JPS6174568A - Purification of ethanol - Google Patents

Purification of ethanol

Info

Publication number
JPS6174568A
JPS6174568A JP59194451A JP19445184A JPS6174568A JP S6174568 A JPS6174568 A JP S6174568A JP 59194451 A JP59194451 A JP 59194451A JP 19445184 A JP19445184 A JP 19445184A JP S6174568 A JPS6174568 A JP S6174568A
Authority
JP
Japan
Prior art keywords
ethanol
column
alkali
impurities
fusel oil
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
Application number
JP59194451A
Other languages
Japanese (ja)
Other versions
JPH0427830B2 (en
Inventor
Hiroshi Takada
高田 弘
Shozo Sumikawa
澄川 昌三
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
K F ENG KK
Original Assignee
K F ENG KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by K F ENG KK filed Critical K F ENG KK
Priority to JP59194451A priority Critical patent/JPS6174568A/en
Publication of JPS6174568A publication Critical patent/JPS6174568A/en
Publication of JPH0427830B2 publication Critical patent/JPH0427830B2/ja
Granted legal-status Critical Current

Links

Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

Landscapes

  • 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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

PURPOSE:To enable the recovery of ethanol in high purity, by adding an alkali to a concentration column, and precipitating the impurities. CONSTITUTION:An alkali metal hydroxide or alkaline earth metal hydroxide, etc. is added to a concentration column between the refluxing position and the fusel oil extraction position. The amount of the alkali is 1-0.3% based on ethanol. Since the impurities having low boiling point or high boiling point are removed by this process, a high-purity ethanol can be produced without repeating the fractionation process.

Description

【発明の詳細な説明】 発1を利 する 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
タノール含有液から蒸留によってエタノールを回収する
に際し途中のa縮塔にアリ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] The present invention relates to a method for purifying ethanol, and more specifically, when recovering ethanol from an ethanol-containing liquid by distillation, alkali is added to a condensation column in the middle to precipitate impurities, This 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
っ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
a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, ethanol is evaporated together with the steam, condensed in a concentrating tower, and dehydrated if necessary in a dehydration tower. A necessary third component is added to generate an azeotropic mixture to recover highly pure ethanol.

一方エタノール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。
On the other hand, the ethanol fermentation liquor contains impurities with low or high boiling points, and these must be removed to obtain ethanol of higher purity.

例えば廃糖蜜を原料とする発酵液はエタノール約8%(
V/V)の他にメタノール、インアシルアルコール、イ
ソブタノール、n−プロパツール、アセトアルデヒド等
が22−150pp含まれる。
For example, fermentation liquid made from blackstrap molasses contains approximately 8% ethanol (
V/V), methanol, inacyl alcohol, isobutanol, n-propanol, acetaldehyde, etc. are contained in an amount of 22-150 pp.

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って除去され、低沸点不
純物は濃縮塔のオーバーヘッ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敗を増して精
留が繰返されている。
High-boiling impurities are usually removed from the concentrator by returning it to the mortar with the fusel oil or from the bottom of the column, and low-boiling impurities are removed from the concentrator downstream of the overhead condenser. However, these methods do not completely remove it, and in order to further increase the purity, the number of losses in the distillation column 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。
Although there is always a demand for ethanol with higher purity than the problem that the invention aims to solve, 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a縮する際にアルカリ
を加えることによっ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 a-condensed 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)=等が用いられ
る。これらのアルカリはawi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%(V/V)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, or potassium or an alkaline earth metal such as KOH, NaOH, Ca (OH)=, etc. These alkalis are added to the AWI column, preferably between its reflux point and fusel oil withdrawal point, at less than 1% (V/V), preferably from 0.3 to 0.01%, relative to 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図に従って説明
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、エタノール含を液は熱交換器1を
経て酸基2に供給されスチームによって加熱され蒸気と
なっ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. Figure 1 shows an example of a process diagram for obtaining ethanol from an ethanol-containing liquid. The ethanol-containing liquid is supplied to an acid group 2 through a heat exchanger 1, heated by steam, becomes steam, and is sent to a concentrating column 3 together with steam. Sent. From the top of the concentration column 3, 95% to 96% ethanol is discharged.

ate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 ate tower 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 passes through a heat exchanger 7 and is transferred to a receiver 8.
A part of it is refluxed to the concentration column 3 and the remainder is supplied to the 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へキサン、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
から酸基に戻される。
The precipitate resulting from the reaction with the alkali is returned to the acid group 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ってもaW
r塔にアルカリを添加することによって低沸点又は高沸
点の不純物を除去することができる。
aW by a modification of the above method or a method other than the above.
By adding alkali to the r column, low or high boiling point impurities can be removed.

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っ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って説明する。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16m
”/Hで酸基(大気圧)に供給し、スチームを同時に3
2’00kg/H供給し、塔頂78℃で操作し、a縮塔
ヘエタノールが送られる。l1itf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1
315L/Hで排出させる。フーゼル油カットノズルよ
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10 L/Hの低沸点不純物を液状
もしくはガス状で抜取る。
Example 16 m of ethanol-containing culture solution (containing 8% ethanol)
”/H to supply acid groups (atmospheric pressure) and steam at the same time.
2'00 kg/H is supplied, the column is operated at 78° C., and ethanol is sent to the a condensation column. The reflux ratio of the l1itf column is 5.0.
95% (V/V) ethanol was added from the top of the column at 1
Discharge at 315L/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。Ethanol leaving the concentration tower is sent to a dehydration tower.

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2000>t; /
 Hを加えて塔頂を64℃で大気圧で操作して1犀水塔
底より99.5%(V/V)以上のエタノールを125
OL/Hで辱る。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。
The dehydration tower was supplied with 1,600 kg/H of cyclohexane and 2,000 tons of steam to form an azeotropic mixture;
After adding H, the top of the column was operated at 64°C and atmospheric pressure, and 99.5% (V/V) or more of ethanol was produced from the bottom of the column.
OL/H humiliates. The obtained ethanol contains acetaldehyde (120 ppm) and ketone (25 ppm).

濃縮塔のフーゼル油カットの位置と還流位置の中間に5
0%(W/W)  N a OH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った。
5 between the fusel oil cut position and the reflux position of the concentrator
When carrying out the same procedure as above except adding 2.5 L/H of 0% (W/W) NaOH (0.2% (V/V) to the product ethanol), there were no traces of both acetaldehyde and ketone. only was recognized.

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って濃
縮塔で沈殿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.

【図面の簡単な説明】[Brief explanation of the drawing]

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。 l:熱交換器、  2:酸基、  3:濃縮塔。
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: Acid group, 3: Concentration column.

Claims (1)

【特許請求の範囲】[Claims] エタノール含有液から濃縮塔を用いる蒸留法によってエ
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。
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.
JP59194451A 1984-09-17 1984-09-17 Purification of ethanol Granted JPS6174568A (en)

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 true JPS6174568A (en) 1986-04-16
JPH0427830B2 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)

Cited By (4)

* Cited by examiner, † Cited by third party
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
WO2005063681A1 (en) * 2003-12-23 2005-07-14 Basf Aktiengesellschaft Method for producing a ethylamine
WO2009123222A1 (en) * 2008-03-31 2009-10-08 宇部興産株式会社 Purification treatment method for fermented alcohol
WO2013035849A1 (en) * 2011-09-09 2013-03-14 宝酒造株式会社 Absolute alcohol manufacturing process and absolute alcohol

Cited By (10)

* Cited by examiner, † Cited by third party
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
WO2005063681A1 (en) * 2003-12-23 2005-07-14 Basf Aktiengesellschaft Method for producing a ethylamine
US7563933B2 (en) 2003-12-23 2009-07-21 Basf Aktiengesellschaft Method for producing an ethylamine
WO2009123222A1 (en) * 2008-03-31 2009-10-08 宇部興産株式会社 Purification treatment method for fermented alcohol
JP2009263355A (en) * 2008-03-31 2009-11-12 Ube Ind Ltd Method for purification-treating fermentation alcohol
CN102037128A (en) * 2008-03-31 2011-04-27 宇部兴产株式会社 Purification treatment method for fermented alcohol
US8053610B2 (en) 2008-03-31 2011-11-08 Ube Industries, Ltd. Method for purifying fermentation alcohol
WO2013035849A1 (en) * 2011-09-09 2013-03-14 宝酒造株式会社 Absolute alcohol manufacturing process and absolute alcohol
JPWO2013035849A1 (en) * 2011-09-09 2015-03-23 宝酒造株式会社 Method for producing anhydrous alcohol, and anhydrous alcohol
US9120724B2 (en) 2011-09-09 2015-09-01 Takara Shuzo Co., Ltd. Method for producing absolute alcohol and absolute alcohol

Also Published As

Publication number Publication date
JPH0427830B2 (en) 1992-05-12

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