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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 PDF

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Publication number
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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water
ionic liquid
tower
alcohol
ethanol
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CN106431836A (en
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朱兆友
李英生
贾慧
刘薇
王英龙
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Qingdao University of Science and Technology
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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
    • 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
    • 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
    • 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)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (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

A kind of technique of extracting rectifying and flash distillation integrated separation alcohol-water object system
[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)

1.一种萃取精馏与闪蒸耦合分离乙醇-水物系的工艺，其特征在于所述工艺包括以下步骤：1. a technique for extractive rectification and flash distillation coupling separation ethanol-water system, is characterized in that described technique comprises the following steps: (1)乙醇-水混合物由塔中下部进入萃取精馏塔内，萃取剂为离子液体溶剂，由塔上部进入塔内；在萃取精馏塔塔内，塔顶物流经冷凝器冷凝后，一部分液体返回塔内回流，一部分液体以纯度为99.5-99.9wt％的乙醇产品采出；塔底物流，经再沸器再沸后，一部分返回塔内，一部分 进入闪蒸罐；(1) ethanol-water mixture enters in the extractive rectification tower from the middle and lower part of the tower, and the extractant is an ionic liquid solvent, and enters into the tower from the upper part of the tower; The liquid is returned to the tower for reflux, and a part of the liquid is extracted as an ethanol product with a purity of 99.5-99.9wt%; the bottom stream of the tower, after being reboiled by the reboiler, is partially returned to the tower, and a part enters the flash tank; (2)在闪蒸罐内实现萃取剂和水的混合物的分离，在闪蒸罐塔顶得到纯度为99.6-99.9wt％的水，经冷凝后直接采出；在闪蒸罐底部得到质量分数为0.2-0.4％的离子液体，由闪蒸罐底部采出， 循环回萃取精馏塔；(2) realize the separation of the mixture of extractant and water in the flash tank, obtain water with a purity of 99.6-99.9wt% at the top of the flash tank, and directly extract it after condensation; obtain the mass fraction at the bottom of the flash tank It is 0.2-0.4% ionic liquid, which is extracted from the bottom of the flash tank and recycled back to the extractive distillation column; 其中所述萃取剂采用离子液体，具体包括1-乙基-3-甲基咪唑四氟硼酸盐和1-乙基-3-甲基咪唑二氰胺盐。Wherein, the extracting agent adopts ionic liquid, and specifically includes 1-ethyl-3-methylimidazolium tetrafluoroborate and 1-ethyl-3-methylimidazolium dicyanamide salt. 2.根据权利要求1所述的一种萃取精馏与闪蒸耦合分离乙醇-水物系的工艺，其特征在于所述萃取精馏塔内径为Φ400-500mm，塔板数为35-45块，操作压力为1atm，乙醇-水混合物在第29-35块塔板进料，萃取剂在第3-6块塔板进料，塔顶温度为77.8-80℃，塔底温度为95-120℃，所述闪蒸罐采用减压操作，操作压力为0.1-0.2atm绝压，温度为108-112℃。2. the technique of a kind of extractive distillation and flash distillation coupling separation ethanol-water system according to claim 1, it is characterized in that described extractive distillation column inner diameter is Φ400-500mm, and the number of plates is 35-45 pieces , the operating pressure is 1atm, the ethanol-water mixture is fed on the 29th-35th trays, the extractant is fed on the 3rd-6th trays, the temperature at the top of the column is 77.8-80 °C, and the temperature at the bottom of the column is 95-120 ℃, the flash tank adopts decompression operation, the operating pressure is 0.1-0.2 atm absolute pressure, and the temperature is 108-112 ℃. 3.根据权利要求1所述的一种萃取精馏与闪蒸耦合分离乙醇-水物系的工艺，其特征在于所述乙醇-水混合物为任意比进料，萃取剂与乙醇-水混合物进料质量比为0.25-1。3. the technique of a kind of extractive rectification according to claim 1 and flash distillation coupling separation ethanol-water system, it is characterized in that described ethanol-water mixture is any ratio feed, and extractant and ethanol-water mixture are fed into. The material-to-mass ratio is 0.25-1.
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CN110028388B (en) * 2019-05-23 2023-01-17 山东科技大学 A method for extracting and rectifying separation of tetrafluoropropanol and water azeotrope with hydrophilic ionic liquid
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 A kind of system of extracting and rectifying methyl acetate and ethanol and using method thereof

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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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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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