CN1405137A - Method for separating acetic acid and water by complexation extraction and rectification - Google Patents
Method for separating acetic acid and water by complexation extraction and rectification Download PDFInfo
- Publication number
- CN1405137A CN1405137A CN 01141847 CN01141847A CN1405137A CN 1405137 A CN1405137 A CN 1405137A CN 01141847 CN01141847 CN 01141847 CN 01141847 A CN01141847 A CN 01141847A CN 1405137 A CN1405137 A CN 1405137A
- Authority
- CN
- China
- Prior art keywords
- acetic acid
- water
- tower
- ratio
- complexing extractant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
THe invention provides a method for separating acetic acid and water by complexation, extraction and rectification process. Said invention utilizes the acting force between organic alkali and acetic acid, which is stronger than that of water, and greatly raises the relative volatilities of acetic acid and water so as to separate them. In the fractionating recrtifying tower with 10-50 theoretical plates it adopts tertiary amine organic alkali as complexation extracting agent, under the condition of normal pressure (or reduced pressure), its solvent ratio is 0.5-5 and refluxing ratio is 0-5, the water whose mass fraction is greater than 99.7% can be obtained from tower top, and in the solvent recovering tower with 5-40 the oretical plates, under the condition of reduced pressure and refluxing ratio of 0.5-5 the acetic acid whose mass fraction is greater than 95.0% can be obtained.
Description
Technical field:
The present invention relates to the method for a kind of separating acetic acid and water, particularly adopt the method separating acetic acid and the water of extracting rectifying.
Background technology:
In the production process of acetic acid, because the relative volatility of acetic acid and water approaches 1, their separation is difficulty comparatively, generally adopts the method for conventional distillation, sequence of constant boiling and rectification both at home and abroad.The technical process of conventional distillation is simple, and operation control is easy, but the stage number that needs is many, and the process energy consumption is big; The used stage number of sequence of constant boiling and rectification is few, but the nonvariant boiling reagent consumption is big, and configuration is complicated, and the process energy consumption is big, and operation control is complicated; US5167774 and US4729818 disclose method separating acetic acid and the water of taking common extracting rectifying, this method selection of Extractant scope is wide, operation control easily, but there are the extraction agent large usage quantity in acetic acid and the separating of water close for relative volatility, weakness such as stage number is many, and energy consumption is bigger.
Summary of the invention:
The present invention is directed to acid-water and alkali-aqueous systems, based on the reversible chemical effect of bronsted lowry acids and bases bronsted lowry with the isolating principle of component to be separated, propose a kind of thought of complexometric extraction rectifying and be used for acetic acid-water system, utilize the interaction force organic bases far away strong between organic bases and the acetic acid and the characteristic of the interaction force between the water, improve the relative volatility of acetic acid and water significantly, they are effectively separated, thereby propose a kind of separating power is strong, flow process is simple, energy consumption the is low separating acetic acid and the method for water.
The present invention adopts the extracting rectifying flow process that comprises extractive distillation column and solvent recovery unit; Select tertiary amines or their liquid mixture as complexing extractant; Wherein the operational condition of extractive distillation column is: have 10-50 piece theoretical plate number, normal pressure (or decompression), solvent ratio 0.5-5, reflux ratio 0-5, tower top temperature is controlled at 99.8 ℃-101.0 ℃, solvent recovery tower has 5-40 piece theoretical tray, normal pressure or decompression, and reflux ratio is 0.5-5.
The selection of above-mentioned complexing extractant is a key problem in technology, except that guaranteeing to have than the strong interaction with acetic acid, also to satisfy to other of solvent require as: moderate boiling point, stable in properties, low price, little etc. to the corrosion of tower.Complexing extractant is to contain the tertiary amines of 6-24 carbon atom or their liquid mixture preferably.
Above-mentioned tertiary amines complexing extractant is that massfraction surpasses 10% liquid mixture.
Above-mentioned tertiary amines complexing extractant is Tributylamine and triamylamine etc.
Effect of the present invention: the present invention is directed to acid-water and alkali-aqueous systems, the thought of complexometric extraction rectifying is proposed, utilize the reversible chemical effect of bronsted lowry acids and bases bronsted lowry that component to be separated is separated, be different from the chemical separation technology commonly used physical action from principle based on intermolecular Van der Waals force, or the thought of the extractive distillation with salt of introducing ion and molecular interaction, particularly this thought is used for separating acetic acid and water, selected to be applicable to the efficient complexing extractant of acetic acid-water system, make the relative volatility of acetic acid and water improve greatly, thereby:
1, significantly improved separating power, following contrast experiment's data are illustrated: experiment condition: massfraction is the acetic acid of 28.87% (acetic acid) and 71.13% (water) and the mixture of water, separates in the rectifying tower with 30 theoretical stages.Behind the total reflux 10min,, tower top temperature is between 99.5 ℃-101.5 ℃, and every 10min gets overhead product and carries out gas chromatographic analysis.The average result of five sub-sampling analyses is:
The mass fraction acetic acid mass fraction of red-tape operati reflux ratio water.
Conventional distillation 1.0 94.87% 5.13%
Complexometric extraction rectifying 1.0 99.7% 0.3%
Conventional distillation 4.0 96.18% 3.82%
It is very difficult greater than 99.7% water that above data declaration conventional distillation method desires to obtain massfraction at the rectifying tower cat head, must further improve reflux ratio.And the present invention can reach separation requirement when less reflux ratio.
2, energy-saving effect is fairly obvious, and under equal stage number and product purity condition, the unit acetic acid energy consumption of sequence of constant boiling and rectification is a 33690KJ/Kg acetic acid, and complexometric extraction rectifying is 11947KJ/Kg acetic acid, and energy-conservation 64.5%.
3, technology is simple, and the present invention adopts the double-column process identical with general extracting rectifying.Therefore adopt this operational path shorter to existing apparatus cycle that undergoes technological transformation, good reliability has very strong practicality.
Description of drawings:
Fig. 1 is the process flow diagram that the present invention adopts the double tower extracting rectifying.
Embodiment:
The present invention adopts the extraction rectification technique that comprises extractive distillation column and solvent recovery tower.Extractive distillation column (stage number is counted from top to bottom), tertiary amines complexing extractant S enters extractive distillation column from 2-5 piece theoretical stage, mixture with any concentration blended acetic acid and water enters from 5-40 piece theoretical stage, under normal pressure (or decompression), solvent ratio 0.5-5, reflux ratio 0-5, tower top temperature is controlled at 99.8 ℃-101.0 ℃, normal pressure or decompression, reflux ratio are 0.5-5.Under this condition, cat head can the extraction massfraction greater than 99.7% water, the emission standard of compliance with environmental protection requirements; Solvent recovery tower (stage number is counted from top to bottom) has 5-40 piece theoretical tray, the complexing extractant S that comes out from extracting rectifying Tata still and the mixture of dense acetic acid enter from 2-30 piece theoretical stage, the working pressure of solvent recovery tower is that 0.05-latm (absolute pressure), reflux ratio are 0.5-5, under this condition, cat head can the extraction massfraction greater than 95.0% acetic acid, the effusive complexing extractant S of tower still recycles.
Embodiment 1:
As shown in Figure 1, experiment flow is made up of extractive distillation column 1 and solvent recovery tower 2.Extractive distillation column has 30 blocks of theoretical trays (stage number is counted from top to bottom), select for use the Tributylamine liquid mixture (mass fraction surpasses 15%) that contains little acetic acid to be complexing extractant, add from the 4th theoretical stage, flow is 10ml/min, the mixture of acetic acid and water adds from the 15th block of theoretical tray, consist of water 71.13wt%, acetic acid 28.87wt%, flow are 10ml/min.Extractive distillation column is operated under normal pressure, and the trim the top of column ratio is 1, and tower top temperature is controlled at 99.5 ℃-101.0 ℃, and overhead product is through gas chromatographic analysis, and the massfraction of water is 99.74%, and the massfraction of acetic acid is 0.26%, reaches separation requirement.Extracting rectifying Tata still soln using pressure difference enters the solvent recovery tower middle part, and solvent recovery tower has 20 blocks of theoretical trays, and working pressure is 0.01-0.05Mpa, and the trim the top of column ratio is 1, and tower still temperature is controlled at 130.0 ℃-160.0 ℃.Cat head can the extraction massfraction greater than 95.0% acetic acid, complexing extractant reclaims in solvent recuperation Tata still, with recycle.
Embodiment 2
With embodiment 1, experiment flow is made up of extractive distillation column and solvent recovery tower.Extractive distillation column has 30 blocks of theoretical trays (stage number is counted from top to bottom), select for use the Tributylamine liquid mixture (mass fraction surpasses 10%) that contains little acetic acid to be complexing extractant, add from the 4th theoretical stage, flow is 10ml/min, the mixture of acetic acid and water adds from the 15th block of theoretical tray, consist of water 71.13wt%, acetic acid 28.87wt%, flow are 10ml/min.Extractive distillation column is operated under normal pressure, and the trim the top of column ratio is 0, and tower top temperature is controlled at 99.5 ℃-101.0 ℃, and overhead product is through gas chromatographic analysis, and the massfraction of water is 99.81%, and the massfraction of acetic acid is 0.19%, reaches separation requirement.Extracting rectifying Tata still soln using pressure difference enters the solvent recovery tower middle part, and solvent recovery tower has 20 blocks of theoretical trays, and working pressure is 0.01-0.05Mpa, and the trim the top of column ratio is 1, and tower still temperature is controlled at 130.0 ℃-160.0 ℃.Cat head can the extraction massfraction greater than 95.0% acetic acid, complexing extractant reclaims in solvent recuperation Tata still, with recycle.Example 3
With embodiment 1, experiment flow is made up of extractive distillation column and solvent recovery tower.Extractive distillation column has 30 blocks of theoretical trays (stage number is counted from top to bottom), select for use the triamylamine liquid mixture (mass fraction surpasses 10%) that contains little acetic acid to be complexing extractant, add from the 4th theoretical stage, flow is 10ml/min, the mixture of acetic acid and water adds from the 15th block of theoretical tray, consist of water 69.97wt%, acetic acid 30.03wt%, flow are 10ml/min.Extractive distillation column is operated under normal pressure, and the trim the top of column ratio is 1, and tower top temperature is controlled at 99.5 ℃-101.0 ℃, and overhead product is through gas chromatographic analysis, and the massfraction of water is 99.77%, and the massfraction of acetic acid is 0.23%, reaches separation requirement.Extracting rectifying Tata still soln using pressure difference enters the solvent recovery tower middle part, and solvent recovery tower has 20 blocks of theoretical trays, and working pressure is 0.01-0.05Mpa, and the trim the top of column ratio is 1, and tower still temperature is controlled at 130.0 ℃-160.0 ℃.Cat head can the extraction massfraction greater than 95.0% acetic acid, complexing extractant reclaims in solvent recuperation Tata still, with recycle.Example 4
With embodiment 1, experiment flow is made up of extractive distillation column and solvent recovery tower.Extractive distillation column has 30 blocks of theoretical trays (stage number is counted from top to bottom), select for use the triamylamine liquid mixture (mass fraction surpasses 15%) that contains little acetic acid to be complexing extractant, add from the 4th theoretical stage, flow is 10ml/min, the mixture of acetic acid and water adds from the 15th block of theoretical tray, consist of water 69.97wt%, acetic acid 30.03wt%, flow are 10ml/min.Extractive distillation column is operated under normal pressure, and the trim the top of column ratio is 0, and tower top temperature is controlled at 99.5 ℃-101.0 ℃, and overhead product is through gas chromatographic analysis, and the massfraction of water is 99.86%, and the massfraction of acetic acid is 0.14%, reaches separation requirement.Extracting rectifying Tata still soln using pressure difference enters the solvent recovery tower middle part, and solvent recovery tower has 20 blocks of theoretical trays, and working pressure is 0.01-0.05Mpa, and the trim the top of column ratio is 1, and tower still temperature is controlled at 130.0 ℃-160.0 ℃.Cat head can the extraction massfraction greater than 95.0% acetic acid, complexing extractant reclaims in solvent recuperation Tata still, with recycle.
Claims (5)
1, the method for a kind of complexometric extraction rectifying separation acetic acid and water, adopt the extracting rectifying flow process, it is characterized in that: with tertiary amines or their liquid mixture as complexing extractant, wherein the operational condition of extractive distillation column is: have 10-50 piece theoretical plate number, normal pressure or decompression, solvent ratio 0.5-5, reflux ratio 0-5, tower top temperature is controlled at 99.8 ℃-101.0 ℃, solvent recovery tower has 5-40 piece theoretical tray, normal pressure or decompression, and reflux ratio is 0.5-5.
2, method according to claim 1 is characterized in that: select to contain the tertiary amines of 6-24 carbon atom or their liquid mixture as complexing extractant.
3, method according to claim 1 is characterized in that: complexing extractant is that massfraction surpasses 10% tertiary amines liquid mixture.
4, method according to claim 1 is characterized in that: complexing extractant is Tributylamine, triamylamine.
5, method according to claim 1 is characterized in that: adopting the extraction rectification technique flow process is the double-column process that comprises rectifying tower and recovery tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011418478A CN1181034C (en) | 2001-09-20 | 2001-09-20 | Method for separating acetic acid and water by complexation extraction and rectification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011418478A CN1181034C (en) | 2001-09-20 | 2001-09-20 | Method for separating acetic acid and water by complexation extraction and rectification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1405137A true CN1405137A (en) | 2003-03-26 |
| CN1181034C CN1181034C (en) | 2004-12-22 |
Family
ID=4676442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011418478A Expired - Fee Related CN1181034C (en) | 2001-09-20 | 2001-09-20 | Method for separating acetic acid and water by complexation extraction and rectification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1181034C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341290A (en) * | 2013-07-30 | 2015-02-11 | 浙江科技学院 | Ionic liquid extractive distillation method for separating acetic acid and water |
| CN104447275A (en) * | 2014-11-28 | 2015-03-25 | 浙江新和成药业有限公司 | Method for purifying acetic acid from acetic acid wastewater |
| WO2015126899A3 (en) * | 2014-02-19 | 2015-11-12 | Api Intellectual Property Holdings, Llc | Processes and apparatus for removal of fermentation inhibitors from biomass hydrolysates |
| CN107176907A (en) * | 2017-06-09 | 2017-09-19 | 安徽丰原发酵技术工程研究有限公司 | A kind of method for extracting malic acid/malate |
-
2001
- 2001-09-20 CN CNB011418478A patent/CN1181034C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341290A (en) * | 2013-07-30 | 2015-02-11 | 浙江科技学院 | Ionic liquid extractive distillation method for separating acetic acid and water |
| WO2015126899A3 (en) * | 2014-02-19 | 2015-11-12 | Api Intellectual Property Holdings, Llc | Processes and apparatus for removal of fermentation inhibitors from biomass hydrolysates |
| CN104447275A (en) * | 2014-11-28 | 2015-03-25 | 浙江新和成药业有限公司 | Method for purifying acetic acid from acetic acid wastewater |
| CN107176907A (en) * | 2017-06-09 | 2017-09-19 | 安徽丰原发酵技术工程研究有限公司 | A kind of method for extracting malic acid/malate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1181034C (en) | 2004-12-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101172941B (en) | Method for recycling acetic acid in dilute acetic acid | |
| CN101306989B (en) | Process for separating acetic acid from water by salt-containing extracting, rectifying and separating | |
| WO2011008927A2 (en) | Recovery of butanol from a mixture of butanol, water, and an organic extractant | |
| WO2011008924A2 (en) | Recovery of butanol from a mixture of butanol, water, and an organic extractant | |
| EP2504303A1 (en) | Recovery of butanol from a mixture of butanol, water, and an organic extractant | |
| CN101028987A (en) | Method and apparatus for extracting, rectifying and separating propane and propylene by separated wall tower | |
| CN1907940A (en) | Azeotropic distillation process for separating acetic acid, methyl acetate and water in the production of an aromatic carboxylic acid | |
| CN101397260B (en) | Technology for recovering dimethylformamide from waste water by combination of saline extraction and rectification method | |
| CN111574375B (en) | Separation method and separation equipment for methyl acrylate crude product gas | |
| CN102070445A (en) | Purification method of ethyl acetate | |
| Han et al. | Separation characteristics of lactic acid in reactive extraction and stripping | |
| CN104610022A (en) | Method for separating ethanol-propyl acetate azeotrope through continuous extractive rectification | |
| CN1181034C (en) | Method for separating acetic acid and water by complexation extraction and rectification | |
| CN112661593B (en) | Method for separating benzene, cyclohexene and cyclohexane by extracting and rectifying mixed solvent containing ionic liquid | |
| CN105646146A (en) | Propyl alcohol-triethylamine azeotropic mixture extraction and rectification method | |
| CN105964007A (en) | Device and process for separating n-butyl alcohol and isobutanol mixture | |
| CN1131200A (en) | Solvent extraction and separation new system of thulium, ytterbium and lutetium | |
| CN1448383A (en) | Process for extracting, preparing and purifying gamma methyllinolenate from algae | |
| CN1982280A (en) | Process for puriying an organic acid | |
| CN101041631A (en) | Improved synthesizing technique for beta-carotene | |
| CN105152926A (en) | Distillation separation method for azeotrope of tert-butanol and methylpropionate by using mixed solvent as extractant | |
| CN1176938C (en) | Refining process of chenodeoxcholic acid | |
| CN212532808U (en) | Methyl acrylate crude product gas separation equipment | |
| CN112679315A (en) | Method for separating low-carbon alcohol-water based on coupling process of ionic liquid mixed extractant and dividing wall tower | |
| CN1146572C (en) | Method for production of ivermectin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |