CN210012777U - Azeotropic distillation separation device for mixed solvent - Google Patents
Azeotropic distillation separation device for mixed solvent Download PDFInfo
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- CN210012777U CN210012777U CN201920827764.6U CN201920827764U CN210012777U CN 210012777 U CN210012777 U CN 210012777U CN 201920827764 U CN201920827764 U CN 201920827764U CN 210012777 U CN210012777 U CN 210012777U
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Abstract
The utility model relates to an azeotropic distillation separation device of mixed solvent, in particular to an azeotropic mixed solvent for rectifying and purifying normal hexane and ethyl acetate, which comprises a rectification mechanism and an extraction separation mechanism, wherein the rectification mechanism comprises a preheating kettle, the rectification mechanism also comprises a rectification tower arranged at the upper end of the preheating kettle, and the rectification tower is communicated with the material outlet end of the preheating kettle; the gaseous material output of rectifying column passes through the condenser and is connected with extraction separating mechanism, the condenser with be provided with the reflux control ware between the extraction separating mechanism, extraction separating mechanism includes the extraction cauldron, extraction separating mechanism still include with a recovery tank and No. two recovery tanks of extraction cauldron intercommunication. The utility model discloses combine together rectification mechanism and extraction mechanism, under the effect of entrainer, with the normal hexane separation and the purification in the mixed solvent, improved mixed solvent's separation and purification effect greatly, and equipment is simple, easily operation.
Description
Technical Field
The utility model belongs to the technical field of the mixed solvent splitter, concretely relates to mixed solvent's azeotropic distillation separator.
Background
Ethyl acetate and n-hexane are widely used in the fields of coatings, medicines, paints and the like, and are often used as organic solvents in large quantities. In industrial processes, waste organic solutions of ethyl acetate and n-hexane are often formed. In order to reduce environmental pollution and save resources, the ethyl acetate and n-hexane waste liquid are required to be recycled and utilized.
At normal pressure, the ethyl acetate and the normal hexane can form the lowest azeotrope, the azeotropic temperature of the azeotrope is 65.2 ℃, and the azeotropic composition is ethyl acetate: n-hexane 0.343:0.657 (mole fraction). The azeotropic system of ethyl acetate and normal hexane can not be efficiently separated by adopting common rectification, therefore, the utility model adopts the azeotropic rectification separation method. In the azeotropic distillation production process, the selection of the entrainer needs to consider not only the degree of separation, but also the process and economic aspects. Meanwhile, the entrainer is required to be simple to recover, have good physical properties and good economic benefit.
The process and the separation and purification equipment not only can efficiently recover the ethyl acetate product in the waste liquid, but also have simple process flow operation, convenient recovery of the entrainer and cyclic utilization.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a simple structure, reasonable in design's azeotropic distillation separator of mixed solvent for solving above-mentioned problem.
The utility model discloses a following technical scheme realizes above-mentioned purpose:
an azeotropic distillation separation device for a mixed solvent, particularly for an azeotropic mixed solvent for rectifying and purifying normal hexane and ethyl acetate, comprises a distillation mechanism and an extraction separation mechanism, wherein the distillation mechanism comprises a preheating kettle, the preheating kettle is provided with a plurality of inlet and outlet ports, including an inlet pipe and a waste liquid discharge pipe, and the distillation mechanism further comprises a distillation tower arranged at the upper end of the preheating kettle, and the distillation tower is communicated with a material outlet end of the preheating kettle;
the gas material output end of the rectifying tower is connected with the extraction separation mechanism through a condenser, a reflux controller is arranged between the condenser and the extraction separation mechanism, the reflux controller is provided with a plurality of material output ends, the extraction separation mechanism comprises an extraction kettle, the input end of the extraction kettle is connected with one material output end of the reflux controller through a connecting pipe, a second control valve is arranged on the connecting pipe between the two, a material circulating pipe is arranged in the middle of the connecting pipe and is communicated with the rectifying tower, and a first control valve is arranged on the material circulating pipe;
the extraction separation mechanism further comprises a first recovery tank and a second recovery tank which are communicated with the extraction kettle, wherein the first recovery tank is used for collecting the n-hexane after extraction separation, and the second recovery tank is used for collecting the entrainer aqueous solution after extraction separation;
the extraction separating mechanism further comprises a third recovery tank and a fourth recovery tank which are connected with the output end of the reflux controller, and each recovery tank is provided with a third control valve and a fourth control valve respectively.
By adopting the technical scheme, the rectification mechanism is combined with the extraction mechanism, n-hexane in the mixed solvent is separated under the action of the entrainer, the subsequent extraction mechanism separates and purifies n-hexane, other components are collected one by one, the separation and purification effects of the mixed solvent are greatly improved, and the device is simple and is easy to operate.
As a further optimization scheme of the utility model, be provided with temperature sensor and heater in the rectifying column, the heater with set up in the output electric connection of the outside controller of rectifying column, temperature sensor's signal output part with the signal input part of controller is connected.
Through adopting above-mentioned technical scheme, when the temperature in the rectifying column is less than the required temperature of rectification, the controller will start the heater and heat the interior material of tower, guarantee that the interior material of tower rectifies under the suitable temperature, when the temperature in the rectifying column is higher than the required temperature of rectification, the work of heater will be stopped to the controller, through setting up temperature sensor, heater and controller, linkage effect between the three, reach the real-time regulation control to the temperature in the rectifying column, can satisfy the rectification operation of different miscella, improve the separation effect of rectification.
As the utility model discloses a further optimization scheme, azeotropic distillation separator still is provided with material circulation mechanism, material circulation mechanism include with the rectifying still that No. two recovery tank outputs are connected, rectifying still's output with preheating the cauldron intercommunication among the rectifying still.
By adopting the technical scheme, the azeotrope after rectification and purification is introduced into the preheating kettle and the rectifying tower again, so that the cyclic utilization of the azeotropic agent is realized, the production cost is reduced, and the utilization rate of the material is improved.
As a further optimization scheme of the utility model, the setting position of No. two control valves is in the lower extreme of material circulating pipe.
By adopting the technical scheme, the controllable circulation of the materials is ensured, and the mutual interference of the material circulation and the extraction separation operation is avoided.
The beneficial effects of the utility model reside in that:
1) the utility model combines the rectification mechanism and the extraction mechanism, under the action of the entrainer, the normal hexane in the mixed solvent is separated, and the subsequent extraction mechanism separates and purifies the normal hexane, other components are collected one by one, the separation and purification effect of the mixed solvent is greatly improved, and the device is simple and easy to operate;
2) the utility model achieves real-time adjustment and control of the temperature in the rectifying tower by arranging the temperature sensor, the heater and the controller and the linkage effect among the three, can meet the rectifying operation of different mixed solvents, and improves the separating effect of rectification;
3) the utility model leads the azeotrope after rectification and purification into the preheating kettle and the rectifying tower again through the material circulating mechanism, thereby realizing the cyclic utilization of the azeotropic agent, reducing the production cost and improving the utilization rate of the material;
4) the utility model discloses simple structure, stability is high, reasonable in design, the realization of being convenient for.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
In the figure: 1. preheating the kettle; 2. a rectifying tower; 3. a condenser; 4. a reflux controller; 5. an extraction kettle; 6. a first recovery tank; 7. a second recovery tank; 8. a rectifying still; 9. a third recovery tank; 10. a fourth recovery tank; 11. a feed pipe; 12. a waste liquid discharge pipe; 24. a first control valve; 45. a second control valve; 49. a third control valve; 410. and a fourth control valve.
Detailed Description
The present application will now be described in further detail with reference to the drawings, it should be noted that the following detailed description is given for illustrative purposes only and is not to be construed as limiting the scope of the present application, as those skilled in the art will be able to make numerous insubstantial modifications and adaptations to the present application based on the above disclosure.
Example 1
As shown in fig. 1, an azeotropic distillation separation device for a mixed solvent, specifically for an azeotropic mixed solvent of n-hexane and ethyl acetate, comprises a distillation mechanism and an extraction separation mechanism, wherein the distillation mechanism comprises a preheating kettle 1, the preheating kettle 1 is provided with a plurality of inlet and outlet ports, and comprises a feed pipe 11 and a waste liquid discharge pipe 12, the feed pipe 11 is used for inputting the mixed solvent to be separated into the preheating kettle 1, and the waste liquid discharge pipe 12 is used for discharging waste liquid finally left in the preheating kettle 1; the rectifying mechanism further comprises a rectifying tower 2 arranged at the upper end of the preheating kettle 1, the rectifying tower 2 is communicated with the material outlet end of the preheating kettle 1, a temperature sensor and a heater are arranged in the rectifying tower 2, the heater is electrically connected with the output end of a controller arranged outside the rectifying tower 2, the signal output end of the temperature sensor is connected with the signal input end of the controller, temperature signals in the rectifying tower 2 are transmitted to the controller through the temperature sensor, when the temperature in the rectifying tower 2 is lower than the required temperature for rectification, the controller heats materials in the tower by starting the heater, the materials in the tower are rectified at a proper temperature, when the temperature in the rectifying tower 2 is higher than the required temperature for rectification, the controller stops the operation of the heater, and by arranging the temperature sensor, the heater and the controller, the linkage effect among the three components achieves the real-time adjustment and control of the temperature in the rectifying tower 2, can meet the rectifying operation of different mixed solvents, and improves the separating effect of rectification.
The gas material output end of the rectifying tower 2 is connected with the extraction and separation mechanism through a condenser 3, a reflux controller 4 is arranged between the condenser 3 and the extraction and separation mechanism, the reflux controller 4 is used for improving the separation effect in the rectifying tower 2, and the reflux controller 4 is provided with a plurality of material output ends; the extraction separation mechanism comprises an extraction kettle 5, the extraction kettle 5 is used for separating mixed liquid of an entrainer and n-hexane, the input end of the extraction kettle 5 is connected with a material output end of the reflux controller 4 through a connecting pipe, a second control valve 45 is arranged on the connecting pipe between the two, a material circulating pipe is arranged in the middle of the connecting pipe, the material circulating pipe is communicated with the rectifying tower 2, a first control valve 24 is arranged on the material circulating pipe, materials in the rectifying tower 2 can be returned to the rectifying tower 2 after rectification through the material circulating pipe, multiple rectification cycles of the materials are achieved, and the rectification effect of the rectifying tower 2 is improved.
The extraction separation mechanism further comprises a first recovery tank 6 and a second recovery tank 7 which are communicated with the extraction kettle 5, wherein the first recovery tank 6 is used for collecting n-hexane after extraction separation, the second recovery tank 7 is used for collecting entrainer aqueous solution after extraction separation, water and n-hexane are utilized for being immiscible by inputting aqueous solvent into the extraction kettle 5, the water bath entrainer is further extracted, separated and purified in the mixed solvent of the n-hexane and the entrainer separated in the rectifying tower 2 and the extraction kettle 5 with the aqueous solvent, the n-hexane in the upper light phase is collected in the first collection tank, the aqueous solution of the entrainer is collected in the second collection tank, and separation and purification of the n-hexane in the n-hexane and ethyl acetate mixed solvent are realized.
Extraction separating mechanism still include with No. three recovery tank 9 and No. four recovery tank 10 that reflux controller 4's output is connected, and each recovery tank is provided with No. three control valve 49 and No. four control valve 410 respectively, No. three recovery tank 9 and No. four recovery tank 10 are arranged in retrieving transition fraction and the ethyl acetate fraction in n-hexane and the ethyl acetate mixed solvent respectively.
In order to realize the sufficient cyclic utilization of the entrainer, the azeotropic distillation separation device is further provided with a material circulation mechanism, the material circulation mechanism comprises a distillation kettle 8 connected with the output end of the second recovery tank 7, the output end of the distillation kettle 8 is communicated with a preheating kettle 1 in the distillation mechanism, the entrainer in the second recovery tank 7 is separated from the hydrosolvent through the distillation kettle 8, and the azeotrope after the distillation and purification is led into the preheating kettle 1 and a distillation tower 2 again, so that the cyclic utilization of the entrainer is realized, the production cost is reduced, and the utilization rate of the material is improved.
It should be noted that the entrainer is an acetone solvent, and the second control valve 45 is arranged at the lower end of the material circulating pipe, so that the controllable circulation of the material is ensured, and the mutual interference between the material circulation and the extraction separation operation is avoided.
The technological process of azeotropic distillation separator for mixed solvent includes the following steps:
stage one: preheating and rectifying purification of mixed solvent
Adding an azeotropic agent acetone solution into a mixed solvent of n-hexane and ethyl acetate, uniformly mixing, inputting into a preheating kettle 1, heating, introducing into a rectifying tower 2, and carrying out rectification and purification, wherein the n-hexane and acetone form an azeotrope and are preferentially led out;
and a second stage: separation and recovery of n-hexane and recycle of acetone solvent
An azeotrope formed by the normal hexane and the acetone which are led into the extraction kettle 5 through the reflux controller 4 is extracted with a water solvent in the extraction kettle 5, the normal hexane solvent and an acetone water solution are separated, and the normal hexane solvent and the acetone water solution are respectively led into a first recovery tank 6 and a second recovery tank 7; the water solution of acetone is rectified and separated from the rectifying still 8, and then is directly led into the preheating still 1 for recycling;
and a third stage: collection of the transition fraction
After the n-hexane is separated, a transition fraction consisting of acetone, n-hexane and ethyl acetate is separated in the rectifying tower 2; the transition fraction is directly led into a third recovery tank 9 through a reflux controller 4 after being condensed;
and a fourth stage: collection of Ethyl acetate
And finally discharging the ethyl acetate solvent from the rectifying tower 2, and introducing the ethyl acetate solvent into a fourth recovery tank 10 from a reflux controller 4, thereby completing the azeotropic distillation separation operation of the whole mixed solvent.
The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention.
Claims (4)
1. An azeotropic distillation separation device of mixed solvent, which is particularly used for rectifying and purifying the azeotropic mixed solvent of normal hexane and ethyl acetate, and is characterized in that: the device comprises a rectifying mechanism and an extraction separation mechanism, wherein the rectifying mechanism comprises a preheating kettle (1), the preheating kettle (1) is provided with a plurality of inlet and outlet ports, the preheating kettle comprises an inlet pipe (11) and a waste liquid discharge pipe (12), the rectifying mechanism further comprises a rectifying tower (2) arranged at the upper end of the preheating kettle (1), and the rectifying tower (2) is communicated with a material outlet end of the preheating kettle (1);
the gas material output end of the rectifying tower (2) is connected with an extraction separation mechanism through a condenser (3), a backflow controller (4) is arranged between the condenser (3) and the extraction separation mechanism, the backflow controller (4) is provided with a plurality of material output ends, the extraction separation mechanism comprises an extraction kettle (5), the input end of the extraction kettle (5) is connected with one material output end of the backflow controller (4) through a connecting pipe, a second control valve (45) is arranged on the connecting pipe between the two, a material circulating pipe is arranged in the middle of the connecting pipe, the material circulating pipe is communicated with the rectifying tower (2), and a first control valve (24) is arranged on the material circulating pipe;
the extraction and separation mechanism further comprises a first recovery tank (6) and a second recovery tank (7) which are communicated with the extraction kettle (5), wherein the first recovery tank (6) is used for collecting n-hexane after extraction and separation, and the second recovery tank (7) is used for collecting an entrainer aqueous solution after extraction and separation;
the extraction separation mechanism further comprises a third recovery tank (9) and a fourth recovery tank (10) which are connected with the output end of the backflow controller (4), and each recovery tank is provided with a third control valve (49) and a fourth control valve (410).
2. The azeotropic distillation separation device for mixed solvents according to claim 1, wherein: the device is characterized in that a temperature sensor and a heater are arranged in the rectifying tower (2), the heater is electrically connected with the output end of a controller arranged outside the rectifying tower (2), and the signal output end of the temperature sensor is connected with the signal input end of the controller.
3. The azeotropic distillation separation device for mixed solvents according to claim 1, wherein: azeotropic distillation separator still is provided with material circulation mechanism, material circulation mechanism include with rectifying still (8) that No. two recovery tank (7) outputs are connected, the output of rectifying still (8) with preheat cauldron (1) intercommunication among the rectifying mechanism.
4. The azeotropic distillation separation device for mixed solvents according to claim 1, wherein: the second control valve (45) is arranged at the lower end of the material circulating pipe.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920827764.6U CN210012777U (en) | 2019-06-03 | 2019-06-03 | Azeotropic distillation separation device for mixed solvent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920827764.6U CN210012777U (en) | 2019-06-03 | 2019-06-03 | Azeotropic distillation separation device for mixed solvent |
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| CN210012777U true CN210012777U (en) | 2020-02-04 |
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