CN103641700A - Method for separating butanone-water azeotrope through extraction distillation - Google Patents
Method for separating butanone-water azeotrope through extraction distillation Download PDFInfo
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- CN103641700A CN103641700A CN201310590242.6A CN201310590242A CN103641700A CN 103641700 A CN103641700 A CN 103641700A CN 201310590242 A CN201310590242 A CN 201310590242A CN 103641700 A CN103641700 A CN 103641700A
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- extractive distillation
- extraction agent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
- C07C45/83—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation by extractive distillation
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention discloses a method for separating a butanone-water azeotrope through extraction distillation. According to the method, an interrupted extraction distillation device is adopted; an ethylene glycol solution containing an ion liquid 1-ethyl-3-methylimidazolium chloride is adopted as an extraction agent; and at a normal pressure, after the extraction agent is added to an extraction distillation tower, a total reflux operation is firstly performed, then butanone, a butanone-water transition section distillate, water and an ethylene glycol-water transition section distillate are sequentially extracted from the top of the extraction distillation tower at different temperatures under different reflux ratio operation conditions, and finally the extraction agent stored in a heating kettle is recycled. The method has the following advantages that: the ion liquid solution of ethylene glycol is adopted as the extraction agent to separate the butanone-water azeotrope, the separated butanone product has high purity, the single-tower operation is adopted, the operation process is flexible and easy to control, and the equipment investment is less.
Description
Technical field
The present invention relates to a kind of method of separation of extractive distillation butanone-water azeotropic mixture, particularly relate to a kind of method of take separation of extractive distillation butanone-water azeotropic mixture that ionic liquid mixed solvent is extraction agent, belong to the isolation technique of butanone-water azeotropic mixture.
Background technology
Butanone is a kind of important industrial chemicals and organic solvent, in removal process, easily produces butanone-water azeotrope, thereby is difficult to separation, if do not reclaimed, not only pollutes the environment, and increases production cost.Extracting rectifying is the effective ways of separated butanone-water azeotropic system with extractive distillation with salt, the solvent that separation of extractive distillation butanone-water azeotrope of bibliographical information adopts is at present ethylene glycol or glycerol, but separation efficiency is lower, extractive distillation with salt adopts the mixture of ethylene glycol and inorganic salt as extraction agent, separation efficiency makes spent glycol high than separately, but inorganic salt solubleness in organic solvent is less, inorganic salt are very limited to separated promoter action, and inorganic salt corrodibility is strong.Ionic liquid is a kind of Novel Extractant of separation of extractive distillation azeotropic mixture, has higher separation efficiency.Ionic liquid is commonly referred to as fusing point lower than the compound being comprised of organic cation and inorganic anion or organic anion of 100 ℃, there is extremely low saturated vapor pressure, good thermostability and chemical stability, and good solubility are class green solvents.Ionic liquid can be separately as the extraction agent of extracting rectifying process, but ionic liquid price is high, and partial ion liquid is solid at normal temperatures, a lot of viscosity of il are large in addition, use separately very inconvenient.If ionic liquid and molecule liquid mixing are used, will address the above problem.The mixed extractant that ionic liquid and molecule liquid form is a kind of Novel Extractant of extracting rectifying, has not yet to see bibliographical information.
Summary of the invention
The object of the present invention is to provide a kind of method of separation of extractive distillation butanone-water azeotropic mixture, high with the isolated butanone product purity of the method, and also equipment is simple, easy handling.
The present invention is realized by the following technical programs, a kind of method of separation of extractive distillation butanone-water azeotropic mixture, the method adopts extracting rectifying device to implement batch fractionating operation, described extracting rectifying device comprises extractive distillation column, the heating kettle connecting at the bottom of extractive distillation column tower, the condenser that extracting rectifying column overhead connects, 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 79.5-80.2 ℃, with reflux ratio (1-2): 1 reaches more than 99.5% butanone product by extractive distillation column overhead extraction containing butanone massfraction, when extracting rectifying tower top temperature is lower than 79 ℃, stop adding extraction agent, start take reflux ratio 2:1 by extractive distillation column overhead extraction temperature section the butanone-water transition section cut as 79 ℃-73 ℃-99 ℃, when extractive distillation column tower top temperature reaches 100 ℃-105 ℃, 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 the separated butanone-water azeotropic mixture of extraction agent, has been realized the high efficiency separation of butanone and water.With the separated butanone-water azeotropic mixture of this extraction agent with take ethylene glycol and compare as the separated butanone-water azeotropic mixture of extraction agent, separation efficiency is high; With with the separated butanone-water azeotropic mixture of pure ionic liquid chlorination 1-ethyl-3-methylimidazole, 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 butanone 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 basin, 2-extractive distillation column, 3-heating kettle, 4-condenser, 5-butanone products pot, 6-butanone-water transition section cut receiving tank, 7-water receiving tank, 8-water-ethylene glycol transition section cut receiving tank, 9-infusion pump.
Embodiment
The idiographic flow of Fig. 1: butanone-water mixture adds in heating kettle 3, open the thermal source of heating kettle and the low-temperature receiver of condenser, when in extractive distillation column, rising steam rising adds entrance to extraction agent, extraction agent is introduced into batch extracting rectified tower top from extraction agent basin 1, total reflux approximately 15 minutes, when reaching 99.5%, butanone mass content starts discharging when above, enter butanone products pot 5, in extractive distillation column overhead fraction, butanone content is lower than 99.2% time, the cut of extracting rectifying tower top extraction enters butanone-water transition section cut receiving tank 6(now, stop adding extraction agent), when in extracting rectifying overhead fraction, water-content is greater than 99%, the material of extraction enters water receiving tank 7, when in extracting rectifying overhead fraction, ethylene glycol content is higher, the cut of extraction enters water-ethylene glycol interim fraction receiving tank 8, when in heating kettle, the composition of extraction agent reaches requirement, stop.Heating kettle is the mixed extractant of high density, utilizes infusion pump to squeeze into extraction agent basin and recycles.The material of two transition sections is put in heating kettle when next batch distills.
Embodiment mono-
Adopt batch extraction rectification device, wherein extractive distillation column diameter is φ 40mm.In-built
net ring filler, bed stuffing height is 1.15m, extraction agent import is apart from tower top 0.15m place.(wherein butanone 89% in heating kettle, to drop into 301.6g butanone-water mixture, water 11%, be mass percent), test the ethylene glycol solution that selected extraction agent is [emim] [cl] (containing [emim] [cl] 13.5%), 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 entrance, it is 5ml/min that control extraction agent adds speed, total reflux operation 15 minutes, when extracting rectifying tower top temperature is 79.5-80.2 ℃, in cut, butanone content is 99.5% beginning discharging, reflux ratio is 1:1, the about 1.5ml/min of discharging speed, in this process, be total to such an extent that butanone qualified product are 187.6g.When extracting rectifying tower top temperature is less than 79.0 ℃, stop adding extraction agent, take reflux ratio as 1:1 extraction butanone-water transition section, in this process, extract tower top temperature and first drop to 73 ℃, then rise to 100 ℃, when extractive distillation column tower top temperature reaches 100 ℃-105 ℃, with reflux ratio 1:1, dewater; When extractive distillation column tower top temperature surpasses 105 ℃, with reflux ratio 4:1 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.
Embodiment bis-
Adopt the experimental installation identical with embodiment mono-.(wherein butanone 89% in heating kettle, to drop into 302g butanone-water mixture, water 11%, be mass percent), test the ethylene glycol solution that selected extraction agent is [emim] [cl] (containing [emim] [cl] 20%), 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 entrance, it is 4.5ml/min that control extraction agent adds speed, total reflux operation 15 minutes, when extracting rectifying tower top temperature is 79.5-80.2 ℃, in cut, butanone content is 99.5% beginning discharging, reflux ratio is 1:1, discharging speed is 1.5ml/min, in this process, be total to such an extent that butanone qualified product are 200g.When extracting rectifying tower top temperature is less than 79.0 ℃, stop adding extraction agent, take reflux ratio as 1:1 extraction butanone-water transition section, in this process, extract tower top temperature and first drop to 73 ℃, then rise to 100 ℃, when extractive distillation column tower top temperature reaches 100 ℃-105 ℃, with reflux ratio 1:1, dewater; When extractive distillation column tower top temperature surpasses 105 ℃, with reflux ratio 4:1 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.
Embodiment tri-
Adopt the experimental installation identical with embodiment mono-.(wherein butanone 89% in heating kettle, to drop into 302g butanone-water mixture, water 11%, be mass percent), test the ethylene glycol solution that selected extraction agent is [emim] [cl] (containing [emim] [cl] 30%), 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 entrance, it is 4ml/min that control extraction agent adds speed, total reflux operation 15 minutes, when extracting rectifying tower top temperature is 79.5-80.2 ℃, in cut, butanone content approximately 99.5% starts discharging, reflux ratio is 1:1, discharging speed is 1.5ml/min, in this process, be total to obtain the about 214g of butanone qualified product.When extracting rectifying tower top temperature is less than 78.5 ℃, stop adding extraction agent, take reflux ratio as 1:1 extraction butanone-water transition section, in this process, extract tower top temperature and first drop to 73 ℃, then rise to 100 ℃, when extractive distillation column tower top temperature reaches 100 ℃-105 ℃, with reflux ratio 1:1, dewater; When extractive distillation column tower top temperature surpasses 105 ℃, with reflux ratio 4:1 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.
Claims (1)
1. the method for a separation of extractive distillation butanone-water azeotropic mixture, the method adopts extracting rectifying device to implement batch fractionating operation, described extracting rectifying device comprises extractive distillation column, the heating kettle connecting at the bottom of extractive distillation column tower, the condenser that extracting rectifying column overhead connects, 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 79.5-80.2 ℃, with reflux ratio (1-2): 1 reaches more than 99.5% butanone product by extractive distillation column overhead extraction containing butanone massfraction, when extracting rectifying tower top temperature is lower than 79 ℃, stop adding extraction agent, start take reflux ratio 2:1 by extractive distillation column overhead extraction temperature section the butanone-water transition section cut as 79 ℃-73 ℃-99 ℃, when extractive distillation column tower top temperature reaches 100 ℃-105 ℃, 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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| CN201310590242.6A CN103641700A (en) | 2013-11-22 | 2013-11-22 | Method for separating butanone-water azeotrope through extraction distillation |
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| CN201310590242.6A CN103641700A (en) | 2013-11-22 | 2013-11-22 | Method for separating butanone-water azeotrope through extraction distillation |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453166A (en) * | 1994-11-07 | 1995-09-26 | Lloyd Berg | Separation of ethanol from 2-butanone by extractive distillation |
| CN1832789A (en) * | 2003-08-05 | 2006-09-13 | 巴斯福股份公司 | Distillative method for separating narrow boiling or azeotropic mixtures using ionic liquids |
| CN101254358A (en) * | 2007-12-05 | 2008-09-03 | 天津大学 | Adding salt intermittent extraction rectification separation method of acetonitrile-water azeotropic mixture |
| CN101284770A (en) * | 2008-07-01 | 2008-10-15 | 南京师范大学 | Extraction and rectification separation method for alkali solution in butanone-water system |
-
2013
- 2013-11-22 CN CN201310590242.6A patent/CN103641700A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453166A (en) * | 1994-11-07 | 1995-09-26 | Lloyd Berg | Separation of ethanol from 2-butanone by extractive distillation |
| CN1832789A (en) * | 2003-08-05 | 2006-09-13 | 巴斯福股份公司 | Distillative method for separating narrow boiling or azeotropic mixtures using ionic liquids |
| CN101254358A (en) * | 2007-12-05 | 2008-09-03 | 天津大学 | Adding salt intermittent extraction rectification separation method of acetonitrile-water azeotropic mixture |
| CN101284770A (en) * | 2008-07-01 | 2008-10-15 | 南京师范大学 | Extraction and rectification separation method for alkali solution in butanone-water system |
Non-Patent Citations (1)
| Title |
|---|
| 陈红梅等: "隔离壁萃取精馏塔分离甲乙酮/水", 《江苏工业学院学报》 * |
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Application publication date: 20140319 |