High solid-liquid separation reaction kettle

Abstract

The utility model discloses a high solid-liquid separation reaction kettle which comprises a reaction kettle body, a stirring mechanism, a wall scraping mechanism and a three-way valve, the bottom of the reaction kettle body is provided with a kettle body conical bottom shell, the top of the reaction kettle body is detachably connected with a kettle body top cover, the stirring mechanism is arranged in the reaction kettle body, and the wall scraping mechanism is fixedly connected with the stirring mechanism. The three-way valve is fixedly mounted at the outlet end of the conical bottom shell of the kettle body, a filtering device is arranged in a connecting pipeline on one side of the three-way valve, and a solid material discharge port is formed in the tail end of a connecting pipeline on the other side. The stirring mechanism and the wall scraping mechanism are matched, so that the stirring process of materials in the reaction kettle is easier, the stirring is more uniform, the residues of the materials on the inner wall of the reaction kettle are less, and the filtering device and the external extraction opening are matched for use, so that the efficient solid-liquid separation in the reaction kettle is realized, and the residual solid product materials on the inner wall of the reaction kettle are reduced; the yield of filtrate can be increased, and the reaction yield is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of solid-liquid separation of output materials in a reaction kettle, in particular to a high-solid-liquid separation reaction kettle. Background Art

[0002] In the process of preparing diiodosilane by reacting anhydrous lithium iodide and dichlorosilane, in addition to liquid diiodosilane, there will also be a large amount of solid products. The slurry formed by mixing the above substances will significantly increase the viscosity of the system, which not only hinders the smooth stirring work during the reaction, but also easily causes the product to remain on the inner wall of the reactor, resulting in a decrease in the reaction yield. Therefore, in a slurry system with high viscosity, how to increase the amount of liquid diiodosilane obtained is an important measure to effectively improve the reaction yield.

[0003] In the prior art, such as the Chinese patent application number CN202311593269.0 "A method for preparing diiodosilane", the application has disclosed a process for distilling diiodosilane by vacuum distillation. However, in this process, part of the diiodosilane will condense on the top cover of the reactor and is not effectively collected, resulting in poor solid-liquid separation of the output material in the reactor. Utility Model Content

[0004] The utility model aims to provide a high solid-liquid separation reactor, which is used to solve the problem of poor solid-liquid separation effect of output materials in the reactor in the prior art.

[0005] The purpose of the utility model can be achieved through the following technical solutions:

[0006] A high solid-liquid separation reactor, comprising:

[0007] The reactor body has a conical bottom shell at the bottom and a detachable top cover at the top;

[0008] A stirring mechanism is arranged in the reactor body;

[0009] A wall scraping mechanism, fixedly connected to the stirring mechanism;

[0010] The three-way valve is fixedly installed at the outlet end of the conical bottom shell of the kettle body. A filtering device is arranged in a connecting pipeline on one side of the three-way valve, and a tail end of a connecting pipeline on the other side is arranged as a solid material discharge port.

[0011] As a further solution of the utility model: the stirring mechanism includes a transmission member, a rotating shaft, a stirring rod and a screw-belt stirring paddle. The transmission member, the rotating shaft and the stirring rod are fixedly connected in sequence from top to bottom. The screw-belt stirring paddle is fixedly connected to the stirring rod, and the transmission member is arranged on the outside of the top cover of the kettle body.

[0012] As a further solution of the utility model: the wall scraping mechanism includes a plurality of scrapers, the scrapers are fixedly connected to the stirring rods via transverse support rods, and the side plate surfaces of the scrapers are in conflict with the vertical inner wall of the reactor body.

[0013] As a further solution of the utility model: a purge mechanism for cleaning the residual solid material on the side plate surface of the scraper is provided in the reactor body.

[0014] As a further solution of the utility model: the purge mechanism includes an air jet disposed above the scraper, the air jet is disposed at one end of an air distribution pipe, the other end of the air distribution pipe is fixedly connected to an air inlet pipe through an air disk, the air inlet pipe is disposed in the axial through hole of the rotating shaft and extends outward from the kettle body top cover, wherein the air distribution pipe is fixedly connected to the rotating shaft.

[0015] As a further solution of the utility model: when the air inlet pipe delivers the purge airflow into the air jet port, a bottom air suction port is correspondingly provided on the conical bottom shell of the kettle body.

[0016] As a further solution of the utility model: the filtering device is a solid-liquid separation filter element net, and an external air suction port is provided on the connecting pipeline where the filtering device is installed.

[0017] As a further solution of the utility model: an air inlet is arranged on the connecting pipeline of the solid material discharge port, and a top air exhaust port is arranged on the top cover of the kettle body.

[0018] As a further solution of the utility model: the reactor body includes a cylindrical tank body connected to the conical bottom shell of the reactor body as an integral structure, a heating chamber and a cooling chamber are respectively arranged on the cavity of the cylindrical tank body, and a temperature sensor is arranged on the conical bottom shell of the reactor body.

[0019] As a further solution of the utility model: an observation window mirror and a feed port are arranged on the top cover of the kettle body.

[0020] Beneficial effects of the utility model:

[0021] (1) The stirring mechanism and the scraping mechanism make the stirring process of the materials in the reactor easier and more uniform, and the materials are less residual on the inner wall of the reactor. In combination with the filtering device and the external air extraction port, efficient solid-liquid separation in the reactor is achieved, thereby reducing the solid product material residual on the inner wall of the reactor, which helps to increase the output of the filtrate and improve the reaction yield;

[0022] (2) By arranging a purge mechanism in the reactor body, the air jet can further blow off the material on the scraper or the inner wall of the reactor, thereby increasing the filtrate output and further improving the reaction yield;

[0023] (3) After the filtrate of liquid diiodosilane is collected, the solid product material is difficult to discharge due to moisture and agglomeration. A certain amount of gas is introduced into the air inlet provided on the connecting pipeline of the solid material discharge port, and the gas is extracted from the top exhaust port. The operation of the gas can make the solid product material looser. After that, the air supply is stopped, and the solid product material can be easily discharged.

[0024] (4) The present application integrates the process design of material reaction and output material separation, which can not only improve the solid-liquid separation effect or separation degree of the reaction, but also further improve the filtrate output and reaction yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The utility model is further described below in conjunction with the accompanying drawings.

[0026] Figure 1 It is a structural schematic diagram of the utility model.

[0027] In the figure: 1. kettle body top cover; 2. kettle body conical bottom shell; 3. three-way valve; 4. observation window mirror; 5. feed port; 6. top air exhaust port; 7. bottom air exhaust port; 8. air inlet pipe; 9. transmission part; 10. rotating shaft; 11. gas disk; 12. gas distribution pipe; 13. jet nozzle; 14. stirring rod; 15. spiral ribbon stirring paddle; 16. scraper; 17. filter device; 18. external air exhaust port; 19. air inlet; 20. temperature sensor; 21. heating chamber; 22. cooling chamber; 23. solid material discharge port. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0029] In the description of the present invention, it should be understood that the terms indicating orientation or positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention; in the description of the present invention, "multiple" and "several" mean at least two, for example two, three, etc., unless otherwise clearly and specifically defined.

[0030] See also Figure 1As shown, the utility model is a high solid-liquid separation reactor, including a reactor body, a stirring mechanism, a scraping mechanism and a three-way valve 3. A conical bottom shell 2 of the reactor body is provided at the bottom of the reactor body, and a top cover 1 of the reactor body can be detachably connected to the top. The stirring mechanism is arranged in the reactor body, and the scraping mechanism is fixedly connected to the stirring mechanism. The three-way valve 3 is fixedly installed at the outlet end of the conical bottom shell 2 of the reactor body. A filtering device 17 is arranged in a connecting pipeline on one side of the three-way valve 3, and a tail end of the connecting pipeline on the other side is arranged as a solid material discharge port 23.

[0031] In the process of preparing diiodosilane by reacting anhydrous lithium iodide and dichlorosilane in the reactor, a stirring mechanism is used to quickly contact and react anhydrous lithium iodide and dichlorosilane to generate liquid diiodosilane and solid product materials. After the reaction is completed, the liquid diiodosilane and the solid product materials need to be separated. The present application uses a three-way valve 3 to form a solid-liquid separation pipeline on the conical bottom shell 2 of the reactor body. The filtering device 17 in the pipeline connected to one side of the three-way valve 3 blocks the solid product material so that the liquid diiodosilane can be discharged from the pipeline connected to this side. After the filtrate of the liquid diiodosilane is collected, the pipeline connected to the other side of the three-way valve 3 is convenient for discharging the solid product material blocked by the filtration and the solid product material remaining in the reactor body, so as to achieve efficient solid-liquid separation in the reactor, thereby reducing the solid product material remaining on the inner wall of the reactor.

[0032] It should be understood that the bottom of the reactor body adopts a conical bottom shell 2 design. Compared with ordinary round-bottom reactors, the conical bottom shell 2 of the reactor body is more conducive to reducing the residue of materials on the inner wall or bottom of the reactor body under the action of gravity.

[0033] In this specific embodiment, the stirring mechanism includes a transmission member 9, a rotating shaft 10, a stirring rod 14 and a screw-belt stirring paddle 15. The transmission member 9, the rotating shaft 10 and the stirring rod 14 are fixedly connected in sequence from top to bottom. The screw-belt stirring paddle 15 is fixedly connected to the stirring rod 14. The transmission member 9 is arranged on the outside of the kettle top cover 1. During the operation of the stirring mechanism in the reactor, it is convenient to transmit the output torque to the transmission member 9 through the driving motor, so as to drive the rotating shaft 10 and the stirring rod 14 to rotate. The stirring rod 14 rotates as a whole to drive the screw-belt stirring paddle 15 to disturb the anhydrous lithium iodide and dichlorosilane mixture, so that the mixture is stirred more evenly, the contact reaction is faster, and there is less material residue on the stirring blades of the screw-belt stirring paddle 15.

[0034] It should be understood that during the process of the rotating shaft 10 driving the rotating action, there is a sealing assembly effect between the rotating shaft 10 and the kettle top cover 1. The preferred structure of the rotating shaft 10 can be an outer shell and a rotor core shaft embedded in the kettle top cover 1, so that the rotor core shaft rotates along the embedded outer shell, thereby realizing the integrated rotation of the stirring rod 14, and the embedded outer shell plays a role of rotational support and sealing for the rotor core shaft.

[0035] In this specific embodiment, the scraping mechanism includes a plurality of scrapers 16, which are fixedly connected to the stirring rod 14 by a transverse support rod, and the side plate surface of the scraper 16 is in conflict with the vertical inner wall of the reactor body. During the operation of the stirring mechanism in the reactor, it is convenient to drive the scraping mechanism to rotate and clean the inner wall of the reactor body, so that the scraper 16 rotates to scrape off the residual material on the inner wall of the reactor body and reduce the adhesion residue of the material on the inner wall; in addition, the scraping mechanism is used in conjunction with the spiral belt stirring paddle 15 to improve the mixing uniformity and reaction rate of the mixture.

[0036] In this specific embodiment, a purge mechanism is provided in the reactor body for cleaning the residual solid material on the side plate surface of the scraper blade 16. Since the scraper mechanism is fixedly connected to the stirring mechanism, residual material is inevitably left on the scraper blade 16 of the scraper mechanism. By adding the purge mechanism, the residual material on the scraper blade 16 can be purged and removed, thereby reducing the residual material on the scraper blade 16 and the inner wall of the reactor, and further improving the filtrate output.

[0037] In this specific embodiment, the purge mechanism includes a jet port 13 arranged above the scraper 16, and the jet port 13 is arranged at one end of the air distribution pipe 12, and the other end of the air distribution pipe 12 is fixedly connected to the air inlet pipe 8 through the air disk 11. The air inlet pipe 8 is arranged in the axial through hole of the rotating shaft 10 and extends outward from the kettle body top cover 1, wherein the air distribution pipe 12 is fixedly connected to the rotating shaft 10. During the operation of the purge mechanism, the purge airflow passes through the air inlet pipe 8, the air disk 11, and the air distribution pipe 12 in sequence to reach the jet port 13 position and be ejected. During the process of the air distribution pipe 12 rotating with the rotating shaft 10, the inner side wall of the reactor body is purged in all directions, and the material is purged downward to the conical bottom shell 2 of the reactor body, and then the purged material can continue to be filtered and the filtrate can be collected, effectively avoiding the residue of the material inside the reactor and improving the reaction yield.

[0038] In this specific embodiment, when the air inlet pipe 8 delivers the purge airflow into the air injection port 13, a bottom air extraction port 7 is provided on the conical bottom shell 2 of the reactor body to facilitate complete discharge of the purge airflow entering the reactor.

[0039] In this specific embodiment, the filter device 17 is a solid-liquid separation filter element net, and an external air suction port 18 is provided on the connecting pipeline where the filter device 17 is installed. When the filter device 17 blocks and separates the solid product material in the liquid diiodosilane, it is convenient to negatively pressure-suction the filtrate through the external air suction port 18. During the filtration, the reactor body can be evacuated to form a pressure difference, thereby improving the filtration efficiency.

[0040] In this specific embodiment, an air inlet 19 is provided on the connecting pipeline of the solid material discharge port 23, and a top air exhaust port 6 is provided on the top cover 1 of the kettle body. After the filtrate of the liquid diiodosilane is collected, the solid product material is easy to be difficult to discharge due to moisture and agglomeration. A certain amount of gas is introduced at the position of the air inlet 19, and the gas is extracted from the top air exhaust port 6. The operation of the gas can make the solid product material looser. After that, the air intake is stopped, and the solid product material can be easily discharged.

[0041] In this specific embodiment, the reactor body includes a cylindrical tank body connected to the conical bottom shell 2 of the reactor body as an integral structure. A heating chamber 21 and a cooling chamber 22 are respectively arranged on the cavity of the cylindrical tank body, and a temperature sensor 20 is arranged on the conical bottom shell 2 of the reactor body. After the material is fed into the reactor body, it is convenient to adjust the temperature of the cooling chamber 22 and the heating chamber 21 to increase or decrease the temperature of the reactor body, and turn on the stirring device during the reaction process so that the spiral ribbon stirring paddle 15 and the scraper 16 continue to stir to ensure that the materials are fully mixed. The set temperature sensor 20 is used to monitor the reaction temperature in the reactor body in real time.

[0042] In this specific embodiment, an observation window 4 and a feed port 5 are provided on the reactor body top cover 1. The feed port 5 is provided to facilitate adding reaction materials into the reactor body, and the observation window 4 is provided to facilitate visually observing the reaction status of the materials in the reactor body.

[0043] The above is a detailed description of an embodiment of the utility model, but the content is only a preferred embodiment of the utility model and cannot be considered to limit the scope of implementation of the utility model. All equivalent changes and improvements made within the scope of application of the utility model should still fall within the scope of the patent coverage of the utility model.

Claims

1. A high solid-liquid separation reactor, characterized in that: include: The reactor body has a conical bottom shell (2) at the bottom and a top cover (1) detachably connected to the reactor body. A stirring mechanism is arranged in the reactor body; A wall scraping mechanism, fixedly connected to the stirring mechanism; A three-way valve (3) is fixedly mounted at the outlet end of the conical bottom shell (2) of the kettle body. A filtering device (17) is arranged in a connecting pipeline on one side of the three-way valve (3), and a tail end of a connecting pipeline on the other side is arranged as a solid material discharge port (23).

2. A high solid-liquid separation reactor according to claim 1, characterized in that: The stirring mechanism comprises a transmission member (9), a rotating shaft (10), a stirring rod (14) and a screw-belt stirring paddle (15); the transmission member (9), the rotating shaft (10) and the stirring rod (14) are fixedly connected in sequence from top to bottom; the stirring rod (14) is fixedly connected to the screw-belt stirring paddle (15); and the transmission member (9) is arranged outside the kettle body top cover (1).

3. A high solid-liquid separation reactor according to claim 2, characterized in that: The wall scraping mechanism comprises a plurality of scrapers (16), wherein the scrapers (16) are fixedly connected to the stirring rod (14) via a transverse support rod, and the side plate surface of the scrapers (16) contacts the vertical inner wall of the reactor body.

4. A high solid-liquid separation reactor according to claim 3, characterized in that: The reactor body is provided with a purge mechanism for cleaning the solid materials remaining on the side plate surface of the scraper (16).

5. A high solid-liquid separation reactor according to claim 4, characterized in that: The purge mechanism includes an air jet (13) arranged above the scraper (16), the air jet (13) being arranged at one end of an air distribution pipe (12), the other end of the air distribution pipe (12) being fixedly connected to an air inlet pipe (8) via an air disk (11), the air inlet pipe (8) being arranged in an axial through hole of the rotating shaft (10) and extending outwardly from the kettle body top cover (1), wherein the air distribution pipe (12) is fixedly connected to the rotating shaft (10).

6. A high solid-liquid separation reactor according to claim 5, characterized in that: When the air inlet pipe (8) delivers the purge airflow into the air injection port (13), a corresponding bottom air extraction port (7) is provided on the conical bottom shell (2) of the kettle body.

7. The high solid-liquid separation reactor according to claim 1, characterized in that: The filtering device (17) is a solid-liquid separation filter element net, and an external air extraction port (18) is provided on the connecting pipeline where the filtering device (17) is installed.

8. The high solid-liquid separation reactor according to claim 1, characterized in that: An air inlet (19) is provided on the connecting pipeline of the solid material discharge port (23), and a top air extraction port (6) is provided on the kettle body top cover (1).

9. The high solid-liquid separation reactor according to claim 1, characterized in that: The reactor body comprises a cylindrical tank body connected to the reactor body conical bottom shell (2) in an integral structure, a heating chamber (21) and a cooling chamber (22) are respectively arranged on the cavity of the cylindrical tank body, and a temperature sensor (20) is arranged on the reactor body conical bottom shell (2).

10. The high solid-liquid separation reactor according to claim 1, characterized in that: The kettle body top cover (1) is provided with an observation window mirror (4) and a feed port (5).

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