CN105418370A - Method for separating mixed alcohol-water by continuous extractive rectification - Google Patents
Method for separating mixed alcohol-water by continuous extractive rectification Download PDFInfo
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- CN105418370A CN105418370A CN201410484677.7A CN201410484677A CN105418370A CN 105418370 A CN105418370 A CN 105418370A CN 201410484677 A CN201410484677 A CN 201410484677A CN 105418370 A CN105418370 A CN 105418370A
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Abstract
The present invention relates to a method for separating mixed alcohol-water by continuous extractive rectification, and relates to a chemical separation method, i.e. a method for separating mixed alcohol-water by continuous extractive rectification with water mixtures such as ethanol, n-propanol and isobutanol. The method comprises the steps: combining extractive rectification with general rectification, and gradually separating the mixed alcohol and the water by using a combined sub-step separation method of multiple towers so as to recover and obtain a component with high purity; achieving separation of the mixed alcohol and the water in an extractive rectification tower B1 by using ethylene glycol as an extractant, wherein atmospheric rectification is used in the tower with a reflux ratio of 1:1 to 10:1, the mixed alcohol is obtained from the tower top, and the solvent and the water are obtain from the tower bottom; recovering most of the solvent in a solvent recovery tower B4 for recycling; and after allowing the mixed alcohol to pass through towers B2 and B3, effectively separating the mixed alcohol, respectively. The method provided by the invention combines extractive rectification with general rectification, breaks azeotropy between alcohol and water by using an extractant, and recovers components with relatively high purity step by step by using multi-tower continuous separation, so that the method has higher economic and environmental benefits.
Description
Technical field
The present invention relates to a kind of chemical separating method, particularly relate to a kind of method of continuous extraction rectifying separation alcohol mixture-water, can be used in alcohol-water mixture, reclaiming valuable alcohols.
Background technology
Along with the day by day exhaustion of petroleum resources, future source of energy structure will turn to based on coal and Sweet natural gas, preparing low-carbon mixed alcohol by synthetic gas fuel is as an alternative produced by Sweet natural gas or gasification, more and more be subject to people's attention, but prepare in the technique of low-carbon alcohol at synthetic gas, inevitable generation a large amount of containing alcohol waste liquid, if by the various waste liquids produced in industrial production directly discharge can cause the serious wasting of resources and environmental pollution, obtain mixture of lower alcohols or the higher alcohols of purity has huge Significance for Environment and economic implications to reclaiming containing alcohol waste liquid.Low-carbon alcohol mixture has broad application prospects, sum up and mainly contain the following aspects: (1), as alternative fuel (2) clean gasoline additive (3) chemical and industrial chemicals (4) one of the means as gelatin liquefaction, realizes the alkylation of coal and solubilized and effectively transport.As liquefied petroleum gas (LPG) (LPG) surrogate; Directly as general chemistry solvent and for efficient power generation etc.
The traditional method of current domestic separation alcohol water system mainly contains: (1) constant boiling rectification method, its major advantage is that mechanization degree is high, output is large, quality is good, deficiency is that sequence of constant boiling and rectification facility investment is large, certainly will increase energy consumption owing to newly adding nonvariant boiling reagent gasification, the health of use to operator of conventional nonvariant boiling reagent benzene is harmful to, thus by gradually replace by the novel process of environmental protection.(2) membrane distillation method, but because mould material production cost is relatively high, therefore membrane separation technique also non-fully matured is not used widely.
Summary of the invention
The object of the present invention is to provide a kind of method of continuous extraction rectifying separation alcohol mixture-water, the method adopts extracting rectifying to be separated alcohol water mixed system with the method that conventional distillation combines, select separating effect preferably extraction agent ethylene glycol, and the more rational technical process of one is proposed, improve plant efficiency, save production cost.
The object of the invention is to be achieved through the following technical solutions:
A method for continuous extraction rectifying separation alcohol mixture-water, said method comprising the steps of:
(1) alcohol-water mixture material enters alcohol-water separation tower B1 in bubble point state, and extraction agent adds continuously near tower top position, and the overhead product of B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, the mixture of extraction solvent and water at the bottom of tower;
(2) B1 overhead product enters ethanol recovery tower B2 through interchanger H1 and pump P2, and tower top obtains high purity ethanol; Obtain the mixture of n-propyl alcohol and isopropylcarbinol at the bottom of tower, then enter n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3, tower top obtains high purity n-propyl alcohol, obtains high purity isopropylcarbinol at the bottom of tower;
(3) introduce solvent recovery tower B4 by the overhead product obtained at the bottom of B1 tower tower through interchanger H1 and pump P1, realize the recovery of solvent ethylene glycol, and recycle.
The method of said a kind of continuous extraction rectifying separation alcohol mixture-water, the extraction agent of extracting rectifying described in it is ethylene glycol, and in rectifying, glycol circulation uses.
The method of said a kind of continuous extraction rectifying separation alcohol mixture-water, described processing condition are as follows: B1 tower: total stage number 82, feed tray 60, reflux ratio 1.35; The total stage number 62 of 2 tower, feed tray 32, reflux ratio 2.63; The total stage number 84 of 3 tower, feed tray 40, reflux ratio 4.67; The total stage number 9 of 4 tower, feed tray 5, reflux ratio 0.47.
Advantage of the present invention and effect are:
The method of a kind of continuous extraction rectifying separation alcohol mixture-water of the present invention, in view of the deficiency in prior art, the maturation and extraction rectifying method possesses skills, solvent selection scope is larger, application is convenient, be easy to the advantages such as industrialization, the method that the present invention adopts extracting rectifying and conventional distillation to combine is separated alcohol water mixed system.1, select separating effect preferably extraction agent ethylene glycol, improve separation efficiency, reduce reflux ratio, saved energy consumption.2 propose the more rational technical process of one, improve plant efficiency, save production cost, have larger energy economy & environment benefit.
Accompanying drawing explanation
The continuous extraction rectification process schema of Fig. 1 designed by the present invention.
Embodiment
As shown in the figure: in figure: B1: extractive distillation column; 2: ethanol recovery tower; 3: n-propyl alcohol isopropylcarbinol Separation and Recovery tower; 4: solvent recovery tower;
Fig. 2 is extracting rectifying Experimental equipment.In figure 1: ethylene glycol storage tank; : containing alcohol waste tank; : spinner-type flowmeter; 4: thermometer; : tower reactor; : tower reactor discharging condenser; : thief hole at the bottom of tower; : tower reactor overhead product storage tank; : overhead product storage tank; 0: electromagnetism reflux ratio controller; 1: tower top thief hole; 2: tower body thief hole; 13 is overhead condenser.
Example 1: continuous extraction rectifying separation alcohol-water mixture flow process is with reference to Fig. 1, extractive distillation column is with reference to Fig. 2, tower body internal diameter is 25mm, tower body filler is 03 $ 3mm stainless steel 0 ring filler, filler part total height is about 1.6m, number of theoretical plate is about 80 pieces, has 3 and 2 tower body thief holes at the rectifying section of extractive distillation column and stripping section, is convenient to detect liquid phase composition content.When experiment starts, first open the water coolant of condenser at the bottom of tower top and tower, close tower top and the valve at the bottom of tower, add in tower reactor solvent ratio be 4:1 ethylene glycol with containing alcohol waste liquid mixed solution 300ml; Connect tower reactor heating power supply, be heated to boiling, until wetting tower body filler.Suitable adjustment heater voltage, keeps total reflux 15 minutes; Open charging valve port, solvent ethylene glycol through spinner-type flowmeter, near the filler position charging at tower top place; Flow out from storage tank 2 containing alcohol waste liquid, position charging enters extractive distillation column in close to tower; Regulate feeding rate by valve port and spinner-type flowmeter, ethylene glycol feed flow rates is 0.644ml/min, is 0.279ml/min containing alcohol waste liquid feed flow rates; Open reflux ratio controller, setting reflux ratio is 1.35, starts backflow; Open tower top valve port and collect overhead distillate; Open tower bottom valve mouth and collect tower bottom flow fluid; Every 5 minutes from thief hole sampling at the bottom of tower top and tower, detect composition content, after composition stablizes 1 hour, detect from 5 tower body thief holes samplings, then within each 15 minutes, get a sample, average.
Example 2: substantially identical with example 1, setting ethylene glycol feed flow rates is 0.644ml/min, is 0.279ml/min containing alcohol waste liquid feed flow rates, and setting reflux ratio is 1 ~ 3.
Example 3: substantially identical with example 1, setting reflux ratio is 1.35, and setting ethylene glycol feed flow rates is 0.4 ~ 0.8ml/min, is 0.2ml/min containing alcohol waste liquid feed flow rates.
Claims (3)
1. a method for continuous extraction rectifying separation alcohol mixture-water, is characterized in that, said method comprising the steps of:
(1) alcohol-water mixture material enters alcohol-water separation tower B1 in bubble point state, and extraction agent adds continuously near tower top position, and the overhead product of B1 tower is ethanol, n-propyl alcohol and isopropylcarbinol, the mixture of extraction solvent and water at the bottom of tower;
(2) B1 overhead product enters ethanol recovery tower B2 through interchanger H1 and pump P2, and tower top obtains high purity ethanol; Obtain the mixture of n-propyl alcohol and isopropylcarbinol at the bottom of tower, then enter n-propyl alcohol isopropylcarbinol recovery tower B3 through interchanger H3 and pump P3, tower top obtains high purity n-propyl alcohol, obtains high purity isopropylcarbinol at the bottom of tower;
(3) introduce solvent recovery tower B4 by the overhead product obtained at the bottom of B1 tower tower through interchanger H1 and pump P1, realize the recovery of solvent ethylene glycol, and recycle.
2. the method for the said a kind of continuous extraction rectifying separation alcohol mixture-water of claim 1, it is characterized in that, the extraction agent of described extracting rectifying is ethylene glycol, and in rectifying, glycol circulation uses.
3. the method for the said a kind of continuous extraction rectifying separation alcohol mixture-water of claim 1, it is characterized in that, described processing condition are as follows: 1 tower: total stage number 82, feed tray 60, reflux ratio 1.35; The total stage number 62 of 2 tower, feed tray 32, reflux ratio 2.63; The total stage number 84 of 3 tower, feed tray 40, reflux ratio 4.67; The total stage number 9 of B4 tower, feed tray 5, reflux ratio 0.47.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410484677.7A CN105418370A (en) | 2014-09-20 | 2014-09-20 | Method for separating mixed alcohol-water by continuous extractive rectification |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410484677.7A CN105418370A (en) | 2014-09-20 | 2014-09-20 | Method for separating mixed alcohol-water by continuous extractive rectification |
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| CN105418370A true CN105418370A (en) | 2016-03-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117674A (en) * | 2017-04-28 | 2017-09-01 | 南京科技职业学院 | A kind of method of extracting rectifying and reaction side line rectification process amino resin waste water |
| CN111377801A (en) * | 2018-12-28 | 2020-07-07 | 国家能源投资集团有限责任公司 | Method and system for refining low carbon alcohol |
| CN112707794A (en) * | 2020-12-25 | 2021-04-27 | 国家能源集团宁夏煤业有限责任公司 | Method for separating propanol from aqueous phase byproduct of Fischer-Tropsch synthesis |
-
2014
- 2014-09-20 CN CN201410484677.7A patent/CN105418370A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117674A (en) * | 2017-04-28 | 2017-09-01 | 南京科技职业学院 | A kind of method of extracting rectifying and reaction side line rectification process amino resin waste water |
| CN107117674B (en) * | 2017-04-28 | 2020-09-29 | 南京科技职业学院 | Method for treating amino resin wastewater by extractive distillation and reaction side-stream distillation |
| CN111377801A (en) * | 2018-12-28 | 2020-07-07 | 国家能源投资集团有限责任公司 | Method and system for refining low carbon alcohol |
| CN111377801B (en) * | 2018-12-28 | 2022-10-11 | 国家能源投资集团有限责任公司 | Method and system for refining low carbon alcohol |
| CN112707794A (en) * | 2020-12-25 | 2021-04-27 | 国家能源集团宁夏煤业有限责任公司 | Method for separating propanol from aqueous phase byproduct of Fischer-Tropsch synthesis |
| CN112707794B (en) * | 2020-12-25 | 2022-11-08 | 国家能源集团宁夏煤业有限责任公司 | Method for separating propanol from aqueous phase byproduct of Fischer-Tropsch synthesis |
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Application publication date: 20160323 |