CN109704919A - Water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method - Google Patents
Water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method Download PDFInfo
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- CN109704919A CN109704919A CN201811624338.9A CN201811624338A CN109704919A CN 109704919 A CN109704919 A CN 109704919A CN 201811624338 A CN201811624338 A CN 201811624338A CN 109704919 A CN109704919 A CN 109704919A
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- extractive distillation
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Abstract
The present invention provides a kind of water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation methods, the present invention destroys water-ethanol azeotropic system using Novel Extractant, it is finally recovered out methanol, the alcohol product of high-purity, flexible operation, cost of equipment less investment, extractant easily recycle, and can be recycled, production cost can be effectively reduced, methanol, purity of alcohol and the yield obtained using technical method of the invention is all larger than 99%.
Description
(1) technical field
The present invention relates to a kind of water-methanol based on choline chloride eutectic solvent-alcohol mixture separation of extractive distillation
Method belongs to the separation technology field of alcohol-water solution.
(2) background technique
Extracted etc. in Chemical Manufactures in heterocyclic compound preparation, medical material synthesis, traditional Chinese medicine ingredients, often use methanol,
The mixture of ethyl alcohol inevitably introduces other impurities, especially water in use process as reaction medium and extractant, because
And generate a large amount of alcohol solution.To reduce production cost and protection environment, methanol, ethyl alcohol need to be separated back from alcohol solution
It receives.
The boiling-point difference of methanol and ethyl alcohol is larger, and not azeotrope with water, it is easy to it is separated from alcohol solution, and ethyl alcohol
With water in 78.2 DEG C of azeotropic, and azeotropic group becomes the ethyl alcohol of 95.6% (mass fraction, similarly hereinafter) and 4.4% water.So processing
The difficult point of alcohol solution is separating alcohol, water binary system.For azeotropic mixture system and nearly azeotropic mixture system, industrial general use
Extracting rectifying is separated, thus the emphasis for being selected to research of extractant.
Eutectic solvent is considered as a kind of novel ionic liquid, is made of ammonium salt and complexant, wherein complexant can
For substances such as urea, carboxylic acid, ethylene glycol.Eutectic solvent has physicochemical properties similar with conventional ion liquid, and has
Have and synthesize the characteristics such as simple and environmental-friendly, and has been widely used in electrochemistry, catalysis, organic synthesis, dissolution, extraction and material
Expect chemical field.As a kind of novel green solvent, eutectic solvent have prepare simple, cheap, non-toxic degradable,
The advantages that saturated vapor forces down, design is strong, extracting rectifying application in can effectively reduce equipment investment, simplify separating technology,
Energy consumption is reduced, there is great application prospect.
(3) summary of the invention
The purpose of the present invention is to provide a kind of water-methanol-alcohol mixture extraction and rectification separation methods.This method chlorine
Change choline-ethylene glycol eutectic solvent as extractant, process is simple, and low energy consumption, the methanol isolated, alcohol product purity
It is high.
Equipment needed for continuous extraction rectification process is made of extractive distillation column, methanol column and solvent recovery tower.Extracting rectifying
Tower is mainly used as the separation of water-ethanol azeotropic system, and separating effect not only needs reasonable process flow and tower structure, but also
The factors such as dosage, feed entrance point to extractant all require.Methanol column is mainly used as the separation of methanol/ethanol system, for
Water-methanol-ethanol system, the present invention use choline chloride-ethylene glycol eutectic solvent for extractant, the behaviour completed by optimization
Make, is finally reached the separation to three.
Technical scheme is as follows:
A kind of water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method, the side
Method comprises the steps of:
(1) water-methanol-alcohol mixture and extractant are added in extractive distillation column, by extractive distillation column overhead extraction
Light component comprising methanol/ethanol, tower reactor produce aqueous and extractant heavy constituent；
The extractant is the eutectic solvent that choline chloride and ethylene glycol are formed with molar ratio 1:2；
The extractive distillation column number of plates be 30~50, operating condition be normal pressure (101.3kPa), solvent ratio be 0.5~
5.0, reflux ratio is 0.5~3.0, and tower top temperature is 65~79 DEG C, and bottom temperature is 120~150 DEG C；
Water-methanol-the alcohol mixture enters in extractive distillation column from the 15th~40 block of column plate of extractive distillation column,
Extractant enters extractive distillation column from the 3rd~10 block of column plate；
(2) light component obtained in step (1) is introduced into methanol column, by methanol column overhead extraction methanol, tower reactor produces second
Alcohol；
The methanol column number of plates is 30~50, and operating condition is normal pressure (101.3kPa), and reflux ratio is 12~20, tower top
Temperature is 64~66 DEG C, and bottom temperature is 77~79 DEG C；
The light component enters in methanol column from the 18th~20 block of column plate of methanol column；
(3) heavy constituent obtained in step (1) is introduced into solvent recovery tower, by solvent recovery tower overhead extraction water, tower reactor
Extractant is produced, and gained extractant is introduced into extractive distillation column and is recycled；
The solvent recovery tower number of plates is 30~50, and operating condition is 10~20kPa, and reflux ratio is 0.8~2.0, tower
Pushing up temperature is 43~48 DEG C, and bottom temperature is 150~155 DEG C；
The heavy constituent enters in solvent recovery tower from the 18th~20 block of column plate of solvent recovery tower.
The present invention has the advantages that destroying water-ethanol azeotropic system using Novel Extractant, it is finally recovered out high-purity
Methanol, alcohol product, flexible operation, cost of equipment less investment, extractant easily recycle, and can be recycled, production can be effectively reduced
Cost.Methanol, purity of alcohol and the yield obtained using technical method of the invention is all larger than 99%.
(4) Detailed description of the invention
Fig. 1 is the device of the invention and flow diagram.
(5) specific embodiment
With reference to the accompanying drawing, by specific embodiment, the present invention is further illustrated, but protection scope of the present invention
It is not limited to that.
It according to shown in Fig. 1, is operated using continuity, by alcohol solution raw material from the essence equipped with 30~50 pieces of theoretical cam curves
It evaporates and enters in extractive distillation column at the 15th~40 block of theoretical tray of tower, extractant enters extraction from the 3rd~10 block of theoretical tray
Take rectifying column；After extracting rectifying, methanol/ethanol mixed liquor enters in methanol column after overhead extraction, after separation, first
Alcohol is produced from methanol column overhead extraction, ethyl alcohol from methanol column tower reactor；The mixed solution of extractant and water is by extractive distillation column tower reactor
Enter solvent recovery tower after extraction, after separation, water continues to lead to from the overhead extraction of solvent recovery tower, extractant after tower reactor extraction
The extractant feed mouth for crossing extractive distillation column enters in extractive distillation column, is recycled.
Embodiment 1:
By process flow shown in attached drawing 1, raw material is formed: methanol 17.3% (mass fraction, the same below), ethyl alcohol 75.2%,
Water 7.5%, treating capacity 1000kg/hr, extractant are choline chloride-ethylene glycol, and technological parameter is as shown in table 1.
The operating parameter of 1 embodiment 1 of table
The top of the distillation column produced quantity 926kg/hr, composition: methanol 18.7%, ethyl alcohol 81.2%.Methanol column overhead extraction amount
173kg/hr contains methanol 99.9%, yield 99.86%；Tower reactor contains ethyl alcohol 99.8%, yield 99.97%.
Embodiment 2:
By process flow shown in attached drawing 1, raw material composition: methanol 20% (mass fraction, the same below), ethyl alcohol 65%, water
15%, treating capacity 1000kg/hr, extractant are choline chloride-ethylene glycol, and technological parameter is as shown in table 2.
The operating parameter of 2 embodiment 2 of table
The top of the distillation column produced quantity 850kg/hr, composition: methanol 29.4%, ethyl alcohol 70.4%.Methanol column overhead extraction amount
200kg/hr contains methanol 99.8%, yield 99.84%；Tower reactor contains ethyl alcohol 99.3%, yield 99.95%.
Comparative example:
By process flow shown in attached drawing 1, raw material is formed: methanol 17.3% (mass fraction, the same below), ethyl alcohol 75.2%,
Water 7.5%, treating capacity 1000kg/hr, extractant are ethylene glycol, and technological parameter is as shown in table 3.
3 operating parameter of table
| Extractive distillation column | Methanol column | Solvent recovery tower | |
| Number of theoretical plate | 34 | 30 | 30 |
| Reflux ratio | 0.8 | 14 | 0.5 |
| Feed entrance point | Raw material: the 26th piece of theoretical plate | 12nd piece of theoretical plate | 25th piece of theoretical plate |
| Solvent ratio | 1.0 | - | - |
| Operating pressure | 101.3kPa | 101.3kPa | 10kPa |
Methanol column overhead contains methanol 92.9%, and tower reactor contains ethyl alcohol 90.67%.
Claims (1)
1. a kind of water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method, feature exist
In the method comprises the steps of:
(1) water-methanol-alcohol mixture and extractant are added in extractive distillation column, include by extractive distillation column overhead extraction
The light component of methanol/ethanol, tower reactor produce aqueous and extractant heavy constituent；
The extractant is the eutectic solvent that choline chloride and ethylene glycol are formed with molar ratio 1:2；
The extractive distillation column number of plates is 30~50, and operating condition is normal pressure, and solvent ratio is 0.5~5.0, reflux ratio 0.5
~3.0, tower top temperature is 65~79 DEG C, and bottom temperature is 120~150 DEG C；
Water-methanol-the alcohol mixture enters in extractive distillation column from the 15th~40 block of column plate of extractive distillation column, extraction
Agent enters extractive distillation column from the 3rd~10 block of column plate；
(2) light component obtained in step (1) is introduced into methanol column, by methanol column overhead extraction methanol, tower reactor produces ethyl alcohol；
The methanol column number of plates is 30~50, and operating condition is normal pressure, and reflux ratio is 12~20, and tower top temperature is 64~66
DEG C, bottom temperature is 77~79 DEG C；
The light component enters in methanol column from the 18th~20 block of column plate of methanol column；
(3) heavy constituent obtained in step (1) is introduced into solvent recovery tower, by solvent recovery tower overhead extraction water, tower reactor extraction
Extractant, and gained extractant is introduced into extractive distillation column and is recycled；
The solvent recovery tower number of plates is 30~50, and operating condition is 10~20kPa, and reflux ratio is 0.8~2.0, tower top temperature
Degree is 43~48 DEG C, and bottom temperature is 150~155 DEG C；
The heavy constituent enters in solvent recovery tower from the 18th~20 block of column plate of solvent recovery tower.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811624338.9A CN109704919A (en) | 2018-12-28 | 2018-12-28 | Water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811624338.9A CN109704919A (en) | 2018-12-28 | 2018-12-28 | Water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662161A (en) * | 2020-06-28 | 2020-09-15 | 浙江工业大学 | Method for separating water-ethanol-isopropanol mixture by extractive distillation |
| CN116836754A (en) * | 2023-05-29 | 2023-10-03 | 河南工业大学 | Method for removing heterocyclic amine from sesame oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449969A (en) * | 2013-09-05 | 2013-12-18 | 天津科林泰克科技有限公司 | Method and production unit for separating methanol-ethanol-isopropanol-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 |
-
2018
- 2018-12-28 CN CN201811624338.9A patent/CN109704919A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449969A (en) * | 2013-09-05 | 2013-12-18 | 天津科林泰克科技有限公司 | Method and production unit for separating methanol-ethanol-isopropanol-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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662161A (en) * | 2020-06-28 | 2020-09-15 | 浙江工业大学 | Method for separating water-ethanol-isopropanol mixture by extractive distillation |
| CN111662161B (en) * | 2020-06-28 | 2023-02-03 | 浙江工业大学 | Method for separating water-ethanol-isopropanol mixture by extractive distillation |
| CN116836754A (en) * | 2023-05-29 | 2023-10-03 | 河南工业大学 | Method for removing heterocyclic amine from sesame oil |
| CN116836754B (en) * | 2023-05-29 | 2024-03-12 | 河南工业大学 | Method for removing heterocyclic amine from sesame oil |
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