A purification device for hexamethyldisilazane production

Abstract

The utility model relates to a kind of purification device for hexamethyldisilazane production applied to the technical field of chemical product purification, realize the inner shell in the distillation kettle main body into which hexamethyldisilazane is input, subsequently through controller opens servo motor drive spindle and drives mixing paddle rotation to its mixing, while through opening heating equipment to multiple spiral heating tube heating, and spiral heating tube and the inner shell side wall of heat-conducting material are pasted, heat can be transferred to the inner shell to hexamethyldisilazane is purified, while mixing paddle is rotationally connected with the heat-conducting ring pasted in the inner wall of inner shell by heat transfer block, spindle and mixing paddle are heat-conducting material, the heat on inner shell can be transferred heat to mixing paddle by heat transfer block at this time, so that mixing paddle is heated when mixing contact to hexamethyldisilazane, during purification, the temperature change in the inner shell can be monitored by multiple temperature sensors, multiple spiral heating tube temperature adjustment can be controlled separately.

Description

Technical Field

[0001] This utility model relates to a purification device, and more particularly to a purification device for the production of hexamethyldisilazane applied in the field of chemical product purification technology. Background Technology

[0002] Hexamethyldisilazane is an important organosilicon compound with wide applications in organic synthesis, semiconductor manufacturing, and other fields. During the production of hexamethyldisilazane, due to the complexity of the reaction process, the product often contains various impurities, such as unreacted raw materials and byproducts. The presence of these impurities can severely affect the product quality and performance of hexamethyldisilazane, thus requiring purification treatment.

[0003] Chinese patent CN217940169U discloses a purification device for hexamethyldisilazane. This invention has the advantages of enabling the reactants to react more thoroughly and increasing the reaction rate, isolating the precipitate after the reaction at the bottom of the reaction cylinder, and discharging the distilled diethyl ether and hexamethyldisilazane from two different outlets during fractional distillation to prevent cross-contamination and improve the purity of the purified product.

[0004] Existing methods for purifying hexamethyldisilazane mainly employ distillation. During distillation, the mixed liquid is heated unevenly in the distillation vessel, resulting in insufficient vaporization of hexamethyldisilazane and thus prolonging the distillation time. Utility Model Content

[0005] The technical problem to be solved by this invention in view of the above-mentioned prior art is that during the distillation process, the mixed liquid is heated unevenly in the distillation vessel, which causes hexamethyldisilazane to not be fully vaporized, thereby prolonging the distillation time.

[0006] To address the aforementioned problems, this utility model provides a purification device for the production of hexamethyldisilazane, comprising a distillation kettle body, a sealing cap with a feed inlet connected to the top of the distillation kettle body by screws, a servo motor fixedly connected to the top of the sealing cap, a rotating shaft detachably connected to the output end of the servo motor, multiple mixing paddles fixedly connected annularly at equal intervals to the side wall of the rotating shaft, an inner shell provided inside the distillation kettle body, and a sandwich formed between the inner shell and the distillation kettle body, a heat-conducting ring fixedly connected to the inner wall of the inner shell, a heat transfer block fixedly connected to the end of the mixing paddle away from the rotating shaft, and the heat transfer block engaging with the heat-conducting ring, multiple sets of spiral heating tubes wound around the outer wall of the inner shell, multiple temperature sensors fixedly connected to the outer wall of the inner shell, a power interface extending to the outside of the distillation kettle body fixedly connected to one end of the spiral heating tubes, and a power supply device connected to the power interface via a wire.

[0007] In the above-mentioned purification device, by setting multiple heat transfer blocks in the body of the distillation vessel, the temperature change inside the inner shell can be monitored in real time. Then, the temperature of the spiral heating tube can be individually controlled to adjust the temperature, so that the temperature inside the inner shell is evenly distributed. At the same time, the heat is transferred to the mixing paddle, which can heat the hexamethyldisilazane when it comes into contact with it during mixing, thereby achieving the effect of uniform heating of the mixed liquid in the body of the distillation vessel.

[0008] As a further improvement of this application, a connecting shaft is connected to the output end of the servo motor, a locking block is fixedly connected to the end of the connecting shaft away from the servo motor, and a locking groove is fixedly connected to the top of the rotating shaft, and the locking groove engages with the locking block.

[0009] As a further improvement of this application, a spiral condenser tube is arranged around the outer wall of the inner shell, which is offset from the spiral heating tube. The input end and output end of the spiral condenser tube are respectively threadedly connected to an output port extending to the body of the distillation vessel.

[0010] As a further improvement of this application, a condenser is provided on the outside of the distillation vessel body. The output end and input end of the condenser are respectively threaded with adapters. The adapters are respectively threaded with multiple corresponding output ports through delivery pipes. Solenoid valves are provided at the connection between the delivery pipe and the adapter.

[0011] As another improvement of this application, a circulation pump is installed inside the condenser, and the output and input ends of the circulation pump are respectively connected to two adapters via connecting pipes.

[0012] As a further improvement to this application, the inner shell, shaft, and hybrid propeller are all made of thermally conductive material.

[0013] As a further improvement to this application, a controller, including a power supply, a condenser, a servo motor, a solenoid valve, and a circulating pump, is fixedly connected to the body of the distillation vessel.

[0014] In summary, the operator opens the feed port and adds hexamethyldisilazane into the inner shell of the distillation vessel. At this time, the output end of the servo motor is engaged with the slot and the rotating shaft via a locking block. Then, the controller activates the servo motor to drive the rotating shaft and rotate the mixing paddle to mix the hexamethyldisilazane. Simultaneously, the heating equipment is activated to heat multiple spiral heating tubes, which are in contact with the heat-conducting material of the inner shell sidewall. This allows heat to be transferred to the inner shell to purify the hexamethyldisilazane. At the same time, the mixing paddle is rotatably connected to the heat-conducting ring attached to the inner shell wall via a heat transfer block. Both the rotating shaft and the mixing paddle are made of heat-conducting material. At this time, the heat on the inner shell can be transferred to the mixing paddle through the heat transfer block, so that the mixing paddle can heat the hexamethyldisilazane during mixing and contact. During the purification process, multiple temperature sensors can monitor the temperature changes inside the inner shell. In case of uneven temperature, multiple spiral heating tubes can be individually controlled to adjust the temperature. Attached Figure Description

[0015] Figure 1 These are isometric views of the distillation kettle according to the first and second embodiments of this application; Figure 2 This is a schematic diagram of the internal structure of the distillation vessel according to the first and second embodiments of this application; Figure 3 This is a schematic diagram of the hybrid propeller installation according to the first embodiment of this application; Figure 4 For this application Figure 3 Enlarged view of point A in the middle; Figure 5 This is a schematic diagram of the spiral heating tube structure according to the first embodiment of this application; Figure 6 This is a schematic diagram of the internal structure of the sealing cap according to the first embodiment of this application.

[0016] Explanation of the labels in the diagram: 1. Distillation vessel body; 2. Sealing cover; 3. Servo motor; 4. Power interface; 5. Output port; 6. Condenser; 7. Adapter; 8. Delivery pipe; 9. Inner shell; 10. Slot; 11. Rotating shaft; 12. Mixing paddle; 13. Spiral heating tube; 14. Spiral condenser tube; 15. Heat-conducting ring; 16. Heat transfer block; 17. Temperature sensor; 18. Locking block; 19. Connecting shaft; 20. Feed inlet. Detailed Implementation

[0017] The two embodiments of this application will be described in detail below with reference to the accompanying drawings.

[0018] First implementation method: Figures 1-6 A purification apparatus for the production of hexamethyldisilazane is shown, comprising a distillation vessel body 1, a sealing cover 2 with a feed inlet 20 connected to the top of the distillation vessel body 1 by screws, a servo motor 3 fixedly connected to the top of the sealing cover 2, a rotating shaft 11 detachably connected to the output end of the servo motor 3, a plurality of mixing paddles 12 fixedly connected annularly at equal intervals to the side wall of the rotating shaft 11, an inner shell 9 provided inside the distillation vessel body 1, and a sandwich formed between the inner shell 9 and the distillation vessel body 1, a heat-conducting ring 15 fixedly connected to the inner wall of the inner shell 9, a heat transfer block 16 fixedly connected to the end of the mixing paddles away from the rotating shaft 11, and the heat transfer block 16 engaging with the heat-conducting ring 15, a plurality of spiral heating tubes 13 wound around the outer wall of the inner shell 9, a plurality of temperature sensors 17 fixedly connected to the outer wall of the inner shell 9, a power interface 4 extending to the outside of the distillation vessel body 1 fixedly connected to one end of the spiral heating tubes 13, and a power supply device connected to the power interface 4 through a wire; The output end of the servo motor 3 is connected to a connecting shaft 19. A locking block 18 is fixedly connected to the end of the connecting shaft 19 away from the servo motor 3. A locking groove 10 is fixedly connected to the top of the rotating shaft 11, and the locking groove 10 engages with the locking block 18. The inner shell 9, the rotating shaft 11 and the mixing paddle 12 are all made of heat-conducting material. The controller power supply, condenser 6, servo motor 3, solenoid valve and circulation pump controller are fixedly connected to the distillation kettle body 1.

[0019] The temperature sensor 17 uses existing technology, and those skilled in the art can select a suitable temperature sensor 17 from the existing technology for installation, such as: PT100 platinum resistance temperature sensor.

[0020] Working principle: The operator opens the feed port 20 and adds hexamethyldisilazane into the inner shell 9 of the distillation vessel body 1. At this time, the output end of the servo motor 3 is engaged with the slot 10 and the rotating shaft 11 through the locking block 18. Then, the controller starts the servo motor 3 to drive the rotating shaft 11 to rotate the mixing paddle 12 to mix it. At the same time, the heating equipment is turned on to heat multiple spiral heating tubes 13. The spiral heating tubes 13 are attached to the heat-conducting material side wall of the inner shell 9, which can transfer heat to the inner shell 9 to mix the hexamethyldisilazane. Purification is carried out, and at the same time, the mixing paddle 12 is rotatably connected to the heat-conducting ring 15 attached to the inner wall of the inner shell 9 through the heat transfer block 16. Both the rotating shaft 11 and the mixing paddle 12 are made of heat-conducting materials. At this time, the heat on the inner shell 9 can be transferred to the mixing paddle 12 through the heat transfer block 16, so that the mixing paddle 12 can be heated when it comes into contact with hexamethyldisilazane. During the purification, the temperature change inside the inner shell 9 can be monitored by multiple temperature sensors 17, so that in the case of uneven temperature, multiple spiral heating tubes 13 can be individually controlled to adjust the temperature. This invention allows for real-time monitoring of temperature changes within the inner shell 9 by setting multiple heat transfer blocks 16 inside the distillation vessel body 1. Subsequently, the temperature of the spiral heating tube 13 can be individually controlled to adjust the temperature, ensuring uniform temperature distribution within the inner shell 9. Simultaneously, heat is transferred to the mixing paddle 12, which can heat the hexamethyldisilazane during mixing, thereby achieving uniform heating of the mixed liquid within the distillation vessel body 1.

[0021] Second implementation method: Figures 1-2The inner shell 9 is shown to be surrounded by a spiral condenser tube 14 that is staggered from the spiral heating tube 13. The input and output ends of the spiral condenser tube 14 are respectively threaded to an output port 5 extending to the outside of the distillation vessel body 1. A condenser 6 is provided on the outside of the distillation vessel body 1. The output and input ends of the condenser 6 are respectively threaded to an adapter 7. The adapter 7 is threaded to multiple corresponding output ports 5 through a delivery pipe 8. A solenoid valve is provided at the connection between the delivery pipe 8 and the adapter 7. A circulation pump is installed in the condenser 6. The output and input ends of the circulation pump are respectively threaded to two adapters 7 through connecting pipes.

[0022] The condenser 6 adopts existing technology, and a suitable condenser 6 from the existing technology shall be selected and installed by a person skilled in the art, such as GLC-80S.

[0023] Working principle: When the temperature inside the inner shell 9 is overheated, the circulation pump in the condenser 6 is turned on first. Then, the solenoid valve connected to the corresponding spiral condenser tube 14 is selectively turned on according to the location to be cooled. The coolant is delivered to the corresponding spiral condenser tube 14 in the distillation vessel body 1 through the delivery pipe 8. The coolant flows around the surface of the inner shell 9 through the spiral condenser tube 14 to cool it down. Finally, it returns to the condenser 6 from the output end for intercooling, thereby achieving the effect of continuous cooling of the inner shell 9. This invention, by setting spiral condenser tubes 14 at intervals from spiral heating tubes 13 on the surface of the inner shell 9, can work with condenser 6 to locally cool the areas inside the inner shell 9 where the temperature is too high, and local cooling can prevent overheating and decomposition.

[0024] In light of current practical needs, the above-described embodiments adopted in this application are not limited to these. Any changes made within the scope of knowledge possessed by those skilled in the art without departing from the concept of this application still fall within the protection scope of this utility model.

Claims

1. A purification apparatus for the production of hexamethyldisilazane, comprising a distillation vessel body (1), characterized in that: The top of the distillation vessel body (1) is connected to a sealing cover (2) with a feed inlet (20) by screws. A servo motor (3) is fixedly connected to the top of the sealing cover (2). A rotating shaft (11) is detachably connected to the output end of the servo motor (3). Multiple mixing paddles (12) are fixedly connected to the side wall of the rotating shaft (11) at equal intervals. An inner shell (9) is provided inside the distillation vessel body (1), and a sandwich is formed between the inner shell (9) and the distillation vessel body (1). A guide is fixedly connected to the inner wall of the inner shell (9). A heat ring (15) is provided. A heat transfer block (16) is fixedly connected to one end of the mixing paddle (12) away from the rotating shaft (11), and the heat transfer block (16) engages with the heat conduction ring (15). Multiple sets of spiral heating tubes (13) are wound around the outer wall of the inner shell (9). Multiple temperature sensors (17) are fixedly connected to the outer wall of the inner shell (9). A power interface (4) extending to the outside of the distillation vessel body (1) is fixedly connected to one end of the spiral heating tube (13), and a power supply device is connected to the power interface (4) through a wire.

2. The purification apparatus for the production of hexamethyldisilazane according to claim 1, characterized in that: The output end of the servo motor (3) is connected to a connecting shaft (19), and a locking block (18) is fixedly connected to the end of the connecting shaft (19) away from the servo motor (3). A slot (10) is fixedly connected to the top of the rotating shaft (11), and the slot (10) engages with the locking block (18).

3. The purification apparatus for the production of hexamethyldisilazane according to claim 1, characterized in that: The outer wall of the inner shell (9) is surrounded by a spiral condenser (14) that is misaligned with the spiral heating tube (13). The input end and output end of the spiral condenser (14) are respectively threaded with an output port (5) extending to the outside of the distillation vessel body (1).

4. The purification apparatus for the production of hexamethyldisilazane according to claim 1, characterized in that: A condenser (6) is provided on the outside of the body (1) of the distillation vessel. The output end and the input end of the condenser (6) are respectively threaded with an adapter (7). The adapter (7) is threaded to multiple corresponding output ports (5) through a delivery pipe (8). A solenoid valve is provided at the connection between the delivery pipe (8) and the adapter (7).

5. The purification apparatus for the production of hexamethyldisilazane according to claim 4, characterized in that: The condenser (6) is equipped with a circulation pump, and the output and input ends of the circulation pump are respectively connected to two adapters (7) by connecting pipes.

6. The purification apparatus for the production of hexamethyldisilazane according to claim 1, characterized in that: The inner shell (9), the rotating shaft (11), and the mixing paddle (12) are all made of thermally conductive material.

7. A purification apparatus for the production of hexamethyldisilazane according to claim 5, characterized in that: The controller, power supply, condenser (6), servo motor (3), solenoid valve and circulation pump are fixedly connected to the body (1) of the distillation vessel.

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