CN105061146A - Batch distillation process for separating isopropanol-acetonitrile azeotrope through mixed extraction agent - Google Patents
Batch distillation process for separating isopropanol-acetonitrile azeotrope through mixed extraction agent Download PDFInfo
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- CN105061146A CN105061146A CN201510418609.5A CN201510418609A CN105061146A CN 105061146 A CN105061146 A CN 105061146A CN 201510418609 A CN201510418609 A CN 201510418609A CN 105061146 A CN105061146 A CN 105061146A
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- acetonitrile
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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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
Abstract
The invention discloses a batch distillation process for separating isopropanol-acetonitrile azeotrope through a mixed extraction agent. The batch distillation process is characterized in that a mixture of ethylene glycol and an ionic liquid is selected to serve as the extraction agent and is added from the upper end of an extraction distillation tower, isopropanol-acetonitrile azeotrope is added to a kettle, the quality of products is controlled by regulating the reflux ratio, and an acetonitrile product, an acetonitrile-isopropanol interim fraction, an isopropanol product and an isopropanol-ethylene glycol interim fraction are sequentially obtained from the top of the tower. The content of the acetonitrile product and the content of the isopropanol product are both higher than 99.5%, and the two interim fractions and the extraction agent at the bottom of the tower can be recovered and used for processing of the next batch of materials. Batch pressure-reduction rectification is adopted, and the batch distillation process has the advantages of simple equipment, few investment, flexible operation, low energy consumption, high product quality and the like and is suitable for medium-scale and small-scale production.
Description
Technical field
The present invention relates to the batch fractionating technique of a kind of mixed extractant separating isopropanol-acetonitrile azeotrope, belong to Virahol-acetonitrile azeotrope extraction and distillation technology.The feature of this technique is that extraction agent is the mixture adding ionic liquid, and operating method for decompression periodical operation, have simple to operate, extraction agent is recyclable, low power consumption and other advantages.
Background technology
Virahol (isopropanol), has another name called dimethylcarbinol, 2-propyl alcohol, also makes IPA in industry, and molecular formula is C
3h
8o, chemical property and ethanol, propyl alcohol are similar, but have the characteristic of secondary alcohol, can dissolve the gas chromatographies such as alkaloid, rubber, shellac, sandarac(h), rosin, frankincense, synthetic resins.In addition, it or the excellent dewaxing medium of bright stock, the extraction agent of Oleum Gossypii semen, frostproofer, water extracter, antifogging agent, have a wide range of applications in medicine, agricultural chemicals, spices, makeup, organic synthesis.Acetonitrile (acetonitrile), has another name called methyl-cyanide, and molecular formula is C
2h
3n, has the special odor being similar to ether, has excellent solvent nature, can dissolve multiple organic and inorganic and gaseous matter.Can be there is the reaction of typical nitrile in acetonitrile, and be used to prepare many typical nitrogenous compounds, is an important organic intermediate.Acetonitrile can be used for the solvent of synthesise vitamins A, cortisone, carbon amine drug and intermediate thereof, also for the manufacture of VITMAIN B1 and amino acid whose active media solvent.Chlorinated solvent can be replaced.In addition for the solvent of the extraction agent of vinyl coating, lipid acid, alcotate, butadiene extraction agent and acrylonitrile synthetic fiber, in textile dyeing, illumination, also has many purposes in spices manufacture and sensitive materials manufacture.But because both exist azeotropic, conventional method cannot obtain two kinds of high-purity materials, thus significantly limit both application, and the technology be therefore separated both exploitation is very necessary.The present invention is intended to for both separation provide a kind of economy, the processing method that easy, separation efficiency is high.
Rectifying is the most frequently used, the most basic separation method of petroleum chemical industry, from rectifying at the beginning of last century, industrialization is used and is started, and had 100 years, distillation technology is also constantly developed, the various technology of periphery also continuous and rectifying combines, and innovates the rectification process made new advances.When living through the energy dilemma eighties in last century, especially after 2008, along with oil price constantly rises, people come to realise raising energy utilization rate, reduce the outlet that energy consumption is only futurity industry, and distillation technology is also like this.It is decompression extracting rectifying that the present invention adopts, in energy consumption, cost of investment, environmental stress, have greater advantage.
Ionic liquid, as the environmentally friendly solvent of one, has the trend of alternative conventional solvent recent years, also becomes the study hotspot of every field, illustrates wide application potential and market outlook.Paper in recent years about ionic liquid becomes progression to increase progressively with patent, and ionic liquid is listed in national strategy development program by the U.S., Europe, Japan especially, company of many transnational groups as: German BASF, German Merck, U.S. Shell, Belgian Bakert, Mitsubishi etc. be devoted to ionic liquid utilisation technology research and development, BASIL (biphasicacidscavengingutilisingionicliquids) deacidification technique that wherein German BASF prepares alkoxyl phenyl phosphine drastically increases efficiency, causes international community's extensive concern.
Why ionic liquid can become study hotspot, and the characteristic excellent with himself is inseparable: compare with ionogen with traditional organic solvent, and ionic liquid has a series of outstanding advantages: 1. almost do not have vapour pressure, non-volatile, colourless, tasteless; 2. larger equilibrium temperature scope is had, good chemical stability and wider electrochemical stability potential window; 3. by the design of zwitterion adjustable its to inorganics, water, organism and structure adaptability, and its acidity can be adjusted to super acid.
Although ionic liquid has numerous advantages, because existing market is expensive, and the large usage quantity of extraction agent, cause production cost very high, therefore rate of utilization is lower.Researchist finds, ionic liquid can form new ionic liquid with coordination agent, effectively can reduce the cost of industrial applications, and have both advantages concurrently simultaneously, conventional coordination agent has ethylene glycol, glycerine etc., the coordination agent that the present invention selects is ethylene glycol, forms mixed solvent with ionic liquid.
Based on the advantage of ionic liquid, the mixed solution of conventional organic solvents and ionic liquid can be used in rectification process as extraction agent, (ionic liquid is non-volatile, rate of loss is extremely low can to effectively reduce the loss of conventional solvent, and recycle), reduce production cost, can improve the quality of products simultaneously.
The method that the novel process that application number is 201410619746.0 1 kinds of methyl alcohol-formic acid propyl ester azeotrope separation of extractive distillations, application number are 201510013539.5 1 kinds of mixed solvent continuous extraction rectifying separation ethanol-toluene azeotropes, extraction agent made by the mixed solvent all adopting N-Methyl pyrrolidone and ionic liquid to form, and application number is the method for 201410619744.1 1 kinds of continuous extraction rectifying separation isopropylcarbinols and ethyl isobutyrate azeotrope, the ionic liquid that mixed extractant adopts is imidazoleacetic acid salt.Compared with above patent of invention, patent of the present invention has obvious novelty in the combination of azeotropic system, mixed extractant.
Existing azeotropic system separation means is divided into two classes substantially: azeotropic distillation and extracting rectifying.Extracting rectifying in product purity, energy consumption comparatively azeotropic distillation there is advantage.Extracting rectifying key is the selection of extraction agent.For alcohol-ester azeotropic system, comparatively conventional extraction agent is ethylene glycol, and current ethylene glycol price is at 4000 ~ 7000 yuan/ton, and novel ion liquid abstraction agent price is then very high.Such as methylimidazole phosphate ion liquid, at present as the Methylimidazole market value of its raw material at 30000 ~ 45000 yuan/ton, and four Sodium phosphorofluoridate prices are at 20000 ~ 30000 yuan/ton, and sodium hexafluoro phosphate price is more up to 180000 yuan/ton.Comparatively conventional solvent, although ionic liquid has many merits as extraction agent, high cost of investment makes its industrial applications very difficult.CN103193590A continuous extraction is separated the method for alcohol mixture-water, the technique of CN102627556A separation of extractive distillation ethyl formate-alcohol-water all adopts ethylene glycol to make extraction agent; The method of CN103193590A ion liquid abstraction rectifying separation Acetic Acid-Water adopts ionic liquid as extraction agent, and above invention all adopts atmospheric distillation technique, and energy consumption cost is larger.Generally speaking, loss of extractant how is reduced and production cost, raising product purity are the problems that current rectification process needs solution badly.
Summary of the invention
In order to solve current extraction rectification technique Problems existing, extraction agent of the present invention adopts coordination agent (ethylene glycol) and ionic liquid to form mixed extractant, can effectively improve product purity and extraction efficiency, reduces production cost and energy consumption.The ionic liquid that the present invention adopts is 1-ethyl-3-methylimidazole diethyl phosphoric acid salt ([emim] [dep]), 1-butyl-3-Methylimidazole dibutyl phosphate salt ([bmim] [dbp]), belongs to the ionic liquid of alkyl imidazole phosphoric acid salt.Not yet find at present the patent, the bibliographical information that are separated about Virahol-acetonitrile azeotropic system or deliver, more have no the technique that ionic liquid applies at this azeotropic system and occur, therefore the present invention makes up current technical vacancy.The maximum advantage of the present invention is the innovation on solvent selection, optimizes separating technology, reduces separating energy consumption, and obtain high-quality Virahol, acetonitrile product, have high promotional value.
The object of the present invention is to provide the batch fractionating technique of a kind of mixed extractant separating isopropanol-acetonitrile azeotrope.This process characteristic is the mixture being that extraction agent is selected ionic liquid and Conventional solvents and formed, and operating method is decompression periodical operation.
A batch fractionating technique for mixed extractant separating isopropanol-acetonitrile azeotrope, this technique major equipment is made up of tower reactor, rectifying tower, condenser, reflux, products pot, interim fraction tank, fresh feed pump, vacuum unit etc.
A batch fractionating technique for mixed extractant separating isopropanol-acetonitrile azeotrope, the present invention is achieved by following process.
Virahol-acetonitrile mixture fresh feed pump 1 adds in tower reactor through mother tube, and ethylene glycol-ionic liquid composition mixed extractant constantly adds from tower top through fresh feed pump, and Solvent quantity and raw material ratio are 2 ~ 4:1, and this tower working pressure is 0.3atm.After mixed extractant enters tower, total reflux operation is carried out to extractive distillation column.When tower top temperature reaches 60 ~ 61 DEG C, with the acetonitrile of reflux ratio 2 ~ 5:1 extraction content >=99.5% to products pot 1; As the acetonitrile product content < less than 98% of extractive distillation column overhead extraction, and tower top temperature higher than 65 DEG C time, stop adding extraction agent, and with reflux ratio 3 ~ 5:1 extraction acetonitrile-Virahol interim fraction to transition tank 1; When tower top temperature reaches 67 ~ 68 DEG C, with reflux ratio 1 ~ 2:1 extraction Virahol to products pot 2, when tower top temperature is higher than 68 DEG C, with reflux ratio 1:1 extraction Virahol-ethylene glycol interim fraction to transition tank 2; When tower top temperature is higher than 140 DEG C, stop.After system cools, tower reactor release purity higher than 99.5% extraction agent, lower batch of material is stand-by.
Extractive distillation column technical parameter is as follows: this tower theoretical plate number is 45 ~ 80, and extractant feed position is 3rd ~ 5 blocks of plates; Reflux ratio is 1 ~ 5, and working pressure is 0.3atm; Extraction agent is ethylene glycol (80 ~ 90wt%) and ionic liquid (10 ~ 20wt%), and extractant feed amount is 2 ~ 4:1 with feedstock ratio, and feeding temperature is 30 ~ 40 DEG C, and pressure is 0.11MPa; Raw material is that Virahol (55wt%) forms with the nearly azeotropic of acetonitrile (45wt%), and feeding temperature is 30 ~ 40 DEG C, and pressure is 0.11MPa.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention and schematic flow sheet.
Embodiment
Embodiment one
A kind of batch fractionating technique of mixed extractant separating isopropanol-acetonitrile azeotrope.Extraction agent selects ethylene glycol and 1-ethyl-3-methylimidazole diethyl phosphoric acid salt ([emim] [dep]) (20wt%); Feed throughput is 1000kg, and raw material consists of Virahol (55wt%) and forms with the nearly azeotropic of acetonitrile (45wt%), and Solvent quantity is 3 ~ 4:1 with feedstock ratio, and extractive distillation column stage number is 60, and extractant feed position is at the 5th block of column plate.Reflux ratio is set as 4, when tower top temperature reaches 60 ~ 61 DEG C, with the acetonitrile of reflux ratio 5:1 extraction content >=99.5% to products pot 1; As the acetonitrile product content < less than 98% of extractive distillation column overhead extraction and tower top temperature higher than 65 DEG C time, stop adding extraction agent, and with reflux ratio 5:1 extraction acetonitrile-Virahol interim fraction to transition tank 1; When tower top temperature reaches 67 ~ 68 DEG C, with reflux ratio 2:1 extraction Virahol to products pot 2, when tower top temperature is higher than 68 DEG C, with reflux ratio 1:1 extraction Virahol-ethylene glycol interim fraction to transition tank 2; When tower top temperature is higher than 140 DEG C, stop.After system cools, tower reactor release purity higher than 99.5% extraction agent, lower batch of material is stand-by.
Embodiment two
Extraction agent selects ethylene glycol and 1-butyl-3-Methylimidazole dibutyl phosphate salt ([bmim] [dbp]), and other conditions are as embodiment one.The acetonitrile obtained follows Virahol product purity all more than 99.5%.
Claims (1)
1. a batch fractionating technique for mixed extractant separating isopropanol-acetonitrile azeotrope, is characterized in that following working method and technical parameter:
1) Virahol-acetonitrile mixture fresh feed pump 1 adds in tower reactor through mother tube, and ethylene glycol-ionic liquid composition mixed extractant constantly adds from tower top through fresh feed pump, and Solvent quantity and raw material ratio are 2 ~ 4:1, and this tower working pressure is 0.3atm; After mixed extractant enters tower, total reflux operation is carried out to extractive distillation column; When tower top temperature reaches 60 ~ 61 DEG C, with the acetonitrile of reflux ratio 2 ~ 5:1 extraction content >=99.5% to products pot 1; As the acetonitrile product content < less than 98% of extractive distillation column overhead extraction, and tower top temperature higher than 65 DEG C time, stop adding extraction agent, and with reflux ratio 3 ~ 5:1 extraction acetonitrile-Virahol interim fraction to transition tank 1; When tower top temperature reaches 67 ~ 68 DEG C, with reflux ratio 1 ~ 2:1 extraction Virahol to products pot 2, when tower top temperature is higher than 68 DEG C, with reflux ratio 1:1 extraction Virahol-ethylene glycol interim fraction to transition tank 2; When tower top temperature is higher than 140 DEG C, stop; After system cools, tower reactor release purity higher than 99.5% extraction agent, lower batch of material is stand-by;
2) extractive distillation column technical parameter: this tower theoretical plate number is 45 ~ 80, extractant feed position is 3rd ~ 5 blocks of plates; Reflux ratio is 1 ~ 5, and working pressure is 0.3atm; Extraction agent is ethylene glycol (80 ~ 90wt%) and ionic liquid (10 ~ 20wt%), and extractant feed amount is 2 ~ 4:1 with feedstock ratio, and feeding temperature is 30 ~ 40 DEG C, and pressure is 0.11MPa; Raw material is that Virahol (55wt%) forms with the nearly azeotropic of acetonitrile (45wt%), and feeding temperature is 30 ~ 40 DEG C, and pressure is 0.11MPa.
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| CN201510418609.5A CN105061146A (en) | 2015-07-17 | 2015-07-17 | Batch distillation process for separating isopropanol-acetonitrile azeotrope through mixed extraction agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220532A (en) * | 2016-07-21 | 2016-12-14 | 青岛科技大学 | A kind of separation of extractive distillation acetonitrile and the method for triethylamine |
| CN110963885A (en) * | 2019-12-25 | 2020-04-07 | 沈阳化工大学 | Method for separating butanone-ethanol azeotrope system by extractive distillation |
| CN113461570A (en) * | 2021-06-24 | 2021-10-01 | 索闻特环保科技(上海)有限公司 | Method for treating mixed liquid containing isopropanol, acetonitrile, triethylamine and water |
Citations (1)
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| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
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Patent Citations (1)
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| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
Non-Patent Citations (1)
| Title |
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| 马利娜等: "1-乙基-3-甲基咪唑二氨腈盐中各类溶质无限稀释活度系数的测定", 《高校化学工程学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220532A (en) * | 2016-07-21 | 2016-12-14 | 青岛科技大学 | A kind of separation of extractive distillation acetonitrile and the method for triethylamine |
| CN106220532B (en) * | 2016-07-21 | 2018-06-22 | 青岛科技大学 | A kind of method of separation of extractive distillation acetonitrile and triethylamine |
| CN110963885A (en) * | 2019-12-25 | 2020-04-07 | 沈阳化工大学 | Method for separating butanone-ethanol azeotrope system by extractive distillation |
| CN113461570A (en) * | 2021-06-24 | 2021-10-01 | 索闻特环保科技(上海)有限公司 | Method for treating mixed liquid containing isopropanol, acetonitrile, triethylamine and water |
| CN113461570B (en) * | 2021-06-24 | 2023-02-17 | 索闻特环保科技(上海)有限公司 | Method for treating mixed liquid containing isopropanol, acetonitrile, triethylamine and water |
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Application publication date: 20151118 |