JPH0288534A - Concentration of ethanol - Google Patents
Concentration of ethanolInfo
- Publication number
- JPH0288534A JPH0288534A JP63239779A JP23977988A JPH0288534A JP H0288534 A JPH0288534 A JP H0288534A JP 63239779 A JP63239779 A JP 63239779A JP 23977988 A JP23977988 A JP 23977988A JP H0288534 A JPH0288534 A JP H0288534A
- Authority
- JP
- Japan
- Prior art keywords
- ethanol
- gas
- extraction
- carbon dioxide
- supercritical
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000000605 extraction Methods 0.000 claims abstract description 46
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 16
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000013361 beverage Nutrition 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、超臨界ガス抽出法によってエタノールを濃縮
する方法の改良に関し、詳細には蒸留法と同等もしくは
それ以上までエタノール純度を高めることのできる濃縮
法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an improvement in a method for concentrating ethanol by a supercritical gas extraction method, and more specifically, to an improvement in a method for concentrating ethanol by a supercritical gas extraction method, and more specifically, to improve a method for concentrating ethanol by using a supercritical gas extraction method, and in particular, to improve a method for concentrating ethanol by using a supercritical gas extraction method. This is about a concentration method that can be used.
［従来の技術］
発酵法によって得られるエタノールには大量の水か共存
しているので、このエタノールを飲料用や工業用として
利用するには濃縮工程が必要となる。エタノールの７ハ
縮には、これまで蒸留法が汎用されている。ところが蒸
留法では、１ｋｇの高純度エタノールを得るのに３００
０〜４０００ Ｋｃａｌ にも及ぶ大エネルギーを必要
とするため製造コストが高く、解決課題の１つとなって
いる。そこで製造コストの低減を期して種々の研究が行
なわれ、たとえば特開昭５６−５６２０１号公報に見ら
れる様な超臨界ガス抽出法を利用した／ａ縮法が提案さ
れている。[Prior Art] Since a large amount of water coexists in ethanol obtained by fermentation, a concentration step is required in order to use this ethanol for beverages or industrial purposes. Until now, distillation has been widely used for the 7-condensation of ethanol. However, with the distillation method, it takes 300 ml to obtain 1 kg of high-purity ethanol.
Since it requires a large amount of energy ranging from 0 to 4000 Kcal, the manufacturing cost is high, and this is one of the problems to be solved. Therefore, various studies have been carried out with the aim of reducing manufacturing costs, and for example, an /a reduction method using a supercritical gas extraction method as seen in Japanese Patent Application Laid-Open No. 56-56201 has been proposed.
この方法は、臨界温度が常温付近にあるガス、たとえば
炭酸ガスを使用し、このガスを超臨界状態（臨界温度、
臨界圧力を超えた温度、圧力の状、ｔｒ！！、）でエタ
ノール含有水溶液に接触させてエタノールを抽出する方
法であり、蒸留法に比べて消費エネルギーを著しく低減
し得るところから経済性の高い方法として注目を集めて
いる。殊に超臨界ガスとして炭酸ガスを使用すれば、抽
出操作を常温付近で行なうことができるので熱エネルギ
ー的に有利であり、且つ溶媒となる炭酸ガスは不燃性、
無毒且つ安価であるといった多くの利点を有しており、
実用化の期待が大きい。This method uses a gas whose critical temperature is around room temperature, such as carbon dioxide, and brings this gas into a supercritical state (critical temperature,
Temperature and pressure that exceed the critical pressure, tr! ! This is a method of extracting ethanol by contacting with an ethanol-containing aqueous solution using a method ( , ), and is attracting attention as a highly economical method because it can significantly reduce energy consumption compared to distillation methods. In particular, if carbon dioxide gas is used as a supercritical gas, the extraction operation can be performed at around room temperature, which is advantageous in terms of thermal energy, and carbon dioxide gas as a solvent is nonflammable and nonflammable.
It has many advantages such as being non-toxic and inexpensive.
There are high expectations for its practical application.
［発明が解決しようとする課題］
ところが元来超臨界ガスのもつ抽出能力は、物性の類似
した複数成分よりなる混合物から目的成分のみを簡単に
しかも効率良く分離し得るほど選択性の優れたものでは
なく、またその溶解能力も通常の液体系溶媒よりかなり
劣っている。たとえば超臨界ガスとして炭酸ガスを用い
てエタノール含有水溶液からエタノールを常温付近（４
０℃程度）で分ｍ？ｌＡ縮する場合には、エタノールの
濃縮限界濃度は第２図に示す通り９０％程度である。[Problem to be solved by the invention] However, the extraction ability of supercritical gas is so selective that it can easily and efficiently separate only the target component from a mixture of multiple components with similar physical properties. Moreover, its dissolving ability is considerably inferior to that of ordinary liquid solvents. For example, using carbon dioxide as a supercritical gas, ethanol is extracted from an ethanol-containing aqueous solution at around room temperature (4
0℃) for minutes? When condensing by 1A, the concentration limit concentration of ethanol is about 90% as shown in FIG.
一方アルコール製品としては、蒸留法によって得られる
エタノールの常圧における共沸点組成（アルコール濃度
９５％）と同等若しくはそれ以上の純度が要求される。On the other hand, alcohol products are required to have a purity equivalent to or higher than the azeotropic point composition (alcohol concentration 95%) at normal pressure of ethanol obtained by distillation.
従って上記要求純度を満足させる為には、超臨界ガス抽
出法によってアルコールを抽出分離した後、更に他の濃
縮手段を講じなければならない。Therefore, in order to satisfy the above required purity, after the alcohol has been extracted and separated by the supercritical gas extraction method, other concentration means must be taken.
本発明はこの様な事情に着目してなされたものであって
、その目的は超臨界ガス抽出法の有する特長を生かし、
且つその欠点であるエタノール高濃度域における選択性
（抽出対象物と非対象物に対する超臨界ガスの抽出選択
性）を改善することにより、超臨界ガス抽出法のみでエ
タノールを９５％程度以上の高純度にまで濃縮し得る様
な方法を確立しようとするものである。The present invention was made in view of these circumstances, and its purpose is to take advantage of the features of the supercritical gas extraction method,
In addition, by improving the selectivity in the high ethanol concentration range (extraction selectivity of supercritical gas with respect to target and non-target substances), which is the drawback, it is possible to extract ethanol with a high concentration of about 95% or more using only the supercritical gas extraction method. The aim is to establish a method that can concentrate to purity.
［課題を解決するための手段］
上記目的を達成することのできた本発明方法の構成は、
炭酸ガスによる超臨界ガス抽出法によってエタノール含
有水溶液からエタノールを濃縮するに当たり、抽出温度
を５０〜７０℃とするところに要旨を有するものである
。[Means for solving the problem] The structure of the method of the present invention that can achieve the above object is as follows:
The gist is that when concentrating ethanol from an ethanol-containing aqueous solution by a supercritical gas extraction method using carbon dioxide gas, the extraction temperature is set at 50 to 70°C.
［作用］
本発明者らは、炭酸ガスによる超臨界ガス抽出法によっ
てエタノール含有水溶液からエタノールの抽出を行なう
場合において、炭酸ガスの抽出選択性を高め得る手段を
求めて鋭意研究を重ねた。[Function] The present inventors have conducted extensive research in search of a means for increasing the selectivity of extraction of carbon dioxide gas when extracting ethanol from an ethanol-containing aqueous solution using a supercritical gas extraction method using carbon dioxide gas.
その結果超臨界ガス抽出法における抽出温度を常温付近
よりも高く設定すれば、炭酸ガスの抽出選択性が向上し
、エタノールの濃縮限界濃度を９５％以上に高め得るこ
とを見出すに至り、本発明を完成した。従来の超臨界ガ
ス抽出法では省エネルギーの観点から抽出温度は常温付
近（３５〜４０℃）に設定されており、抽出温度につい
ては何ら検討されていなかった。As a result, it was discovered that if the extraction temperature in the supercritical gas extraction method is set higher than around room temperature, the extraction selectivity of carbon dioxide gas can be improved and the concentration limit concentration of ethanol can be increased to 95% or more. completed. In the conventional supercritical gas extraction method, the extraction temperature is set around normal temperature (35 to 40°C) from the viewpoint of energy saving, and no consideration has been given to the extraction temperature.
これに対し本発明者らが超臨界ガス抽出法における抽出
温度とエタノール濃縮限界濃度との関係について調査し
たところ、第１図に示す様な結果が得られた。第１図に
見られる様に、抽出温度が高まるにつれてエタノールの
濃縮限界濃度が上昇することが判明した。またエタノー
ルの濃縮限界４度を９５％以上にするには、抽出温度を
５０℃以上にすればよいことが分かった。尚濃縮限界濃
度は抽出温度が７０℃程度のとぎにほぼ１００％となり
、７０℃を超える抽出温度を設定しても無意味であり、
製造コスト低減という観点から好ましくない。この様な
ところから本発明では抽出温度を５０〜７０℃の範囲に
限定した。On the other hand, when the present inventors investigated the relationship between extraction temperature and ethanol concentration limit concentration in supercritical gas extraction method, results as shown in FIG. 1 were obtained. As seen in FIG. 1, it was found that the concentration limit concentration of ethanol increased as the extraction temperature increased. It was also found that in order to increase the ethanol concentration limit of 4 degrees Celsius to 95% or higher, the extraction temperature should be set to 50 degrees Celsius or higher. The concentration limit concentration becomes almost 100% when the extraction temperature is about 70°C, so it is meaningless to set an extraction temperature higher than 70°C.
This is not preferable from the viewpoint of reducing manufacturing costs. For this reason, in the present invention, the extraction temperature is limited to a range of 50 to 70°C.
以下本発明を実施例によって更に詳細に説明するが、下
記実施例は本発明を限定する性質のものではなく、前・
後記の趣旨に徴して設計変更することはいずれも本発明
の技術的範囲に含まれるものである。Hereinafter, the present invention will be explained in more detail with reference to examples, but the following examples are not intended to limit the present invention.
Any design changes for the purposes described below are included within the technical scope of the present invention.
［実施例］
第３図は本発明方法を実施する為に構成されるエタノー
ル濃縮プロセスの一例を示するフロー図であり、１は抽
出塔、２は気液分離器、３は圧縮機を夫々示す。[Example] Figure 3 is a flow diagram showing an example of an ethanol concentration process configured to carry out the method of the present invention, in which 1 is an extraction column, 2 is a gas-liquid separator, and 3 is a compressor. show.
第３図において、抽出塔１の中部から原料（１０％濃度
のエタノール含有水溶液）Ａを１０ｋｇ／時間の割合で
供給する一方、抽出塔！の底部からは圧縮機３によって
加圧された超臨界状態の炭酸ガスＣを吹込み、抽出温度
６０℃、圧力１００ ａｔｍの条件でエタノール濃縮を
行なった。In FIG. 3, while raw material (10% ethanol-containing aqueous solution) A is supplied from the middle of the extraction tower 1 at a rate of 10 kg/hour, the extraction tower 1! Carbon dioxide C in a supercritical state pressurized by the compressor 3 was blown into the bottom of the tank, and ethanol concentration was carried out at an extraction temperature of 60° C. and a pressure of 100 atm.
尚このとき抽出塔１から導出される濃縮エタノール含有
ガスはラインＬ、からバルブＶを経て気液分離器２へ送
り、気液分離器２で分離された炭酸ガスはラインし２か
ら圧縮機３へ送って循環使用し、該分離器２で分離され
る高純度エタノールの一部はラインＬ３を経て抽出塔１
へ返送すると共に、一部はラインＬ４から製品Ｓとして
連続的に抜ぎ出した。At this time, the concentrated ethanol-containing gas derived from the extraction tower 1 is sent from line L to the gas-liquid separator 2 via valve V, and the carbon dioxide separated by the gas-liquid separator 2 is sent from line 2 to the compressor 3. A part of the high-purity ethanol separated by the separator 2 is sent to the extraction column 1 through line L3.
At the same time, a portion was continuously extracted as product S from line L4.
その結果、濃度が約９７％という高濃度の製品エタノー
ルＳが得られた。As a result, a highly concentrated product ethanol S with a concentration of about 97% was obtained.
［発明の効果コ
本発明は以上の様に構成されており、エタノール含有水
（８液から超臨界ガス抽出法のみで９５％以上という高
純度のエタノールを得ることができ、蒸留法等に比べて
エタノールの精製に要する消費エネルギーを大幅に低減
し得ることになった。[Effects of the Invention] The present invention is constructed as described above, and it is possible to obtain ethanol with a high purity of 95% or more from ethanol-containing water (8 liquids) using only the supercritical gas extraction method, which is more efficient than distillation methods. As a result, the energy consumption required for refining ethanol can be significantly reduced.
第１図は抽出温度がエタノール濃縮限界濃度に与える影
晋を示すグラフ、第２図は４０℃におけるエタノール？
！ＡＦａ限界濃度を示すグラフ、第３図は本発明を実施
する為に構成されるエタノール濃縮プロセスの一例を示
するフロー図である。
１・・・抽出塔 ２・・・気液分離器３・・・
圧縮機
Ａ・・・原料（エタノール含有水溶液）Ｃ・・・超臨界
炭酸ガス
Ｓ・・・製品エタノールFigure 1 is a graph showing the effect of extraction temperature on the ethanol concentration limit concentration, and Figure 2 is ethanol at 40°C.
! FIG. 3 is a graph showing the AFa limit concentration and is a flow diagram showing an example of an ethanol concentration process configured to carry out the present invention. 1... Extraction tower 2... Gas-liquid separator 3...
Compressor A... Raw material (ethanol-containing aqueous solution) C... Supercritical carbon dioxide gas S... Product ethanol
Claims (1)
有水溶液からエタノールを濃縮するに当たり、抽出温度
を５０〜７０℃とすることを特徴とするエタノールの濃
縮方法。A method for concentrating ethanol, which comprises concentrating ethanol from an ethanol-containing aqueous solution by a supercritical gas extraction method using carbon dioxide gas, the extraction temperature being set at 50 to 70°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63239779A JPH0288534A (en) | 1988-09-27 | 1988-09-27 | Concentration of ethanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63239779A JPH0288534A (en) | 1988-09-27 | 1988-09-27 | Concentration of ethanol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0288534A true JPH0288534A (en) | 1990-03-28 |
| JPH0456017B2 JPH0456017B2 (en) | 1992-09-07 |
Family
ID=17049769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63239779A Granted JPH0288534A (en) | 1988-09-27 | 1988-09-27 | Concentration of ethanol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0288534A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5656201A (en) * | 1979-09-28 | 1981-05-18 | Little Inc A | Method and device for separating organic liquid solute from mixture with solvent of said solute |
-
1988
- 1988-09-27 JP JP63239779A patent/JPH0288534A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5656201A (en) * | 1979-09-28 | 1981-05-18 | Little Inc A | Method and device for separating organic liquid solute from mixture with solvent of said solute |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0456017B2 (en) | 1992-09-07 |
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