Liquid-liquid reaction cooling crystallization device
By setting a reflux tube and a stirring paddle in the reaction cylinder of the liquid-liquid reaction cooling crystallization device, and using the refrigerant system of the cooling cylinder, the problem of improving reaction efficiency and separation effect without increasing energy consumption in the existing equipment is solved, and an efficient liquid-liquid reaction cooling crystallization process is achieved.
Patent Information
- Application Number
- CN202420653257.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-01
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2034-04-01
AI Technical Summary
Existing liquid-liquid reaction crystallization equipment is difficult to improve reaction efficiency without increasing energy consumption and realize effective separation of crystals and solutions, especially in areas where the temperature difference between reaction crystallization and precipitation crystallization is large.
A liquid-liquid reaction cooling crystallization device is designed, including a reaction cylinder and a cooling cylinder. By setting a reflux tube and a stirring paddle in the reaction cylinder, the material mixing degree is increased by centrifugal force, and the temperature is reduced through the refrigerant system of the cooling cylinder, so as to achieve effective separation of crystals.
Without increasing energy consumption, the reaction efficiency and the separation effect between the crystal and the solution are improved, the product output rate and quality are improved, and it is suitable for areas with large temperature differences in reaction crystallization and precipitation crystallization.
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Figure CN222658620U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to a liquid-liquid reaction cooling crystallization device, belonging to the technical field of crystallization equipment. Background Art
[0002] Reaction crystallization refers to the process of chemical reaction between gas and liquid or between liquid and liquid to produce insoluble or insoluble solid phase substances. The utility model mainly focuses on liquid-liquid reaction crystallization. Liquid-liquid reaction crystallization is an important method in the production and refining process of chemical pharmaceutical and implant industry products. At present, the equipment used for liquid-liquid reaction crystallization is diverse. Improving the reaction efficiency of the reaction crystallizer plays a decisive role in improving work efficiency. Improving the mixing degree of the system is one of the important ways to speed up the reaction speed. After the liquid-liquid reaction is completed, in most cases, the temperature of the reactant system is high, resulting in the high solubility of the crystal in the solution and it is not easy to precipitate completely, which affects the product yield to a certain extent. Cooling crystallization refers to cooling and cooling down to make the crystallization system a supersaturated solution, and the fine crystals produced after the reaction gradually precipitate from the system. This method effectively solves the problem that the temperature of the liquid-liquid reactant system is high and the crystals after the reaction are high in the solution and not easy to precipitate completely. Because the temperature requirements of the two methods of reaction crystallization and cooling crystallization are quite different, there is currently no method that can combine the two well.
[0003] In order to improve the working efficiency of the reaction crystallizer, the prior art has adopted a variety of means: for example, the patent with application announcement number CN210752662U discloses a reaction crystallization kettle device, which includes an equipment shell, an inner sleeve, a rotating motor on the top of the device, a rotating shaft sleeved with a reducer, a vertical rod fixedly connected to the reducer rotating shaft, a rotating seat is provided on the side of the vertical rod, and a rotating rod is fixedly sleeved inside the rotating seat. By arranging a rotating rod and a horizontal stirring rod on the side of the vertical rod, the medium in the inner sleeve is flipped up and down and stirred left and right, respectively, to improve the reaction efficiency of the medium. For another example, the patent application publication number CN2640593Y discloses a precipitation crystallization reactor device, which is divided into two parts: a reaction tank and a precipitation crystallization zone. The reaction tank is composed of a head and a tank body, which is provided with a feed port and a discharge port. An inverted cone is provided in the tank body, which divides the inner cavity of the reaction tank into a precipitation reaction zone inside the cone and a precipitation crystallization zone outside the cone. A pipe mouth for drawing out the upper solution of the precipitation crystallization zone is provided on the tank body. The device can realize continuous production of precipitation crystallization of protein solutions, and has a good precipitation separation effect.
[0004] The above-mentioned prior art improves the reaction efficiency or precipitation separation effect by improving the equipment structure, but patent CN210752662U increases kinetic energy consumption, and continuous stirring is not conducive to static separation of crystals, which brings a large workload for subsequent filtration or centrifugal separation. Patent CN2640593Y does not take into account the temperature difference between reaction crystallization and precipitation crystallization, or in other words, the patent is only applicable to the field where the temperature difference between reaction crystallization and precipitation crystallization is small, and the patent has no outstanding improvement opinions on improving the reaction efficiency of reaction crystallization. Therefore, it is particularly important to invent a device that improves the reaction efficiency without increasing energy consumption and realizes the effective separation of crystals and solutions on the basis of enhanced reaction degree. Utility Model Content
[0005] In order to solve the above problems, the utility model proposes a liquid-liquid reaction cooling crystallization device, which is suitable for the field where the temperature difference between reaction crystallization and precipitation crystallization is large, can improve the reaction efficiency without increasing energy consumption, and can also achieve effective separation of crystals and solution on the basis of enhanced reaction degree, thereby improving product output rate and quality.
[0006] In order to solve the above technical problems, the technical solution adopted by the utility model is:
[0007] A liquid-liquid reaction cooling crystallization device comprises a cooling cylinder and a reaction cylinder located above the cooling cylinder and partially extending into the interior of the cooling cylinder and connected to the cooling cylinder through a reaction cylinder discharge buffer tube at the bottom, wherein a cooling cylinder crystal discharge port is arranged at the bottom of the cooling cylinder, a cooling cylinder solution discharge port is arranged at the top, and two rotatable cooling cylinder stirring paddles extending from the bottom and extending into both sides of the reaction cylinder discharge buffer tube respectively are arranged at the bottom end of the interior, a reaction cylinder feed port is arranged at the top of the reaction cylinder, and a rotatable reaction cylinder stirring paddle extending from the top into the bottom is arranged inside, multiple layers of blades are evenly installed on the central axes of the cooling cylinder stirring paddle and the reaction cylinder stirring paddle, a reflux pipe is arranged on the side wall of the reaction cylinder, the reflux pipe horizontally passes through the reaction cylinder wall and the cooling cylinder wall in an arc shape along the stirring direction, and the outlet is tangent to the cooling cylinder wall, and then refluxes downward to the central axis position of the reaction cylinder stirring paddle, the reflux port is located below the blade, and a reflux pipe control valve is arranged on the reflux pipe.
[0008] A further improvement of the technical solution of the utility model is that the upper part of the reaction cylinder is a cylindrical straight section, the lower part is a conical or semi-elliptical structure, and the reaction cylinder discharge buffer pipe is located at the bottom of the conical or semi-elliptical structure, the bottom of the cooling cylinder is set as a conical structure, and the volume ratio of the reaction cylinder and the cooling cylinder is 1:1.0-5.0.
[0009] A further improvement of the technical solution of the utility model is that a cleaning port connected to the interior of the reaction cylinder, a reaction cylinder gas overflow port and an instrument installation hole for installing temperature and pressure instruments are provided on the top of the reaction cylinder, and valves are provided on the cleaning port and the reaction cylinder gas overflow port.
[0010] A further improvement of the technical solution of the utility model is that a first drive motor for providing power to the reaction tube stirring paddle is arranged on the top of the reaction tube, and the main shaft of the first drive motor passes through the top plate of the reaction tube and is connected to the reaction tube stirring paddle.
[0011] A further improvement of the technical solution of the utility model is that: the outer wall of the reaction tube is provided with a heat-insulating layer jacket, a reaction tube heat source inlet is provided at a higher position on one side of the heat-insulating layer jacket, a reaction tube heat source outlet is provided at a lower position on the other side of the jacket, and valves are provided on the reaction tube heat source inlet and the reaction tube heat source outlet.
[0012] A further improvement of the technical solution of the utility model is that: the power mechanism of the cooling cylinder stirring paddle includes a magnetic drive component and a second drive motor, the magnetic drive component is located at the inner bottom end of the cooling cylinder and is connected to the bottom of the cooling cylinder stirring paddle, the second drive motor is located outside the cooling cylinder and an isolation sleeve matching the magnetic drive component is provided on the top of the main shaft, and the cooling cylinder crystal discharge port includes cooling cylinder crystal discharge port one and cooling cylinder crystal discharge port two, which are respectively located on both sides of the second drive motor.
[0013] A further improvement of the technical solution of the utility model is that a cooling cylinder refrigerant jacket is provided on the outer wall of the cooling cylinder, a cooling cylinder refrigerant inlet with a valve is provided at a lower position of the cooling cylinder refrigerant jacket, and a cooling cylinder refrigerant outlet with a valve is provided at a higher position on the other side.
[0014] A further improvement of the technical solution of the utility model is that a lifting lug connected to the platform is welded on the upper side wall of the cooling cylinder, a cooling cylinder thermometer penetrating into the interior of the cooling cylinder is arranged on one side of the bottom, and a manhole is arranged on the side wall of the cooling cylinder, and the diameter of the manhole is not less than 400 mm.
[0015] A further improvement of the technical solution of the utility model is that the diameter of the reaction tube discharge buffer tube is 50mm-120mm, and a buffer tube refrigerant jacket is arranged on the tube wall, a reaction tube discharge buffer tube refrigerant inlet penetrating the outer wall of the cooling tube is arranged at a lower position on one side of the buffer tube refrigerant jacket, and a reaction tube discharge buffer tube refrigerant outlet penetrating the outer wall of the cooling tube is arranged at a higher position on the opposite side.
[0016] A further improvement of the technical solution of the utility model is that: the reflux pipes are arranged in multiple groups symmetrically or asymmetrically along the circumference of the reaction tube, and each group of reflux pipes is provided with multiple reflux pipes and distributed vertically along the reaction tube.
[0017] Due to the adoption of the above technical solution, the technical progress achieved by the utility model is:
[0018] The utility model is suitable for fields where the temperature difference between reaction crystallization and precipitation crystallization is large, and can improve the reaction efficiency without increasing energy consumption. At the same time, it can also realize the effective separation of crystals and solutions on the basis of enhanced reaction degree, thereby improving product output rate and quality.
[0019] The reflux pipe provided in the utility model utilizes the centrifugal force generated when the reaction barrel stirring paddle rotates to increase the degree of material mixing, that is, the centrifugal force on the center of the reaction barrel stirring paddle is small and the liquid level is low, while the centrifugal force on the liquid at the barrel wall is large and the liquid level is high. When the reflux pipe control valve is opened, the liquid is acted upon by the centrifugal force and enters the lower part of the central axis of the reaction barrel stirring paddle from the upper layer of the reaction barrel along the reflux pipe for mixing, thereby increasing the degree of turbulence of the upper and lower liquids, achieving full mixing between the liquids in the barrel and achieving the purpose of improving the reaction efficiency. At the same time, the reflux pipe does not require additional power or energy consumption. By adding refrigerant and rotating the cooling barrel stirring paddle, the temperature in the cooling barrel is reduced, the uniformity of the mixed solution is improved, the solubility of the crystal in the mixed solution is reduced while also ensuring the uniformity of the crystallization, thereby achieving the purpose of improving the product output rate and quality.
[0020] The top of the reaction cylinder of the utility model is provided with a cleaning port with a valve switch, which facilitates the cleaning of the inside of the reaction cylinder and prevents the cylinder from being polluted by the external environment.
[0021] The top of the reaction cylinder of the utility model is provided with a reaction cylinder gas overflow port with a valve switch, so that the gas that may be generated by the reaction in the cylinder can be smoothly discharged out of the cylinder, thereby ensuring the safety of the equipment.
[0022] The top of the reaction cylinder of the utility model is provided with instrument mounting holes for temperature and pressure instruments, through which the real-time temperature and pressure inside the reaction cylinder can be observed, thus ensuring the stable operation of the equipment.
[0023] The heat-insulating jacket outside the reaction tube of the utility model effectively isolates the reaction tube and the cooling tube, and can ensure that the temperatures of each are independent and do not interfere with each other.
[0024] The power mechanism of the cooling cylinder stirring paddle of the utility model is a magnetic driving component and a second driving motor. The inside and outside of the system are isolated without mechanical seals, thereby ensuring the overall sealing of the equipment.
[0025] The utility model provides a cooling cylinder thermometer at the bottom of the cooling cylinder, which can monitor the temperature in the cooling cylinder in real time and make timely adjustments to ensure that the cooling and crystallization work proceeds in an orderly manner.
[0026] The utility model provides a refrigerant jacket on the outer wall of the cooling cylinder and the outer wall of the discharge buffer tube of the reaction cylinder. A refrigerant inlet is provided at a lower position on one side of the cooling jacket, and a refrigerant outlet is provided at a higher position on the other side. The height setting of the refrigerant inlet and outlet can fill the refrigerant in the refrigerant jacket, thereby achieving a better cooling effect.
[0027] The utility model has lifting ears welded on the upper side wall of the cooling cylinder for connection with the platform, which facilitates the movement and transportation of the equipment and ensures the stability of the equipment during operation.
[0028] The utility model provides a manhole with a diameter not less than 400 mm on the side wall of the cooling cylinder, which is convenient for users to better observe the crystallization situation in the cooling cylinder and control the crystallization process. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1 It is a schematic diagram of the structure of the utility model;
[0030] Among them, 1. reaction cylinder; 2. reaction cylinder feed port; 3. first drive motor; 4. cleaning port; 5. reaction cylinder gas overflow port; 6. instrument installation hole; 7. cooling cylinder solution discharge port; 8. cooling cylinder refrigerant outlet; 9. reaction cylinder heat source outlet; 10. reaction cylinder discharge buffer tube refrigerant inlet; 11. cooling cylinder; 12. cooling cylinder stirring paddle; 13. cooling cylinder thermometer; 14. second drive motor; 15. magnetic drive assembly; 16. cooling cylinder crystal discharge port; 161. cooling cylinder crystal discharge port one; 162. cooling cylinder crystal discharge port two; 17. cooling cylinder refrigerant inlet; 18. reaction cylinder discharge buffer tube; 19. manhole; 20. reaction cylinder discharge buffer tube refrigerant outlet; 21. reflux pipe; 22. reflux pipe control valve; 23. reaction cylinder heat source inlet; 24. reaction cylinder stirring paddle; 25. lifting ear. DETAILED DESCRIPTION
[0031] The present invention is further described in detail below in conjunction with the embodiments:
[0032] The liquid-liquid reaction cooling crystallization device of the utility model has a compact structure and high material reaction efficiency, and can improve the reaction efficiency without increasing the energy consumption of the equipment. At the same time, the use of low-temperature cooling helps to reduce the solubility of the output crystal in the solution and improve the output rate.
[0033] like Figure 1 As shown, the device specifically includes a reaction cylinder 1 and a cooling cylinder 11. The reaction cylinder 1 is located above the cooling cylinder 11 and partially extends into the interior of the cooling cylinder 11. It is connected to the cooling cylinder 11 through a reaction cylinder discharge buffer tube 18 at the bottom. The volume ratio of the reaction cylinder 1 and the cooling cylinder 11 is generally set to 1:1.0-5.0, and is 1:3 in this embodiment.
[0034] The upper part of the reaction cylinder 1 is a cylindrical straight section, and the lower part can be a conical structure or a semi-elliptical structure. The present embodiment is a conical structure, and a reaction cylinder discharge buffer tube 18 is arranged at the bottom of the conical structure. The reaction cylinder discharge buffer tube 18 is cylindrical, with a diameter between 50 mm and 120 mm, and 100 mm in the present embodiment. The reaction cylinder discharge buffer tube 18 extends downward into the cooling cylinder 11.
[0035] The top of the reaction tube 1 is provided with a reaction tube feed port 2, a cleaning port 4, a reaction tube gas overflow port 5 and an instrument mounting hole 6 which are communicated with the interior of the reaction tube 1. A temperature and pressure instrument is installed on the instrument mounting hole 6 for measuring the temperature and pressure in the reaction tube. The top of the reaction tube 1 is also provided with a first drive motor 3. The main shaft of the first drive motor 3 passes through the top plate of the reaction tube 1 and is connected to the reaction tube stirring paddle 24 for driving the reaction tube stirring paddle 24 to rotate. A plurality of layers of blades are arranged on the central axis of the reaction tube stirring paddle 24 from top to bottom. In this embodiment, there are three layers. The blades can be in different forms such as spiral and rectangular. In this embodiment, they are rectangular.
[0036] The outer wall of the reaction tube 1 is provided with an insulation layer jacket, a reaction tube heat source inlet 23 is provided at a higher position on one side of the insulation layer jacket, and a reaction tube heat source outlet 9 is provided at a lower position on the opposite side, and valves are provided on the reaction tube heat source inlet 23 and the reaction tube heat source outlet 9.
[0037] The side wall of the reaction tube 1 is also provided with a reflux pipe 21. The reflux pipe 21 passes through the reaction tube wall and the cooling tube wall in an arc shape horizontally along the stirring direction, and the outlet is tangent to the cooling tube wall, and then refluxes downward to the central axis position of the reaction tube stirring paddle 24. The reflux port is located below the blade. Such a structural arrangement enables the liquid to flow smoothly into the reflux pipe 21 during the stirring process, and the centrifugal force generated when the reaction tube stirring paddle 24 rotates is used to enhance the material mixing intensity, that is, the centrifugal force at the center position of the reaction tube stirring paddle 24 is small, the liquid level is low, and the centrifugal force at the tube wall is large, and the liquid level is high. The reflux pipe control valve 22 is opened, and the liquid is acted upon by the centrifugal force and enters the lower part of the central axis of the reaction tube stirring paddle 24 from the upper layer of the reaction tube 1 along the reflux pipe 21 for mixing, thereby increasing the turbulence of the upper and lower liquids, achieving full mixing between the liquids in the tube, and achieving the purpose of improving the reaction efficiency. At the same time, the reflux pipe 21 does not require additional power and energy consumption.
[0038] The reflux pipes 21 are arranged in multiple groups symmetrically or asymmetrically along the circumference of the reaction tube 1 , and each group of reflux pipes 21 is provided with multiple reflux pipes and distributed vertically along the reaction tube 1 . In this embodiment, three reflux pipes are arranged in each group, and each reflux pipe 21 is provided with a reaction tube reflux pipe control valve 22 .
[0039] A buffer tube refrigerant jacket is arranged on the wall of the reaction tube discharge buffer tube 18, a reaction tube discharge buffer tube refrigerant inlet 10 penetrating the outer wall of the cooling tube is arranged at a lower position on one side of the buffer tube refrigerant jacket, and a reaction tube discharge buffer tube refrigerant outlet 20 penetrating the outer wall of the cooling tube is arranged at a higher position on the opposite side.
[0040] The bottom of the cooling cylinder 11 is arranged as a conical structure, and the inner bottom end is arranged with two rotatable cooling cylinder stirring paddles 12 extending from the bottom and extending into the two sides of the reaction cylinder discharge buffer pipe 18 respectively. A plurality of layers of blades are arranged on the central axis of each cooling cylinder stirring paddle 12, and this embodiment has 4 layers. The mechanism for providing power for the cooling cylinder stirring paddle 12 includes a magnetic drive component 15 and a second drive motor 14. The magnetic drive component 15 is located at the inner bottom end of the cooling cylinder 11 and is connected to the bottom of the cooling cylinder stirring paddle 12. The second drive motor 14 is located outside the cooling cylinder 11 and an isolation sleeve matching the magnetic drive component 15 is arranged at the top of the main shaft.
[0041] The outer wall of the cooling cylinder 11 is provided with a cooling cylinder refrigerant jacket, a cooling cylinder refrigerant inlet 17 with a valve is provided at a lower position of the cooling cylinder refrigerant jacket, and a cooling cylinder refrigerant outlet 8 with a valve is provided at a higher position on the other side.
[0042] Two cooling cylinder crystal discharge ports 16 are provided at the bottom of the cooling cylinder 11, which are respectively located on both sides of the second driving motor. A cooling cylinder solution discharge port 7 is provided at a higher position on one side of the cooling cylinder 11. After the reacted materials are fully retained and separated in the cooling cylinder 11, the solution is discharged through the cooling cylinder solution discharge port 7.
[0043] A cooling cylinder thermometer 13 extending into the barrel is arranged at one side of the bottom of the cooling cylinder 11, a lifting lug 25 is arranged at a higher position on one side of the cooling cylinder 11, and a manhole is arranged on one side of the cooling cylinder 11. The diameter of the manhole is not less than 400 mm, and is 500 mm in this embodiment.
[0044] Working principle: First, turn on the first drive motor 3 to drive the reaction barrel stirring paddle 24 to rotate. After the material to be reacted is added to the reaction barrel 1 from the reaction barrel feed port 2 at the top of the reaction barrel 1, open the valve of the reaction barrel heat source inlet 23, introduce the heat source, and control the appropriate temperature to allow a liquid-liquid reaction to occur in the reaction barrel 1. The reaction material is subjected to the centrifugal force generated by the rotation of the blades on the reaction barrel stirring paddle 24 in the reaction barrel 1. The liquid level near the center of the reaction barrel stirring paddle 24 will be concave, and the liquid level near the inner wall of the reaction barrel 1 will be convex. The corresponding reaction barrel reflux pipe control valve 22 is opened according to the height of the liquid level each time. Under the action of centrifugal force, the mixed liquid refluxes from the upper edge of the reaction barrel 1 to the position below the central axis of the reaction barrel stirring paddle 24 through the reflux pipe 21, thereby achieving a better mixing reaction of the material to be reacted.
[0045] Open the valves at the refrigerant inlet 10 and the refrigerant outlet 20 of the reaction tube discharge buffer tube, and introduce the refrigerant. When the liquid after sufficient mixing and reaction in the reaction tube 1 enters the bottom reaction tube discharge buffer tube 18, the heat of this part of the liquid is replaced, and then the liquid enters the cooling tube 11. Open the valves at the refrigerant inlet 17 and the refrigerant outlet 8 of the cooling tube, and introduce the refrigerant. Start the second drive motor 14. The cooling tube 11 has a large internal space and a low temperature. After the liquid after the reaction is fully retained and crystallized in the cooling tube 11, the solution is discharged through the cooling tube solution outlet 7 under the action of an external water pump, and the crystals containing a small amount of mother liquor go to the separation equipment through the cooling tube crystal outlet 1 161 and the cooling tube crystal outlet 2 162.
Claims
1. A liquid-liquid reaction cooling crystallization device, characterized in that: The invention comprises a cooling cylinder (11) and a reaction cylinder (1) located above the cooling cylinder (11) and partially extending into the interior of the cooling cylinder (11) and connected to the cooling cylinder (11) through a reaction cylinder discharge buffer pipe (18) at the bottom, wherein the bottom of the cooling cylinder (11) is provided with a cooling cylinder crystal discharge port (16), the top of the cooling cylinder (11) is provided with a cooling cylinder solution discharge port (7), the bottom of the interior is provided with two rotatable cooling cylinder stirring paddles (12) extending from the bottom and extending into the two sides of the reaction cylinder discharge buffer pipe (18) respectively, and the top of the reaction cylinder (1) is provided with a reaction cylinder feed port (2 ), a reaction cylinder stirring paddle (24) is arranged inside and extends from the top to the bottom and is rotatable, and multiple layers of blades are evenly installed on the central axis of the cooling cylinder stirring paddle (12) and the reaction cylinder stirring paddle (24). A reflux pipe (21) is arranged on the side wall of the reaction cylinder (1). The reflux pipe (21) passes through the reaction cylinder wall and the cooling cylinder wall in an arc shape horizontally along the stirring direction, and the outlet is tangent to the cooling cylinder wall, and then refluxes downward to the central axis position of the reaction cylinder stirring paddle (24). The reflux port is located below the blades, and a reflux pipe control valve (22) is arranged on the reflux pipe (21).
2. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The upper part of the reaction cylinder (1) is a cylindrical straight section, and the lower part is a conical or semi-elliptical structure, and the reaction cylinder discharge buffer pipe (18) is located at the bottom of the conical or semi-elliptical structure, and the bottom of the cooling cylinder (11) is set as a conical structure, and the volume ratio of the reaction cylinder (1) and the cooling cylinder (11) is 1:1.0-5.
0.
3. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The top of the reaction cylinder (1) is provided with a cleaning port (4) connected to the interior of the reaction cylinder (1), a reaction cylinder gas overflow port (5) and an instrument installation hole (6) on which temperature and pressure instruments are installed, and valves are provided on the cleaning port (4) and the reaction cylinder gas overflow port (5).
4. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: A first drive motor (3) for providing power to the reaction tube stirring paddle (24) is arranged on the top of the reaction tube (1), and a main shaft of the first drive motor (3) passes through the top plate of the reaction tube (1) and is connected to the reaction tube stirring paddle (24).
5. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The outer wall of the reaction tube (1) is provided with a heat-insulating layer jacket, a reaction tube heat source inlet (23) is provided at a higher position on one side of the heat-insulating layer jacket, a reaction tube heat source outlet (9) is provided at a lower position on the other side of the jacket, and valves are provided on the reaction tube heat source inlet (23) and the reaction tube heat source outlet (9).
6. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The power mechanism of the cooling cylinder stirring paddle (12) includes a magnetic drive component (15) and a second drive motor (14), wherein the magnetic drive component (15) is located at the inner bottom end of the cooling cylinder (11) and is connected to the bottom of the cooling cylinder stirring paddle (12), the second drive motor (14) is located outside the cooling cylinder (11) and an isolation sleeve matching the magnetic drive component (15) is provided at the top of the main shaft, and the cooling cylinder crystal discharge port (16) includes a cooling cylinder crystal discharge port 1 (161) and a cooling cylinder crystal discharge port 2 (162), which are respectively located on both sides of the second drive motor (14).
7. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The outer wall of the cooling cylinder (11) is provided with a cooling cylinder refrigerant jacket, a cooling cylinder refrigerant inlet (17) with a valve is provided at a lower position of the cooling cylinder refrigerant jacket, and a cooling cylinder refrigerant outlet (8) with a valve is provided at a higher position on the other side.
8. The liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: A lifting lug (25) connected to the platform is welded on the upper side of the side wall of the cooling cylinder (11), a cooling cylinder thermometer (13) extending deep into the cooling cylinder (11) is arranged on one side of the bottom, and a manhole (19) is also arranged on the side wall of the cooling cylinder (11), and the diameter of the manhole (19) is not less than 400 mm.
9. A liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The diameter of the reaction tube discharge buffer tube (18) is 50mm-120mm, and a buffer tube refrigerant jacket is provided on the tube wall. A reaction tube discharge buffer tube refrigerant inlet (10) penetrating the outer wall of the cooling tube is provided at a lower position on one side of the buffer tube refrigerant jacket, and a reaction tube discharge buffer tube refrigerant outlet (20) penetrating the outer wall of the cooling tube is provided at a higher position on the opposite side.
10. The liquid-liquid reaction cooling crystallization device according to claim 1, characterized in that: The reflux pipes (21) are arranged in a plurality of groups symmetrically or asymmetrically along the circumference of the reaction cylinder (1), and each group of reflux pipes (21) is provided with a plurality of reflux pipes (21) distributed vertically along the reaction cylinder (1).
Citation Information
Patent Citations
Reaction crystallization kettle device for ethylene glycol antimony
CN210752662U