JPH0427830B2 - - Google Patents
Info
- Publication number
- JPH0427830B2 JPH0427830B2 JP59194451A JP19445184A JPH0427830B2 JP H0427830 B2 JPH0427830 B2 JP H0427830B2 JP 59194451 A JP59194451 A JP 59194451A JP 19445184 A JP19445184 A JP 19445184A JP H0427830 B2 JPH0427830 B2 JP H0427830B2
- Authority
- JP
- Japan
- Prior art keywords
- ethanol
- tower
- column
- alkali
- impurities
- 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 - Lifetime
Links
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 77
- 238000000034 method Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000004821 distillation Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 description 10
- 239000001760 fusel oil Substances 0.000 description 9
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- 238000009835 boiling Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000000855 fermentation Methods 0.000 description 5
- 230000004151 fermentation Effects 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002699 waste 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Description
【発明の詳細な説明】
発明を利用する分野
本発明はエタノールの精製法に関し、さらに詳
しくはエタノールを含有液から蒸留によつてエタ
ノールを回収するに際し途中の濃縮塔にアルカリ
を加えて不純物を沈澱させ、エタノールを高純度
で回収する方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for purifying ethanol, and more specifically, when recovering ethanol from a liquid containing ethanol by distillation, an alkali is added to a concentrating column midway through the process to precipitate impurities. The present invention relates to a method for recovering ethanol with high purity.
従来技術
エタノール含有液例えばエタノール発酵液から
蒸留によつてエタノールを回収するには例えば発
酵液にスチームを加えてエタノールをスチームと
共に蒸発させ濃縮塔で濃縮し、必要に応じて脱水
塔で要すれば脱水するに必要な第３成分を加えて
共沸混合物を生成させて純度の高いエタノールを
回収することが行われる。Prior Art To recover ethanol from an ethanol-containing liquid, such as an ethanol fermentation liquid, by distillation, for example, steam is added to the fermentation liquid, the ethanol is evaporated together with the steam, concentrated in a concentrating column, and if necessary, in a dehydration column, if necessary. A third component necessary for dehydration is added to generate an azeotropic mixture to recover highly pure ethanol.
一方エタノールの発酵液には低沸点もしくは高
沸点の不純物が含まれており、より高純度のエタ
ノールを得るにはこれらを除去しなければならな
い。例えば廃糖密を原料とする発酵液はエタノー
ル約８％（／）の他にメタノール、イソアシ
ルアルコール、イソブタノール、ｎ−プロパノー
ル、アセトアルデヒド等が２−150ppm含まれる。 On the other hand, the ethanol fermentation liquor contains impurities with low or high boiling points, and these must be removed to obtain higher purity ethanol. For example, a fermentation liquid made from waste molasses contains about 8% (/) of ethanol, as well as 2-150 ppm of methanol, isoacyl alcohol, isobutanol, n-propanol, acetaldehyde, etc.
高沸点不純物は通常濃縮塔からフーゼル油と共
にあるいは塔底から醪塔へ戻すことによつて除去
され、低沸点不純物は濃縮塔のオーバーヘツドコ
ンデンサーの後流から除去されている。しかし、
これらの方法で完全に除去されず、より純度を上
げるためには蒸留塔の数を増して精留が繰返され
ている。 High-boiling impurities are usually removed from the concentrating column either with the fusel oil or by returning it to the mortar from the bottom, and low-boiling impurities are removed downstream of the overhead condenser of the concentrating column. but,
These methods do not remove it completely, and in order to further increase the purity, the number of distillation columns is increased and rectification is repeated.
発明が解決しようとする問題点
より純度の高いエタノールは常に求められてい
るが精留を繰返すことはエネルギーを多量に消費
し、コストを上げる。より簡単なる方法で不純物
を除去する方法の開発が求められている。Problems to be Solved by the Invention Ethanol with higher purity is always in demand, but repeating rectification consumes a large amount of energy and increases costs. There is a need for the development of a simpler method for removing impurities.
問題を解決するための手段
本発明によれば醪塔でエタノール含有液に蒸気
を加えてエタノールを濃縮塔へ送りそこで濃縮す
る際にアルカリを加えることによつて不純物が沈
澱物として除去できる。これは不純物がアルカリ
と反応して沈澱物を作ると考えられることによ
る。Means for Solving the Problems According to the present invention, impurities can be removed as precipitates by adding steam to the ethanol-containing liquid in the mortar tower and sending the ethanol to the concentrating tower, where it is concentrated by adding alkali. This is because impurities are thought to react with alkali to form precipitates.
用いられるアルカリはナトリウム、カルシウ
ム、カリウム等のアルカリ金属又はアルカリ土類
金属の水酸化物例えばKOH，NaOH，Ca（OH）2
等が用いられる。これらのアルカリは濃縮塔、好
ましくはその還流の位置とフーゼル油抜出し個所
の間にエタノールに対し１％（／）以下、好
ましくは0.3〜0.01％添加される。 The alkali used is a hydroxide of an alkali metal such as sodium, calcium, potassium or an alkaline earth metal such as KOH, NaOH, Ca(OH) 2
etc. are used. These alkalis are added to the concentration column, preferably between the reflux point and the fusel oil withdrawal point, in an amount of not more than 1% (/), preferably 0.3 to 0.01%, based on the ethanol.
アルカリは通常50重量％以下の濃度のものが用
いられる。 The alkali used usually has a concentration of 50% by weight or less.
本発明をより詳しく説明するために第１図に従
つて説明する。第１図はエタノール含有液からエ
タノールを得る工程図の１例を示し、エタノール
含有液は熱交換器１を経て醪塔２に供給されスチ
ームによつて加熱され蒸気となつてスチームと共
に濃縮塔３に送られる。濃縮塔３の塔頂から95％
〜96％のエタノールが排出される。 The present invention will be explained in more detail with reference to FIG. FIG. 1 shows an example of a process diagram for obtaining ethanol from an ethanol-containing liquid. The ethanol-containing liquid is supplied to a mortar tower 2 through a heat exchanger 1, heated by steam, turned into steam, and transferred together with steam to a concentrating tower 3. sent to. 95% from the top of concentration tower 3
~96% ethanol is emitted.
濃縮塔３の底部にフーゼル油取出口４が設けら
れフーゼル油が適宜抜き取られる。アルカリ供給
口５は還流口６とフーゼル油取出し口の間に設け
られる。 A fusel oil outlet 4 is provided at the bottom of the concentrating column 3, and the fusel oil is appropriately extracted. The alkali supply port 5 is provided between the reflux port 6 and the fusel oil outlet.
塔頂からのエタノール濃縮液は熱熱交換器７を
経て受器８に送られ、その１部は濃縮塔３へ還流
され残部は脱水塔９へ供給される。 The ethanol concentrate from the top of the column is sent to a receiver 8 via a heat exchanger 7, a part of which is refluxed to a concentrating column 3, and the remainder is supplied to a dehydration column 9.
脱水塔には必要に応じて三成分系共沸混合物を
形成させるための第３の成分例えばシクロヘキサ
ン、ベンゼン等が加えられる。精製エタノールは
脱水塔の塔底から得られる。 If necessary, a third component such as cyclohexane, benzene, etc. is added to the dehydration tower to form a ternary azeotrope. Purified ethanol is obtained from the bottom of the dehydration tower.
アルカリとの反応による沈澱物は濃縮塔ドレイ
ン抜出口から醪塔に戻される。 The precipitate resulting from the reaction with the alkali is returned to the moromi tower through the concentrator drain outlet.
上記方法の変法あるいは上記以外の方法によつ
ても濃縮塔にアルカリを添加することによつて低
沸点又は高沸点の不純物を除去することができ
る。 Low-boiling point or high-boiling point impurities can be removed by a modification of the above method or by a method other than the above method by adding alkali to the concentration column.
本発明方法はエタノール発酵液のみならずエタ
ノールを含有する溶液であればいずれも対象とな
り、エタノールを回収する際に適用することによ
つて高純度で安価に回収できる。 The method of the present invention is applicable not only to ethanol fermentation liquid but also to any solution containing ethanol, and by applying it when recovering ethanol, it can be recovered with high purity and at low cost.
以下本発明の態様を実施例によつて説明する。 Aspects of the present invention will be explained below using Examples.
実施例
エタノール含有培養液（エタノール８％含有）
を16m3／Ｈで醪塔（大気圧）に供給し、スチーム
を同時に3200Kg／Ｈ供給し、塔頂78℃で操作し、
濃縮塔へエタノールが送られる。濃縮塔を還流比
5.0で操作し、塔頂より95％（Ｖ／Ｖ）のエタノ
ールを1315L／Ｈで排出させる。フーゼル油カツ
トノズルより50L／Ｈでフーゼル油を取出し、熱
交換器７の後流の熱交換基１０より10L／Ｈの低
沸点不純物を液状もしくはガス状で抜取る。Example Ethanol-containing culture solution (containing 8% ethanol)
was supplied to the mortar tower (atmospheric pressure) at 16 m 3 /H, steam was simultaneously supplied at 3200 Kg / H, and the tower was operated at 78°C.
Ethanol is sent to the concentration column. Reflux ratio of concentration tower
5.0, and 95% (V/V) ethanol is discharged from the top of the column at 1315 L/H. Fusel oil is taken out at 50 L/H from a fusel oil cut nozzle, and 10 L/H of low boiling point impurities are taken out in liquid or gas form from a heat exchange group 10 downstream of the heat exchanger 7.
濃縮塔を出たエタノールは脱水塔に送られる。
脱水塔には共沸混合物を形成させるためのシクロ
ヘキサン1600Kg／Ｈ及びスチームを2000Kg／Ｈを
加えて塔頂を64℃で大気圧で操作して脱水塔底よ
り99.5％（Ｖ／Ｖ）以上のエタノールを1250L／
Ｈで得る。得られたエタノール中にアセトアルデ
ヒド（120ppm）及びケトン（25ppm）が含まれ
ている。 Ethanol leaving the concentration tower is sent to a dehydration tower.
To the dehydration tower, 1,600 kg/h of cyclohexane and 2,000 kg/h of steam were added to form an azeotropic mixture, and the top of the tower was operated at 64°C and atmospheric pressure to produce a concentration of 99.5% (V/V) or more from the bottom of the dehydrating tower. 1250L/ethanol
Get it with H. The obtained ethanol contains acetaldehyde (120 ppm) and ketone (25 ppm).
濃縮塔のフーゼル油カツトの位置と還流位置の
中間に50％（Ｗ／Ｗ）NaOHを2.5L／Ｈ〔製品エ
タノールに対し0.2％（Ｖ／Ｖ）〕を添加する他は
上記と同様に実施した場合はアセトアルデヒド、
ケトンは共に痕跡しか認められなかつた。 Carry out in the same manner as above, except that 2.5 L/H of 50% (W/W) NaOH [0.2% (V/V) relative to product ethanol] is added between the fusel oil cut position and the reflux position of the concentration tower. If so, acetaldehyde,
Only traces of ketones were detected.
発明の効果
低沸点又は高沸点の不純物がアルカリの添加に
よつて濃縮塔で沈澱物として簡単に除去でき、精
留を繰返すことなく高純度のエタノールを安価に
得ることができる。Effects of the Invention Impurities with low or high boiling points can be easily removed as precipitates in a concentration column by adding alkali, and high purity ethanol can be obtained at low cost without repeating rectification.
第１図は本発明によるエタノールの製造工程の
１例を示す。
各記号は以下の装置を示す。１……熱交換器、
２……醪塔、３……濃縮塔、４……フーゼル油取
出口、５……アルカリ供給口、６……還流口、７
……熱交換器、８……受器、９……脱水塔、１０
……熱交換器。
FIG. 1 shows an example of the ethanol production process according to the present invention. Each symbol indicates the following equipment. 1... heat exchanger,
2... Mortar tower, 3... Concentration tower, 4... Fusel oil outlet, 5... Alkali supply port, 6... Reflux port, 7
... Heat exchanger, 8 ... Receiver, 9 ... Dehydration tower, 10
……Heat exchanger.
Claims (1)
によつてエタノールを回収する際に該濃縮塔にア
ルカリを添加することを特徴とするエタノールの
精製法。1. A method for purifying ethanol, which comprises adding an alkali to a concentrating column when recovering ethanol from an ethanol-containing liquid by a distillation method using a concentrating column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59194451A JPS6174568A (en) | 1984-09-17 | 1984-09-17 | Purification of ethanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59194451A JPS6174568A (en) | 1984-09-17 | 1984-09-17 | Purification of ethanol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6174568A JPS6174568A (en) | 1986-04-16 |
| JPH0427830B2 true JPH0427830B2 (en) | 1992-05-12 |
Family
ID=16324786
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59194451A Granted JPS6174568A (en) | 1984-09-17 | 1984-09-17 | Purification of ethanol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6174568A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63107703A (en) * | 1986-10-27 | 1988-05-12 | Daicel Chem Ind Ltd | Distillation separating method for azeotropic mixture |
| DE10361503A1 (en) * | 2003-12-23 | 2005-07-28 | Basf Ag | Process for the preparation of an ethylamine |
| US8053610B2 (en) | 2008-03-31 | 2011-11-08 | Ube Industries, Ltd. | Method for purifying fermentation alcohol |
| US9120724B2 (en) | 2011-09-09 | 2015-09-01 | Takara Shuzo Co., Ltd. | Method for producing absolute alcohol and absolute alcohol |
-
1984
- 1984-09-17 JP JP59194451A patent/JPS6174568A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6174568A (en) | 1986-04-16 |
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