CN104829426A - Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent - Google Patents
Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent Download PDFInfo
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- CN104829426A CN104829426A CN201510260352.5A CN201510260352A CN104829426A CN 104829426 A CN104829426 A CN 104829426A CN 201510260352 A CN201510260352 A CN 201510260352A CN 104829426 A CN104829426 A CN 104829426A
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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
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on a choline chloride/urea low-co-melting solvent. The technology is characterized in that a mixed solution of ethylene glycol and choline chloride/urea is taken as an extraction agent, wherein the mass fraction of choline chloride/urea is 5%-15%. The extraction and rectification operation process is as follows: an extraction and rectification tower is operated under normal pressure, the number of tower plates is 20-50, the reflux ratio is controlled within (1-7):1, the tower top temperature is controlled within 68-69DEG C, and the tower kettle temperature is controlled within 187-189DEG C; and the number of the tower plates of a solvent reclamation tower is 30-60, the solvent reclamation tower is operated under normal pressure, the reflux ratio is controlled within (4-8):1, the tower top temperature is controlled within 82-83DEG C, and the tower bottom temperature is controlled within 195-197DEG C. By virtue of the technology, high-purity isopropyl ether and isopropyl alcohol products can be obtained finally; and the technology has the advantages of simplicity in operation, low cost, small ambient pressure and the like.
Description
Technical field
The present invention relates to a kind of based on the low isopropyl ether-azeotropic thing continuous extraction rectification process being total to melt and dissolved dose of choline chloride/urea, it is characterized in that the low melt and dissolved dose of application in this separating technology altogether of choline chloride/urea.
Background technology
Isopropyl ether has another name called diisopropyl ether, boiling point is 68.5 DEG C, water insoluble, is dissolved in most organic solvents such as alcohol, ether, benzene, chloroform, isopropyl ether itself is also good organic solvent simultaneously, the industrial dewaxing technique often diisopropyl ether and other solvent being applied to paraffinic base oil product.Also be applied to the aspects such as pharmacy, smokeless powder, coating and paint cleaning as solvent, diisopropyl ether has high-octane rating and anti-freezing property, can be used as gasoline blender.Virahol boiling point is 82.5 DEG C, is important Chemicals and raw material.Be mainly used in pharmacy, makeup, plastics, spices, coating etc.Isopropyl ether-the isopropanol mixture produced in the production processes such as Virahol by product, because Virahol and isopropyl ether form azeotrope, (massfraction of isopropyl ether is 83.7 %, azeotropic temperature 66.2 DEG C) and be difficult to be separated, and separation method energy consumption is large, therefore develop the separation method of isopropyl ether-azeotropic mixture, increase technology content and there is important practical significance.
In the industrial production, have numerous separation methods, but the most frequently used or make product reach desirable purity and requirement by rectifying because rectifying not only equipment is simple, easy to operate, and compared to novel separation methods such as membrane sepn, on cost drops into, also there is very large advantage.Conventional rectifying mode comprises: extracting rectifying, azeotropic distillation, salt distillation and variable-pressure rectification.Extracting rectifying due to advantages such as himself energy consumption are low, it is little to pollute, solvent can be recycled, cost-saving, thus becomes the desirable method of system being separated relative volatility and being less than 1.The present invention adopts the method for extracting rectifying equally, is separated isopropyl ether-azeotropic system.The report that patent also not relevant at present or document are separated both.
Low common melt and dissolved dose is a kind of novel ionic liquid, by ammonium salt (R
1r
2r
3r
4n
+x
-) form with coordination agent, wherein coordination agent can be the materials such as urea, carboxylic acid, ethylene glycol.Low common melt and dissolved dose has and physicochemical property like conventional ion liquid phase, and has characteristics such as synthesizing simple and environmental friendliness, and has been widely used in electrochemistry, catalysis, organic synthesis, dissolving, extraction and technical field of material chemistry.Compared to traditional ionic liquid, low common melt and dissolved dose has better characteristic: almost without vapour pressure, low melting point, non-combustible, good thermostability, electrochemical stability, good Effective Conductivity, and use cost comparatively conventional ion liquid is lower, there is great application prospect.Low common melt and dissolved dose that adopts in the present invention is choline chloride/urea, not yet has its patent being applied in isopropyl ether-azeotropic system or bibliographical information at present.
Summary of the invention
The present invention is separated by adopting the azeotrope of method to isopropyl ether-Virahol of extracting rectifying, extraction agent select ethylene glycol and choline chloride/urea low melt and dissolved dose altogether, compared with traditional separation method, in energy consumption, product purity, environmental stress and running cost, all there is advantage.
Continuous extraction rectification process required equipment is made up of extractive distillation column and solvent recovery tower substantially.Extractive distillation column is mainly used as isopropyl ether and is separated with Virahol-extraction agent system, and its separating effect not only needs rational technical process and tower structure, and has requirement to the factors such as consumption, feed entrance point, extraction control of extraction agent.For the azeotropic system of isopropyl ether-Virahol, the present invention adopts ethylene glycol and choline chloride/urea to make extraction agent, by the operation optimized, finally reaches the separation to both.
The present invention is achieved by following technical scheme.
A kind of based on the low isopropyl ether-azeotropic thing continuous extraction rectification process being total to melt and dissolved dose of choline chloride/urea, it is characterized in that the mixed solution that extraction agent employing ethylene glycol and choline chloride/urea form, and extraction agent enters from the tower top of extractive distillation column, the azeotrope of isopropyl ether-Virahol enters from the middle and lower part of tower body.
According to the analysis entering material in tower, this technique obtains isopropyl ether at the tower top of extraction tower, obtains Virahol, obtain mixed extractant at the bottom of tower at the tower top of solvent recovery tower, and extraction agent refluxes, and reenters extraction tower, supplements.
The boiling point of the mixed extractant formed due to extraction agent ethylene glycol and choline chloride/urea is higher, and rectification under vacuum can be adopted to reduce energy consumption.
Extracting rectifying operating process is as follows: extractive distillation column operational condition is normal pressure, and control of reflux ratio is 1 ~ 7:1, and the temperature of tower top controls at 68 ~ 69 DEG C, and bottom temperature controls at 187 ~ 189 DEG C.Tower top can obtain the isopropyl ether of purity higher than 99 % with this understanding.The tower bottoms of extractive distillation column is the mixture of the isopropyl ether containing extraction agent, Virahol and minute quantity.The tower bottoms of extractive distillation column is introduced solvent recovery tower, extraction agent is separated with Virahol.The operational condition of solvent recovery tower is normal pressure, and control of reflux ratio is at 4 ~ 8:1.Tower top temperature controls, at 82 ~ 83 DEG C, to control at 195 ~ 197 DEG C at the bottom of tower.Overhead extraction Virahol, the extraction agent of tower reactor returns extractive distillation column, supplementing as solvent.
Method of the present invention is applicable to process the azeotropic mixture of isopropyl ether and Virahol composition or the mixture close to azeotropic composition.
Use of the present invention is based on the low altogether melt and dissolved dose of double-column process as extraction agent separation of extractive distillation isopropyl ether and Virahol of choline chloride/urea as shown in Figure 1: the stage number of T1 is 20 ~ 50.As shown in the figure, extraction agent is from the upper feed inlet (at 3rd ~ 10 theoretical stages) of T1, and namely 1. the mouth of pipe adds, then more than opening for feed form extraction agent recovery zone.The partial extraction agent upwards of this column plate is progressively reduced to zero.The azeotropic mixture of isopropyl ether and Virahol adds from T1 middle and lower part, and namely the mouth of pipe 2., and the stage number of rectifying section is 15 ~ 40.From the bottom up, in gas phase, the concentration of isopropyl ether progressively improves, and in liquid phase, the concentration of Virahol improves gradually.The stage number of stripping section is 5 ~ 20, and its effect extracts isopropyl ether from dropping liq, makes the concentration of isopropyl ether in tower reactor progressively drop to zero.The operational condition of T1 is normal pressure, the mass ratio of extraction agent and stock liquid is 1 ~ 4:1, the temperature of tower top controls at 68 ~ 69 DEG C, bottom temperature controls at 187 ~ 189 DEG C, with this understanding, can tower top can obtain purity higher than 99% isopropyl ether, overhead product is through condensation, 3. part turns back to T1 through pipeline, and extraction part is through pipeline 5. extraction, and control of reflux ratio is at 1 ~ 7:1.4. tower bottoms containing Virahol enters T2 by tower bottom pipeline and carries out being separated of extraction agent and Virahol.
The stage number of T2 is 30 ~ 60 pieces, operational condition is normal pressure, tower top temperature controls at 82 ~ 83 DEG C, and control at the bottom of tower at 195 ~ 197 DEG C, overhead product is through condensation, reflux ratio is 4 ~ 8:1, pipeline 7. extraction be Virahol, may Virahol containing minute quantity with ethylene glycol, remaining at the bottom of tower is extraction agent, and through piping 8. can and the pipeline being back to T1 tower 1., supplementing as extraction agent.
The present invention makees extraction agent by adopting low common melt and dissolved dose of ethylene glycol-choline chloride/urea, uses two-tower rectification, is separated, obtains highly purified isopropyl ether and Virahol respectively in two column overhead to isopropyl ether with the azeotropic mixture of Virahol.In the process, extraction agent select low altogether melt and dissolved dose with the mixed solution of ethylene glycol two kinds of solvents, combine that cost is low, technology is novel, environmental stress is little, the low numerous advantage of operation easier, meet the idea of development of green chemical industry.
Describe the present invention below in conjunction with specific embodiment.Scope of the present invention is not limited with embodiment, but the scope of requirement of having the right is limited.
Accompanying drawing explanation
Fig. 1 extracting rectifying double-column process schematic diagram.
Embodiment
Embodiment 1:
Based on low isopropyl ether and the azeotropic thing continuous extraction rectification process being total to melt and dissolved dose of choline chloride/urea, its process flow sheet as shown in Figure 1.T1 stage number is 50, and with 90wt% ethylene glycol and 10wt% choline chloride/urea as extraction agent, add from the 3rd block of column plate, flow is 300kg/hr.The mixture of isopropyl ether and Virahol adds from the 40th block of column plate, and flow is 100kg/hr, and wherein the massfraction of isopropyl ether is 80%.Normal pressing operation, trim the top of column is than controlling as 3:1, and tower top temperature is 68 ~ 69 DEG C, and bottom temperature is 187 ~ 189 DEG C, overhead product by analysis, for purity higher than 99% isopropyl ether product, the tower reactor thing of T1 enters T2.T2 has 50 blocks of column plates, and reflux ratio is 6:1, and from the 40th piece of column plate charging, operational condition is normal pressure, tower top temperature 82 ~ 83 DEG C, bottom temperature 195 ~ 197 DEG C.After testing, tower top finally obtain purity higher than 99% Virahol, the tower reactor thing of T2 returns T1 and recycles.
Embodiment 2:
Extractive distillation column double-column process is with embodiment 1.Make extraction agent with 85wt% ethylene glycol and 15wt% choline chloride/urea, stage number is 30, and from the 3rd piece of column plate charging, flow is 200kg/hr.The mixture of isopropyl ether and Virahol adds from the 22nd piece of theoretical stage, and flow is 100kg/hr, forms identical with embodiment 1.T1 operates at ambient pressure, and reflux ratio is 3:1.Now tower top temperature is 68 ~ 69 DEG C, bottom temperature 187 ~ 189 DEG C.Overhead product through gas chromatographic analysis, obtain purity higher than 99% isopropyl ether product.T2 stage number is 60, and other operational conditions are with embodiment 1, and tower reactor thing returns T1 and recycles.
Claims (1)
1. isopropyl ether-azeotropic thing continuous extraction the rectification process based on low common melt and dissolved dose of choline chloride/urea, it is characterized in that operating method is continuous rectification, the mixed solution adopting ethylene glycol and choline chloride/urea is extraction agent, wherein the massfraction of choline chloride/urea is 5% ~ 15%, extractive distillation column operational condition is normal pressure, stage number is 20 ~ 50, control of reflux ratio is 1 ~ 7:1, the temperature of tower top controls at 68 ~ 69 DEG C, bottom temperature controls at 187 ~ 189 DEG C, solvent recovery tower stage number is 30 ~ 60, operational condition is normal pressure, control of reflux ratio is at 4 ~ 8:1, tower top temperature controls at 82 ~ 83 DEG C, control at the bottom of tower at 195 ~ 197 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510260352.5A CN104829426A (en) | 2015-05-21 | 2015-05-21 | Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent |
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| CN201510260352.5A CN104829426A (en) | 2015-05-21 | 2015-05-21 | Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518618A (en) * | 2016-10-08 | 2017-03-22 | 济南大学 | Method for continuously extracting, rectificating and separating isopropanol-isopropyl ether azeotrope by mixed solvent |
| CN107954859A (en) * | 2017-12-11 | 2018-04-24 | 万华化学集团股份有限公司 | A kind of method for separating acrylic acid/triisobutylene azeotropic mixture |
| 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 |
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| JPH0363239A (en) * | 1989-08-02 | 1991-03-19 | Mitsui Toatsu Chem Inc | Method for purifying diisopropyl ether |
| CN101792367A (en) * | 2010-03-12 | 2010-08-04 | 江苏工业学院 | Intermittent extraction, distillation and separation method of isopropanol-diisopropyl ether-water mixture |
| CN103467245A (en) * | 2013-09-23 | 2013-12-25 | 河北科技大学 | Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent |
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2015
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Patent Citations (3)
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| JPH0363239A (en) * | 1989-08-02 | 1991-03-19 | Mitsui Toatsu Chem Inc | Method for purifying diisopropyl ether |
| CN101792367A (en) * | 2010-03-12 | 2010-08-04 | 江苏工业学院 | Intermittent extraction, distillation and separation method of isopropanol-diisopropyl ether-water mixture |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518618A (en) * | 2016-10-08 | 2017-03-22 | 济南大学 | Method for continuously extracting, rectificating and separating isopropanol-isopropyl ether azeotrope by mixed solvent |
| CN106518618B (en) * | 2016-10-08 | 2019-03-29 | 济南大学 | A kind of method of mixed solvent continuous extraction rectifying separating isopropanol-isopropyl ether azeotropic mixture |
| CN107954859A (en) * | 2017-12-11 | 2018-04-24 | 万华化学集团股份有限公司 | A kind of method for separating acrylic acid/triisobutylene azeotropic mixture |
| CN107954859B (en) * | 2017-12-11 | 2020-11-24 | 万华化学集团股份有限公司 | Method for separating acrylic acid/triisobutene azeotrope |
| 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 |
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Application publication date: 20150812 |