JPH0578535B2 - - Google Patents
Info
- Publication number
- JPH0578535B2 JPH0578535B2 JP60275995A JP27599585A JPH0578535B2 JP H0578535 B2 JPH0578535 B2 JP H0578535B2 JP 60275995 A JP60275995 A JP 60275995A JP 27599585 A JP27599585 A JP 27599585A JP H0578535 B2 JPH0578535 B2 JP H0578535B2
- Authority
- JP
- Japan
- Prior art keywords
- alcohol
- liquid
- solvent
- raw material
- boiling point
- 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 56
- 239000002904 solvent Substances 0.000 claims description 48
- 239000012535 impurity Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 34
- 238000009835 boiling Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 10
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 238000005191 phase separation Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 description 48
- 150000001298 alcohols Chemical class 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000001760 fusel oil Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 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
- -1 amashiyo Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004090 dissolution 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
- 239000003049 inorganic solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 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
- 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
-
- 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
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Extraction Or Liquid Replacement (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、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分離濃縮しうる方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for separating and concentrating highly pure alcohol from fermented alcohol and the like in an energy-saving manner.
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〜
20wt％と低いため、約95〜100wt％まで濃縮する
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 between 10 and 10.
Since it is low at 20wt%, it is necessary to concentrate it to about 95-100wt%.
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、経済的に不利であり、これに替わる
省エネルギー型の濃縮法の開発が望まれている。 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.Therefore, an alternative energy-saving concentration method has been developed. is desired.
従来、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、エチレン、エタン
を用いてアルコールを水より抽出・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、この濃縮された発酵アルコール
中には高沸点不純物（C4〜C5系フーゼル油）等
の副生成物が混入しており、これらも分離除去す
る必要があるが、この分離除去法として従来は蒸
留法による精留塔が用いられており、この際、濃
縮アルコールを再昇温せねばならず、熱負荷が増
大し、省エネルギー的な方法とは云えないという
欠点があつた。 BACKGROUND ART Conventionally, as an energy-saving concentration method, a method has been proposed in which alcohol is extracted and separated from water using carbon dioxide, ethylene, or ethane in a supercritical or quasi-critical state and concentrated. (JP-A-56-56201 and JP-A-59-141528) However, by-products such as high-boiling impurities (C 4 - C 5 fusel oil) are mixed in this concentrated fermented alcohol. These also need to be separated and removed, but conventionally, a rectification column using a distillation method has been used for this separation and removal method, but in this case, the concentrated alcohol has to be heated again, which increases the heat load and saves energy. The drawback was that it could not be called a practical method.
本発明は、アルコール、水、高沸点不純物等の
混合物から実質的に水、高沸点不純物が含まれな
いアルコールを分離回収する際に、省エネルギー
型の分離回収法を行うことができる方法を提供し
ようとするものである。
The present invention provides an energy-saving separation and recovery method when separating and recovering alcohol substantially free of water and high-boiling point impurities from a mixture of alcohol, water, high-boiling point impurities, etc. That is.
すなわち、本発明はアルコール及び高沸点不純
物からなる有機液体溶質と水との原料混合物を向
流接触抽出装置の上部より供給し、又臨界温度が
該アルコールの沸点より低い溶剤を該向流接触抽
出装置の下部より供給し、該原料混合物と該溶剤
を、該溶剤を超臨界状態又は擬臨界状態になるよ
うな条件下で向流接触させ、該向流接触抽出装置
の上部より軽液を、下部より重液を取り出し、次
に、該軽液は実質的に高沸点不純物が相分離する
に必要な圧力まで減圧後、不純物分離槽に導入し
重質不純物液と軽質精製液に分離し、該重質不純
物液を前記向流接触抽出装置の原料混合物供給部
分と溶剤供給部分との間に導入するとともに、該
軽質精製液を溶剤分離槽に導入し、溶解溶剤と濃
縮アルコールが相分離するに必要な圧力まで減圧
後、該濃縮アルコールの一部を該原料混合物供給
部分より上部に導入することを特徴とするアルコ
ール濃縮精製法である。
That is, in the present invention, a raw material mixture of an organic liquid solute consisting of alcohol and high-boiling impurities and water is supplied from the upper part of a countercurrent catalytic extraction device, and a solvent whose critical temperature is lower than the boiling point of the alcohol is supplied to the countercurrent catalytic extraction device. The raw material mixture and the solvent are brought into countercurrent contact under conditions that bring the solvent into a supercritical or quasi-critical state, and the light liquid is supplied from the upper part of the countercurrent contact extraction device. The heavy liquid is taken out from the lower part, and then the light liquid is depressurized to the pressure necessary for substantially high-boiling point impurities to undergo phase separation, and then introduced into an impurity separation tank and separated into a heavy impurity liquid and a light purified liquid, The heavy impurity liquid is introduced between the raw material mixture supply section and the solvent supply section of the countercurrent contact extraction device, and the light purified liquid is introduced into the solvent separation tank, so that the dissolved solvent and concentrated alcohol are phase-separated. This alcohol concentration and purification method is characterized in that after the pressure is reduced to the pressure required for this, a part of the concentrated alcohol is introduced into the upper part of the raw material mixture supply section.
本発明の原料混合物は、主に発酵アルコールで
あり代表的組成は
水 80〜90wt％
アルコール類 10〜20wt％
高沸点不純物（C4〜C5系フーゼル油） 0.1wt％
である。アルコール類とは、メチルアルコール、
エチルアルコール、プロパノール、ブタノール等
である。 The raw material mixture of the present invention is mainly fermented alcohol, and its typical composition is 80 to 90 wt% water, 10 to 20 wt% alcohol, and 0.1 wt% high boiling point impurities ( C4 to C5 fusel oil). Alcohols include methyl alcohol,
Ethyl alcohol, propanol, butanol, etc.
又、溶解溶剤としては、特開昭56−56201号公
報にみられるように、CO2、C2H4、C2H6等の他
に、臨界温度がアルコールの沸点以下である無機
又は有機の溶剤が使用可能である。表１に、主な
溶剤を示す。 In addition to CO 2 , C 2 H 4 , C 2 H 6 , etc., inorganic or organic solvents whose critical temperature is below the boiling point of alcohol can be used as dissolving solvents, as shown in JP-A No. 56-56201. solvents can be used. Table 1 shows the main solvents.
表 １
溶剤名 臨界温度（℃）
CO2 31.1
C2H4 9.7
C2H6 32.4
C3H8 96.8
C4H10 152.0
H2S 100.4
N2O 36.5
特に、臨界温度が常温に近い程又アルコールと
の親和力の大きい溶剤程省エネルギー効果は大き
く、好ましい溶剤である。又、これらは混合して
も使用できる。一般に溶解溶剤は原料アルコール
１重量部に対して２〜10重量部添加されるが、ア
ルコールとしての親和力の大きい溶解溶剤の場合
は、その添加量は上記範囲より少にすることがで
きる。 Table 1 Solvent name Critical temperature (°C) CO 2 31.1 C 2 H 4 9.7 C 2 H 6 32.4 C 3 H 8 96.8 C 4 H 10 152.0 H 2 S 100.4 N 2 O 36.5 In particular, the closer the critical temperature is to room temperature, the more A solvent that has a greater affinity with alcohol has a greater energy saving effect and is therefore a preferable solvent. Moreover, these can be used even if mixed. Generally, the dissolving solvent is added in an amount of 2 to 10 parts by weight per 1 part by weight of the raw material alcohol, but if the dissolving solvent has a high affinity for alcohol, the amount added can be smaller than the above range.
本発明にいう超臨界状態とは、溶解溶剤の臨界
温度以上かつ臨界圧力以上の温度、圧力条件での
状態を意味し、擬臨界状態とは、溶解溶剤に臨界
温度Tc以下で、対臨界温度TR＝Ｔ／Tc（但し、
0.90＜Tr＜1.0）の温度Ｔで、圧力はその温度に
おける溶解溶剤の飽和蒸気圧以上の状態を意味す
る。擬臨界状態では超臨界状態より溶解溶剤の溶
解度が増す場合があるが、溶解速度は減少する傾
向にある。 The supercritical state in the present invention refers to a state in which the temperature and pressure are higher than the critical temperature and critical pressure of the dissolving solvent, and the quasi-critical state is a state in which the dissolving solvent is under the critical temperature Tc and below the critical temperature. T R = T/Tc (however,
At a temperature T of 0.90<Tr<1.0), the pressure means a state equal to or higher than the saturated vapor pressure of the dissolving solvent at that temperature. Although the solubility of the dissolving solvent may increase in the quasi-critical state compared to the supercritical state, the dissolution rate tends to decrease.
向流接触装置は、充填塔、棚段塔又は多段抽出
塔等が好ましい。 The countercurrent contact device is preferably a packed column, a tray column, a multistage extraction column, or the like.
以下、本発明の一実施例を第１図に従つて詳述
する。 An embodiment of the present invention will be described in detail below with reference to FIG.
原料混合物１重量部を上記向流接触装置３の上
部１より、又溶解溶剤２〜10重量部を下部２より
供給し、該溶解溶剤の臨界状態又は擬臨界状態で
向流接触させることにより、軽質の溶解溶剤相は
上昇しながら、原料混合物相よりアルコール類を
選択的に押出し、上部６より軽液として取り出さ
れる。溶解溶剤の添加量は、溶解溶剤がアルコー
ル類との親和力が大きい場合は減ずることができ
る。 By supplying 1 part by weight of the raw material mixture from the upper part 1 of the countercurrent contacting device 3 and 2 to 10 parts by weight of the dissolving solvent from the lower part 2, and carrying out countercurrent contact in the critical state or quasi-critical state of the dissolving solvent, As the light dissolved solvent phase rises, it selectively pushes out alcohols from the raw material mixture phase and is taken out from the upper part 6 as a light liquid. The amount of the dissolving solvent added can be reduced if the dissolving solvent has a high affinity with alcohols.
一方、原料混合物相はアルコール類を抽出され
ながら下部へ重液となり下降し、下部５より抜き
出される。 On the other hand, the raw material mixture phase descends to the lower part as a heavy liquid while the alcohols are extracted, and is extracted from the lower part 5.
上部６よりの軽液は、溶解溶剤及びアルコール
の他に少量の高沸点不純物と水を含んでおり、水
と不純物は製品の規格上好ましくないものであ
り、分離除去する必要がある。 The light liquid from the upper part 6 contains a small amount of high-boiling point impurities and water in addition to the dissolving solvent and alcohol, and water and impurities are unfavorable in terms of product specifications and must be separated and removed.
溶解溶剤中への水及び不純物の溶解度は、溶解
溶剤の密度にほぼ比例しており、圧力を下げるか
又は温度を上げて溶解溶剤の密度の低下させるこ
とにより、水及び不純物の内、高沸点の物質がま
ず溶解溶剤から相分離する。 The solubility of water and impurities in a dissolving solvent is approximately proportional to the density of the dissolving solvent, and by lowering the pressure or increasing the temperature to lower the density of the dissolving solvent, water and impurities with high boiling points can be removed. The substance first undergoes phase separation from the dissolved solvent.
温度を上げることは、熱効率の低下をもたらす
ので好ましくないので、圧力を下げることにより
溶解溶剤の密度を下げるのが好ましい。しかし、
圧力を下げすぎると、溶解溶剤の溶解度が大巾に
減少し、アルコール類も多量相分離するのでその
量を把握して圧力を制御する必要がある。 Since increasing the temperature is undesirable as it causes a decrease in thermal efficiency, it is preferable to decrease the density of the dissolving solvent by decreasing the pressure. but,
If the pressure is lowered too much, the solubility of the dissolving solvent will decrease significantly and a large amount of alcohol will phase separate, so it is necessary to control the pressure by controlling the amount.
本発明はかかる現象を利用することにより、濃
縮アルコールの純度を向上させるものである。即
ち、前記軽液は減圧弁７により、高沸点不純物を
選択的に相分離するように減圧され、ライン８よ
り不純物分離槽９に導入され、軽質精製液と重質
不純物液とに分離される。該軽質精製液は、溶解
溶剤の他にアルコールとごく微量の水及び高沸点
不純物の混合物である。又、重質不純物液は、水
及び高沸点不純物とごく少量のアルコールと溶解
溶剤からなる混合物である。 The present invention utilizes this phenomenon to improve the purity of concentrated alcohol. That is, the light liquid is depressurized by a pressure reducing valve 7 to selectively phase-separate high-boiling point impurities, and is introduced into an impurity separation tank 9 through a line 8, where it is separated into a light purified liquid and a heavy impurity liquid. . The light purified liquid is a mixture of alcohol, a very small amount of water, and high-boiling point impurities in addition to the dissolving solvent. The heavy impurity liquid is a mixture of water, high boiling point impurities, a very small amount of alcohol, and a dissolving solvent.
該軽質精製液は、１３より抜き出され、減圧弁
１４により溶解溶剤とアルコールが相分離するに
必要な圧力まで減圧後、ライン１５より溶解溶剤
分離槽１６に導入する。 The light purified liquid is extracted from 13, reduced in pressure by a pressure reducing valve 14 to a pressure necessary for phase separation of the dissolved solvent and alcohol, and then introduced into a dissolved solvent separation tank 16 through a line 15.
該溶解溶剤分離槽１６からライン１７を経由し
て取出されるアルコール中には微量の水及び高沸
点不純物を含んでいるが、該アルコールの一部を
ライン２０を介して該向流接触装置４の上部に循
環する。この還流効果により、該アルコールの純
度が大巾に向上する。又、該アルコールの純度は
循環流量の増加とともに向上する。 The alcohol taken out from the dissolved solvent separation tank 16 via line 17 contains trace amounts of water and high boiling point impurities, and a portion of the alcohol is transferred via line 20 to the countercurrent contactor 4. circulate to the top of the. This reflux effect greatly improves the purity of the alcohol. Also, the purity of the alcohol increases with increasing circulation flow rate.
溶解溶剤分離槽１６の上部からは、ライン１
８、減圧弁１９を介し、ライン２２より溶解溶剤
が回収され再使用される。 From the top of the dissolved solvent separation tank 16, line 1
8. The dissolving solvent is recovered from the line 22 via the pressure reducing valve 19 and reused.
一方、不純物分離槽９の下部からライン１０を
経由して取出される重質不純物中には少量のアル
コールが溶解しており、製品アルコールの損失を
防止するために回収する必要がある。 On the other hand, a small amount of alcohol is dissolved in the heavy impurities taken out from the lower part of the impurity separation tank 9 via the line 10, and needs to be recovered to prevent loss of product alcohol.
本発明においては、該重質不純物を前記向流接
触装置３にライン１１を経て再度導入することに
より、アルコールの損失を防止するとともに、高
沸点重質不純物を分離除去するものである。該重
質不純物の導入部は、その組成に応じて決定され
るが、好ましくは原料混合物導入部１と溶解溶剤
導入部２との間である。 In the present invention, by reintroducing the heavy impurities into the countercurrent contactor 3 via the line 11, loss of alcohol is prevented and high boiling point heavy impurities are separated and removed. The introduction section for the heavy impurities is determined depending on the composition, but is preferably between the raw material mixture introduction section 1 and the dissolving solvent introduction section 2.
なお第１図中、２１は製品アルコール取出しラ
イン、１２は重質不純物排出ラインである。 In FIG. 1, 21 is a product alcohol take-out line, and 12 is a heavy impurity discharge line.
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
エチルアルコール10wt％、C4〜C5系フーゼル
油0.1wt％、水89.9wt％の原料混合物１重量部と、
溶解溶剤として二酸化炭素を６重量部及びエタン
を0.5重量部を、内径50mm、長さ３ｍの充填塔の
上部より１ｍの部位及び下部より30cmの部位に供
給し、圧力150atm、温度40℃で向流接触させ、
塔頂より軽液を塔底より重液を取り出し、該軽液
を不純物分離槽で圧力90atmに減圧し、軽質精製
液と重質不純物液に分離し、該重質不純物液は充
填塔の下部から1.5ｍの部位に全量戻した。Example 1 part by weight of a raw material mixture of 10 wt% ethyl alcohol, 0.1 wt% C4 - C5 fusel oil, and 89.9 wt% water,
6 parts by weight of carbon dioxide and 0.5 parts by weight of ethane as dissolving solvents were supplied to a part 1 m from the top and 30 cm from the bottom of a packed column with an inner diameter of 50 mm and a length of 3 m, and the mixture was heated at a pressure of 150 atm and a temperature of 40°C. contact with the flow,
A light liquid is taken out from the top of the column and a heavy liquid is taken out from the bottom of the column.The light liquid is reduced to a pressure of 90 atm in an impurity separation tank and separated into a light purified liquid and a heavy impurity liquid.The heavy impurity liquid is taken out at the bottom of the packed column. The entire amount was returned to a site 1.5 m from the site.
又、該軽質精製液は溶解溶剤分離層で圧力
30atmに減圧し、溶解溶剤と濃縮エチルアルコー
ルに相分離し、該濃縮エチルアルコールの90％を
該充填塔の上部に循環した。 In addition, the light purified liquid is subjected to pressure in the dissolving solvent separation layer.
The pressure was reduced to 30 atm, the dissolving solvent and concentrated ethyl alcohol were phase-separated, and 90% of the concentrated ethyl alcohol was circulated to the upper part of the packed column.
そして、全体が定常になるまで運転し、その結
果原料エチルアルコールの99.0wt％が回収され、
その中の水及び高沸点不純物の濃度は各々5.1wt
％、98ppmであつた。 Then, the operation was continued until the whole became steady, and as a result, 99.0wt% of the raw material ethyl alcohol was recovered.
The concentration of water and high boiling point impurities in it is 5.1wt each.
%, 98ppm.
比較例 １
実施例１において、重質不純物液及び濃縮エチ
ルアルコールを充填塔に戻さずに運転したとこ
ろ、原料エチルアルコールの90.0wt％しか回収さ
れなかつた。水及び高沸点不純物の濃度は各々
10wt％、1000ppmであつた。Comparative Example 1 In Example 1, when the heavy impurity liquid and concentrated ethyl alcohol were operated without being returned to the packed column, only 90.0 wt% of the raw material ethyl alcohol was recovered. The concentrations of water and high boiling point impurities are each
It was 10wt% and 1000ppm.
比較例 ２
実施例１において、重質不純物液のみを充填塔
に戻さずに運転したところ、原料エチルアルコー
ルの97.0wt％が回収されたが、水及び高沸点不純
物の濃度は各々9wt％、800ppmであつた。Comparative Example 2 In Example 1, when only the heavy impurity liquid was operated without returning it to the packed column, 97.0 wt% of the raw material ethyl alcohol was recovered, but the concentrations of water and high boiling point impurities were 9 wt% and 800 ppm, respectively. It was hot.
本発明は、以上詳記したようにアルコール、
水、高沸点不純物の混合物を、臨界付近の溶解溶
剤を使用し常温付近で圧力を３段階に制御して、
これらの混合物を分離するものであり、分離速度
が早く装置のコンパクト化が可能となるととも
に、熱的負荷が軽減されて省エネルギー効果を生
ずるものである。
As detailed above, the present invention provides alcohol,
A mixture of water and high-boiling point impurities is controlled at three levels of pressure at room temperature using a near-critical dissolving solvent.
These mixtures are separated, and the separation speed is fast, making it possible to make the device more compact, and the thermal load is reduced, resulting in an energy-saving effect.
第１図は、本発明を実施するためのフローシー
トである。
FIG. 1 is a flow sheet for implementing the present invention.
Claims (1)
体溶質と水との原料混合物を向流接触抽出装置の
上部より供給し、又臨界温度が該アルコールの沸
点より低い溶剤を該向流接触抽出装置の下部より
供給し、該原料混合物と該溶剤を、該溶剤を超臨
界状態又は擬臨界状態になるような条件下で向流
接触させ、該向流接触抽出装置の上部より軽液
を、下部より重液を取り出し、次に、該軽液は実
質的に高沸点不純物が相分離するに必要な圧力ま
で減圧後、不純物分離槽に導入し重質不純物液と
軽質精製液に分離し、該重質不純物液を前記向流
接触抽出装置の原料混合物供給部分と溶剤供給部
分との間に導入するとともに、該軽質精製液を溶
剤分離槽に導入し、溶解溶剤と濃縮アルコールが
相分離するに必要な圧力まで減圧後、該濃縮アル
コールの一部を前記向流接触抽出装置の原料混合
物供給部分より上部に導入することを特徴とする
アルコール濃縮精製法。1. A raw material mixture of an organic liquid solute consisting of alcohol and high-boiling point impurities and water is supplied from the upper part of the countercurrent catalytic extraction apparatus, and a solvent whose critical temperature is lower than the boiling point of the alcohol is supplied from the lower part of the countercurrent catalytic extraction apparatus. The raw material mixture and the solvent are brought into countercurrent contact under conditions that bring the solvent into a supercritical or quasi-critical state, and the light liquid is supplied from the upper part of the countercurrent contact extraction apparatus and the heavy liquid is supplied from the lower part. Next, the light liquid is depressurized to the pressure required to substantially phase-separate high-boiling point impurities, and then introduced into an impurity separation tank where it is separated into a heavy impurity liquid and a light purified liquid, and the heavy impurities are separated. The liquid is introduced between the raw material mixture supply part and the solvent supply part of the countercurrent contact extraction device, and the light purified liquid is introduced into the solvent separation tank, and the pressure necessary for phase separation of the dissolved solvent and concentrated alcohol is applied. 1. A method for concentrating and purifying alcohol, which comprises introducing a portion of the concentrated alcohol into an upper part of the countercurrent catalytic extraction device from the raw material mixture supply section after the pressure is reduced to .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60275995A JPS62135440A (en) | 1985-12-10 | 1985-12-10 | Method for concentrating and purifying alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60275995A JPS62135440A (en) | 1985-12-10 | 1985-12-10 | Method for concentrating and purifying alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62135440A JPS62135440A (en) | 1987-06-18 |
| JPH0578535B2 true JPH0578535B2 (en) | 1993-10-29 |
Family
ID=17563302
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60275995A Granted JPS62135440A (en) | 1985-12-10 | 1985-12-10 | Method for concentrating and purifying alcohol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62135440A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3850772T2 (en) * | 1987-07-24 | 1994-11-03 | Japan As Represented By Minist | Experience in concentrating and cleaning alcohol. |
| US5250271A (en) * | 1987-07-24 | 1993-10-05 | Minister Of International Trade & Industry | Apparatus to concentrate and purify alcohol |
| JPS6430592A (en) * | 1987-07-24 | 1989-02-01 | Tsusho Sangyo Daijin | Concentration and purification of alcohol |
-
1985
- 1985-12-10 JP JP60275995A patent/JPS62135440A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62135440A (en) | 1987-06-18 |
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