A tetraethyl orthosilicate production apparatus

Abstract

This invention discloses a production equipment for tetraethyl orthosilicate (TEO), relating to the field of TEO production. The equipment includes a frame on which a reaction vessel is mounted. A hydraulic rod for adjusting the position of the vessel lid is also mounted on the frame. The hydraulic rod is fixed to the frame, and its output end is fixed to the vessel lid. A thermometer and a pressure gauge for temperature and pressure detection are mounted on the vessel lid, with their probes located inside the reaction vessel. A motor is also mounted on the vessel lid. This TEO production equipment employs a feeding mechanism that allows for intermittent feeding and uniform dispersion of solid materials without disrupting the internal pressure of the equipment. This effectively avoids excessive single-feeding of solid materials, which could lead to sedimentation and affect the normal mixing reaction, thus ensuring the optimal mixing effect.

Description

Technical Field

[0001] This invention relates to the field of tetraethyl orthosilicate production technology, specifically to a production equipment for tetraethyl orthosilicate. Background Technology

[0002] Tetraethyl orthosilicate (TEOS) is an important organosilicon compound widely used in coatings, adhesives, ceramic precursors and other fields. At present, the production of tetraethyl orthosilicate mainly relies on the reaction of high-purity silicon powder with anhydrous ethanol as a catalyst. The reaction temperature is 200℃-300℃ and the reaction pressure is 2-5 MPa. In order to ensure the normal progress of the reaction, a high-pressure reactor is required for production. In the existing production process of tetraethyl orthosilicate, the raw materials are generally directly fed into a high-pressure reactor. In the actual reaction process, high-purity silicon powder will be deposited in large quantities at the bottom of the high-pressure reactor due to its own gravity, which will prevent the materials from being fully mixed and reacted, thus affecting the normal progress of the process. Summary of the Invention

[0003] The purpose of this invention is to provide a production apparatus for tetraethyl orthosilicate to solve the problems mentioned in the background art.

[0004] To achieve the above objectives, the present invention provides the following technical solution: a production equipment for tetraethyl orthosilicate, comprising a frame, a reaction vessel mounted on the frame, a hydraulic rod for adjusting the position of the vessel lid mounted on the frame, the hydraulic rod being fixed to the frame and the output end of the hydraulic rod being fixed to the vessel lid, a thermometer and a pressure gauge for temperature and pressure detection mounted on the vessel lid, the detection heads of the thermometer and pressure gauge being located inside the reaction vessel, a motor mounted on the vessel lid, the output end of the motor being connected to a rotating shaft with a bearing connected to the vessel lid; The self-locking mechanism uses air pressure to achieve self-locking between the frame and the vessel lid. The self-locking mechanism is installed on the vessel lid at equal angles. The feeding mechanism is used for intermittent feeding and automatic dispersion of powder. The feeding mechanism is connected to the lid of the vessel and to the rotating shaft.

[0005] Preferably, heating tubes are installed at equal angles inside the reactor, and a discharge valve is fixed on the lower end face of the reactor. The heating tubes can heat the material and ensure the normal progress of the material reaction.

[0006] Preferably, the vessel lid is equipped with a feed pipe for fluid feeding and a feed valve for powder feeding, with the feed valve located above the feeding mechanism. The vessel lid is also equipped with an air inlet connected to a high-pressure pump via a conduit, and a pressure relief solenoid valve is installed on the vessel lid. The pressure relief solenoid valve enables automatic pressure relief inside the device, preventing excessive internal pressure from affecting the normal operation of the device.

[0007] Preferably, the self-locking mechanism includes a fixing box fixed at equal angles inside the vessel lid, and the fixing box has a through hole. The lower end of the fixing box is fixed with a positioning shaft that is nested with the positioning seat. Meanwhile, the positioning seat is fixed at equal angles inside the reactor. Through the nesting action between the positioning shaft and the positioning seat, the positioning between the vessel lid and the reactor can be achieved.

[0008] Preferably, a piston head is slidably connected inside the fixed box, and a first spring is fixed between the piston head and the fixed box. A piston rod is also fixed to the piston head, and the piston rod is slidably connected to the fixed box. The piston rod can be moved by air pressure, thereby providing a basic guarantee for realizing the self-locking between the vessel lid and the reactor.

[0009] Preferably, one end of the piston rod is rotatably connected to the connecting rod, and the other end of the connecting rod is rotatably connected to the limiting plate. The limiting plate and the positioning shaft are slidably connected. At the same time, the limiting plate and the positioning seat are nested to achieve the positioning function. When the piston rod moves, it can provide a basic force for the movement of the limiting plate in conjunction with the transmission action of the connecting rod, thereby providing a basic guarantee for locking and unlocking between the limiting plate and the positioning seat.

[0010] Preferably, a stirring rod is installed on the rotating shaft, and a self-priming impeller is installed at the lower end of the rotating shaft. A pusher plate is also fixed at an equal angle on the rotating shaft, and the pusher plate is installed at an inclination. The pusher plate is set in the storage box. The stirring rod can realize the stirring effect of the material. In conjunction with the self-priming impeller, a negative pressure zone can be generated, thereby automatically sucking the material deposited in the reaction vessel into the self-priming impeller and dispersing it to the outside through the side opening of the self-priming impeller, thus effectively ensuring the mixing effect of the material.

[0011] Preferably, the feeding mechanism includes a storage box fixed on the lid of the vessel, and a fixing plate is fixed inside the lower opening of the storage box. The fixing plate and the vertical rod are slidably connected. At the same time, a sealing ball is fixed at the upper end of the vertical rod. The sealing ball cooperates with the lower opening of the storage box to achieve a seal. Through the function of the sealing ball, a basic guarantee can be provided for the intermittent feeding of materials in the storage box.

[0012] Preferably, a sliding groove ring is fixed to the lower end face of the storage box, and the sliding groove ring is slidably connected to the dispersing disc. The dispersing disc is fixed on the rotating shaft, and a circular plate is slidably connected inside the dispersing disc. The circular plate is slidably connected to the rotating shaft. Through the rotation of the dispersing disc, the material can be effectively dispersed, thereby ensuring the uniform mixing of the material.

[0013] Preferably, a sliding rod is fixed to the lower end face of the circular plate, and the sliding rod is slidably connected to the dispersing disk. A second spring is fixed between the sliding rod and the protective cylinder, and the protective cylinder is fixed to the lower end face of the dispersing disk. Through the elastic action of the second spring, a basic force can be provided for the automatic reset of the circular plate, thereby ensuring the normal operation of the device.

[0014] Compared with the prior art, the beneficial effects of the present invention are: 1. The production equipment for tetraethyl orthosilicate adopts a feeding mechanism, which can achieve intermittent feeding and uniform dispersion of solid materials during the operation of the equipment without disrupting the internal pressure. This effectively avoids excessive feeding of solid materials at one time, which could lead to material sedimentation and affect the normal mixing reaction, thus ensuring the mixing reaction effect of the materials. 2. The production equipment for tetraethyl orthosilicate adopts a pneumatic self-locking mechanism. Compared with the traditional bolt locking mechanism, it can make the assembly and disassembly of the reactor and the lid more convenient, thus facilitating later maintenance and repair. It can also ensure the stability of the connection between the reactor and the lid during the reaction process, and ensure that the reactor and the lid cannot be opened during the process, thereby avoiding the safety accident caused by the high temperature gas and material spraying out due to excessive internal pressure. Attached Figure Description

[0015] Figure 1 This is a frontal three-dimensional structural diagram of the device of the present invention; Figure 2 This is a three-dimensional structural diagram of the overall front cross-section of the device of the present invention; Figure 3 This is a frontal cross-sectional three-dimensional structural diagram of the self-locking mechanism of the present invention; Figure 4 For the present invention Figure 3 Enlarged structural diagram at point A in the middle; Figure 5 This is a three-dimensional structural diagram of the rotating axis of the present invention viewed from below; Figure 6 This is a frontal cross-sectional three-dimensional structural diagram of the storage box of the present invention; Figure 7 This is a schematic diagram of the three-dimensional structure of the dispersion disk of the present invention, viewed from below.

[0016] In the diagram: 1. Frame; 2. Reactor; 201. Heating tube; 202. Discharge valve; 3. Hydraulic rod; 4. Reactor lid; 401. Feed pipe; 402. Feed valve; 403. Gas inlet; 404. Pressure relief solenoid valve; 5. Self-locking mechanism; 501. Fixing box; 502. Through hole; 503. Positioning shaft; 504. Positioning seat; 505. Piston head; 506. First spring; 507. Piston 508. Rod; 509. Connecting rod; 500. Limiting plate; 6. Motor; 7. Rotating shaft; 701. Stirring rod; 702. Self-priming impeller; 703. Pushing plate; 8. Discharging mechanism; 801. Storage box; 802. Fixing plate; 803. Vertical rod; 804. Sealing ball; 805. Sliding groove ring; 806. Dispersing disc; 807. Circular plate; 808. Sliding rod; 809. Second spring; 810. Protective cylinder. Detailed Implementation

[0017] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0018] Please see Figures 1-7 The present invention provides a technical solution: a production equipment for tetraethyl orthosilicate, including a frame 1, a reaction vessel 2 mounted on the frame 1, a hydraulic rod 3 for adjusting the position of the vessel cover 4 mounted on the frame 1, the hydraulic rod 3 being fixed to the frame 1, and the output end of the hydraulic rod 3 being fixed to the vessel cover 4, a thermometer and a pressure gauge for temperature and pressure detection mounted on the vessel cover 4, the detection heads of the thermometer and pressure gauge being located inside the reaction vessel 2, a motor 6 mounted on the vessel cover 4, and the output end of the motor 6 being connected to a rotating shaft 7 with a bearing connected to the vessel cover 4; The self-locking mechanism 5 uses air pressure to achieve self-locking between the frame 1 and the vessel lid 4. The self-locking mechanism 5 is installed on the vessel lid 4 at equal angles. The feeding mechanism 8 is used for intermittent feeding and automatic dispersion of powder. The feeding mechanism 8 is connected to the lid 4 and the rotating shaft 7.

[0019] Heating tubes 201 are installed at equal angles inside the reactor 2, and a discharge valve port 202 is fixed on the lower end face of the reactor 2; a feed pipe 401 for fluid feeding is installed on the reactor cover 4, and a feed valve port 402 for powder feeding is installed on the reactor cover 4, and the feed valve port 402 is located above the feeding mechanism 8; an air inlet 403 is installed on the reactor cover 4 and connected to a high-pressure pump through a conduit, and a pressure relief solenoid valve 404 is also installed on the reactor cover 4. When using the production equipment for tetraethyl orthosilicate, such as Figures 1-7 As shown, anhydrous ethanol is first added to reactor 2 through feed pipe 401, followed by the catalyst (cuprous chloride) through feed pipe 401. After addition, the valve connected to feed pipe 401 is closed, and then high-purity silicon powder is added through feed valve 402. The high-purity silicon powder is then stored in storage box 801 (ensuring that the high-purity silicon powder does not directly contact the anhydrous ethanol and catalyst during addition). After addition, feed valve 402 is closed, sealing the entire device. Then... The high-pressure pump, conduit, and air inlet 403 can pressurize the device with air. The pressure gauge is used to detect the pressure and keep the internal pressure of the device between 3.5 MPa and 3.5 MPa. The heating tube 201 can then be used to heat the material. The temperature gauge can be used to detect the material temperature and keep it at 250℃. This ensures the normal reaction of the material in the subsequent process. During the pressurization process, when the internal pressure of the device exceeds 3.5 MPa, the pressure relief solenoid valve 404 can automatically release the pressure to ensure the safety of the internal pressure of the device. A stirring rod 701 is mounted on the rotating shaft 7, and a self-priming impeller 702 is mounted on the lower end of the rotating shaft 7. A pusher plate 703 is also fixed at an equal angle on the rotating shaft 7, and the pusher plate 703 is installed at an angle. The pusher plate 703 is located inside the storage box 801. The feeding mechanism 8 includes a storage box 801 fixed to the lid 4, and a fixing plate 802 is fixed inside the lower opening of the storage box 801. The fixing plate 802 is slidably connected to the vertical rod 803. A sealing ball 804 is fixed to the upper end of the vertical rod 803, and the sealing ball 804 is matched with the lower opening of the storage box 801. The system achieves a seal; a sliding ring 805 is fixed to the lower end face of the storage box 801, and the sliding ring 805 is slidably connected to the dispersing disc 806. The dispersing disc 806 is fixed to the rotating shaft 7, and a circular plate 807 is slidably connected inside the dispersing disc 806. The circular plate 807 is slidably connected to the rotating shaft 7. A sliding rod 808 is fixed to the lower end face of the circular plate 807, and the sliding rod 808 is slidably connected to the dispersing disc 806. A second spring 809 is fixed between the sliding rod 808 and the protective cylinder 810, and the protective cylinder 810 is fixed to the lower end face of the dispersing disc 806. After the materials are added, such as Figures 1-7As shown, high-purity silicon powder entering the storage box 801 falls onto the circular plate 807 through the lower opening of the storage box 801. As the gravity of the silicon powder increases, the circular plate 807 overcomes the preload of the second spring 809 and moves downward. Combined with the sliding guide action between the slide rod 808 and the dispersing disc 806, the stability of the circular plate 807's movement is ensured. When the circular plate 807 moves downward, it separates from the vertical rod 803, causing the sealing ball 804 to move downward synchronously under its own gravity and the force of the silicon powder flow. This, combined with the sliding guide action between the slide rod 808 and the dispersing disc 806, ensures the stability of the circular plate 807's movement. The sliding guide action between the sealing ball 804 and the fixed plate 802 ensures the stability of the movement of the sealing ball 804 until the sealing ball 804 engages with the lower opening of the storage box 801 to achieve a seal, thus completing one feeding operation. Then, the motor 6 is started, which drives the rotating shaft 7, stirring rod 701, self-priming impeller 702, dispersing disc 806, and circular plate 807 to rotate. At this time, under the action of centrifugal force, the high-purity silicon powder on the circular plate 807 is continuously and evenly sprinkled into the reaction vessel 2 through the side opening of the dispersing disc 806. Combined with the action of the stirring rod 701, the materials can be stirred and mixed, facilitating the reaction. When the high-purity powder sinks under its own weight, the rotation of the self-priming impeller 702 creates a negative pressure inside, drawing the sinking high-purity powder into the impeller 702 and dispersing it outwards again through the side openings of the impeller 702, thus effectively ensuring the mixing effect of the materials. Furthermore, as the dispersing disc 806 and the circular plate 807 rotate to disperse the materials, the circular plate 807... As the material on plate 7 decreases, when the remaining weight of silicon powder on plate 807 is lower than the pre-tightening force of spring 809, plate 807 moves upward under the action of spring 809. When plate 807 contacts vertical rod 803, vertical rod 803 can move upward under the action of spring 809, thereby causing sealing ball 804 to move upward and release the seal of the lower opening of storage box 801, allowing material in the lower opening of storage box 801 to fall again, thus realizing intermittent feeding and automatic dispersion of material. The self-locking mechanism 5 includes a fixed box 501 fixed at equal angles inside the vessel lid 4, and a through hole 502 is provided on the fixed box 501. A positioning shaft 503 is fixed at the lower end of the fixed box 501 and nested with the positioning seat 504. The positioning seat 504 is fixed at equal angles inside the reactor 2. A piston head 505 is slidably connected inside the fixed box 501, and a first spring 506 is fixed between the piston head 505 and the fixed box 501. A piston rod 507 is also fixed on the piston head 505, and the piston rod 507 is slidably connected to the fixed box 501. One end of the piston rod 507 is rotatably connected to a connecting rod 508, and the other end of the connecting rod 508 is rotatably connected to a limiting plate 509. The limiting plate 509 is slidably connected to the positioning shaft 503, and the limiting plate 509 and the positioning seat 504 are nested to achieve a positioning function. During the use of the device, when pressurizing the device by supplying air inside, such as Figures 1-4 As shown, as the internal pressure of the device increases, high-pressure gas enters the fixed box 501 through the through hole 502, causing the piston head 505 to move downward under the force of the gas pressure. This causes the piston rod 507 to move downward synchronously. During the downward movement of the piston rod 507, in conjunction with the transmission action of the connecting rod 508, the limiting plate 509 is forced to slide outward towards the positioning shaft 503 until the limiting plate 509 and the positioning seat 504 are nested together, thus locking the lid 4 and the reactor 2. This ensures that during the reaction process, the high pressure inside the device prevents the lid 4 and the reactor 2 from opening, avoiding the safety accident caused by the high internal pressure leading to the opening of the lid and the ejection of high-temperature gas and materials. This is the working principle of the tetraethyl orthosilicate production equipment.

[0020] It should be noted that, in this document, the terms “comprising,” “including,” or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0021] This article uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only for the purpose of helping to understand the method and core ideas of the present invention. The above descriptions are only preferred embodiments of the present invention. It should be noted that due to the limitations of textual expression, while there are objectively infinite specific structures, those skilled in the art can make several improvements, modifications, or changes without departing from the principles of the present invention, and can also combine the above technical features in an appropriate manner. These improvements, modifications, changes, or combinations, or the direct application of the inventive concept and technical solution to other situations without modification, should all be considered within the scope of protection of the present invention.

Claims

1. A production apparatus for tetraethyl orthosilicate, comprising a frame (1), wherein a reaction vessel (2) is mounted on the frame (1), and a hydraulic rod (3) for adjusting the position of a vessel lid (4) is also mounted on the frame (1), wherein the hydraulic rod (3) is fixed to the frame (1), and the output end of the hydraulic rod (3) is fixed to the vessel lid (4), characterized in that: The thermometer and pressure gauge for temperature and pressure detection are installed on the lid (4), and the detection heads of the thermometer and pressure gauge are located inside the reactor (2). The lid (4) is equipped with a motor (6), and the output end of the motor (6) is connected to the rotating shaft (7) with the bearing connected to the lid (4). The self-locking mechanism (5) uses air pressure to achieve self-locking between the frame (1) and the lid (4). The self-locking mechanism (5) is installed on the lid (4) at equal angles. The feeding mechanism (8) is used for intermittent feeding of powder and automatic dispersion of powder. The feeding mechanism (8) is connected to the lid (4) and to the rotating shaft (7).

2. The production equipment for tetraethyl orthosilicate according to claim 1, characterized in that: Heating tubes (201) are installed at equal angles inside the reactor (2), and a discharge valve (202) is fixed on the lower end face of the reactor (2).

3. The production equipment for tetraethyl orthosilicate according to claim 1, characterized in that: The lid (4) is equipped with a feed pipe (401) for fluid feeding and a feed valve (402) for powder feeding. The feed valve (402) is located above the feeding mechanism (8). The lid (4) is equipped with an air inlet (403) that is connected to a high-pressure pump through a conduit. The lid (4) is also equipped with a pressure relief solenoid valve (404).

4. The production equipment for tetraethyl orthosilicate according to claim 1, characterized in that: The self-locking mechanism (5) includes a fixed box (501) fixed at an equal angle inside the lid (4), and the fixed box (501) has a through hole (502), and the lower end of the fixed box (501) is fixed with a positioning shaft (503) nested with the positioning seat (504), while the positioning seat (504) is fixed at an equal angle inside the reactor (2).

5. The production equipment for tetraethyl orthosilicate according to claim 4, characterized in that: A piston head (505) is slidably connected inside the fixed box (501), and a first spring (506) is fixed between the piston head (505) and the fixed box (501). A piston rod (507) is also fixed on the piston head (505), and the piston rod (507) is slidably connected to the fixed box (501).

6. The production equipment for tetraethyl orthosilicate according to claim 5, characterized in that: The piston rod (507) is rotatably connected to one end of the connecting rod (508), and the other end of the connecting rod (508) is rotatably connected to the limiting plate (509). The limiting plate (509) is slidably connected to the positioning shaft (503), and the limiting plate (509) and the positioning seat (504) are nested to achieve the positioning function.

7. The production equipment for tetraethyl orthosilicate according to claim 1, characterized in that: A stirring rod (701) is installed on the rotating shaft (7), and a self-priming impeller (702) is installed at the lower end of the rotating shaft (7). A pusher plate (703) is also fixed at an equal angle on the rotating shaft (7). The pusher plate (703) is installed at an inclination and is located in the storage box (801).

8. The production equipment for tetraethyl orthosilicate according to claim 1, characterized in that: The feeding mechanism (8) includes a storage box (801) fixed on the lid (4), and a fixing plate (802) is fixed inside the lower opening of the storage box (801). The fixing plate (802) and the vertical rod (803) are slidably connected. At the same time, a sealing ball (804) is fixed at the upper end of the vertical rod (803). The sealing ball (804) cooperates with the lower opening of the storage box (801) to achieve sealing.

9. The production equipment for tetraethyl orthosilicate according to claim 8, characterized in that: The lower end face of the storage box (801) is also fixed with a sliding groove ring (805), and the sliding groove ring (805) is slidably connected to the dispersing disc (806). The dispersing disc (806) is fixed on the rotating shaft (7), and a circular plate (807) is slidably connected inside the dispersing disc (806). The circular plate (807) is slidably connected to the rotating shaft (7).

10. The production equipment for tetraethyl orthosilicate according to claim 9, characterized in that: A sliding rod (808) is fixed to the lower end face of the circular plate (807), and the sliding rod (808) is slidably connected to the dispersing disk (806). A second spring (809) is fixed between the sliding rod (808) and the protective cylinder (810), while the protective cylinder (810) is fixed to the lower end face of the dispersing disk (806).

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