CN219783871U - Continuous double-phase liquid-phase extraction separation device for solid phase removal - Google Patents
Continuous double-phase liquid-phase extraction separation device for solid phase removal Download PDFInfo
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- CN219783871U CN219783871U CN202320768165.8U CN202320768165U CN219783871U CN 219783871 U CN219783871 U CN 219783871U CN 202320768165 U CN202320768165 U CN 202320768165U CN 219783871 U CN219783871 U CN 219783871U
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- tube
- reaction tube
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- separation
- discharge
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- 238000000926 separation method Methods 0.000 title claims abstract description 41
- 239000007791 liquid phase Substances 0.000 title claims abstract description 20
- 239000012071 phase Substances 0.000 title claims abstract description 14
- 238000000605 extraction Methods 0.000 title claims abstract description 13
- 239000007790 solid phase Substances 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000003860 storage Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 4
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 210000003298 dental enamel Anatomy 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000010924 continuous production Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 12
- 239000007788 liquid Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 229910001629 magnesium chloride Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000001311 chemical methods and process Methods 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910000856 hastalloy Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A continuous double-phase liquid phase extraction separation device for solid phase removal comprises a reaction tube (1) and a separation tube (2); a penetrating stirring paddle (3) is arranged in the reaction tube along the central shaft, a flow separation baffle (4) is arranged on the inner wall, 2 feed inlets are arranged at the lower end, 1 discharge outlet is arranged at the upper end, and a reaction tube heat insulation jacket (5) is sleeved on the outer side surface; the middle part of the separating tube is provided with a feed inlet, the upper end and the lower end are respectively provided with 1 discharge port, and the outer side surface of the separating tube is sleeved with a separating tube heat-insulating jacket (11); the discharge port of the reaction tube is connected with the feed port of the separation tube through a feed pipeline; the reaction tube is characterized in that 2 feed inlets of the reaction tube are respectively connected with a raw material tank (6) through a feed pipeline, a feed pump (7) and a flowmeter (8) are arranged on the feed pipeline, and discharge outlets at the upper end and the lower end of the separation tube are connected with a storage tank (9) through discharge pipelines. The utility model can realize the continuous process of the two-phase liquid phase extraction separation, improves the production efficiency and the product stability, and has no harsh requirements on equipment.
Description
Technical Field
The utility model belongs to the technical field of devices for removing solid impurities in a liquid phase in a chemical process, and particularly relates to a double-phase liquid-phase extraction separation device for removing a solid phase.
Background
A large number of chemical reactions are involving solids, and many chemical processes involve the removal of solid impurities in the liquid phase. Currently, tank reactors are still in large scale, and therefore, as a process in chemical processes, solid impurity removal is still performed in a batch or semi-batch process in the tank reactor. Because the removal of certain solid impurities has obvious heat release, the adoption of the kettle type reactor has certain danger; when using a tank reactor, the efficiency is generally improved by increasing the volume or number of reaction equipment, and the process is controlled more severely. Under the increasing importance of the national security production, the impurity removal process is changed, the production efficiency is improved, and the method has a very positive effect on promoting the development of the industry.
The continuous operation based on the tubular reactor is a feasible way for improving the production efficiency and the safety. However, at present, continuous operation is mainly focused on chemical reaction processes, but is rarely applied to washing and other processes.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model provides a continuous double-phase liquid-phase extraction separation device for solid phase removal, so as to improve the production efficiency, the process safety and the product stability in the process.
The technical scheme adopted by the utility model is as follows:
a continuous double-phase liquid phase extraction separation device for solid phase removal comprises a reaction tube and a separation tube; the reaction tube is internally provided with stirring paddles along a central shaft, the inner wall of the reaction tube is provided with a flow separation baffle, the lower end of the reaction tube is provided with 2 feed inlets, the upper end of the reaction tube is provided with 1 discharge outlet, and the outer side surface of the reaction tube is sleeved with a reaction tube heat insulation jacket; the middle part of the separating tube is provided with a feed inlet, the upper end and the lower end are respectively provided with 1 discharge port, and the outer side surface of the separating tube is sleeved with a separating tube heat-insulating jacket; the discharge port of the reaction tube is connected with the feed port of the separation tube through a feed pipeline; the reaction tube is characterized in that 2 feed inlets of the reaction tube are respectively connected with a raw material tank through a feed pipeline, a feed pump and a flowmeter are arranged on the feed pipeline, and discharge outlets at the upper end and the lower end of the separation tube are connected with a storage tank through discharge pipelines.
Further, the reaction tube is an enamel reaction tube or a quartz reaction tube.
Further, the separating tube is an enamel separating tube or a quartz separating tube.
Further, the stirring paddle is a penetrating stirring paddle, and comprises a central shaft and stirring paddles which are arranged at intervals along the height of the central shaft, and the top of the central shaft extends out of the reaction tube and is connected with a motor.
Further, a flow control valve is arranged on the discharging pipeline.
The utility model can continuously inject the liquid phase target product containing solid phase impurities and the washing liquid into the reaction tube according to a certain proportion, start the stirrer and the circulating water, and carry out the reaction in the reaction tube. After the reaction tube is filled, the mixed solution after the reaction is completed flows to the separation tube. Due to the density difference of the two phases, the mixed solution is layered up and down in the separation tube. After the separating tube is filled, a discharge hole at the lower end of the separating tube is opened to a certain extent, heavy components flow out from the discharge hole, and light components flow out from the discharge hole at the upper end of the separating tube.
The utility model can realize complete continuous removal of solid impurities in the liquid phase, improves the stability of products, improves the production efficiency, greatly reduces the process danger, and is safe and reliable.
Drawings
Fig. 1 is a schematic view of the apparatus of the present utility model.
Description of the embodiments
In order to make the technical scheme and advantages of the present utility model more apparent, the present utility model will be further described in detail with reference to the following examples.
As shown in FIG. 1, the continuous two-phase liquid phase extraction and separation device comprises a reaction tube 1 and a separation tube 2. The reaction tube is internally provided with a stirring paddle 3 along the central shaft, the inner wall is provided with a flow separation baffle 4 for reducing the circular motion of liquid, the lower end is provided with 2 feed inlets, the upper end is provided with 1 discharge port, and the outer side face is sleeved with a reaction tube heat-insulation jacket 5. The stirring paddle 3 is a penetrating stirring paddle and comprises a central shaft 3a and stirring paddles 3b which are arranged at intervals along the height of the central shaft, and the top of the central shaft extends out of the reaction tube and is connected with a motor 10. The stirring paddle is driven by a motor to rotate. The middle part of the separating tube is provided with a feed inlet, the upper end and the lower end are respectively provided with 1 discharge port, and the outer side surface is sleeved with a separating tube heat-insulating jacket 11. The discharge port of the reaction tube is connected with the feed port of the separation tube through a feed pipeline; the 2 feed inlets of reaction tube are connected with the feed tank 6 through the feed pipeline respectively, are provided with feed pump 7 and flowmeter 8 on the feed pipeline, the discharge gate of lower extreme passes through ejection of compact pipeline connection storage tank 9 on the separator tube. Two of the feed tanks, one for storing liquid phase chemicals containing solid phase impurities and one for storing washing liquid. The reaction tube is an enamel reaction tube or a quartz reaction tube, and the separation tube is an enamel separation tube or a quartz separation tube, so that acid and alkali corrosion resistance can be realized. A flow control valve may be provided on the discharge line to control the discharge.
Examples
The device provided by the utility model is used for removing sodium chloride suspended in ethyl acetate. The reaction tube is made of quartz, the height is 1200mm, the inner diameter of the reaction tube is 80mm, the volume occupied by stirring is deducted, and the single tube liquid holdup (namely the volume of the reaction cavity) is about 3.6L; the separating tube is made of quartz, the height of the separating tube is 1500mm, the inner diameter of the separating tube is 50mm, and the liquid holdup of a single tube is about 2.94L.
Closing a discharge hole at the lower end of the separation tube, continuously injecting ethyl acetate containing sodium chloride stored in one raw material tank and washing water stored in the other raw material tank into the reaction tube at the rates of 40mL/min and 60mL/min respectively, starting a motor, rotating a stirring paddle, adjusting the rotating speed to 150rad/min, starting circulating water, and adjusting the temperature to 30 ℃. After about 40min, the material reached the outlet of the reaction tube and flowed to the separation tube. And (5) continuously injecting materials. The material flowing to the separating tube is layered in the tube, the upper layer is ethyl acetate, and the lower layer is washing water containing sodium chloride. After about 70min, the separating tube is filled with the material, a discharge hole at the lower end of the separating tube is opened, and the discharge amount is adjusted to 60mL/min. At this time, the washing water containing sodium chloride flows out from the lower discharge port to the lower storage tank, and pure ethyl acetate flows out from the upper discharge port to the upper storage tank.
Examples
The device of the utility model is used for removing suspended magnesium chips in diethyl ether. The quality of the reaction tube is preferably quartz, the height is 1200mm, the inner diameter of the reaction tube is 80mm, the volume occupied by stirring is subtracted, and the single tube liquid holdup (i.e. the volume of the reaction cavity) is about 3.6L; the quality of the separating tube is preferably quartz, the height of the separating tube is 1500mm, the inner diameter of the separating tube is 50mm, and the liquid holdup of a single tube is about 2.94L. Other suitable materials, such as hastelloy, may be used for the reaction and separation tubes.
Closing a discharge hole at the lower end of the separation tube, continuously injecting diethyl ether containing magnesium chips and washing diluted hydrochloric acid respectively stored in two raw material tanks into the reaction tube at the rates of 25mL/min and 25mL/min, starting a motor, rotating a stirring paddle, adjusting the rotating speed to 300rad/min, starting circulating water, and adjusting the temperature to 5 ℃. The hydrogen generated in the reaction process flows along the reaction tube to the separation tube and flows out from a discharge hole at the upper end of the separation tube. After about 80 minutes, the liquid phase material reached the outlet of the reaction tube and flowed to the separation tube. And (5) continuously injecting materials. The material flowing to the separating tube is layered in the tube, the upper layer is diethyl ether, and the lower layer is mixed solution of magnesium chloride and hydrogen chloride. After about 140min, the separating tube is filled with the material, a discharge hole at the lower end of the separating tube is opened, and the discharge amount is adjusted to 25mL/min. At this time, the mixed solution of magnesium chloride and hydrogen chloride flows out from the lower discharge port to enter the lower storage tank, and pure diethyl ether flows out from the upper discharge port to enter the upper storage tank.
Examples
The device provided by the utility model is used for removing suspended magnesium chloride in butyl ether. The reaction tube is enamel, the height is 3500mm, the inner diameter of the reaction tube is 400mm, the occupied volume of the stirring paddle is deducted, and the single tube liquid holdup (namely the volume of the reaction cavity) is about 220L; the separating tube is enamel, the height is 3000mm, the inner diameter is 280mm, and the single tube liquid holdup is about 185L.
Closing a discharge hole at the lower end of the separation tube, continuously injecting butyl ether containing magnesium chloride and washing water respectively stored in two raw material tanks into the reaction tube at the speed of 3L/min and 12L/min respectively, starting a motor, rotating a stirring paddle, adjusting the rotating speed to 75rad/min, starting circulating water, and adjusting the temperature to 25 ℃. After about 15 minutes, the liquid phase material reached the outlet of the reaction tube and flowed to the separation tube. And (5) continuously injecting materials. The material flowing to the separating tube is layered in the tube, the upper layer is butyl ether, and the lower layer is magnesium chloride water solution. After about 30min, the separating tube is filled with the material, the discharge ports at the upper end and the lower end are opened, and the discharge amount is adjusted to be 12L/min. At this time, the magnesium chloride aqueous solution flows out from the lower discharge port and enters the lower storage tank, and the pure butyl ether flows out from the upper discharge port and enters the upper storage tank.
It should be noted that the foregoing is only used for further detailed description of the technical solution of the present utility model, and should not be construed as limiting the scope of the application, and that the non-essential modifications made by those skilled in the art based on the disclosure of the present utility model are all within the scope of the present utility model.
Claims (5)
1. A continuous two-phase liquid phase extraction separation device for solid phase removal, characterized in that the device comprises a reaction tube (1) and a separation tube (2); a stirring paddle (3) is arranged in the reaction tube along the central shaft, a flow separation baffle (4) is arranged on the inner wall, 2 feed inlets are arranged at the lower end, 1 discharge outlet is arranged at the upper end, and a reaction tube heat insulation jacket (5) is sleeved on the outer side surface; the middle part of the separating tube is provided with a feed inlet, the upper end and the lower end are respectively provided with 1 discharge port, and the outer side surface of the separating tube is sleeved with a separating tube heat-insulating jacket (11); the discharge port of the reaction tube is connected with the feed port of the separation tube through a feed pipeline; the reaction tube is characterized in that 2 feed inlets of the reaction tube are respectively connected with a raw material tank (6) through a feed pipeline, a feed pump (7) and a flowmeter (8) are arranged on the feed pipeline, and discharge outlets at the upper end and the lower end of the separation tube are connected with a storage tank (9) through discharge pipelines.
2. A continuous two-phase liquid phase extraction separation apparatus for solid phase removal according to claim 1, wherein the reaction tube (1) is an enamel reaction tube or a quartz reaction tube.
3. The continuous two-phase liquid phase extraction separator for solid phase removal according to claim 1, wherein the separator tube is an enamel separator tube or a quartz separator tube.
4. A continuous two-phase liquid phase extraction separation apparatus for solid phase removal according to claim 1, 2 or 3, wherein the stirring paddle (3) is a penetrating stirring paddle, comprising a central shaft (3 a) and stirring paddles (3 b) arranged at intervals along the height of the central shaft, and the top of the central shaft extends to the outside of the reaction tube and is connected with a motor (10).
5. A continuous two-phase liquid phase extraction separation apparatus for solid phase removal according to claim 1 or 2 or 3, wherein a flow control valve is provided on the discharge line.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320768165.8U CN219783871U (en) | 2023-04-10 | 2023-04-10 | Continuous double-phase liquid-phase extraction separation device for solid phase removal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320768165.8U CN219783871U (en) | 2023-04-10 | 2023-04-10 | Continuous double-phase liquid-phase extraction separation device for solid phase removal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN219783871U true CN219783871U (en) | 2023-10-03 |
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ID=88156593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202320768165.8U Active CN219783871U (en) | 2023-04-10 | 2023-04-10 | Continuous double-phase liquid-phase extraction separation device for solid phase removal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN219783871U (en) |
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2023
- 2023-04-10 CN CN202320768165.8U patent/CN219783871U/en active Active
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