CN1745868A - Extraction rectifying method and rectifier with separated wall - Google Patents
Extraction rectifying method and rectifier with separated wall Download PDFInfo
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- CN1745868A CN1745868A CN 200510041506 CN200510041506A CN1745868A CN 1745868 A CN1745868 A CN 1745868A CN 200510041506 CN200510041506 CN 200510041506 CN 200510041506 A CN200510041506 A CN 200510041506A CN 1745868 A CN1745868 A CN 1745868A
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Abstract
An extracting-rectifying tower with isolating wall features that its isolating wall is vertically arranged from tower top to lower part of tower to divide the internal space of said tower in to three subspaces. The material to be separated and the extract come in one subspace for extracting and rectifying. The product is output from tower top. The extract and another material come in extracting-rectifying segment for separation. The extract is recovered for cyclic use. The mixed material is recovered through recovery tower for reuse. Its advantages are omitting one tower and low energy consumption.
Description
Technical field
The invention belongs to a kind of novel extraction separation method, refer in particular to a kind of extraction rectifying method and device, in a partition wall rectifying column, finish the separation process of extracting rectifying process and extractant and component simultaneously with partition wall rectifying column.
Background technology
Partition wall rectifying column (DWC) is to establish a vertical wall in rectifying column, this vertical wall can be arranged on the middle part of tower, also vertical wall can be extended to cat head or tower still, the DWC tower is separated two parts that wall separates can common rectifying section or stripping section, or common rectifying section and stripping section are arranged simultaneously.U.S. Pat 20040011706, US200310116420 etc. disclose and have adopted the DWC tower to separate the method for ternary mixture, adopt the DWC tower than double-column process energy-conservation 30%, and equipment investment can be saved more than 30%, these patents all only are applied to distillation process with the DWC tower, are not applied to the extracting rectifying process.
Extraction rectification technique is suitable for separating azeotrope or the approaching system of boiling-point difference owing to have advantages such as equipment investment is low, energy Mao is low.As the separation for preparing absolute ethyl alcohol and hydrocarbon mixture.
Existing extraction rectification technique mainly is to add the relative volatility that extractant changes needs separation component in extractive distillation column, and component is separated, recycle after then extractant being reclaimed, that is to say, carry out extracting rectifying earlier, and then carry out extractant and reclaim.So general extracting rectifying flow process needs three towers, promptly extractive distillation column, extractant recovery tower reclaim the solvent that comes out from extracting rectifying Tata still, a material recovery tower separates the material that steams from extractant recovery tower top, makes its separation obtain another kind of product.Obviously, the employed equipment of this method is more, and complex operation.
Summary of the invention
The purpose of this invention is to provide and a kind ofly in the partition wall rectifying column extracting rectifying and extractant are separated the method and apparatus of finishing simultaneously, two towers of its need can be finished separation requirement.
The present invention is achieved in that
Device of the present invention is the extractive distillation column that has partition wall, it is a vertical partition wall extends to tower from the top of tower bottom, the height of dividing wall is less than the total height of tower, partition wall is divided into three parts with extractive distillation column inside, wherein the top of tower is separated wall and is divided into left and right sides two parts, the part that communicates in the lower end of partition wall is the total stripping section of the left and right sides, top two parts of tower, on the right side in next door, tower top two charging apertures are arranged, top is the charging aperture of extractant, and the middle part is the material feeding mouth.
Method of the present invention is: extractant, raw material enters in the tower from the extractant feed mouth of extractive distillation column right upper portion and the material inlet of bottom respectively, through extracting rectifying, need the cat head discharging of separation component from charging aperture one side, obtain the product A of required purity, the extractant that contains B component and a small amount of A enters the tower still and distills, because the extractant boiling point is very high, so A, B is easy to separate, the material that contains B component and a small amount of A will be from the left side discharging of partition wall, entering the material recovery tower further separates, simultaneously, the tower still obtains pure extractant, and this extractant returns salty multiple use of extractant feed.
The present invention compared with the prior art, its outstanding substantive distinguishing features and marked improvement is:
1. compare with existing extracting rectifying equipment, can save an extractant rectifying column, can save equipment investment more than 30%.
2. adopt the partition wall extractive distillation column to reduce by 30% the amount of boiling again,, can save energy above 50% for some specific flow processs.Saved energy greatly.
Description of drawings
Fig. 1 is technological process of the present invention and apparatus sketch
Fig. 2 is traditional extracting rectifying flow process
Fig. 3 is for adopting the extracting rectifying flow process of partition wall extractive distillation column
In the drawings, 1,2,3 is three different zones, and 7 is extractive distillation column, and 8 is the extractant recovery tower, and 9 is the material recovery tower, and 5,10,13 is condenser, and 6,11,14 is return tank, and 4,12,15 is reboiler, and 16 is intermediate storage tank.
The specific embodiment
In the technological process shown in Figure 1, one vertical partition wall that extends to the bottom of tower from the top is arranged in the extractive distillation column, because the height of dividing wall is less than the total height of tower, so two zones communicate in the lower end of dividing wall, vertical partition wall in the partition wall extractive distillation column forms zone 1 and 2 and lower area 3 at rectifier, also comprises tower still reboiler 4, overhead condenser 5 and return tank 6.
The extracting rectifying effect is mainly played in zone 1, and mixed material is A, B two component mixtures, from the middle part charging of tower, extractant is from the top charging of tower, because extractant has changed the relative volatility of A, B two components in the incoming mixture, and component A is steamed from cat head, obtains net product A.Extractant, B component and a small amount of component A enter tower bottom reboiler 4 by zone 3.
Zone 2 main effects are that extractant is separated with the B component that contains a small amount of component A.Because the effect of extractant, major part is extractant and B component from the material that regional 1 side is got off, because the boiling-point difference of extractant and institute's separation component has 25 ℃ at least, so extractant separates with B component accessible region territory 2, the discharging position in zone 2 is determined with the complexity of separating of component by extractant.Do not contain extractant from 2 materials that come out of zone, for containing the binary mixture of a small amount of A, this mixture enters in the material recovery tower again and further handles.
The effect of heating up in a steamer of proposing is mainly worked in zone 3, and extractant and other component are separated in zone 3, and process can obtain pure extractant from the tower still after carrying and heating up in a steamer, and this extractant can return salty multiple use of extractant feed.Another of zone 3 act as enough steam to zone 1 and zone 2 is provided, and carries out smoothly to guarantee separation energy.
Embodiment 1
Material (weight ratio: alcohol 95 %, water 5%, azeotrope) from the middle part charging of partition wall extractive distillation column zone 1 side, flow velocity 250g/h, add extractant ethylene glycol simultaneously from tower top, flow velocity 1000g/h, the weight ratio of extractant and material is 4: 1, cat head discharging steam is after condenser 5 condensations, enter return tank 6, partial reflux, part is as the product discharging.Tower still still liquid returns salty multiple use of extractant feed, enters the ethanol recovery tower in the discharging of regional 2 middle side parts, and the discharging of ethanol recovery tower cat head is an azeotrope, returns charging and handles again, and the tower still is a pure water.
The tower operating condition is as follows:
Pressure: 0.1Mpa
Reflux ratio: 2: 1
Material feed state: saturated vapor
80-82 ℃ of extractant feed temperature
Reboiler temperature 210-212 ℃
Overhead product shows through gas chromatographic analysis: by weight: ethanol is 99.4% in the overhead product, and water is 0.6%, and tower bottoms is that middle ethylene glycol is 99.4%, and water is 0.6%, and ethanol is 43.1% in the side line extraction product, and water is 56.9%.
Embodiment 2
Material (weight ratio: normal heptane 64%, toluene 36%) from the middle part charging of the extractive distillation column of partition wall zone 1 side, flow velocity 250g/h adds extractant phenol, flow velocity 500g/h simultaneously from tower top, the weight ratio of extractant and material is 2: 1, cat head discharging steam enters return tank 6, partial reflux after condenser 5 condensations, part is as the product discharging, and the cat head discharging is a normal heptane.Tower still still liquid returns salty multiple use of extractant feed, enters the toluene recovery tower in the discharging of regional 2 middle side parts, and the discharging of toluene recovery tower cat head is returned charging and handled again, and the tower still is a toluene.
The tower operating condition is as follows:
Pressure: 0.1Mpa
Reflux ratio: 3: 1
Material feed state: saturated vapor
105-115 ℃ of extractant feed temperature
Reboiler temperature 195-200 ℃
Overhead product shows through gas chromatographic analysis: by weight: normal heptane is 99.2% in the overhead product, and toluene is 0.8%, and tower bottoms is that phenol is 99.3%, and toluene is 0.4%, and normal heptane is 14.7% in the side line extraction product, and toluene is 85.3%.
Claims (2)
1. the extraction rectifying method that has the partition wall rectifying column, it is characterized in that extractant, raw material enters in the tower from the extractant feed mouth of extractive distillation column right upper portion and the material inlet of bottom respectively, through extracting rectifying, need the cat head discharging of separation component from charging aperture one side, obtain the product A of required purity, the extractant that contains B component and a small amount of A enters the tower still and distills, the material that contains B component and a small amount of A will be from the left side discharging of partition wall, entering the material recovery tower further separates, simultaneously, the tower still obtains pure extractant, and this extractant returns salty multiple use of extractant feed.
2. realize the described device of claim 1 with extraction rectifying method of partition wall rectifying column, it is characterized in that a vertical partition wall extends to the bottom of tower from the top of tower, the height of dividing wall is less than the total height of tower, partition wall is divided into three parts with extractive distillation column inside, wherein the top of tower is separated wall and is divided into left and right sides two parts, the part that communicates in the lower end of partition wall is the total stripping section of the left and right sides, top two parts of tower, on the right side in next door, tower top two charging apertures are arranged, top is the charging aperture of extractant, and the middle part is the material feeding mouth.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510041506 CN1745868A (en) | 2005-08-17 | 2005-08-17 | Extraction rectifying method and rectifier with separated wall |
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| CN 200510041506 CN1745868A (en) | 2005-08-17 | 2005-08-17 | Extraction rectifying method and rectifier with separated wall |
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| CN1745868A true CN1745868A (en) | 2006-03-15 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417930B (en) * | 2008-11-28 | 2011-10-12 | 湖南阿斯达生化科技有限公司 | Method and apparatus for separating and purifying ethyl vanillin by decompression and continuous distillation in dividing wall column |
| CN105749575A (en) * | 2014-12-17 | 2016-07-13 | 新特能源股份有限公司 | Divided wall distillation column for recovery of tail gas absorption liquid and condensate liquid in polysilicon production, method and processing system |
| CN107400064A (en) * | 2016-05-18 | 2017-11-28 | 辽宁石油化工大学 | A kind of divided wall extractive distillation column refines the method containing water-acetonitrile |
| CN111989142A (en) * | 2018-03-29 | 2020-11-24 | 环球油品有限责任公司 | Controlling split flow of liquid reflux in divided wall column |
| CN112403015A (en) * | 2020-11-03 | 2021-02-26 | 汇智工程科技股份有限公司 | Device and method for separating acetone-n-heptane mixture by extractive distillation |
| CN113181681A (en) * | 2021-05-24 | 2021-07-30 | 烟台大学 | Device and method for separating butane and butene from mixed carbon four through partition wall extractive distillation |
-
2005
- 2005-08-17 CN CN 200510041506 patent/CN1745868A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417930B (en) * | 2008-11-28 | 2011-10-12 | 湖南阿斯达生化科技有限公司 | Method and apparatus for separating and purifying ethyl vanillin by decompression and continuous distillation in dividing wall column |
| CN105749575A (en) * | 2014-12-17 | 2016-07-13 | 新特能源股份有限公司 | Divided wall distillation column for recovery of tail gas absorption liquid and condensate liquid in polysilicon production, method and processing system |
| CN105749575B (en) * | 2014-12-17 | 2017-12-19 | 新特能源股份有限公司 | The divided-wall distillation column of tail gas absorption liquid and condensate liquid recovery in production of polysilicon, method, processing system |
| CN107400064A (en) * | 2016-05-18 | 2017-11-28 | 辽宁石油化工大学 | A kind of divided wall extractive distillation column refines the method containing water-acetonitrile |
| CN111989142A (en) * | 2018-03-29 | 2020-11-24 | 环球油品有限责任公司 | Controlling split flow of liquid reflux in divided wall column |
| CN111989142B (en) * | 2018-03-29 | 2022-06-21 | 环球油品有限责任公司 | Controlling split flow of liquid reflux in divided wall column |
| CN112403015A (en) * | 2020-11-03 | 2021-02-26 | 汇智工程科技股份有限公司 | Device and method for separating acetone-n-heptane mixture by extractive distillation |
| CN113181681A (en) * | 2021-05-24 | 2021-07-30 | 烟台大学 | Device and method for separating butane and butene from mixed carbon four through partition wall extractive distillation |
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