CN203677981U - Ionic liquid extractive distillation experimental device - Google Patents
Ionic liquid extractive distillation experimental device Download PDFInfo
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- CN203677981U CN203677981U CN201420011205.5U CN201420011205U CN203677981U CN 203677981 U CN203677981 U CN 203677981U CN 201420011205 U CN201420011205 U CN 201420011205U CN 203677981 U CN203677981 U CN 203677981U
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- extractive distillation
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Abstract
The utility model discloses an ionic liquid extractive distillation experimental device and relates to a chemical engineering experiment device. The device comprises an ionic liquid storage tank, an azeotrope raw material storage tank, a tower bottom, a tower top distillate storage tank and a flash tank. An ethyl acetate-isopropanol waste solvent mixture and other azeotrope series needing to be subjected to extractive distillation separation are filled in the azeotrope raw material storage tank; the azeotrope raw materials are heated from the azeotrope storage tank by virtue of a heat exchanger and enter an extractive distillation tower. The influence of factors such as the ionic liquid addition amount, a top reflux ratio, a system feeding amount and feeding thermal conditions on the plate efficiency and other tower performances can be calculated by measuring the feeding amount and the content of tower top and bottom distillate, and the ionic liquid is recovered in a flash tank. The device is designed by combining the characteristics of low volatility and high separation performance in the ionic liquid. According to the device, related aspects such as the operating conditions, the tower performance and stability of the ionic liquid in the ionic liquid extractive distillation process can be researched.
Description
Technical field
The utility model relates to a kind of chemical engineering experiment device, particularly relates to a kind of ion liquid abstraction rectification experimental apparatus.
Background technology
The azeotropic system of the conventional industrial chemicals composition such as ethyl acetate-isopropyl alcohol need separate by special extract rectification methods such as extracting rectifyings, and the traditional extraction agent of extracting rectifying is organic solvent, and its shortcoming is that consumption is large, energy consumption is high.In this case, the defect of the vapour pressure ignored of ionic liquid, advantage can the make up organic solvent such as chemical stability is good, boiling point is high, can be recycled, therefore becomes international study hotspot.The physical characteristics such as the separating power of ionic liquid and density, viscosity, surface tension, dissolubility all can affect its practical application.What at present research was more is its relatively can degree of sending out on azeotropic system impact, and less to the research of relevant device design and operation, the utility model device is mainly to design for the relation of research ion liquid abstraction agent combination property and tower.
Summary of the invention
The purpose of this utility model is to provide a kind of ion liquid abstraction rectification experimental apparatus, and the feature that this device combines the low volatility of ionic liquid, high separating property designs.Can study related fields such as operating condition in ion liquid abstraction distillation process and tower performance, ionic liquid stability by this device.
The purpose of this utility model is achieved through the following technical solutions:
A kind of ion liquid abstraction rectification experimental apparatus, comprises ionic liquid storage tank; Azeotropic system storage tank; Spinner flowmeter; Thermometer; Tower reactor; Tower reactor discharging condenser; Sample tap at the bottom of tower; Flash tank; Overhead storage tank; Electromagnetism reflux ratio controller; Tower top sample tap; Tower body thermometer; For overhead condenser; Centrifugal pump, described rectifying column is connected with overhead reflux device by electromagnetism reflux ratio controller, and ionic liquid is connected by pipeline with system to be separated, is provided with valve and flowmeter in pipeline; Rectifying column injection port, overhead storage tank and tower reactor distillate storage tank are established sample tap, in the pipeline after flash tank, establish sample tap; Rectifying column tower top, tower reactor are provided with thermocouple thermometer, and flash tank is provided with thermocouple and gauge measurement flash temperature and pressure; Tower top cooling water pipeline is connected with condenser at the bottom of tower, at the bottom of tower top and tower, is equipped with outlet valve, is provided with inlet valve in tower reactor, and tower body is equiped with filler.The filler position at tower top place is provided with charging aperture; Storage tank is connected with position charging aperture and extractive distillation column in tower, and its connecting place is provided with valve and spinner flowmeter, at the bottom of extractive distillation column, is connected with flash tank.
Described a kind of ion liquid abstraction rectification experimental apparatus, the tower body of described extractive distillation column tower is surrounded by heat-preservation cotton outward.
Described a kind of ion liquid abstraction rectification experimental apparatus, the rectifying section of described extractive distillation column and stripping section are respectively equipped with 3 and 2 thermocouple thermometers.
Described a kind of ion liquid abstraction rectification experimental apparatus, described tower body internal diameter is 25mm, tower body filler is 3 3mm stainless steel θ ring fillers, the about 1.5m of filler part total height, plate number is 50.
Advantage of the present utility model and effect are:
The utility model provides a kind of device of studying ion liquid abstraction rectifying separation and azeotropic system, and the feature that this device combines the low volatility of ionic liquid, high separating property designs.Device comprises sample tap at the bottom of ionic liquid storage tank, azeotropic system storage tank, spinner flowmeter, thermometer, tower reactor, tower reactor discharging condenser, tower, overhead storage tank, electromagnetism reflux ratio controller, tower top sample tap, sample introduction sample tap, overhead condenser, centrifugal pump etc.Can study related fields such as operating condition in ion liquid abstraction distillation process and tower performance, ionic liquid stability by this device.
Accompanying drawing explanation
Fig. 1 is that the utility model entirety forms schematic diagram.
The specific embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the utility model is described in further detail.
Fig. 1 is device and the flow process signal that the utility model adopts.Comprise extractive distillation column and extractant agent recovery flash tank.
In figure: 1: ionic liquid storage tank; 2: azeotropic system storage tank; 3: spinner flowmeter; 4: thermometer; 5: tower reactor; 6: tower reactor discharging condenser; 7: sample tap at the bottom of tower; 8: flash tank; 9: overhead storage tank; 10: electromagnetism reflux ratio controller; 11: tower top sample tap; 12: tower body thermometer; 13: be overhead condenser; 14: centrifugal pump.
The extractive distillation column tower body of the utility model experimental provision is all surrounded by heat-preservation cotton outward, is respectively equipped with 3 and 2 thermocouple thermometers at rectifying section and the stripping section of extractive distillation column.Tower body internal diameter is 25mm, and tower body filler is 3 3mm stainless steel θ ring fillers, the about 1.5m of filler part total height, and it is 90-120 ℃ that number of theoretical plate is about 50 extractive distillation column tower reactor temperature.Ion liquid abstraction agent adds from the top of extractive distillation column, and azeotropic system material liquid adds from rectifying column middle part.The mixture obtaining at the bottom of extractive distillation column tower enters in flash distillation recycling can, and flash tank decompression operation reclaims the ionic liquid obtaining and is cycled to repeat use.
Embodiment 1: extracting rectifying flow process as shown in Figure 1.When experiment starts, first open the cooling water of condenser at the bottom of tower top and tower, close the outlet valve at the bottom of tower top and tower, in tower reactor, add ionic liquid and ethyl acetate isopropyl alcohol mixed liquor 300ml that ratio of solvent (mass ratio) is 0.5:1; Close inlet valve, connect tower reactor heating power supply, be heated to boiling, until wetting tower body filler.Suitably regulate heating voltage; Keep infinite reflux, after stable system, open input and output material valve port, after lyate ion heating liquid through spinner flowmeter, in the filler position charging near tower top place; Ethyl acetate isopropyl alcohol flows out from storage tank 2, enters extractive distillation column approaching position charging aperture in tower; Regulate and monitoring feed rate by valve and spinner flowmeter, ionic liquid feed flow rates is 0.6ml/min, is 0.4ml/min containing alcohol waste liquid feed flow rates; Setting reflux ratio is 1.5, starts to reflux; Open tower top valve port and collect overhead distillate, open tower bottom valve mouth and collect tower bottom flow fluid, collect feeding liquid from feeding pipe, and monitor temperature changes.
Extracting rectifying tower bottom product isopropyl alcohol and ionic liquid mixture enter solvent recovery flash tank, and flash temperature is 100 ℃, the stable rear ionic liquid concentration of measuring.
Embodiment 2: extracting rectifying flow process as shown in Figure 1.When experiment starts, first open the cooling water of condenser at the bottom of tower top and tower, close the outlet valve at the bottom of tower top and tower, in tower reactor, add ionic liquid and ethyl acetate isopropyl alcohol mixed liquor 300ml that ratio of solvent (mass ratio) is 0.8:1; Close inlet valve, connect tower reactor heating power supply, be heated to boiling, until wetting tower body filler.Suitably regulate heating voltage, keep infinite reflux, after stable system, open input and output material valve port, after lyate ion heating liquid through spinner flowmeter, in the filler position charging near tower top place; Ethyl acetate isopropyl alcohol flows out from storage tank 2, enters extractive distillation column approaching position charging in tower; Regulate feed rate by valve and spinner flowmeter, ionic liquid feed flow rates is 0.5ml/min, is 0.3ml/min containing alcohol waste liquid feed flow rates; Setting reflux ratio is 2.0, starts to reflux; Open tower top valve port and collect overhead distillate, open tower bottom valve mouth collection tower bottom flow and go out liquid system, collect feeding liquid from feeding pipe, and monitor temperature changes.
Extracting rectifying tower bottom product isopropyl alcohol and ionic liquid mixture enter solvent recovery flash tank, and flash temperature is 100 ℃, the stable rear ionic liquid concentration of measuring.
Embodiment 3: extracting rectifying flow process as shown in Figure 1.When experiment starts, first open the cooling water of condenser at the bottom of tower top and tower, close the outlet valve at the bottom of tower top and tower, in tower reactor, add ionic liquid and ethyl acetate isopropyl alcohol mixed liquor 300ml that ratio of solvent (mass ratio) is 1:1; Close inlet valve, connect tower reactor heating power supply, be heated to boiling, until wetting tower body filler.Suitably regulate heating voltage, keep infinite reflux, after stable system, open input and output material valve port, after lyate ion heating liquid through spinner flowmeter, in the filler position charging near tower top place; Ethyl acetate isopropyl alcohol flows out from storage tank 2, enters extractive distillation column approaching position charging in tower; Regulate feed rate by valve port and spinner flowmeter, ionic liquid feed flow rates is 0.4ml/min, is 0.3ml/min containing alcohol waste liquid feed flow rates; Setting reflux ratio is 2.5, starts to reflux; Open tower top valve port and collect overhead distillate, open tower bottom valve mouth and collect tower bottom flow fluid, collect feeding liquid from feeding pipe, and monitor temperature changes.
Extracting rectifying tower bottom product isopropyl alcohol and ionic liquid mixture enter solvent recovery flash tank, and flash temperature is 100 ℃, the stable rear ionic liquid concentration of measuring.
Claims (4)
1. an ion liquid abstraction rectification experimental apparatus, comprises ionic liquid storage tank; Azeotropic system storage tank; Spinner flowmeter; Thermometer; Tower reactor; Tower reactor discharging condenser; Sample tap at the bottom of tower; Flash tank; Overhead storage tank; Electromagnetism reflux ratio controller; Tower top sample tap; Tower body thermometer; For overhead condenser; Centrifugal pump, is characterized in that, described rectifying column is connected with overhead reflux device by electromagnetism reflux ratio controller, and ionic liquid is connected by pipeline with system to be separated, is provided with valve and flowmeter in pipeline; Rectifying column injection port, overhead storage tank and tower reactor distillate storage tank are established sample tap, in the pipeline after flash tank, establish sample tap; Rectifying column tower top, tower reactor are provided with thermocouple thermometer, and flash tank is provided with thermocouple and gauge measurement flash temperature and pressure; Tower top cooling water pipeline is connected with condenser at the bottom of tower, at the bottom of tower top and tower, is equipped with outlet valve, is provided with inlet valve in tower reactor, and tower body is equiped with filler; The filler position at tower top place is provided with charging aperture; Storage tank is connected with position charging aperture and extractive distillation column in tower, and its connecting place is provided with valve and spinner flowmeter, at the bottom of extractive distillation column, is connected with flash tank.
2. a kind of ion liquid abstraction rectification experimental apparatus according to claim 1, is characterized in that, the tower body of described extractive distillation column tower is surrounded by heat-preservation cotton outward.
3. a kind of ion liquid abstraction rectification experimental apparatus according to claim 2, is characterized in that, the rectifying section of described extractive distillation column and stripping section are respectively equipped with 3 and 2 thermocouple thermometers.
4. a kind of ion liquid abstraction rectification experimental apparatus according to claim 3, is characterized in that, the tower body internal diameter of described extractive distillation column is 25mm, and tower body filler is 3 3mm stainless steel θ ring fillers, the about 1.5m of filler part total height, and plate number is 50.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104383711A (en) * | 2014-11-21 | 2015-03-04 | 沈阳化工大学 | Device and method for separating tert-butanol from water by taking 1-(2-chloroethyl)-3-methylimidazole chloride as extraction agent |
CN105413218A (en) * | 2015-12-17 | 2016-03-23 | 南京科技职业学院 | Immobilized type ionic liquid catalytic reaction rectification device |
-
2014
- 2014-01-09 CN CN201420011205.5U patent/CN203677981U/en not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104383711A (en) * | 2014-11-21 | 2015-03-04 | 沈阳化工大学 | Device and method for separating tert-butanol from water by taking 1-(2-chloroethyl)-3-methylimidazole chloride as extraction agent |
CN104383711B (en) * | 2014-11-21 | 2016-08-24 | 沈阳化工大学 | It is the devices and methods therefor of extractant tert-butyl alcohol from water with chlorination 1-(2-chloroethyl)-3-methylimidazole |
CN105413218A (en) * | 2015-12-17 | 2016-03-23 | 南京科技职业学院 | Immobilized type ionic liquid catalytic reaction rectification device |
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C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140702 Termination date: 20180109 |
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CF01 | Termination of patent right due to non-payment of annual fee |