferably 87 to 89 ° C., and at the top of the tower at 75 to 80 ° C. by steam blown from a steam inlet 9 at the bottom of the tower. The low-boiling impurities are continuously discharged from a discharge port 10 at the top of the tower, a part thereof is returned to a rectification tower 2 through a reflux receiving tank 11 by a conduit 12, and the rest is discharged out of the system by a discharge pipe 13.
【００１４】このようにして、連続的に操作することに
より、オキサゾールを除去された精製アセトニトリルが
高い回収率で取り出し口８より抜き出される。例えば、
オキサゾール含有率０．５〜１０．０重量％の粗製アセ
トニトリルを処理すれば、オキサゾール含有率がトレー
スないし３０ｗｔｐｐｍ又はそれ以下になるまで除去す
ることができる。また、アセトニトリルの回収率は８５
〜９５％と高く、この高い回収率を維持したまま水分２
０〜１００ｗｔｐｐｍの非常に乾燥したアセトニトリル
を得ることができる。By operating continuously in this way, purified acetonitrile from which oxazole has been removed is withdrawn from the outlet 8 at a high recovery rate. For example,
Treatment of crude acetonitrile with an oxazole content of 0.5-10.0% by weight can be removed until the oxazole content is traced to 30 wtppm or less. The recovery rate of acetonitrile was 85
９５95%, and while maintaining this high recovery rate, water 2
Very dry acetonitrile of 0-100 wtppm can be obtained.
【００１５】[0015]
【００１６】[0016]
【実施例１】図１に示す蒸発缶１の原料供給口３から、
水２．５重量％、アンモニア０．１重量％、オキサゾー
ル５．６重量％、アクリル酸ナトリウム１２０ｗｔｐｐ
ｍ、酢酸ナトリウム３０ｗｔｐｐｍを含む粗製アセトニ
トリルを毎時６００ｋｇの割合で供給し、スチームによ
って缶内温度８４℃に維持した。排出口４から水１０．
０重量％、アセトニトリル９０．０重量％、アクリル酸
ナトリウム０．１８重量％、酢酸ナトリウム０．０４５
重量％を含有したアセトニトリルを毎時４０ｋｇの割合
で抜き出した。取り出し口５から一次精製アセトニトリ
ルを蒸気状で取り出し、４０段の精留塔２の２７段目に
おける供給口７から供給し、スチームによって、塔底温
度８８℃、塔頂温度７６℃、還流比１３に維持した。こ
のようにして、塔頂より水１２．４重量％、オキサゾー
ル３５．３重量％、その他アセトニトリル５２．３重量
％を含む留出物を毎時１０５．０ｋｇ得た。一方、抜き
出し口８よりアセトニトリルを毎時４５５．０ｋｇで抜
き出したところ、水４０ｗｔｐｐｍ、アンモニア２０ｗ
ｔｐｐｍ、オキサゾール１０ｗｔｐｐｍを含むアセトニ
トリルが連続的に８，０００時間得られた。この場合、
アセトニトリルの回収率は８８％であった。Embodiment 1 From the raw material supply port 3 of the evaporator 1 shown in FIG.
2.5% by weight of water, 0.1% by weight of ammonia, 5.6% by weight of oxazole, 120wtpp of sodium acrylate
m, crude acetonitrile containing 30 wtppm of sodium acetate was supplied at a rate of 600 kg / hour, and the temperature in the vessel was maintained at 84 ° C. by steam. 10. Water from outlet 4
0% by weight, acetonitrile 90.0% by weight, sodium acrylate 0.18% by weight, sodium acetate 0.045%
Acetonitrile containing weight percent was withdrawn at a rate of 40 kg per hour. The primary purified acetonitrile is taken out from the outlet 5 in the form of vapor, supplied from the supply port 7 at the 27th stage of the 40-stage rectification column 2, and the bottom temperature is 88 ° C., the top temperature is 76 ° C., and the reflux ratio is 13 by steam. Maintained. In this way, 105.0 kg / h of a distillate containing 12.4% by weight of water, 35.3% by weight of oxazole, and 52.3% by weight of acetonitrile were obtained from the top of the column. On the other hand, when acetonitrile was withdrawn at 455.0 kg / h from the outlet 8, water 40wtppm, ammonia 20w
Acetonitrile containing tppm and 10 wtppm of oxazole was continuously obtained for 8,000 hours. in this case,
The recovery of acetonitrile was 88%.
【００１７】[0017]
【発明の効果】本発明のアセトニトリル精製法によれ
ば、粗製アセトニトリル中に含まれるオキサゾールに水
を添加して分離除去する際、精留塔を一旦停止して、生
成した沈殿物の分離操作をすることなく連続的にアセト
ニトリルを精製できる。According to the acetonitrile purification method of the present invention, when water is added to oxazole contained in crude acetonitrile for separation and removal, the rectification column is temporarily stopped, and the operation of separating the formed precipitate is performed. The acetonitrile can be continuously purified without performing the step.
【図面の簡単な説明】 図１は本発明方法を実施するための装置の１例を示す説
明図である。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is an explanatory view showing one example of an apparatus for carrying out the method of the present invention.
【図１】FIG.
１、蒸発缶 ２、精留塔 ３、供給口 ４、排出口 ５、取り出し口 ６、水蒸気導入口 ７、供給口 ８、取り出し口 ９、水蒸気導入口 １０、排出口 １１、還流受槽 １２、導管 １３、排出管 1, evaporator 2, rectification tower 3, supply port 4, discharge port 5, take-out port 6, steam inlet port 7, supply port 8, take-out port 9, steam inlet port 10, discharge port 11, reflux receiving tank 12, conduit 13. Discharge pipe
Claims (4)
ル酸塩を含有する粗製アセトニトリルをあらかじめ蒸発
缶に供給し、該粗製アセトニトリルを濃縮し、残存する
アセトニトリルと共に酢酸塩およびアクリル酸塩を蒸発
装置の下部より除去し、一方該蒸発缶上部よりオキサゾ
ール、水を含有する１次精製アセトニトリルを精留塔へ
供給し連続精留を行い、塔頂よりオキサゾールを水及び
少量のアセトニトリルと共に共沸混合物として濃縮分離
し、塔下部より精製アセトニトリルを回収することを特
徴とするアセトニトリルの精製法。1. A crude acetonitrile containing oxazole, water, acetate and acrylate is supplied to an evaporator in advance, the crude acetonitrile is concentrated, and the acetate and acrylate together with the remaining acetonitrile are removed from the lower part of the evaporator. The primary purified acetonitrile containing oxazole and water was supplied from the upper part of the evaporator to the rectification column for continuous rectification, and the oxazole was concentrated and separated as an azeotrope with water and a small amount of acetonitrile from the top of the column. And recovering purified acetonitrile from the bottom of the column.
キサゾールをそれぞれ水との共沸組成にするに充分な量
であることを特徴とする請求項１記載のアセトニトリル
の精製法。2. The method for purifying acetonitrile according to claim 1, wherein the amount of water contained is sufficient to make each of acetonitrile and oxazole have an azeotropic composition with water.
８ｋｇ／ｃｍ2Ｇ、温度８１〜１１８℃の範囲であるこ
とを特徴とする請求項１記載のアセトニトリルの精製
法。3. The condition of the evaporator under a pressure of 1.0 to 2.0.
The method for purifying acetonitrile according to claim 1, wherein the temperature is 8 kg / cm 2 G and the temperature is 81 to 118 ° C.
給がガス状であることを特徴とする請求項１記載のアセ
トニトリルの精製法。4. The method for purifying acetonitrile according to claim 1, wherein the supply of the primary purified acetonitrile to the rectification column is gaseous.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17911096A JP3907749B2 (en) | 1996-07-09 | 1996-07-09 | Purification method of acetonitrile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17911096A JP3907749B2 (en) | 1996-07-09 | 1996-07-09 | Purification method of acetonitrile |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1025272A true JPH1025272A (en) | 1998-01-27 |
| JP3907749B2 JP3907749B2 (en) | 2007-04-18 |
Family
ID=16060197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17911096A Expired - Lifetime JP3907749B2 (en) | 1996-07-09 | 1996-07-09 | Purification method of acetonitrile |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3907749B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020121969A (en) * | 2019-01-29 | 2020-08-13 | 旭化成株式会社 | Method for purifying (meth)acrylonitrile and method for manufacturing (meth)acrylonitrile |
| CN114213282A (en) * | 2021-12-21 | 2022-03-22 | 山东博苑医药化学股份有限公司 | Acetonitrile recovery method containing acid acetonitrile waste solvent |
| CN114671476A (en) * | 2022-05-06 | 2022-06-28 | 江苏盈天化学有限公司 | Device and method for continuously recovering high-purity acetonitrile from waste liquid |
| CN115180756A (en) * | 2022-06-10 | 2022-10-14 | 武汉北湖云峰环保科技有限公司 | Acetonitrile waste liquid purification and recovery device and method |
-
1996
- 1996-07-09 JP JP17911096A patent/JP3907749B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020121969A (en) * | 2019-01-29 | 2020-08-13 | 旭化成株式会社 | Method for purifying (meth)acrylonitrile and method for manufacturing (meth)acrylonitrile |
| CN114213282A (en) * | 2021-12-21 | 2022-03-22 | 山东博苑医药化学股份有限公司 | Acetonitrile recovery method containing acid acetonitrile waste solvent |
| CN114671476A (en) * | 2022-05-06 | 2022-06-28 | 江苏盈天化学有限公司 | Device and method for continuously recovering high-purity acetonitrile from waste liquid |
| CN115180756A (en) * | 2022-06-10 | 2022-10-14 | 武汉北湖云峰环保科技有限公司 | Acetonitrile waste liquid purification and recovery device and method |
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| Publication number | Publication date |
|---|---|
| JP3907749B2 (en) | 2007-04-18 |
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