CN1106710A - Single-tower atmospheric intermittent extractive rectification method - Google Patents
Single-tower atmospheric intermittent extractive rectification method Download PDFInfo
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- CN1106710A CN1106710A CN 94118258 CN94118258A CN1106710A CN 1106710 A CN1106710 A CN 1106710A CN 94118258 CN94118258 CN 94118258 CN 94118258 A CN94118258 A CN 94118258A CN 1106710 A CN1106710 A CN 1106710A
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- tower
- distillation column
- extractive distillation
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Abstract
The said method is suitable for the separation of azeotrope and mixture with very little boiling point difference, and it is realized in an equipment comprising extracting rectification tower, evaporator, solvent temp controlling tank. Technologically, it features that the raw material liquid is introduced batchwise into the evaporator, from which the vapor phase enters the tower, partial liquid condensed in the tower returns to the evaporator and the solvent recovered directly inside the tower is pumped for reuse. Compared with continuous extractive rectification process, the said method is simple, flexible and easy to control. In addition, it can also realize batch-type extractive rectification of multicomponent mixture.
Description
The invention belongs to a kind of innovation of extracting rectifying, it has widened the application of extracting rectifying.
Traditional extracting rectifying has only the continued operation mode, and for the separation of two component mixtures, the system that needs two towers formations just can finish, and one of them is an extractive distillation column, and another is a solvent recovery tower.Material to be separated is sent into extractive distillation column continuously by pump in the operation, and the heavy ends material at the bottom of the tower and the mixed liquor of solvent are also sent into solvent recovery tower continuously by pump, and the solvent delivery after will being reclaimed by pump is again gone into extraction tower and recycled.For the separation of multicomponent mixture, then the tower that need be made of a plurality of towers that comprise solvent recovery tower (the tower number is identical with the component number of mixture to be separated) is to finish.Because two towers or a plurality of tower of continuous extraction rectifying mode must guarantee synchronous steady state operation, thereby its equipment is more, the systematic comparison complexity not only need to be equipped with the perfect control instrument, and operation easier is bigger.It is applicable to larger production occasion, and for small scale, in batches less, the production process of periodic intermittent, industry such as fine chemistry industry for example, the continuous extraction distillation technology fails to be applied always.
The object of the present invention is to provide a kind of single-tower atmospheric intermittent extractive rectification method, this method be specially adapted to production scale little, in batches less, the azeotropic mixture of periodic intermittent or the separation of the minimum mixture of boiling-point difference.
For achieving the above object, the present invention adopts following technical proposals to be realized.At the extractive distillation column that is provided with washing section, extracting rectifying section, exhausting section, tower still by, and on the device that constituted of evaporimeter, solvent temperature controlling groove, circulating pump, overhead condenser, return tank, product receiving tank, carry out under the normal pressure batch extracting rectified, its technology characteristics is: one, disposable being stored in the evaporimeter of material liquid to be separated, and this evaporimeter is vapour phase and enters in the tower from the extracting rectifying pars infrasegmentalis of extractive distillation column certainly, and part condensate material is back in the evaporimeter by the top of exhausting section in the tower.Two, solvent (extractant) is disposable is stored in the tower still, delivers to the solvent temperature controlling groove through circulating pump, and advances tower by this groove from the extracting rectifying section top of tower with suitable temperature, dirty then and directly flow back in the tower still after the extractive distillation column exhausting section is reclaimed.
Accompanying drawing is a process flow diagram of the present invention.Wherein 1 is evaporimeter, 2 is the tower still, and 3 is circulating pump, and 4 is the exhausting section of extractive distillation column, 5 is the exhausting section condenser of extractive distillation column, 6 is the solvent temperature controlling groove, and 7 is the rectifying section of extractive distillation column, and 8,9 is receiving tank, 10 distillate valve for product, 11 is the washing section of extractive distillation column, and 12 is return tank, and 13 is overhead condenser.
Specific implementation process of the present invention: at first with the disposable input evaporimeter 1 of material liquid to be separated, the solvent temperature controlling groove 6 of more a part of solvent (extractant) being packed into, and make its liquid level just in time reach overfall, pack another part solvent into tower still 2 to the operate as normal liquid level at last.Tower still 2 at first begins heating, when the solvent in the tower still reaches the set point of temperature value, start circulating pump 3 and make solvent begin circulation, after this should suitably regulate the cooling water flow that adds heat and solvent temperature controlling groove of tower still respectively, their temperature is remained in separately the set point of temperature scope always.This moment, evaporimeter began heating, opened the cooling water of the exhausting section condenser 5 of overhead condenser 13 and extractive distillation column simultaneously.Steam begins to rise into tower after the boiling of the material liquid in the evaporimeter, and after the liquid level rising of return tank 12 reached normal operation position, then the driving of extractive distillation column startup was finished.After this should keep the stable of each strand fluid flow in the operation.Along with continuing of operation, purity liquid can improve gradually until the product purity that reaches regulation in the return tank of top of the tower 12.Open and suitably regulate product this moment and flow out valve 10, begin the product distillate is collected into corresponding receiving tank gradually.Purity liquid descends gradually in return tank, and jar in a mean concentration when being about to be lower than product purity and requiring, close product and flow out valve 10, stop all heating and all cooling waters simultaneously, stop circulating pump 3, this moment EO.
Compare with traditional continuous extraction rectifying, the characteristics of single tower batch fractionating method of the present invention are: equipment is simple, small investment, flexible operation, control are convenient, be specially adapted in the industries such as fine chemistry industry and pharmacy small scale, in batches less, the feed separation process of periodic intermittent.
The present invention is not only applicable to the batch extracting rectified separation of bi-component azeotropic mixture and the minimum mixture of boiling-point difference, and can realize the batch extracting rectified of multicomponent mixture.Therefore, the present invention has good application prospects.
Embodiment 1:
Raw material to be separated: industrial alcohol (is formed: alcohol 95 %, water: 5%)
Alcohol product purity: greater than 99%
Solvent: ethylene glycol (purity 99%) (above-mentioned composition is percetage by weight)
It is as follows to adopt batch extracting rectified (packed tower) to implement the separation processes data:
70 millimeters of tower internal diameter: Φ (the Dixon ring filler of interior dress Φ 4 * 4)
Extracting rectifying section number of theoretical plate: 35
Washing section number of theoretical plate: 4
Exhausting section number of theoretical plate: 10
Ratio of solvent: 6.0
Reflux ratio: 4.0～8.5
Tower still temperature: 210～215 ℃
Solvent is gone into the tower temperature: 80～82 ℃
Embodiment 2:
Raw material to be separated is formed: normal heptane 35%, hexahydrotoluene 35%, toluene 30%
Normal heptane product purity: greater than 98.5%
Methyl cyclohexanol product purity: greater than 98.5%
Solvent: phenol (purity 99%) (above-mentioned composition is percetage by weight)
It is as follows to adopt batch extracting rectified (packed tower) to implement the separation processes data:
70 millimeters of tower internal diameter: Φ (the Dixon ring filler of interior dress Φ 4 * 4)
Extracting rectifying section number of theoretical plate: 20
Washing section number of theoretical plate: 5
Exhausting section number of theoretical plate: 12
Ratio of solvent: 7.5
Reflux ratio: 6.0～11.0
Tower still temperature: 192～201 ℃
Solvent is gone into the tower temperature: 104～120 ℃
Claims (1)
1, a kind of single-tower atmospheric intermittent extractive rectification method, it is the extractive distillation column that is provided with washing section, extracting rectifying section, exhausting section, tower still by, and implement on evaporimeter, solvent temperature controlling groove, the device that circulating pump, overhead condenser, return tank, receiving tank constituted, its technology characteristics is:
(1) material to be separated is disposable is stored in the evaporimeter, and this evaporimeter is gas phase and enters in the tower from the extracting rectifying pars infrasegmentalis of extractive distillation column certainly, and part condensate material is back in the evaporimeter by the top of the exhausting section of extractive distillation column in the tower,
(2) in the disposable tower still that is stored in extractive distillation column of solvent (extractant), deliver to the solvent temperature controlling groove through circulating pump, and advance tower by this groove from the extracting rectifying section top of extractive distillation column with suitable temperature, dirty then and after the extractive distillation column exhausting section is reclaimed, directly flow back in the tower still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94118258 CN1106710A (en) | 1994-11-18 | 1994-11-18 | Single-tower atmospheric intermittent extractive rectification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94118258 CN1106710A (en) | 1994-11-18 | 1994-11-18 | Single-tower atmospheric intermittent extractive rectification method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1106710A true CN1106710A (en) | 1995-08-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN 94118258 Pending CN1106710A (en) | 1994-11-18 | 1994-11-18 | Single-tower atmospheric intermittent extractive rectification method |
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| CN (1) | CN1106710A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317049C (en) * | 2005-07-26 | 2007-05-23 | 天津大学 | Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue |
| CN100363409C (en) * | 2006-08-06 | 2008-01-23 | 湖南百利工程科技有限公司 | Technique of refining solvent in process of producing synthetic rubber |
| CN100387688C (en) * | 2005-11-17 | 2008-05-14 | 中国矿业大学 | Oil coal cinder extracting process and equipment |
| CN100418940C (en) * | 2006-09-28 | 2008-09-17 | 天津大学 | Theoretical plate aided double temperature control intermittent rectifying process for separating isopropanol from n-propanol |
| CN102180791A (en) * | 2011-04-13 | 2011-09-14 | 天津大学 | Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification |
| CN102247709A (en) * | 2011-04-12 | 2011-11-23 | 彭长根 | Environment-friendly type low-temperature extraction agent and preparation method thereof |
| CN102350075A (en) * | 2011-07-11 | 2012-02-15 | 李保国 | Purification apparatus for organic solvents |
| CN106563285A (en) * | 2016-10-10 | 2017-04-19 | 天津科技大学 | Rectification apparatus for high-salinity material |
-
1994
- 1994-11-18 CN CN 94118258 patent/CN1106710A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317049C (en) * | 2005-07-26 | 2007-05-23 | 天津大学 | Batch extractive distillation separating method of acetonitrile-methylbenzene azeotropic mixtrue |
| CN100387688C (en) * | 2005-11-17 | 2008-05-14 | 中国矿业大学 | Oil coal cinder extracting process and equipment |
| CN100363409C (en) * | 2006-08-06 | 2008-01-23 | 湖南百利工程科技有限公司 | Technique of refining solvent in process of producing synthetic rubber |
| CN100418940C (en) * | 2006-09-28 | 2008-09-17 | 天津大学 | Theoretical plate aided double temperature control intermittent rectifying process for separating isopropanol from n-propanol |
| CN102247709A (en) * | 2011-04-12 | 2011-11-23 | 彭长根 | Environment-friendly type low-temperature extraction agent and preparation method thereof |
| CN102247709B (en) * | 2011-04-12 | 2014-07-30 | 彭长根 | Environment-friendly type low-temperature extraction agent and preparation method thereof |
| CN102180791A (en) * | 2011-04-13 | 2011-09-14 | 天津大学 | Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification |
| CN102350075A (en) * | 2011-07-11 | 2012-02-15 | 李保国 | Purification apparatus for organic solvents |
| CN106563285A (en) * | 2016-10-10 | 2017-04-19 | 天津科技大学 | Rectification apparatus for high-salinity material |
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