JPH0327337A - Concentration and purification of alcohol - Google Patents
Concentration and purification of alcoholInfo
- Publication number
- JPH0327337A JPH0327337A JP1160697A JP16069789A JPH0327337A JP H0327337 A JPH0327337 A JP H0327337A JP 1160697 A JP1160697 A JP 1160697A JP 16069789 A JP16069789 A JP 16069789A JP H0327337 A JPH0327337 A JP H0327337A
- Authority
- JP
- Japan
- Prior art keywords
- alcohol
- solvent
- boiling point
- concentration
- supplied
- 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 73
- 238000000746 purification Methods 0.000 title description 2
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 238000009835 boiling Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 8
- 239000012141 concentrate Substances 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000005494 condensation Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- -1 amashiyo Chemical class 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000007858 starting material 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
- Y02P20/141—Feedstock
Landscapes
- Extraction Or Liquid Replacement (AREA)
- 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〕
本発明はアルコールの濃縮精製方法に関し、合成アルコ
ール、食品工業における使用済アルコール水溶液及び特
に発酵アルコール等から高純度のアルコールを省エネル
ギー的に濃縮精製するのに適した方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for concentrating and purifying alcohol, and is an energy-saving method for concentrating and purifying high-purity alcohol from synthetic alcohol, aqueous solutions of used alcohol in the food industry, and especially fermented alcohol. Concerning the appropriate method to do so.
甘しよ、さつまいも、とうもろこし等の炭水化物を原料
とする発酵アルコールは、飲料用及び工業用として重要
な出発原料であるが、発酵法で得られるアルコール水溶
液のアルコール濃度は１０〜２ ０ Ｗｔ％と低いため
、約９５〜１００ｗｔ％筐で濃縮する必要がある。Fermented alcohol made from carbohydrates such as amashiyo, sweet potato, and corn is an important starting material for beverages and industrial use, but the alcohol concentration of the alcohol aqueous solution obtained by the fermentation method is 10 to 20 wt%. Since the concentration is low, it is necessary to concentrate it in a box of about 95 to 100 wt%.
従来、この濃縮法として蒸留法が用いられてきたが、大
部分を占める水も８０〜１００℃まで昇温せねばならず
、経済的に不利であシ、これに替わる省エネルギー型の
濃縮法の開発が望筐れている。Conventionally, distillation has been used as a concentration method, but water, which makes up most of the water, must be heated to 80 to 100°C, which is economically disadvantageous, and an energy-saving concentration method has been proposed instead. Development is expected.
一方、省エネルギー型の濃縮法として超臨界状態又は擬
臨界状態の炭酸ガスを用いてアルコールを水よう抽出・
分離して濃縮する方法が提案されている。（特開昭５６
−５６２０１及び同５９−１４１５２８号公報）
しかしながら、炭酸ガスを溶剤として用いた場合アルコ
ールの選択的抽出には限界があシ、最大ｍ縮度は約９
１ ｗｔ％が限界であク、これ以上に濃縮することは不
可能であることが最近報告されている。又、炭酸ガス中
へのアルコールの溶解度は十分に大きくないことより、
大量の炭酸ガス（１０％アルコール水溶液１重量部に対
し１５重量部以上）を必要とするという問題点かあｂ，
その改善が望まれている。On the other hand, as an energy-saving concentration method, alcohol can be extracted by hydrolytic extraction using carbon dioxide gas in a supercritical or quasi-critical state.
A method of separating and concentrating has been proposed. (Unexamined Japanese Patent Publication No. 56
(No. 56201 and No. 59-141528) However, when carbon dioxide gas is used as a solvent, there is a limit to the selective extraction of alcohol, and the maximum degree of condensation is approximately 9.
It has recently been reported that 1 wt% is the limit and it is impossible to concentrate more than this. Also, since the solubility of alcohol in carbon dioxide gas is not large enough,
The problem is that a large amount of carbon dioxide gas (15 parts by weight or more per 1 part by weight of 10% alcohol aqueous solution) is required.
Improvement is desired.
このため、現在アルコール濃縮度を向上させ、かつアル
コール溶解度を大きくできる方法が望まれている。For this reason, there is currently a need for a method that can improve alcohol concentration and increase alcohol solubility.
本発明はアルコール濃縮度を９０〜９ ５ Ｗｔ％に保
持し、かつ、アルコール溶解度が大きくでき少量の溶剤
量でアルコールを濃縮回収できる経済的なアルコール濃
縮方法を提供しようとするものである。The present invention aims to provide an economical method for concentrating alcohol, which maintains the alcohol concentration at 90 to 95 Wt%, increases alcohol solubility, and can concentrate and recover alcohol using a small amount of solvent.
すなわち本発明は向流接触装置中部の原料供給口より、
アルコール水溶液を供給し、該向流接触装置の下部よ，
！７ ｃｏｓ溶剤を供給し、該原料供給口より下部にお
いてはＣｏ，溶剤を該アルコールの沸点（常圧沸点）の
温度以上かつ臨界圧力以上に保持し、該原料供給口よう
上部においてはＣｏ，溶剤を該アルコールの沸点（常圧
沸点）温度以下に保持することにより、該抽出塔上部よ
り実質的に水分が分離された濃縮アルコールを回収する
ことを特徴とするアルコールの濃縮轄製方法である。That is, in the present invention, from the raw material supply port in the middle of the countercurrent contactor,
An aqueous alcohol solution is supplied to the bottom of the countercurrent contactor,
! 7 Cos solvent is supplied below the raw material supply port, and the solvent is maintained at a temperature above the boiling point (normal pressure boiling point) of the alcohol and above the critical pressure, and above the raw material supply port, Co and the solvent are This is a method for concentrating alcohol, which is characterized by recovering concentrated alcohol from which water has been substantially separated from the upper part of the extraction column by maintaining the alcohol at a temperature below the boiling point (normal pressure boiling point) of the alcohol.
本発明は一般的には全てのアルコール水溶液の濃縮精製
に適用しうるものであるが、その一例として発酵アルコ
ールについて云えば、アルコール濃度は約１０ｗｔ％前
後で残シは水が主成分である。The present invention is generally applicable to the concentration and purification of all aqueous alcohol solutions, but as an example of fermented alcohol, the alcohol concentration is approximately 10 wt% and the remainder is mainly water.
以下、本発明の一実施態様を第１図に従って詳述する。Hereinafter, one embodiment of the present invention will be described in detail with reference to FIG.
第１図において、１は向流接触装置（このものは、充填
塔、棚段塔又は多段抽出塔であることが好ましい。）、
２は原料であるアルコールを含む水溶液の゜供給ライン
、３はＣＯ，溶剤の供給ライン、４は向流接触装置１の
下部の重液（水が主或分）の取出しライン、５は向流接
触装置１の上部の軽液（ ＣＯ，溶剤と濃縮アルコール
分）の取出しライン、６は原料供給ライン２より上部の
アルコール濃縮部、７は原料供給ライン２より下部のア
ルコール回収部、８は冷却用熱交換器である。In FIG. 1, 1 is a countercurrent contactor (this is preferably a packed column, plate column, or multistage extraction column);
2 is a supply line for an aqueous solution containing alcohol as a raw material, 3 is a CO and solvent supply line, 4 is a take-out line for heavy liquid (mainly water) at the bottom of the countercurrent contactor 1, and 5 is a countercurrent A take-out line for light liquid (CO, solvent and concentrated alcohol) at the top of the contactor 1, 6 an alcohol concentration section above the raw material supply line 2, 7 an alcohol recovery section below the raw material supply line 2, and 8 a cooling section. It is a heat exchanger for
原料のアルコール水溶液１重量部を原料供給ライン２よ
り、又ＣＯ，溶剤１０〜１５重量部を供給ライン３より
向流接触装置１に供給し、該ＣＯ，溶剤を回収部７にて
アルコール水溶液と向流接触させることにより、密度の
低いＣＯ，溶剤相は上昇しながらアルコール水溶液よう
アルコールを選択的に抽出し、軽液取出しライン５より
軽液として取シ出される。1 part by weight of an alcohol aqueous solution as a raw material is supplied through a raw material supply line 2, and 10 to 15 parts by weight of CO and a solvent are supplied through a supply line 3 to a countercurrent contactor 1, and the CO and solvent are converted into an alcohol aqueous solution in a recovery section 7. By bringing them into countercurrent contact, the CO and solvent phases with low density rise while selectively extracting alcohol like an aqueous alcohol solution, and are taken out as a light liquid through the light liquid extraction line 5.
本発明者は回収部７においてはｃｏ！溶剤を該アルコー
ルの沸点の温度以上かつ臨界圧力以上に保持することに
より、アルコールのｃｏ雪への溶解度が大巾に向上し、
重液抜出し２イン４からのアルコールの損失を防止する
に必要なＣＯ雪溶剤の使用量を大巾に低減できることを
見出した。The present inventor is co! By maintaining the solvent at a temperature above the boiling point of the alcohol and above the critical pressure, the solubility of the alcohol in cocoon snow is greatly improved,
It has been found that the amount of CO snow solvent required to prevent loss of alcohol from the heavy liquid extraction 2-in-4 can be significantly reduced.
この回収部７においては温度は約８０℃〜１７０℃が好
！シ〈、最も好ましい温度は８０〜１３０℃である。圧
力は７ ５ ａｔｍ以上が好ましいが、最も好ましくは
１００〜２ ０ ０ ａｔｍである。これ以上の圧力で
は装置コストの増大となシ好ましくない。In this recovery section 7, the temperature is preferably about 80°C to 170°C! The most preferable temperature is 80 to 130°C. The pressure is preferably 75 atm or higher, most preferably 100 to 200 atm. A pressure higher than this is undesirable as it increases the cost of the device.
次に、本発明者はＣＯ，溶剤相をアルコール濃縮部６に
おいて、冷却用熱交換器８にて冷却して該アルコールの
沸点温度以下にすることにより水分が選択的にＣｏ，溶
剤相よｂ相分離し、濃縮部６を重液となって下降し、Ｃ
Ｏ２溶剤和中のアルコール濃度が９０〜９ ５ ｗｔ％
（ ＣＯ２のない状態）１で濃縮されることを見出した
。Next, the present inventor cooled the CO and solvent phases in the alcohol concentrating section 6 with a cooling heat exchanger 8 to lower the temperature to below the boiling point of the alcohol, thereby selectively removing moisture from the CO and solvent phases. The phase separates and descends through the concentration section 6 as a heavy liquid.
Alcohol concentration in O2 solvent is 90-95 wt%
(in the absence of CO2) was found to be concentrated at 1.
ｓｌＩＩ部６ではＣｏ，溶剤を液体状態とする温度、圧
力が必要である。温度は１０〜７ａ４℃が好喧しいが、
最も好１しくは１０〜６０℃であう、圧力は回収部７と
同等の条件が好筐しい。In the slII section 6, a temperature and pressure are required to make Co and the solvent into a liquid state. The temperature is preferably 10-7a4℃,
Most preferably, the temperature is 10 to 60°C, and the pressure is preferably the same as that in the recovery section 7.
以下、本発明の実施例をあげて本発明を詳細に説明する
。Hereinafter, the present invention will be explained in detail by giving examples of the present invention.
（実施例１）
アルコール１０ｗｔ％、水９０ｗｔ％からなる原料１重
量部を、内径５０■、長さ７ｍの充填塔形式の向流接触
装置の上部よＦ）２ｍの部分に供給し、又Ｃｏ，溶剤を
該装置の底部より５〜２０重量の範囲で供給し、回収部
の温度を種々変化させた試験を行ない、該装置の塔頂及
び塔底のアルコール濃度を分析し、表１の結果を得た。(Example 1) 1 part by weight of a raw material consisting of 10 wt% alcohol and 90 wt% water was supplied to a part 2 m above the top of a packed column type countercurrent contactor with an inner diameter of 50 cm and a length of 7 m. , A test was conducted in which a solvent was supplied from the bottom of the device in a range of 5 to 20 weight, and the temperature of the recovery section was varied, and the alcohol concentration at the top and bottom of the device was analyzed. The results are shown in Table 1. I got it.
なお濃縮部の温度は４０℃にした。Note that the temperature of the concentration section was set to 40°C.
アルコール回収率は、既存の蒸留法の９９ｗｔ％を基準
とし、９９ｖｔ％以上を合格（Ｏ印）、９ ５ ｗｔ％
以下を不合格（ ×Ｌ ９ ６ ｗｔ％以上であるが９
９ｗｔ％以下をやや合格（Δ印）とした。The alcohol recovery rate is based on 99wt% of the existing distillation method, and passes 99vt% or higher (O mark), 95 wt%.
Fail the following (×L 9 6 wt% or more but 9
A value of 9 wt% or less was considered somewhat acceptable (Δ mark).
本結果より、次のことが見出された。From this result, the following was discovered.
Ｃｏ，溶剤を用いることにより、回収部の温度を８０〜
１７０℃、好ましくは８０〜１３０℃とすることによ）
Ｃ０３浴剤量が大巾に低減できた。（１ ０％アルコー
ル水溶液１重量部に対して１０重量部で十分であった。By using Co and solvent, the temperature of the recovery section can be kept at 80~80℃.
170°C, preferably 80-130°C)
The amount of C03 bath additives was significantly reduced. (10 parts by weight was sufficient for 1 part by weight of a 10% alcohol aqueous solution.
）
圧力は１００〜５ ０ ０ ａｔｍの範囲で十分てあつ
た。) The pressure was sufficient in the range of 100 to 500 atm.
又、アルコール＠縮度はいづれの場合も９１〜９ ２
ｗｔ％の範囲内であった。Also, the alcohol@condensation degree is 91 to 92 in any case.
It was within the range of wt%.
表１：
実施例１の結果
（実施例２）
実施例１に説明した向流接触装置を用い、同じアルコー
ル原料１重量部に対しＣＯ，溶剤を１０重量部供給し、
回収部の圧力は濃縮部の圧力と同じにし、温度を１１０
℃とし、濃縮部の温度を種々変化させた試験を行ない、
表２の結果を得た。Table 1: Results of Example 1 (Example 2) Using the countercurrent contactor described in Example 1, 10 parts by weight of CO and solvent were supplied to 1 part by weight of the same alcohol raw material,
The pressure in the recovery section is the same as that in the concentration section, and the temperature is 110℃.
℃, and conducted tests by varying the temperature of the concentrating section.
The results shown in Table 2 were obtained.
塔頂の溶剤相中のアルコール濃度が約９０ｖｔ％以上の
場合を合格（０印）と判定した。A case where the alcohol concentration in the solvent phase at the top of the column was about 90 vt% or more was judged to be passed (marked 0).
この結果、濃縮部の温度は１０〜７１１４℃、好１し〈
は１０〜６０℃とすることにより、９０ｗｔ％以上の含
水アルコールに濃縮できることが見出された。As a result, the temperature of the concentrating section was 10 to 7114℃, which was good.
It has been found that by controlling the temperature to 10 to 60°C, it can be concentrated to 90 wt% or more of hydrous alcohol.
するに際し、該アルコールの沸点温度以上かつ臨界圧力
以上のＣＯ２を用いることにより少量のＣＯ，でアルコ
ールを９ ９ ｗｔ％以上抽出回収し、更にＣＯ，を該
アルコールの沸点以下に冷却してアルコールの選択性を
向上させアルコール濃度を９ ０ ｗｔ％以上に濃縮で
きるものであシ、少量の溶剤使用のため装置のコンパク
ト化及びエネルギー負荷が軽減される経済的な効果を生
ずるとともに、製品価値の高い９ ０ ｗｔ％以上のア
ルコールを得るという効果を奏する。In this process, more than 99 wt% of alcohol is extracted and recovered with a small amount of CO by using CO2 at a temperature higher than the boiling point temperature and critical pressure of the alcohol, and then the CO2 is further cooled to below the boiling point of the alcohol to extract and recover the alcohol It can improve selectivity and concentrate the alcohol concentration to 90 wt% or more, and because it uses a small amount of solvent, it has an economical effect of making the equipment more compact and reducing energy load, and it also has high product value. This has the effect of obtaining alcohol of 90 wt% or more.
第１図は、本発明を実施するための向流接触装置の概略
図である。
〔発明の効果〕FIG. 1 is a schematic diagram of a countercurrent contacting apparatus for practicing the invention. 〔Effect of the invention〕
Claims (1)
を供給し、該向流接触装置の下部よりＣＯ＿２溶剤を供
給し、該原料供給口より下部においてはＣＯ＿２溶剤を
該アルコールの沸点の温度以上かつ臨界圧力以上に保持
し、該原料供給口より上部においてはＣＯ＿２溶剤を該
アルコールの沸点の温度以下に保持することにより、該
抽出塔上部より実質的に水分が分離された濃縮アルコー
ルを回収することを特徴とするアルコールの濃縮精製方
法。An aqueous alcohol solution is supplied from the raw material supply port in the middle of the countercurrent contactor, and a CO_2 solvent is supplied from the lower part of the countercurrent contactor, and at the lower part of the raw material supply port, the CO_2 solvent is heated at a temperature higher than the boiling point of the alcohol and at a temperature higher than the boiling point of the alcohol. By maintaining the pressure above the critical pressure and maintaining the CO_2 solvent at a temperature below the boiling point of the alcohol above the raw material supply port, concentrated alcohol from which water has been substantially separated is recovered from the top of the extraction column. A method for concentrating and purifying alcohol, characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1160697A JPH0327337A (en) | 1989-06-26 | 1989-06-26 | Concentration and purification of alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1160697A JPH0327337A (en) | 1989-06-26 | 1989-06-26 | Concentration and purification of alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0327337A true JPH0327337A (en) | 1991-02-05 |
| JPH0536419B2 JPH0536419B2 (en) | 1993-05-31 |
Family
ID=15720516
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1160697A Granted JPH0327337A (en) | 1989-06-26 | 1989-06-26 | Concentration and purification of alcohol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0327337A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5284983A (en) * | 1991-06-07 | 1994-02-08 | Basic Industries Bureau of Ministry of International Trade and Industry | Process for purifying aqueous crude ethanol solution |
-
1989
- 1989-06-26 JP JP1160697A patent/JPH0327337A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5284983A (en) * | 1991-06-07 | 1994-02-08 | Basic Industries Bureau of Ministry of International Trade and Industry | Process for purifying aqueous crude ethanol solution |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0536419B2 (en) | 1993-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4324567A (en) | Separation of gaseous components from a gaseous mixture by physical scrubbing | |
| US5294304A (en) | Process for the recovery of absolute ethanol by vapor compression extractive distillation | |
| JPH04193304A (en) | Condensing and refining method for alcohol | |
| US3644432A (en) | Process for recovering ethylene oxide | |
| US3816976A (en) | Process for the purification of acetylene and ethylene | |
| JPH0327337A (en) | Concentration and purification of alcohol | |
| JPH0329393B2 (en) | ||
| US2714573A (en) | Process for recovering volatile flavors | |
| JPS6229990A (en) | Purification of ethanol | |
| JPS6229988A (en) | Purification of ethanol from aqueous solution thereof | |
| JPH02184643A (en) | Production of anhydrous alcohol | |
| JPS6225985A (en) | Method of concentrating and purifying alcohol | |
| EP0354243B1 (en) | Process for concentrating and purifying alchohol | |
| JPH0420914B2 (en) | ||
| EP0453569B1 (en) | Manufacture of absolute alcohol | |
| JPH0327336A (en) | Dehydration of alcohol | |
| JPS6225983A (en) | Method of concentrating and purifying alcohol | |
| JPH02184388A (en) | Method and equipment for concentrating and purifying alcohol | |
| JPH035432A (en) | Method for dehydrating alcohol with n-butane | |
| JPH035431A (en) | Method for dehydrating alcohol with propylene | |
| JPS62135440A (en) | Method for concentrating and purifying alcohol | |
| JPH0333000B2 (en) | ||
| JPH0811161B2 (en) | Method for separating impurities in high-concentration ethanol | |
| JPH0129188B2 (en) | ||
| JPS6225984A (en) | Method of concentrating and purifying alcohol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term |