CN216170007U - Inorganic salt-organic solvent separator - Google Patents
Inorganic salt-organic solvent separator Download PDFInfo
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- CN216170007U CN216170007U CN202122589600.4U CN202122589600U CN216170007U CN 216170007 U CN216170007 U CN 216170007U CN 202122589600 U CN202122589600 U CN 202122589600U CN 216170007 U CN216170007 U CN 216170007U
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Abstract
The utility model relates to an inorganic salt-organic solvent separation device, and belongs to the technical field of chemical industry. The device comprises a solvent distillation tank, a condenser, an organic solvent recovery tank, an azeotrope recovery tank, a vacuum mechanism and an inorganic salt solution collection tank; wherein the organic solvent is an organic solvent which has a boiling point lower than that of water and forms an azeotrope with water; the top of the solvent distillation tank is respectively provided with a water inlet and a feed inlet, and the outside of the solvent distillation tank is provided with a heating mechanism; the gas phase import of condenser is connected through the top of pipeline with the solvent distillation retort, and the liquid phase export of condenser is connected with organic solvent recovery jar and azeotrope recovery jar through the pipeline respectively, and organic solvent recovery jar and azeotrope recovery jar are connected with vacuum mechanism through the pipeline respectively, and the inorganic salt solution collecting vessel passes through the pipeline and is connected with the bottom of solvent distillation retort. The device can realize the effective separation of inorganic salt and organic solvent.
Description
Technical Field
The utility model relates to an inorganic salt-organic solvent separation device, and belongs to the technical field of chemical industry.
Background
The solid-liquid reaction with the participation of inorganic salt is a common reaction mode in fine chemical engineering. In order to increase the concentration of inorganic salts in the reaction system and increase the reaction rate, a strongly polar solvent such as methanol, ethanol, n-propanol, isopropanol or acetonitrile is often selected as a reaction medium. Although the use of such solvents can effectively improve the production efficiency, the inorganic salt is dissolved therein to form a solution with extremely high viscosity due to the strong polarity of the solvents, and simultaneously, a large amount of solid remains at the bottom, thereby improving the difficulty of the post-reaction treatment. If conventional distillation processes are used, the organic solvent is only partially evaporated and recovered, and a large amount of the solvent remains in the system due to strong interaction with the inorganic salts. The salts contain organic matters and can only be treated by adopting an incineration method, thereby causing the waste of raw materials and causing environmental pollution.
SUMMERY OF THE UTILITY MODEL
In view of the above, the present invention aims to provide an inorganic salt-organic solvent separation apparatus.
In order to achieve the purpose, the technical scheme of the utility model is as follows:
an inorganic salt-organic solvent separation device comprises a solvent distillation tank, a condenser, an organic solvent recovery tank, an azeotrope recovery tank, a vacuum mechanism and an inorganic salt solution collection tank; wherein the organic solvent is an organic solvent which has a boiling point lower than that of water and forms an azeotrope with water; the top of the solvent distillation tank is respectively provided with a water inlet and a feed inlet, and the outside of the solvent distillation tank is provided with a heating mechanism; the gas phase import of condenser is connected through the top of pipeline with the solvent distillation retort, and the liquid phase export of condenser is connected with organic solvent recovery jar and azeotrope recovery jar through the pipeline respectively, and organic solvent recovery jar and azeotrope recovery jar are connected with vacuum mechanism through the pipeline respectively, and the inorganic salt solution collecting vessel passes through the pipeline and is connected with the bottom of solvent distillation retort.
The method for separating inorganic salt from organic solvent by using the device comprises the following steps:
(1) adding inorganic salt-organic solvent to be separated into a solvent distillation tank through a feeding hole, controlling the pressure of a vacuum mechanism control device to be-0.1 MPa to normal pressure, starting a heating mechanism to heat the solvent distillation tank, condensing distillate materials through a condenser, then feeding the distillate materials into an organic solvent recovery tank until no materials are distilled, and finishing distillation.
(2) Adding water preheated to above 50 ℃ into the solvent distillation tank through a water inlet to dissolve residual materials.
(3) The pressure of a vacuum mechanism control device is between-0.1 MPa and normal pressure, a heating mechanism is started to heat a solvent distillation tank, a distillate material is condensed by a condenser and then enters an azeotrope recovery tank, the concentration of an organic solvent in the distillate material is monitored in real time, and when the distillate material does not contain the organic solvent, heating is stopped; and collecting the water phase at the bottom of the solvent distillation tank into an inorganic salt solution collection tank.
Furthermore, a stirring mechanism is arranged in the solvent distillation tank.
Further, vacuum mechanism includes vacuum buffer tank and vacuum pump, organic solvent retrieves jar and azeotrope and retrieves jar and be connected with vacuum buffer tank through the pipeline respectively, and vacuum buffer tank passes through the pipeline and is connected with the vacuum pump.
Furthermore, the connecting pipelines are all provided with valves.
Further, the organic solvent is methanol, ethanol, n-propanol, isopropanol or acetonitrile.
Advantageous effects
The inorganic salt-organic solvent separation device firstly recovers the organic solvent through primary distillation; adding water to dissolve residual materials, completely releasing the residual organic solvent in the inorganic salt, completely recovering the azeotrope from the solution by adopting secondary distillation according to the characteristic that the azeotrope formed by the polar solvent and the water is easy to separate, and converting the azeotrope into materials with economic value; finally, the inorganic salt exists in the form of aqueous solution with good fluidity, the viscosity of the system is effectively reduced, the inorganic salt smoothly flows out from the bottom of the tank, and the inorganic salt without organic solvent can be recovered by processes such as spray drying and the like. The device realizes the effective separation of inorganic salt and organic solvent.
Drawings
Fig. 1 is a schematic structural diagram of the apparatus described in embodiment 1 of the present invention.
The device comprises a solvent distillation tank, a solvent 2-condenser, an organic solvent 3-recovery tank, an azeotrope 4-recovery tank, a vacuum buffer tank 5-a vacuum pump 6-an inorganic salt solution collection tank 7-a water inlet 11-a feed inlet 12-a heating mechanism 13-and a stirring mechanism 14-and is characterized in that the solvent distillation tank is connected with the inorganic salt solution collection tank through a pipeline.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
An inorganic salt-organic solvent separation device comprises a solvent distillation tank 1, a condenser 2, an organic solvent recovery tank 3, an azeotrope recovery tank 4, a vacuum mechanism and an inorganic salt solution collection tank 7, wherein the organic solvent is an organic solvent which has a boiling point lower than that of water and forms an azeotrope with the water; the top of the solvent distillation tank 1 is respectively provided with a water inlet 11 and a feed inlet 12, and the outside of the solvent distillation tank 1 is provided with a heating mechanism 13; the gas phase import of condenser 2 is connected with the top of solvent distillation retort 1 through the pipeline, and the liquid phase export of condenser 2 is connected with organic solvent recovery tank 3 and azeotrope recovery tank 4 through the pipeline respectively, and organic solvent recovery tank 3 and azeotrope recovery tank 4 are connected with vacuum mechanism through the pipeline respectively, and inorganic salt solution collection tank 7 is connected with the bottom of solvent distillation retort 1 through the pipeline.
The method for separating inorganic salt from organic solvent by using the device comprises the following steps:
(1) adding inorganic salt-organic solvent to be separated into a solvent distillation tank 1 through a feeding hole 12, controlling the pressure of a vacuum mechanism control device to be-0.1 MPa to normal pressure, starting a heating mechanism 13 to heat the solvent distillation tank 11, condensing distillate materials through a condenser 2, then feeding the distillate materials into an organic solvent recovery tank 3 until no materials are distilled, and ending distillation.
(2) Water preheated to 50 ℃ or higher is added to the solvent distillation tank 1 through the water inlet 11 to dissolve the residual materials.
(3) The pressure of a vacuum mechanism control device is-0.1 MPa to normal pressure, a heating mechanism 13 is started to heat a solvent distillation tank 11, a distillate material is condensed by a condenser 2 and then enters an azeotrope recovery tank 4, the concentration of an organic solvent in the distillate material is monitored in real time, and when the distillate material does not contain the organic solvent, heating is stopped; the water phase at the bottom of the solvent distillation tank 11 is collected into an inorganic salt solution collection tank 7.
And a stirring mechanism 14 is arranged in the solvent distillation tank 1.
The vacuum mechanism comprises a vacuum buffer tank 5 and a vacuum pump 6, the organic solvent recovery tank 3 and the azeotrope recovery tank 4 are respectively connected with the vacuum buffer tank 5 through pipelines, and the vacuum buffer tank 5 is connected with the vacuum pump 6 through a pipeline.
And valves are arranged on the connecting pipelines.
The organic solvent is methanol, ethanol, n-propanol, isopropanol or acetonitrile.
Example 2
A method for separating zinc chloride-isopropanol, the method steps comprising:
(1) adding 1000g of zinc chloride-isopropanol mixed material into a 2L solvent distillation tank 1, reducing the pressure of the system to-0.095 MPa through a vacuum mechanism, starting a heating mechanism for heating, and gradually raising the temperature along with the continuous discharging process until the temperature reaches 90 ℃. The evaporated material is converted into liquid state by a condenser 2 and enters an organic solvent recovery tank 3 for collection. Finally, 586g of liquid material were collected and isopropanol was analyzed by gas chromatography with a purity of 98%.
(2) After completion of the distillation, 400g of water preheated to 60 ℃ was added from the water inlet 11 to the solvent distillation pot 1 to dissolve the residual material into an aqueous solution.
(3) The pressure of the system is reduced to-0.095 MPa by a vacuum mechanism, a heating mechanism is started to heat, and the temperature is gradually increased along with the continuous discharging process until the temperature reaches 90 ℃. The evaporated material is converted into liquid state by the condenser 2 and enters the azeotrope recovery tank 4 for collection. A small amount of distillate was taken every 10min and analyzed by infrared spectrometer, and when the distillate contained no more isopropanol, distillation was stopped and 66g of distillate was collected. The aqueous phase was taken from the bottom of the solvent distillation pot 1 to an inorganic salt solution collection pot 7, and 725g of the aqueous phase was collected.
Example 3
A method for separating potassium fluoride-methanol, the method steps comprising:
(1) adding 1000g of potassium fluoride-methanol mixed material into a 2L solvent distillation tank 1, starting a heating mechanism to heat under normal pressure, and gradually raising the temperature along with the continuous discharging process until the temperature reaches 90 ℃. The evaporated material is converted into liquid state by a condenser 2 and enters an organic solvent recovery tank 3 for collection. Finally, 677g of a liquid material was collected, and methanol having a purity of 99% was analyzed by gas chromatography.
(2) After completion of the distillation, 300g of water preheated to 60 ℃ was added from the water inlet 11 to the solvent distillation pot 1 to dissolve the residual material into an aqueous solution.
(3) Under normal pressure, a heating mechanism is started to heat, and the temperature is gradually increased along with the continuous discharging process until the temperature reaches 90 ℃. The evaporated material is converted into liquid state by the condenser 2 and enters the azeotrope recovery tank 4 for collection. A small amount of distillate was taken every 10min and analyzed by infrared spectrometer, and when the distillate contained no more isopropanol, distillation was stopped and 16g of distillate was collected. The aqueous phase was taken from the bottom of the solvent distillation tank 1 to an inorganic salt solution collection tank 7, and 593g of the aqueous phase was collected altogether.
Example 4
A process for the separation of sodium chloride-ethanol, the process steps comprising:
(1) adding 1000g of sodium chloride-ethanol mixed material into a 2L solvent distillation tank 1, reducing the pressure of the system to-0.05 MPa through a vacuum mechanism, starting a heating mechanism for heating, and gradually raising the temperature along with the continuous discharging process until the temperature reaches 80 ℃. The evaporated material is converted into liquid state by a condenser 2 and enters an organic solvent recovery tank 3 for collection. Finally, 533g of liquid material was collected, and ethanol having a purity of 98% was analyzed by gas chromatography.
(2) After completion of the distillation, 400g of water preheated to 60 ℃ was added from the water inlet 11 to the solvent distillation pot 1 to dissolve the residual material into an aqueous solution.
(3) The pressure of the system is reduced to-0.05 MPa by a vacuum mechanism, a heating mechanism is started to heat, and the temperature is gradually increased along with the continuous discharging process until the temperature reaches 90 ℃. The evaporated material is converted into liquid state by the condenser 2 and enters the azeotrope recovery tank 4 for collection. A small amount of distillate was taken every 10min and analyzed by infrared spectrometer, and when the distillate contained no more isopropanol, distillation was stopped and 43g of fraction was collected. The aqueous phase was taken from the bottom of the solvent distillation tank 1 to an inorganic salt solution collection tank 7, and 799g of the aqueous phase was collected altogether.
In summary, the present invention includes but is not limited to the above embodiments, and any equivalent substitutions or partial modifications made under the spirit and principle of the present invention should be considered within the protection scope of the present invention.
Claims (5)
1. An inorganic salt-organic solvent separation device, characterized in that: comprises a solvent distillation tank (1), a condenser (2), an organic solvent recovery tank (3), an azeotrope recovery tank (4), a vacuum mechanism and an inorganic salt solution collection tank (7); wherein the organic solvent is an organic solvent which has a boiling point lower than that of water and forms an azeotrope with water; the top of the solvent distillation tank (1) is respectively provided with a water inlet (11) and a feed inlet (12), and the outside of the solvent distillation tank (1) is provided with a heating mechanism (13); the gas phase inlet of the condenser (2) is connected with the top of the solvent distillation tank (1) through a pipeline, the liquid phase outlet of the condenser (2) is respectively connected with the organic solvent recovery tank (3) and the azeotrope recovery tank (4) through pipelines, the organic solvent recovery tank (3) and the azeotrope recovery tank (4) are respectively connected with a vacuum mechanism through pipelines, and the inorganic salt solution collection tank (7) is connected with the bottom of the solvent distillation tank (1) through a pipeline.
2. The inorganic salt-organic solvent separating apparatus as claimed in claim 1, wherein: and a stirring mechanism (14) is arranged in the solvent distillation tank (1).
3. The inorganic salt-organic solvent separating apparatus as claimed in claim 1, wherein: the vacuum mechanism comprises a vacuum buffer tank (5) and a vacuum pump (6), the organic solvent recovery tank (3) and the azeotrope recovery tank (4) are respectively connected with the vacuum buffer tank (5) through pipelines, and the vacuum buffer tank (5) is connected with the vacuum pump (6) through a pipeline.
4. The inorganic salt-organic solvent separating apparatus as claimed in claim 1, wherein: and valves are arranged on the connecting pipelines.
5. The inorganic salt-organic solvent separating apparatus as claimed in claim 1, wherein: the organic solvent is methanol, ethanol, n-propanol, isopropanol or acetonitrile.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122589600.4U CN216170007U (en) | 2021-10-26 | 2021-10-26 | Inorganic salt-organic solvent separator |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122589600.4U CN216170007U (en) | 2021-10-26 | 2021-10-26 | Inorganic salt-organic solvent separator |
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| CN216170007U true CN216170007U (en) | 2022-04-05 |
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2021
- 2021-10-26 CN CN202122589600.4U patent/CN216170007U/en active Active
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