JP2676900B2 - Method for producing ethanol concentrate - Google Patents
Method for producing ethanol concentrateInfo
- Publication number
- JP2676900B2 JP2676900B2 JP1092978A JP9297889A JP2676900B2 JP 2676900 B2 JP2676900 B2 JP 2676900B2 JP 1092978 A JP1092978 A JP 1092978A JP 9297889 A JP9297889 A JP 9297889A JP 2676900 B2 JP2676900 B2 JP 2676900B2
- Authority
- JP
- Japan
- Prior art keywords
- ethanol
- distillation column
- pervaporation
- producing
- membrane
- 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 - Fee Related
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は比較的低濃度のエタノール水溶液からエタノ
ール優先透過型浸透気化膜を利用してエタノール濃縮液
を製造する新規な方法に関するものであり、アルコール
発酵液からのアルコールの濃縮・分離、特に連続発酵法
等のアルコール発酵液からのアルコールの濃縮・分離に
好ましく用いられる。TECHNICAL FIELD The present invention relates to a novel method for producing an ethanol concentrate from an ethanol aqueous solution having a relatively low concentration by using an ethanol preferential permeation type pervaporation membrane, It is preferably used for concentration / separation of alcohol from an alcohol fermentation broth, particularly for concentration / separation of alcohol from an alcohol fermentation broth such as a continuous fermentation method.
（従来の技術） 液体混合物の分離方法としては最もひろく実用化され
ている技術の一つは蒸留法である。また近年、逆浸透法
および浸透気化法（Pervaporation法）等の分離膜を使
用する方法が鋭意研究されている。(Prior Art) One of the most widely used techniques for separating a liquid mixture is a distillation method. In recent years, a method using a separation membrane such as a reverse osmosis method and a pervaporation method (Pervaporation method) has been intensively studied.
比較的低濃度の揮発性有機液体水溶液を濃縮する場
合、蒸留法は大量の水分を蒸発させて分離するため多大
な分離エネルギーが必要である。例えば、発酵法による
エタノールの製造では連続発酵法や固定化酵素法のよう
なバイオテクノロジーを駆使した新規な方法の発酵生産
性は著しく高い。にもかかわらず発酵液中のエタノール
濃度が従来の回分式発酵法より低濃度のため、蒸留法に
よる濃縮・分離のエネルギーが増大してむしろエタノー
ルの製造コストが不利になると云われている。また、化
学工業の製造プロセスでは、しばしば低濃度の揮発性有
機液体水溶液が生成するが、蒸留法等の従来技術で濃縮
・分離して回収するにはコストがかかりすぎて経済性が
失われるため、公害源や焼却処理等により資源の浪費の
原因となっている。In the case of concentrating a volatile organic liquid aqueous solution having a relatively low concentration, the distillation method requires a large amount of separation energy because a large amount of water is evaporated and separated. For example, in the production of ethanol by a fermentation method, the fermentation productivity of a novel method utilizing biotechnology such as a continuous fermentation method or an immobilized enzyme method is remarkably high. Nevertheless, it is said that since the concentration of ethanol in the fermentation liquid is lower than that of the conventional batch fermentation method, the energy for concentration and separation by the distillation method is increased, and the production cost of ethanol is rather disadvantageous. Also, in the manufacturing process of the chemical industry, a low concentration volatile organic liquid aqueous solution is often generated, but it is too costly and economically disadvantageous to concentrate and separate and recover it by a conventional technique such as a distillation method. However, it causes waste of resources due to pollution sources and incineration.
このため、少量成分で有用な有機液体成分を選択的に
透過させる膜分離技術が分離に要するエネルギーが原理
的に最も少なくてすむ理想的分離方法として期待されて
いる。しかし、逆浸透法は水を選択的に透過・分離する
方法であり、大量成分である水を透過させるためエネル
ギー的に有利とはいえず、また濃度の上昇に伴う浸透圧
の増大と操作圧力の限界との関係で高濃度の濃縮液を得
ることは困難である。他方、浸透気化法は特定の成分を
高い分離率で選択的に透過・捕集しうる膜分離法として
期待され精力的に研究開発の努力が注がれている。水溶
液を対象とする場合には水を優先的に透過させる浸透気
化法で分離性能の著しく高い浸透気化膜が開発され実用
化の段階に近付きつつあり、高濃度液の脱水技術として
注目されている。しかし、有機液体水溶液から有機液体
を選択的に透過させる高性能の浸透気化膜の開発は現在
まだ基礎的研究の段階にあり、本技術を直ちに実用化と
するのに十分な分離性能の高い浸透気化膜はまだ開発さ
れていない。しかし、揮発性有機液体水溶液から有機液
体を優先的に透過させる浸透気化膜としては特開昭60−
75306、61−277430、62−201605、およびEP−0254758
（A1）等に提案された分離膜が比較的高い分離性能を有
していて注目される。For this reason, a membrane separation technique for selectively permeating a useful organic liquid component with a small amount of a component is expected as an ideal separation method which requires the least energy for separation in principle. However, the reverse osmosis method is a method of selectively permeating and separating water, which is not energy-efficient because it allows water, which is a large component, to permeate.In addition, the osmotic pressure increases with increasing concentration and the operating pressure increases. It is difficult to obtain a concentrated solution having a high concentration in relation to the limits of the above. On the other hand, the pervaporation method is expected as a membrane separation method capable of selectively permeating and collecting a specific component at a high separation rate, and research and development efforts are being vigorously pursued. In the case of aqueous solutions, a pervaporation membrane with remarkably high separation performance has been developed by the pervaporation method that preferentially permeates water, and it is approaching the stage of practical use, and it is attracting attention as a dehydration technology for high concentration liquids . However, the development of a high-performance pervaporation membrane that selectively permeates an organic liquid from an organic liquid aqueous solution is still in the basic research stage, and a high-performance permeation membrane with sufficient separation performance to immediately commercialize this technology. Evaporation film has not been developed yet. However, as a pervaporation membrane that preferentially permeates an organic liquid from a volatile organic liquid aqueous solution, it is disclosed in JP-A-60-
75306, 61-277430, 62-201605, and EP-0254758
It is noteworthy that the separation membrane proposed in (A1) has relatively high separation performance.
この様な状況を背景にして、揮発性有機液体水溶液か
ら有機液体を優先的に透過させる浸透気化膜を用いた分
離方法の研究の例はまだ非常に少なく、特開昭58−5810
8、59−216605、61−56085等に提案されているような方
法および学会等で、揮発性有機液体優先透過型浸透気化
膜の使用方法あるいは揮発性有機液体優先透過型浸透気
化膜と水優先透過型浸透気化膜とを組合せて使用すると
いう基本的概念に関する基礎的定性的研究が提案されて
いるという状況であり、具体的に経済性を検討して工業
的に有利であることを確かめた例は非常に少ない。Against this background, there are still very few examples of studies on a separation method using a pervaporation membrane that preferentially permeates an organic liquid from a volatile organic liquid aqueous solution.
8, 59-216605, 61-56085, etc., and methods of using volatile organic liquid preferential permeation vaporization membrane or volatile organic liquid preferential permeation vaporization membrane and water priority at academic conferences. The situation is that a basic qualitative research on the basic concept of using in combination with a permeation type pervaporation membrane has been proposed, and it was confirmed that it was industrially advantageous by specifically examining the economic efficiency. Very few examples.
（発明が解決しようとする課題） 本発明者らはこのような事情を鑑み、現実的に入手可
能な分離性能のエタノール優先透過型膜を用いた浸透気
化法を蒸留法と組合せた、工業的規模で経済的に有利な
エタノール濃縮液の製造方法を提供しようとするもので
ある。(Problems to be Solved by the Invention) In view of such circumstances, the present inventors have proposed an industrial method in which a pervaporation method using an ethanol preferential permeation type membrane having practically available separation performance is combined with a distillation method. It is intended to provide a method for producing an ethanol concentrate which is economically advantageous on a scale.
（課題を解決するための手段） 本願発明は、15重量％以下のエタノール水溶液を原料
として、エタノール優先透過型浸透気化膜を有する浸透
気化装置を用いてエタノール濃縮液を製造するに際し、
該浸透気化膜の透過側蒸気を凝縮器で捕集した後、蒸留
塔の中段に供給して更に濃縮することを特徴とするエタ
ノール濃縮液の製造方法に関する。(Means for Solving the Problems) The present invention, when an ethanol aqueous solution of 15% by weight or less is used as a raw material, when producing an ethanol concentrate using a pervaporation apparatus having an ethanol preferential permeation type pervaporation membrane,
The present invention relates to a method for producing an ethanol concentrated solution, which comprises collecting vapor on the permeation side of the pervaporation membrane with a condenser and then supplying it to the middle stage of a distillation column for further concentration.
第１図は本願発明の低濃度揮発性有機液体水溶液の濃
縮液の製造方法の概略図である。すなわち、熱交換器１
を介して低濃度のエタノール水溶液を加温し、エタノー
ル優先透過型浸透気化膜からなる浸透気化装置２の１次
側に原料水溶液を供給する。膜の２次側は凝縮器３を介
して真空ポンプ４で所定の減圧度に保持してあり、エタ
ノールに富む透過蒸気を凝縮器で冷却・液化して捕集す
る。次いで凝縮液は熱交換器５で加温して蒸留塔６の中
段に供給する。蒸留塔の塔頂からエタノールを主とする
蒸気を抜出し浸透気化装置２の熱交換器７で低濃度のエ
タノール供給液を加熱した後、凝縮してくるエタノール
濃縮液の一部を蒸留塔に還流し、残りの部分の凝縮液を
製品のエタノール濃縮液として取り出す。８は蒸留塔の
加熱器である。エタノール優先透過型浸透気化膜からな
る浸透気化装置２の１次側からの回収液は発酵槽等の原
料供給液の補給液として再利用する。FIG. 1 is a schematic diagram of a method for producing a concentrated liquid of a low-concentration volatile organic liquid aqueous solution of the present invention. That is, the heat exchanger 1
A low-concentration aqueous ethanol solution is heated via the, and the raw material aqueous solution is supplied to the primary side of the pervaporation apparatus 2 composed of an ethanol preferential permeation type pervaporation membrane. The secondary side of the membrane is maintained at a predetermined degree of reduced pressure by a vacuum pump 4 via a condenser 3, and the permeated vapor rich in ethanol is cooled and liquefied by the condenser to be collected. Next, the condensate is heated by the heat exchanger 5 and supplied to the middle stage of the distillation column 6. After the vapor mainly consisting of ethanol is extracted from the top of the distillation column and the low-concentration ethanol feed liquid is heated by the heat exchanger 7 of the pervaporation apparatus 2, a part of the condensed ethanol concentrate is refluxed to the distillation column. Then, the remaining condensate is taken out as the ethanol concentrate of the product. Reference numeral 8 is a heater for the distillation column. The liquid recovered from the primary side of the pervaporation apparatus 2 composed of the ethanol preferential permeation type pervaporation membrane is reused as a replenisher for the raw material supply liquid such as the fermentation tank.
揮発性有機液体優先透過型浸透気化装置２に用いる膜
は、揮発性有機液体の水に対する分離係数αEtOHが５〜
100程度の膜が使用でき、特に10〜50の範囲の膜が好ま
しく使用できる。全透過速度は0.1kg m-2h-1以上である
ことが好ましい。現実的に入手できる膜としてはαEtOH
＝20〜40、透過速度＝0.3〜3kg m-2h-1の範囲の膜が特
に好ましく使用できできる。このような揮発性有機液体
優先透過型浸透気化膜の例としては、ポリ（１−トリメ
チルシリルピロピン−１）、ポリ（１−トリメチルシリ
ルピロピン−１）またはポリフェニルプロピンにジメチ
ルシロキサン鎖をグラフトさせたポリマの膜、およびフ
ルオロアルキルエステルをグラフトさせたポリスチレン
等の膜、およびこれらの複合膜がある。分離性能が上述
の様な範囲にあり図１の様なフローで濃縮液を製造する
場合には、揮発性有機液体優先透過型浸透気化装置の原
料液と透過成分の量と濃度および熱量が好ましい範囲に
バランスする条件が存在するために本願発明の方法が有
利となるのである。膜モジュールの形式は平膜のプレー
トアンドフレーム型、スパイラル巻型、中空糸型等いず
れの形式のものでも好ましく使用できる。The membrane used in the volatile organic liquid preferential permeation vaporizer 2 has a separation coefficient α EtOH of water of the volatile organic liquid of 5 to 5
A membrane of about 100 can be used, and a membrane in the range of 10 to 50 can be preferably used. The total permeation rate is preferably 0.1 kg m -2 h -1 or more. Α EtOH is a practically available film
= 20 to 40, permeation rate = 0.3 to 3 kg m -2 h -1 membranes can be used particularly preferably. Examples of such a volatile organic liquid preferential permeation type pervaporation membrane include poly (1-trimethylsilylpyropine-1), poly (1-trimethylsilylpyropine-1) or polyphenylpropyne grafted with a dimethylsiloxane chain. Polymer films, and films such as polystyrene grafted with fluoroalkyl esters, and composite films thereof. When the separation performance is in the above range and the concentrated liquid is produced by the flow as shown in FIG. 1, the amount and concentration of the raw material liquid and the permeation component and the amount of heat of the volatile organic liquid preferential permeation type vaporizer are preferable. The method of the present invention is advantageous because of the existence of the conditions that balance the ranges. The membrane module may be of any type such as a flat membrane plate-and-frame type, a spiral wound type, and a hollow fiber type.
蒸留塔の段数としては、供給液の濃度と浸透気化膜の
性能、浸透気化装置での回収率、蒸留塔の還流比、目的
とする濃度等によって変るので一概に規定することはで
きないが、エタノールを濃縮して濃縮アルコールを製造
する目的から云えば、おおよそ10段以上好ましくは20段
以上あれば十分であると考えられる。The number of stages of the distillation column varies depending on the concentration of the feed liquid and the performance of the pervaporation membrane, the recovery rate in the pervaporation device, the reflux ratio of the distillation column, the target concentration, etc. For the purpose of producing concentrated alcohol by condensing the alcohol, it is considered that about 10 stages or more, preferably 20 stages or more is sufficient.
原料液である低濃度のエタノール水溶液としては、本
発明の趣旨から云えば約15％以下のエタノール水溶液に
適用することが必要である。さらに好ましくは例えば連
続発酵法の発酵液の様に５〜10％程度のエタノール水溶
液に対して本発明を適用する場合に本発明の効果を有利
に発揮できる。連続発酵法としては、発酵液を槽から連
続的に取り出し回収液を発酵槽に補給液として還流する
方法、菌体を固定化して発酵させる方法、アルコール発
酵酵素を固定化して発酵させる方法等いずれの方法でも
よい。発酵液を槽から連続的に取り出し回収液を発酵槽
に補給液として還流する方法では、発酵液から菌体を限
外濾過法および／または沈降法等で除去して本発明を適
用するのが好ましい。As a low-concentration aqueous ethanol solution which is a raw material liquid, it is necessary to apply it to an aqueous ethanol solution of about 15% or less for the purpose of the present invention. More preferably, the effect of the present invention can be advantageously exhibited when the present invention is applied to an aqueous ethanol solution of about 5 to 10%, such as a fermentation broth of a continuous fermentation method. Examples of the continuous fermentation method include a method in which the fermented liquid is continuously taken out from the tank and the recovered liquid is refluxed as a replenisher in the fermenter, a method in which cells are immobilized and fermented, a method in which alcohol fermentation enzyme is immobilized and fermented, etc. Method is also acceptable. In the method of continuously taking out the fermented liquid from the tank and refluxing the recovered liquid to the fermenter as a replenishing liquid, the present invention is applied by removing cells from the fermented liquid by an ultrafiltration method and / or a sedimentation method or the like. preferable.
（発明の作用効果） 図１に示した各装置ユニットの操作条件は、原料供給
液の濃度、浸透気化装置２の分離性能、回収液の条件、
蒸留塔の条件等によって変るので一概に示すことはでき
ない。(Effects of the Invention) The operating conditions of each device unit shown in FIG. 1 are as follows: the concentration of the raw material supply liquid, the separation performance of the pervaporation device 2, the condition of the recovery liquid,
It cannot be categorized as it varies depending on the conditions of the distillation column.
しかし、例えばエタノール等の数％〜10数％の水溶液
を原料供給液として、αEtOH＝30、透過速度＝1.0kg m
-2h-1程度の性能の浸透気化膜を揮発性有機液体優先透
過型浸透気化装置２に使用するとすれば、供給液の温度
は35〜80℃さらに好ましくは60〜75℃の範囲がよい。該
浸透気化装置２からの回収液は、供給液と熱交換器１で
予備加温して供給する。該浸透気化装置の温度は膜モジ
ュールに組み込まれた熱交換器および／または外部循環
式熱交換器により、蒸留塔の塔頂蒸気を熱源として所定
温度に保持する。凝縮器３で冷却・捕集された浸透気化
法濃縮液は蒸留塔の塔底からの排出液を熱源として熱交
換器５で予備加熱して蒸留塔に供給する。本発明によれ
ば、浸透気化法に必要な蒸発潜熱を蒸留操作で必要とす
る蒸気の冷却操作と組合せて熱エネルギーを有効に利用
すると同時に、浸透気化操作および蒸留操作で発生する
比較的低温の熱源を有効に利用して熱エネルギーの節減
に成功している。However, for example, using an aqueous solution of several% to several tens% such as ethanol as the raw material supply liquid, α EtOH = 30, permeation rate = 1.0 kg m
If a pervaporation membrane having a performance of about -2 h -1 is used in the volatile organic liquid preferential permeation type pervaporation apparatus 2, the temperature of the supply liquid is preferably 35 to 80 ° C, more preferably 60 to 75 ° C. . The recovered liquid from the pervaporation apparatus 2 is preheated with the supply liquid and the heat exchanger 1 and supplied. The temperature of the pervaporation apparatus is maintained at a predetermined temperature by using the top vapor of the distillation column as a heat source by a heat exchanger incorporated in the membrane module and / or an external circulation heat exchanger. The permeation method concentrated liquid cooled and collected in the condenser 3 is preheated in the heat exchanger 5 using the liquid discharged from the bottom of the distillation column as a heat source and supplied to the distillation column. According to the present invention, the latent heat of vaporization necessary for the pervaporation method is combined with the vapor cooling operation required for the distillation operation to effectively utilize the heat energy, and at the same time, the relatively low temperature generated by the pervaporation operation and the distillation operation is used. We have succeeded in saving heat energy by effectively using the heat source.
またさらに、該浸透気化装置２の膜の２次側の圧力は
１次側の温度と膜の分離性能に依存するが、供給液温度
を高く設定すれば２次側圧力は100Torr前後で運転が可
能となる。この場合は、該浸透気化装置２の透過蒸気の
凝縮器の冷却を20〜30℃程度の冷水で行なうことが可能
であり、冷却装置の電力費を大幅に節減することが可能
となる。Furthermore, although the pressure on the secondary side of the membrane of the pervaporation apparatus 2 depends on the temperature on the primary side and the separation performance of the membrane, if the feed liquid temperature is set high, the secondary side pressure will operate at around 100 Torr. It will be possible. In this case, the condenser of the permeated vapor of the pervaporation apparatus 2 can be cooled with cold water at about 20 to 30 ° C., and the power cost of the cooling apparatus can be significantly reduced.
（実施例） 以下に実施例によって具体的に本願発明を説明する
が、本発明の適用範囲が本実施例によって制約されない
ことはいうまでもない。(Examples) Hereinafter, the present invention will be specifically described with reference to examples, but it goes without saying that the scope of application of the present invention is not limited by the examples.
図１に示す方法で６％のエタノール水溶液を濃縮し
た。揮発性有機液体優先透過型浸透気化装置２にはエタ
ノール濃度３〜15％の水溶液に対して60〜70℃の条件の
平均性能がαEtOH＝30、透過速度＝1.0kg m-2h-1の性能
を有するポリ（１−トリメチルシリルプロピン−１）の
平膜を、フィルタープレス型のプレートアンドフレーム
式モジュールに組み込んで使用した。A 6% aqueous ethanol solution was concentrated by the method shown in FIG. The volatile organic liquid preferential permeation type pervaporation apparatus 2 has an average performance of α EtOH = 30 and a permeation rate = 1.0 kg m -2 h -1 at an aqueous solution having an ethanol concentration of 3 to 15% under conditions of 60 to 70 ° C. A flat membrane of poly (1-trimethylsilylpropyne-1) having the following performance was used in a plate-and-frame type module of a filter press type.
３％のエタノール溶液を31.6kg h-1の速度で熱交換器
１で35℃から59℃に予備加温して、揮発性有機液体優先
透過型浸透気化装置２に供給した。熱交換器１の熱源と
しては該浸透気化装置の１次側供給液出口から70℃で2
9.9kg h-1の割合で抜出される回収液の余熱を利用し
た。排出された回収液の温度は約40℃であった。浸透気
化装置の供給液温度は外部循環式の熱交換器７を使用し
て、蒸留塔の塔頂から抜出した蒸気を熱源に使って70℃
に保持した。蒸気量は4.05kg h-1であった。A 3% ethanol solution was preheated from 35 ° C. to 59 ° C. in the heat exchanger 1 at a rate of 31.6 kg h −1 and supplied to the volatile organic liquid preferential permeation vaporizer 2. The heat source for the heat exchanger 1 is 2 at 70 ° C from the outlet of the supply liquid on the primary side of the pervaporation device.
The residual heat of the recovered liquid extracted at a rate of 9.9 kg h -1 was used. The temperature of the discharged recovery liquid was about 40 ° C. The temperature of the liquid supplied to the pervaporation apparatus is 70 ° C by using the heat exchanger 7 of the external circulation type and using the steam extracted from the top of the distillation column as the heat source.
Held. The amount of steam was 4.05 kg h -1 .
該浸透気化装置２の２次側の圧力は冷却トラップ３を
介して100Torrに真空ポンプ４で圧力調節器を使って保
持した。トラップは25℃の冷水で冷却した。トラップに
は1.70kg h-1の割合で59％のエタノールが凝縮した。ト
ラップ３に貯まる約30℃の凝縮液を定量ポンプで1.70kg
h-1の割合で抜きだし、熱交換器５で蒸留塔搭底の100
℃の排出液0.62kg h-1で予備加熱をして52℃にし、段数
20段の蒸留塔の中段に供給した。蒸留塔の加熱器からは
ゲージ圧0.8kg cm-2の水蒸気1.8kg h-1で加熱した。塔
頂蒸気の冷却・凝縮は浸透気化装置の外部循環式の熱交
換器７で行ない、1.08kg h-1を製品のエタノール濃縮液
として取り出し、297kg h-1を蒸留塔に還流量した。製
品のエタノール濃縮液の濃度は93％であった。The pressure on the secondary side of the pervaporation apparatus 2 was maintained at 100 Torr via the cooling trap 3 with a vacuum pump 4 using a pressure regulator. The trap was cooled with cold water at 25 ° C. 59% ethanol was condensed in the trap at a rate of 1.70 kg h -1 . 1.70kg of the condensate at about 30 ℃ stored in trap 3
It is withdrawn at a rate of h -1 and the heat exchanger 5 is used to remove 100
Effluent at ℃ 0.62kg h -1 to preheat to 52 ℃,
It was fed to the middle stage of a 20-stage distillation column. From the heater of the distillation column, steam was heated with a gauge pressure of 0.8 kg cm -2 and steam of 1.8 kg h -1 . Cooling and condensation of the overhead vapor is performed in the heat exchanger 7 of the external circulation type pervaporation device, taken out 1.08 kg h -1 as ethanol concentrate product was amount refluxed 297kg h -1 to a distillation column. The concentration of the ethanol concentrate of the product was 93%.
以上の結果から、エタノール1kg当りの蒸気の使用量
は1.8kg、電力の使用量は5WHと見積もられた。従来法の
蒸留の場合には蒸気3.2kgを要すると算定される。蒸気
のコストを３円/kg、電気代を0.015円/WHと仮定して見
積もると、本発明では5.48円／エタノール−kgであり、
従来の蒸留法では10.4円／エタノール−kgとなる。すな
わち、本願発明によれば分離に要するエネルギーコスト
が顕著に節減できる。From the above results, it was estimated that the amount of steam used per kg of ethanol was 1.8 kg and the amount of electric power used was 5 WH. In the case of conventional distillation, it is calculated that 3.2 kg of steam is required. Assuming that the cost of steam is 3 yen / kg and the electricity bill is 0.015 yen / WH, it is 5.48 yen / ethanol-kg in the present invention,
With the conventional distillation method, it is 10.4 yen / ethanol-kg. That is, according to the present invention, the energy cost required for separation can be significantly reduced.
なお、エタノール95％の水溶液に対して70℃でαH20
＝1200、透過速度＝0.35kg m-2h-1の性能を示すキトサ
ンを活性層とする複合中空糸膜からなる水優先透過型浸
透気化装置を蒸留法に代えた方法を比較例として検討し
た。フローシートを図２に示した。本比較例の場合には
エタノール1kg当り蒸気の使用量が2.45kg、電力の使用
量は0.135WHで、9.38円／エタノール−kgと見積もられ
た。比較例２に対しても本発明例の方が著しく分離のエ
ネルギーが少なくて済む事が明らかである。In addition, α H20 at 70 ° C against an aqueous solution of 95% ethanol.
= 1200, permeation rate = 0.35 kg m -2 h -1 A comparative example was investigated in which the water preferential permeation type vaporizer consisting of a composite hollow fiber membrane with chitosan as the active layer was replaced with a distillation method. . The flow sheet is shown in FIG. In the case of this comparative example, the amount of steam used per kg of ethanol was 2.45 kg, and the amount of electric power used was 0.135 WH, and it was estimated to be 9.38 yen / ethanol-kg. It is clear that the invention example also requires significantly less energy for separation than the comparative example 2.
第１図は本発明にかかるエタノール濃縮液の製造方法を
示すフローシートである。図中、１、５、および７は熱
交換器を示す。２は揮発性有機液体優先透過型浸透気化
装置である。３は凝縮器を、４は真空ポンプを示す。６
は蒸留塔を示し、８は蒸留塔の加熱器である。 第２図は比較例にかかるエタノール濃縮液の製造方法を
示すフローシートである。図中1a、1bは熱交換器を示
す。2aはエタノール優先透過型浸透気化装置を、2bは水
優先透過型浸透気化装置である。3aおよび3bは凝縮器、
4a、4bは真空ポンプを示す。5aおよび5bはそれぞれ浸透
気化装置の付属する熱交換器を示している。FIG. 1 is a flow sheet showing a method for producing an ethanol concentrate according to the present invention. In the figure, 1, 5, and 7 indicate heat exchangers. 2 is a volatile organic liquid preferential permeation type pervaporation apparatus. 3 is a condenser and 4 is a vacuum pump. 6
Is a distillation column, and 8 is a heater for the distillation column. FIG. 2 is a flow sheet showing a method for producing an ethanol concentrate according to a comparative example. In the figure, 1a and 1b indicate heat exchangers. 2a is an ethanol preferential permeation type vaporizer, and 2b is a water preferential permeation type vaporizer. 3a and 3b are condensers,
4a and 4b show vacuum pumps. 5a and 5b show heat exchangers attached to the pervaporation apparatus, respectively.
Claims (4)
して、エタノール優先透過型浸透気化膜を有する浸透気
化装置を用いてエタノール濃縮液を製造するに際し、該
浸透気化膜の透過側蒸気を凝縮器で捕集した後、蒸留塔
の中段に供給して更に濃縮することを特徴とするエタノ
ール濃縮液の製造方法。1. When producing an ethanol concentrate using an ethanol aqueous solution of 15% by weight or less as a raw material and using a pervaporation apparatus having an ethanol preferential permeation type pervaporation membrane, the vapor on the permeation side of the pervaporation membrane is condensed into a condenser. The method for producing an ethanol concentrated solution, which comprises collecting in an intermediate stage of a distillation column and further concentrating the solution.
気化装置の１次側の供給液を加温した後、凝縮させて一
部を蒸留塔に還流し、残りの凝縮液を製品として取り出
すことを特徴とする請求項１記載のエタノール濃縮液の
製造方法。2. The steam withdrawn from the top of the distillation column warms the feed liquid on the primary side of the pervaporation apparatus, then condenses it and partially refluxes it to the distillation column. The method for producing an ethanol concentrate according to claim 1, which is taken out as a product.
供給される冷却された凝縮液と熱交換をさせて予備加熱
した後、蒸留塔に供給することを特徴とする請求項２記
載のエタノール濃縮液の製造方法。3. The column bottom liquid discharged from the distillation column and the cooled condensate supplied to the distillation column are heat-exchanged to be preheated and then supplied to the distillation column. 2. The method for producing an ethanol concentrate according to 2.
られた発酵液であることを特徴とする請求項１記載のエ
タノール濃縮液の製造方法。4. The method for producing an ethanol concentrate according to claim 1, wherein the low-concentration aqueous ethanol solution is a fermentation broth obtained by continuous fermentation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1092978A JP2676900B2 (en) | 1989-04-14 | 1989-04-14 | Method for producing ethanol concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1092978A JP2676900B2 (en) | 1989-04-14 | 1989-04-14 | Method for producing ethanol concentrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02273636A JPH02273636A (en) | 1990-11-08 |
| JP2676900B2 true JP2676900B2 (en) | 1997-11-17 |
Family
ID=14069481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1092978A Expired - Fee Related JP2676900B2 (en) | 1989-04-14 | 1989-04-14 | Method for producing ethanol concentrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2676900B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011101542A1 (en) * | 2010-02-19 | 2011-08-25 | St1 Biofuels Oy | Method and apparatus for heat restoration in a pervaporation process concentrating ethanol |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5750331B2 (en) * | 2010-08-05 | 2015-07-22 | 新日鉄住金エンジニアリング株式会社 | Membrane separation device and membrane separation method |
| JP6440156B2 (en) * | 2014-07-29 | 2018-12-19 | オルガノ株式会社 | Organic solvent purification system and method |
| JP6636111B2 (en) * | 2018-09-14 | 2020-01-29 | オルガノ株式会社 | Organic solvent purification system and method |
| JP7473171B2 (en) * | 2020-05-01 | 2024-04-23 | イーセップ株式会社 | Liquid composition adjustment system |
| WO2024004839A1 (en) * | 2022-06-28 | 2024-01-04 | 日東電工株式会社 | Membrane separation device, membrane separation system, and method for operating membrane separation device |
| WO2024058081A1 (en) * | 2022-09-14 | 2024-03-21 | 日東電工株式会社 | Membrane separation system and method for operating membrane separation system |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5940048B2 (en) * | 1977-08-19 | 1984-09-27 | 昭和電工株式会社 | How to separate liquid mixtures |
| JPS6042210B2 (en) * | 1981-07-29 | 1985-09-20 | 昭和電工株式会社 | Method for producing anhydrous ethanol |
| JPS5948427A (en) * | 1982-09-14 | 1984-03-19 | Showa Denko Kk | Preparation of anhydrous ethanol |
| JPS61158774A (en) * | 1984-12-29 | 1986-07-18 | Tokyo Electric Power Co Inc:The | Device for purifying ethanol |
| JPS63254987A (en) * | 1987-04-13 | 1988-10-21 | Ube Ind Ltd | Dehydration and concentration of alcoholic fermentation liquor |
-
1989
- 1989-04-14 JP JP1092978A patent/JP2676900B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011101542A1 (en) * | 2010-02-19 | 2011-08-25 | St1 Biofuels Oy | Method and apparatus for heat restoration in a pervaporation process concentrating ethanol |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02273636A (en) | 1990-11-08 |
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