CN103601618A - Method for extracting, rectifying and separating alcohol-water azeotropic mixture - Google Patents
Method for extracting, rectifying and separating alcohol-water azeotropic mixture Download PDFInfo
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- CN103601618A CN103601618A CN201310591239.6A CN201310591239A CN103601618A CN 103601618 A CN103601618 A CN 103601618A CN 201310591239 A CN201310591239 A CN 201310591239A CN 103601618 A CN103601618 A CN 103601618A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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Abstract
The invention discloses a method for extracting, rectifying and separating an alcohol-water azeotropic mixture. The method adopts chlorinated 1-ethyl-3-methyl imidazole liquor of glycol as an extracting agent to carry out batch extracting rectifying operation under a normal pressure and comprises the following operation processes: introducing the extracting agent into an extracting and rectifying tower to carry out total-reflux operation to produce an alcohol product, alcohol-water transition section fraction, water and glycol-water transition section fraction, wherein raffinate in a parked heating kettle is used as the extracting agent for cycle use. The method disclosed by the invention has the advantage that the ion liquid liquor of the glycol is adopted as the extracting agent to separate the alcohol-water azeotropic mixture, the alcohol product obtained by separating is high in purity, single-tower operation is adopted, operation process is flexible and easy to control, and device investment is little.
Description
Technical field
The present invention relates to a kind of method of separation of extractive distillation ethanol-water azeotropic mixture, particularly relate to a kind of method of take the separation of extractive distillation ethanol-water azeotropic mixture that ionic liquid mixed solvent is extraction agent, belong to the isolation technique of ethanol-water azeotropic mixture.
Background technology
Extracting rectifying is a kind of common method of Separation of Mixtures with Same Boiling Point, generally adopts molecule liquid as extraction agent.Except molecule liquid, people start to adopt ionic liquid as the extraction agent of extracting rectifying in recent years.Ionic liquid refers to that fusing point is lower than the compounds being comprised of organic cation and inorganic anion or organic anion of 100 ℃.For many azeotropic systems, ion liquid abstraction agent has than the better separating effect of molecule liquid extractant, but ionic liquid price is high, and a lot of ion liquid abstraction agent fusing point is higher efficiently, be solid at normal temperatures, during therefore separately as extraction agent, use very inconvenient.If ionic liquid and molecule liquid mixing are formed to mixed solvent as extraction agent, will overcome its shortcoming separately.Ethanol is a kind of important industrial chemicals and organic solvent, is easy to form difficult separated azeotropic mixture with water.In a lot of chemical processes, relate to the separation of ethanol-water azeotropic mixture, the green high-efficient isolation technique of therefore developing ethanol-water azeotropic mixture is significant.More about article and the patent of separating ethanol-water azeotropic mixture, there is not yet publish with molecule liquid and ionic liquid mixed solvent, make the extracting rectifying of the ethanol-water azeotropic system of extraction agent.
Summary of the invention
The present invention aims to provide a kind of method of separation of extractive distillation ethanol-water azeotropic mixture.The facility investment that the method adopts is few, and operational condition is easy to control, and the purity of alcohol obtaining is high.
The present invention is realized by the following technical programs.A kind of method of separation of extractive distillation ethanol-water azeotropic mixture, the method adopts extracting rectifying device to implement batch fractionating operation, described extracting rectifying device comprises extractive distillation column, at the bottom of extractive distillation column tower, connect heating kettle, extracting rectifying column overhead connects condenser, after condenser, connect receiving tank, extractive distillation column tower body connects extraction agent basin, it is characterized in that comprising following process: adopting the ethylene glycol solution of the chlorination 1-ethyl-3-methylimidazole [emim] [cl] that mass content is 10-80% is extraction agent, extractive distillation column operates with following condition: under normal pressure, when the rising steam rising that still to be heated produces adds entrance to the extraction agent of extractive distillation column, by entering the extraction agent of extractive distillation column and the volume ratio of extracting rectifying tower top liquid return amount for (0.5-5): 1, the extraction agent that by temperature is 25-80 ℃ is introduced extraction agent rectifying tower by extraction agent basin, when extracting rectifying tower top temperature is 78.5-80 ℃, with reflux ratio (1-5): 1 reaches more than 99% alcohol product by extractive distillation column overhead extraction containing ethanol massfraction, when extracting rectifying tower top temperature is during lower than 78.2 ℃, stop adding extraction agent, with reflux ratio (1-5): 1 by extractive distillation column overhead extraction alcohol-water transition section cut, when extractive distillation column tower top temperature reaches 100 ℃, with reflux ratio (1-4): 1 dehydration, when extractive distillation column tower top temperature surpasses 105 ℃, with reflux ratio (1-6): 1 by extractive distillation column overhead extraction ethylene glycol-water transition section cut, when in extractive distillation column overhead product, water-content is less than 0.1%, stop cooling, still residual liquid infusion pump is squeezed into extraction agent basin and is recycled as extraction agent.
Advantage of the present invention, the solution of the ionic liquid chlorination 1-ethyl-3-methylimidazole of employing molecule liquid glycol, as extraction agent separating ethanol-water azeotropic mixture, has been realized the high efficiency separation of second alcohol and water.With this extraction agent separating ethanol-water azeotropic mixture with take ethylene glycol and compare as extraction agent separating ethanol-water azeotropic mixture, separation efficiency is high; With with pure ionic liquid chlorination 1-ethyl-3-methylimidazole separating ethanol-water azeotropic mixture, compare, separation costs is low, and solved pure ionic liquid because of fusing point compared with the high problem that is easy to cause Crystallization Plugging pipeline with and fusing after the larger problem of viscosity; The alcohol product purity that separation obtains is high, adopts single tower operation, and operating process is easy to control flexibly, and facility investment is few.
Accompanying drawing explanation
Fig. 1 is device and the schematic flow sheet that the present invention adopts.
In figure: 1-extraction agent header tank, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-alcohol product tank, 6-alcohol-water interim fraction receiving tank, 7-water receiving tank, 8-ethylene glycol-water interim fraction receiving tank, 9-infusion pump.
Embodiment
The idiographic flow of Fig. 1: ethanol-water azeotropic mixture is joined in heating kettle 3, thermal source in the low-temperature receiver of open cold condenser and heating kettle, when the steam that rises in extractive distillation column arrival extraction agent adds entrance, start to add extraction agent, extraction agent is introduced to extractive distillation column from header tank 1 through the extraction agent charging opening of extractive distillation column 2, total reflux 15 minutes, when reaching 99%, tower top ethanol mass fraction starts discharging when above, distillate material and enter alcohol product tank 5, the ethanol mass fraction distillating when tower top is lower than 99% time, stop adding extraction agent, distillate alcohol-water transition section, enter alcohol-water interim fraction receiving tank 6, when in overhead product, the mass fraction of water is greater than 99%, distillate material and enter water receiving tank 7, in overhead product, the mass fraction of water is lower than 97.5% time, extraction water-ethylene glycol transition section cut, enter water-ethylene glycol receiving tank 8, until the mass fraction of water is less than 0.1% in overhead product, stop.In heating kettle, be now the mixture of ionic liquid and ethylene glycol, be introduced in header tank and recycle.Mixture in two transition sections when distilling, next batch is put in heating kettle.
Embodiment mono-
Adopt the diameter of extractive distillation column to be φ 40mm, in-built
net ring filler, bed stuffing height is 1.15m, extraction agent import is apart from tower top 0.15m place.At heating kettle, drop into 297.4g ethanol-water mixture (alcohol 95 % wherein, water 5%, be mass percent), testing selected mixed extractant is the mixture (ionic liquid massfraction 14%) of chlorination 1-ethyl-3-methylimidazole ([EMIM] Cl) and ethylene glycol, open heating kettle thermal source and condenser low-temperature receiver, extractive distillation column brings into operation, when in extractive distillation column, rising steam rising adds entrance to extraction agent, extraction agent is added in extractive distillation column by extraction agent import, control extraction agent and add speed 258ml/h, total reflux operation 15 minutes, when extracting rectifying tower top temperature is 78.5-79.5 ℃, when ethanol content is 99.6% in overhead product, start discharging, reflux ratio is 1:1, discharging speed is 85ml/h, in this process, be total to such an extent that ethanol qualified product are 215g.When extracting rectifying tower top temperature stops adding extraction agent during lower than 78.2 ℃, extraction alcohol-water interim fraction, reflux ratio is 1:1, when tower top temperature is 100 ℃, recovered water, when in overhead product, the mass fraction of water is less than 98.5%, with reflux ratio 3:1 extraction water-ethylene glycol interim fraction, until the mass fraction of water is less than 0.1% in overhead product, stop.After parking, the material in heating kettle is ethylene glycol and ionic liquid mixture, is introduced into extraction agent header tank, as next batch extracting rectifying extraction agent, recycles.
Embodiment bis-
Adopt the extracting rectifying device identical with embodiment mono-, carry out following operation: at heating kettle, drop into 298.2g ethanol-water mixture (alcohol 95 % wherein, water 5%, be mass percent), testing selected mixed extractant is the mixture (ionic liquid massfraction 25%) of chlorination 1-ethyl-3-methylimidazole ([EMIM] Cl) and ethylene glycol, open heating kettle thermal source and condenser low-temperature receiver, extractive distillation column brings into operation, when in extractive distillation column, rising steam rising adds entrance to extraction agent, extraction agent is added in extractive distillation column by extraction agent import, control extraction agent and add speed 230ml/h, total reflux operation 15 minutes, when extracting rectifying tower top temperature is 78.5-79.5 ℃, when ethanol content is 99.5% in cut, start discharging, reflux ratio is 1:1, discharging speed is 85ml/h, in this process, be total to such an extent that ethanol qualified product are 226g.When extracting rectifying tower top temperature stops adding extraction agent during lower than 78 ℃, extraction alcohol-water interim fraction, reflux ratio is 1:1, when tower top temperature is 100 ℃, recovered water, when in overhead product, the mass fraction of water is less than 97.5%, with reflux ratio 4:1 extraction water-ethylene glycol interim fraction, until the mass fraction of water is less than 0.1% in overhead product, stop.After parking, the material in heating kettle is ethylene glycol and ionic liquid mixture, is introduced into extraction agent header tank, as next batch extracting rectifying extraction agent, recycles.
Embodiment tri-
Adopt the extracting rectifying device identical with embodiment mono-, carry out following operation: at heating kettle, drop into 300.1 ethanol-water mixtures (alcohol 95 % wherein, water 5%, be mass percent), testing selected mixed extractant is the mixture (ionic liquid massfraction 30%) of chlorination 1-ethyl-3-methylimidazole ([EMIM] Cl) and ethylene glycol, open heating kettle thermal source and condenser low-temperature receiver, extractive distillation column brings into operation, when in extractive distillation column, rising steam rising adds entrance to extraction agent, extraction agent is added in extractive distillation column by extraction agent import, control extraction agent and add speed 200ml/h, total reflux operation 15 minutes, when extracting rectifying tower top temperature is 78.5-79.5 ℃, when ethanol content is 99.5% in cut, start discharging, reflux ratio is 1:1, discharging speed is 90ml/h, in this process, be total to such an extent that ethanol qualified product are 235g.When extracting rectifying tower top temperature stops adding extraction agent during lower than 78.2 ℃, extraction alcohol-water interim fraction, reflux ratio is 1:1, when tower top temperature is 100 ℃, recovered water, when in overhead product, the mass fraction of water is less than 97.5%, with reflux ratio 3:1 extraction water-ethylene glycol interim fraction, until the mass fraction of water is less than 0.1% in overhead product, stop.After parking, the material in heating kettle is ethylene glycol and ionic liquid mixture, is introduced into extraction agent header tank, as next batch extracting rectifying extraction agent, recycles.
Claims (1)
1. the method for a separation of extractive distillation ethanol-water azeotropic mixture, the method adopts extracting rectifying device to implement batch fractionating operation, described extracting rectifying device comprises extractive distillation column, at the bottom of extractive distillation column tower, connect heating kettle, extracting rectifying column overhead connects condenser, after condenser, connect receiving tank, extractive distillation column tower body connects extraction agent basin, it is characterized in that comprising following process: adopting the ethylene glycol solution of the chlorination 1-ethyl-3-methylimidazole that mass content is 10-80% is extraction agent, extractive distillation column operates with following condition: under normal pressure, when the rising steam rising that still to be heated produces adds entrance to the extraction agent of extractive distillation column, by entering the extraction agent of extractive distillation column and the volume ratio of extracting rectifying tower top liquid return amount for (0.5-5): 1, the extraction agent that by temperature is 25-80 ℃ is introduced extraction agent rectifying tower by extraction agent basin, when extracting rectifying tower top temperature is 78.5-80 ℃, with reflux ratio (1-5): 1 reaches more than 99% alcohol product by extractive distillation column overhead extraction containing ethanol massfraction, when extracting rectifying tower top temperature is during lower than 78.2 ℃, stop adding extraction agent, with reflux ratio (1-5): 1 by extractive distillation column overhead extraction alcohol-water transition section cut, when extractive distillation column tower top temperature reaches 100 ℃, with reflux ratio (1-4): 1 dehydration, when extractive distillation column tower top temperature surpasses 105 ℃, with reflux ratio (1-6): 1 by extractive distillation column overhead extraction ethylene glycol-water transition section cut, when in extractive distillation column overhead product, water-content is less than 0.1%, stop cooling, still residual liquid infusion pump is squeezed into extraction agent basin and is recycled as extraction agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628520A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-propyl formate azeotropic mixture |
| CN106431836A (en) * | 2016-09-19 | 2017-02-22 | 青岛科技大学 | Technology for separating ethyl alcohol-water system by means of extractive distillation and flash coupling |
| CN110028388A (en) * | 2019-05-23 | 2019-07-19 | 山东科技大学 | A method of with hydrophilic ionic-liquid separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
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| CN101254358A (en) * | 2007-12-05 | 2008-09-03 | 天津大学 | Adding salt intermittent extraction rectification separation method of acetonitrile-water azeotropic mixture |
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2013
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| CN101254358A (en) * | 2007-12-05 | 2008-09-03 | 天津大学 | Adding salt intermittent extraction rectification separation method of acetonitrile-water azeotropic mixture |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628520A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-propyl formate azeotropic mixture |
| CN106431836A (en) * | 2016-09-19 | 2017-02-22 | 青岛科技大学 | Technology for separating ethyl alcohol-water system by means of extractive distillation and flash coupling |
| CN106431836B (en) * | 2016-09-19 | 2019-03-29 | 青岛科技大学 | A kind of technique of extracting rectifying and flash distillation integrated separation alcohol-water object system |
| CN110028388A (en) * | 2019-05-23 | 2019-07-19 | 山东科技大学 | A method of with hydrophilic ionic-liquid separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
| CN110028388B (en) * | 2019-05-23 | 2023-01-17 | 山东科技大学 | Method for separating tetrafluoropropanol and water azeotrope by using hydrophilic ionic liquid extraction and rectification |
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Application publication date: 20140226 |