CN106431836B - A kind of technique of extracting rectifying and flash distillation integrated separation alcohol-water object system - Google Patents
A kind of technique of extracting rectifying and flash distillation integrated separation alcohol-water object system Download PDFInfo
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- CN106431836B CN106431836B CN201610829622.4A CN201610829622A CN106431836B CN 106431836 B CN106431836 B CN 106431836B CN 201610829622 A CN201610829622 A CN 201610829622A CN 106431836 B CN106431836 B CN 106431836B
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- C—CHEMISTRY; METALLURGY
- 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
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- C—CHEMISTRY; METALLURGY
- 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
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- C—CHEMISTRY; METALLURGY
- 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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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention is a kind of extracting rectifying and the technique for flashing integrated separation alcohol-water object system, which is extractant using ionic liquid, and ethyl alcohol can be improved to the relative volatility of water, improve separative efficiency, obtain alcohol product.The ionic liquid is 1- ethyl-3-methylimidazole tetrafluoroborate and 1- ethyl-3-methylimidazole dicyan amine salt.The ion liquid abstraction agent that the present invention uses can improve the relative volatility of ethyl alcohol in ethanol-water system, reduce solvent ratio.Obtain the ethyl alcohol that purity is greater than 99.9%.The present invention forms the process flow can be recycled of the ionic liquid of steady and continuous using the process flow of extracting rectifying and flash distillation integrated separation alcohol-water.
Description
[technical field]
The invention belongs to chemical separating purification arts, and in particular to a kind of extracting rectifying and flash separation alcohol-water object system
Technique.
[background technique]
In chemical industry and pharmaceutical industry, ethyl alcohol is important solvent and raw material, and demand is continuously increased.It returns in the industrial production
It receives and utilizes high purity ethanol, this extremely has economic significance for enterprise.Since ethyl alcohol and water will form azeotropic mixture, azeotropic temperature is
It 78.15 DEG C, is difficult to efficiently separate it using conventional distillation method.In recent years, since ionic liquid has extremely low steaming
The excellent property such as vapour pressure, low melting point, thermal stability, nontoxic, non-corrosive, designability, for ionic liquid as extraction
The extracting rectifying of agent expands research and practice.As the type of ionic liquid is more and more, select in entire production process
Advantageous ionic liquid can solve the problems such as energy conservation, environmental pollution, equipment investment.
Patent (CN103073388A) discloses a kind of composite extractant separating alcohol-water with ionic liquid and inorganic salts
Method, but the Solvent quantity of this method is big, flows back bigger, energy consumption is higher, and because using inorganic salts, has to process units
Corrosivity.
Patent (CN103435445A) discloses a kind of with ionic liquid or the double solvents of ionic liquid and organic solvent
For the method for extractant separating alcohol-water object system, energy consumption and production cost are reduced, and obtained high purity ethanol, yield
Greater than 99.0%.Patent (CN103601618A) is related to a kind of method of separation of extractive distillation ethanol-water azeotropic object, and this method is adopted
Spent glycol and chlorination 1- ethyl-3-methylimidazole are that mixed solvent carries out batch extracting rectified operation, Application Example knot
Fruit: alcohol product purity is up to 99.5%.
For the extracting rectifying process using ionic liquid as extractant, the selection of ionic liquid is crucial.It is above-mentioned existing
Isolation technics present in defect and deficiency be: have ignored the properties such as viscosity, the thermal stability of ionic liquid to production process
Influence；The cost of separation process is relatively high；And product quality is affected to a certain extent；Process flow is complicated.With tradition
Organic solvent extraction separation process compare, the separation of ionic liquid and water or organic matter only need to using simple distillation without
Complicated distillation process, and ionic liquid can be recycled, almost free of losses.
The green high-efficient isolation technics of exploitation ethanol-water mixture is of great significance, related separating alcohol-water mixture
Article and patent in there is not yet publish with ionic liquid 1- ethyl-3-methylimidazole tetrafluoroborate and 1- ethyl-
The technique that 3- methylimidazole dicyan amine salt carries out extracting rectifying as extractant and flashes integrated separation alcohol-water object system.This hair
The ionic liquid of bright use is advantageous to entire production process due to liquid condition, viscosity are smaller under room temperature.
[summary of the invention]
The object of the present invention is to provide a kind of extracting rectifying and flash distillation integrated separation alcohol-water object system device and method,
After isolating ethyl alcohol using ion liquid abstraction rectifying to alcohol-water object system, by extractive distillation column tower reactor containing extractant and
Aqueous mixtures carry out vacuum flashing, reduce the energy consumption during production operation, and the equipment investment that this method uses is few, operates item
Part is easily controllable, and obtained purity of alcohol is higher.
The present invention is to be realized by the following technical programs.
A kind of method of extracting rectifying and flash separation alcohol-water object system, this method are implemented to connect using extracting rectifying device
Continuous distillation operation, the extracting rectifying device include extractive distillation column, and extractive distillation column tower bottom connects reboiler, tower top connection
Condenser, condenser connect receiving tank later, and ionic liquid recycles flash tank, it is characterised in that including following procedure: alcohol-water
Mixture is entered in extractive distillation column by tower middle and lower part, and extractant is ion liquid solvent, is entered in tower by tower top；It is extracting
In rectifying tower, overhead stream is after condenser condenses, and a part of liquid returns to reflux in tower, and a part of liquid is as high-purity
Alcohol product extraction；After reboiler boils again, a part returns in tower tower base stream, and a part enters flash tank；
The separation that the mixture of extractant and water is realized in flash tank, obtains the water of high-purity in flash tank tower top, passes through
It is directly produced after condensation；The ionic liquid that mass fraction is 0.2-0.4% is obtained in flash tank bottom, is adopted by flash tank bottom
Out, it is recycled back to extractive distillation column；Wherein the extractant uses ionic liquid, specifically includes 1- ethyl-3-methylimidazole tetrafluoro
Borate and 1- ethyl-3-methylimidazole dicyan amine salt.
The extractive distillation column internal diameter is Φ 400-500mm, and the number of plates is 35-45 block, operating pressure 1atm, ethyl alcohol-
Aqueous mixtures are fed in 29-35 block column plate, and extractant is fed in 3-6 block column plate, and tower top temperature is 77.8-80 DEG C, tower bottom
Temperature is 95-120 DEG C, and the flash tank uses decompression operation, and operating pressure is 0.1-0.2atm absolute pressure, temperature 108-112
℃。
The ion liquid solvent is preferably 1- ethyl-3-methylimidazole tetrafluoroborate and 1- ethyl -3- methyl miaow
Azoles dicyan amine salt.
Two kinds of ingredient arbitrary proportions in the ethanol-water mixture material.
Two kinds of composition qualities are than being preferably ethyl alcohol: water=0.25-1 in the alcohol-water object system.
The invention has the benefit that the ionic liquid can improve the relative volatility of the ethyl alcohol in alcohol-water object system,
Reduce solvent ratio.When the mass fraction of ionic liquid reaches 17%-50%, the azeotropic point of alcohol-water can be made to disappear.By answering
Known with embodiment, when the mass ratio of ionic liquid and alcohol-water object system is 1:3, extracting rectifying can be carried out well, obtained
Ethyl alcohol greater than 99.5%.For alcohol-water object system, ionic liquid 1- ethyl-3-methylimidazole tetrafluoroborate and 1- ethyl-
3- methylimidazole dicyan amine salt and water have preferable intersolubility, can be acted on by chemical affinity, hydrogen bond force etc. and water, improve second
Alcohol uses ionic liquid using simple be distilled to recover, drop so that ionic liquid additional amount is less for the relative volatility of water
The low energy consumption and investment of separation process.
[Detailed description of the invention]
A kind of Fig. 1: flow diagram of extracting rectifying and flash distillation integrated separation alcohol-water object system of the present invention.
Wherein, T1-extractive distillation column；T2-flash tank；F1-extractive distillation column material inlet；F2-extractant feed mouth；
B1-extractive distillation column tower bottom discharge port；B2-cycling extraction agent outlet；D1-alcohol product outlet；D2-water out；1-reboiler；
2,3-condensers.
[specific embodiment]
Embodiment 1: the internal diameter of extractive distillation column is Φ 500mm, number of theoretical plate 40, operating pressure 101.325kPa,
It is 95 DEG C that operating reflux ratio, which is 1.8, tower top temperature is controlled in 77 DEG C, bottom temperature, 25 DEG C of ionic liquid 1- ethyl -3- methyl
Tetrafluoroborate is entered by the 6th block of plate, 25 DEG C of mass fraction be -80% aqueous mixtures of 20% ethyl alcohol by the 34th block of plate with
The flow of 1000kg/h enters, and the mass ratio for controlling ionic liquid and alcohol-water is 1:3, tower top upflowing vapor by condenser into
Row condensation.For phegma by the overhead reflux of extractive distillation column, Produced Liquid is the ethyl alcohol of mass fraction 99.5%.Extractive distillation column
Tower reactor is the mixture of 1- ethyl-3-methylimidazole tetrafluoroborate and water, and phegma returns after reboiler boils again in 126 DEG C
Stream, remaining enters flash tank, and operating pressure 0.12atm, the control of flash tank temperature are at 112 DEG C.The bottom of flash tank is quality
Score is the ionic liquid of 0.4% water.
Embodiment 2: the internal diameter of extractive distillation column is Φ 400mm, number of theoretical plate 35, operating pressure 101.325kPa,
It is 109 DEG C that operating reflux ratio, which is 2.1, tower top temperature is controlled in 77.8 DEG C, bottom temperature, 25 DEG C of ionic liquid 1- ethyl -3-
Methyl imidazolium tetrafluoroborate is entered by the 6th block of plate, and 25 DEG C of mass fraction is -70% aqueous mixtures of 30% ethyl alcohol by the 29th piece
Plate is entered with the flow of 1000kg/h, and the mass ratio for controlling ionic liquid and alcohol-water is 1:2.5, and tower top upflowing vapor is by cold
Condenser is condensed.For phegma by the overhead reflux of extractive distillation column, Produced Liquid is the ethyl alcohol of mass fraction 99.6%.Extraction essence
The tower reactor for evaporating tower is the mixture of 1- ethyl-3-methylimidazole tetrafluoroborate and water, and phegma is boiled through reboiler in 120 DEG C again
After flow back, remaining enter flash tank, operating pressure 0.15atm, flash tank temperature control at 109 DEG C.The bottom of flash tank is
Mass fraction is the ionic liquid of 0.3% water.
Embodiment 3: the internal diameter of extractive distillation column is Φ 400mm, number of theoretical plate 35, operating pressure 101.325kPa,
It is 107 DEG C that operating reflux ratio, which is 2.6, tower top temperature is controlled in 77.8 DEG C, bottom temperature, 25 DEG C of ionic liquid 1- ethyl -3-
Methyl imidazolium tetrafluoroborate is entered by the 6th block of plate, and 25 DEG C of mass fraction is -60% aqueous mixtures of 40% ethyl alcohol by the 30th piece
Plate is entered with the flow of 1000kg/h, and the mass ratio for controlling ionic liquid and alcohol-water is 1:2, and tower top upflowing vapor is by condensing
Device is condensed.For phegma by the overhead reflux of extractive distillation column, Produced Liquid is the ethyl alcohol of mass fraction 99.6%.Extracting rectifying
The tower reactor of tower is the mixture of 1- ethyl-3-methylimidazole tetrafluoroborate and water, and phegma is through reboiler after 120 DEG C boil again
Reflux, remaining flash tank, operating pressure 0.18atm, the control of flash tank temperature are at 110 DEG C.The bottom of flash tank is quality point
Number is the ionic liquid of 0.3% water.
Embodiment 4: the internal diameter of extractive distillation column is Φ 500mm, number of theoretical plate 40, operating pressure 101.325kPa,
It is 119 DEG C that operating reflux ratio, which is 1.2, tower top temperature is controlled in 78.0 DEG C, bottom temperature, 25 DEG C of ionic liquid 1- ethyl -3-
Methylimidazole dicyan amine salt is entered by the 5th block of plate, and 25 DEG C of mass fraction is -80% aqueous mixtures of 20% ethyl alcohol by the 32nd block of plate
Entered with the flow of 1000kg/h, the mass ratio for controlling ionic liquid and alcohol-water is 1:4, and tower top upflowing vapor is by condenser
It is condensed.For phegma by the overhead reflux of extractive distillation column, Produced Liquid is the ethyl alcohol of mass fraction 99.8%.Extractive distillation column
Tower reactor be 1- ethyl-3-methylimidazole dicyan amine salt and water mixture, phegma after reboiler boils again in 127 DEG C return
Stream, remaining enters flash tank, and operating pressure 0.14atm, the control of flash tank temperature are at 108 DEG C.The bottom of flash tank is quality
Score is the ionic liquid of 0.1% water.
Embodiment 5: the internal diameter of extractive distillation column is Φ 500mm, number of theoretical plate 45, operating pressure 101.325kPa,
Operating reflux ratio is the control of 1.8, tower top temperature at 80 DEG C, and bottom temperature is 112 DEG C, 25 DEG C of ionic liquid 1- ethyl -3- first
Base imidazoles dicyan amine salt is entered by the 3rd block of plate, 25 DEG C of mass fraction be -70% aqueous mixtures of 30% ethyl alcohol by the 31st block of plate with
The flow of 1000kg/h enters, and the mass ratio for controlling ionic liquid and alcohol-water is 1:3, tower top upflowing vapor by condenser into
Row condensation.For phegma by the overhead reflux of extractive distillation column, Produced Liquid is the ethyl alcohol of mass fraction 99.9%.Extractive distillation column
Tower reactor is the mixture of 1- ethyl-3-methylimidazole dicyan amine salt and water, and phegma flows back after reboiler boils again in 126 DEG C,
Remaining enters flash tank, and operating pressure 0.16atm, the control of flash tank temperature are at 120 DEG C.The bottom of flash tank is mass fraction
For the ionic liquid of 0.1% water.
Embodiment 6: the internal diameter of extractive distillation column is Φ 500mm, number of theoretical plate 40, operating pressure 101.325kPa,
It is 120 DEG C that operating reflux ratio, which is 2.0, tower top temperature is controlled in 77.9 DEG C, bottom temperature, 25 DEG C of ionic liquid 1- ethyl -3-
Methylimidazole dicyan amine salt is entered by the 4th block of plate, and 25 DEG C of mass fraction is -60% aqueous mixtures of 40% ethyl alcohol by the 35th block of plate
Entered with the flow of 1000kg/h, the mass ratio for controlling ionic liquid and alcohol-water is 1:3, and tower top upflowing vapor is by condenser
It is condensed.For phegma by the overhead reflux of extractive distillation column, Produced Liquid is the ethyl alcohol of mass fraction 99.9%.Extractive distillation column
Tower reactor be 1- ethyl-3-methylimidazole dicyan amine salt and water mixture, phegma after reboiler boils again in 126 DEG C return
Stream, remaining enters flash tank, and operating pressure 0.2atm, the control of flash tank temperature are at 112 DEG C.The bottom of steaming pot is mass fraction
For the ionic liquid of 0.2% water.
Claims (3)
1. the technique of a kind of extracting rectifying and flash distillation integrated separation alcohol-water object system, it is characterised in that the technique includes following
Step:
(1) ethanol-water mixture is entered in extractive distillation column by tower middle and lower part, and extractant is ion liquid solvent, by tower top
Into in tower；In extractive distillation column tower, overhead stream is after condenser condenses, a part of liquid return reflux in tower, and one
Liquid separation body is produced with purity for the alcohol product of 99.5-99.9wt%；Tower base stream, after reboiler boils again, a part is returned
In tower, a part enters flash tank；
(2) separation that the mixture of extractant and water is realized in flash tank, obtaining purity in flash tank tower top is 99.6-
The water of 99.9wt%, directly produces after condensing；The ionic liquid that mass fraction is 0.2-0.4% is obtained in flash tank bottom,
It is produced by flash tank bottom, is recycled back to extractive distillation column；
Wherein the extractant uses ionic liquid, specifically includes 1- ethyl-3-methylimidazole tetrafluoroborate and 1- ethyl -3-
Methylimidazole dicyan amine salt.
2. the technique of a kind of extracting rectifying according to claim 1 and flash distillation integrated separation alcohol-water object system, feature exist
It is Φ 400-500mm in the extractive distillation column internal diameter, the number of plates is 35-45 block, operating pressure 1atm, alcohol-water mixing
Object is fed in 29-35 block column plate, and extractant is fed in 3-6 block column plate, and tower top temperature is 77.8-80 DEG C, and column bottom temperature is
95-120 DEG C, the flash tank uses decompression operation, and operating pressure is 0.1-0.2atm absolute pressure, and temperature is 108-112 DEG C.
3. the technique of a kind of extracting rectifying according to claim 1 and flash distillation integrated separation alcohol-water object system, feature exist
It is any than charging in the ethanol-water mixture, extractant and ethanol-water mixture charge-mass ratio are 0.25-1.
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| 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 |
| CN112795397B (en) * | 2019-11-14 | 2023-02-07 | 中国石油天然气股份有限公司 | Composite solvent for separating cyclane and aromatic hydrocarbon from naphtha |
| CN113248378A (en) * | 2021-05-31 | 2021-08-13 | 鹤壁腾飞清洁能源有限公司 | System for extracting and rectifying methyl acetate and ethanol and using method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3152968A (en) * | 1958-06-27 | 1964-10-13 | Celanese Corp | Recovery of methylene chloride from a mixed solvent system by extractive distillation with water |
| CN103073388A (en) * | 2013-01-28 | 2013-05-01 | 北京化工大学 | Method for separating alcohol from water through ion liquid extraction and rectification |
| CN103435445A (en) * | 2013-08-20 | 2013-12-11 | 天津科林泰克科技有限公司 | Method for separating mixture of ethanol alcohol and water |
| CN103601618A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating alcohol-water azeotropic mixture |
-
2016
- 2016-09-19 CN CN201610829622.4A patent/CN106431836B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3152968A (en) * | 1958-06-27 | 1964-10-13 | Celanese Corp | Recovery of methylene chloride from a mixed solvent system by extractive distillation with water |
| CN103073388A (en) * | 2013-01-28 | 2013-05-01 | 北京化工大学 | Method for separating alcohol from water through ion liquid extraction and rectification |
| CN103435445A (en) * | 2013-08-20 | 2013-12-11 | 天津科林泰克科技有限公司 | Method for separating mixture of ethanol alcohol and water |
| CN103601618A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating alcohol-water azeotropic mixture |
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