Raw material hydrolysis reactor for preparing hexamethyldisiloxane
By designing a raw material hydrolysis reactor for the preparation of hexamethyldisiloxane with precise control over the feeding rate and temperature, the problem of violent reaction caused by improper feeding rate was solved, and the product purity and reaction efficiency were improved.
Patent Information
- Application Number
- CN202520261797.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-18
- Publication Date
- 2025-12-19
- Estimated Expiration
- 2035-02-18
AI Technical Summary
In the existing technology, improper control of the feeding rate of hexamethyldisiloxane raw material leads to violent reactions, making it difficult to control the release of heat, affecting the reaction time and temperature, resulting in intermolecular condensation reactions and reducing purity.
A raw material hydrolysis reactor including a flow meter, an electric heating module and a stirring system was designed. By precisely controlling the feeding rate and temperature, combined with a two-way stirring structure, the reaction is ensured to proceed uniformly.
This method improves the purity of hexamethyldisiloxane, avoids violent reactions, and ensures the controllability and efficiency of the reaction.
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Figure CN223683550U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to a chemical industry technical field especially relates to a raw material hydrolysis reactor for preparing hexamethyldisiloxane. BACKGROUND
[0002] Hexamethyldisiloxane is an organosilicon compound, colorless transparent liquid at room temperature, has lower viscosity and boiling point, and good volatility and thermal stability, is mainly used as the raw material of producing silicone oil, silicone rubber, silicone resin and other organosilicon products, also is used for improving the leveling and gloss of paint, ink, cosmetics, is used as surfactant and release agent.
[0003] The patent with the authorized announcement number CN212017796U discloses a hydrolysis device for producing hexamethyldisiloxane, including a reaction tank, a stirrer, a feed pipe network, an annular mixing pipe is fixedly installed in the reaction tank near the upper end position, a plurality of groups of evenly distributed liquid outlets are opened on the mixing pipe, the feed pipe network penetrates into the inside of the reaction tank from the side wall of the top end of the reaction tank, and a discharge pipe is installed at the bottom of the reaction tank;The patent proposes that the preliminary mixing feed pipe network and annular mixing pipe are used before the material is fed into the reaction tank, and are provided with a rotating disc and a stirring paddle combined stirrer, so that the raw materials are rapidly and fully mixed;But when using the patent to hydrolyze the hexamethyldisiloxane raw material, the speed control in the process of raw material feeding is not proper, and violent reaction is easy to occur, and a large amount of heat is released, so that the reaction time and reaction temperature in the reaction tank are difficult to control, the condensation reaction between hexamethyldisiloxane molecules occurs, and polysiloxane with higher molecular weight is formed, thereby affecting the purity of hexamethyldisiloxane during preparation.
[0004] Therefore, it is necessary to design a raw material hydrolysis reactor for preparing hexamethyldisiloxane, which can accurately feed. UTILITY MODEL CONTENTS
[0005] In order to overcome the defects that when the existing patent is used to hydrolyze the hexamethyldisiloxane raw material, the speed control in the process of raw material feeding is not proper, and violent reaction is easy to occur, and a large amount of heat is released, so that the reaction time and reaction temperature in the reaction tank are difficult to control, the condensation reaction between hexamethyldisiloxane molecules occurs, and polysiloxane with higher molecular weight is formed, thereby affecting the purity of hexamethyldisiloxane during preparation, the utility model provides a raw material hydrolysis reactor for preparing hexamethyldisiloxane, which can accurately feed.
[0006] The utility model discloses a technical scheme is: a kind of raw material hydrolysis reactor for preparing hexamethyldisiloxane, including support seat, shell, reaction vessel, motor, rotating rod, stirring plate, feed pipe, discharge pipe, first valve and gas outlet pipe, multiple support seats are installed in shell lower part, reaction vessel is arranged in shell interior, motor is installed in shell top, rotating rod is connected with rotating rod on the output shaft of motor by coupling, rotating rod penetrates shell and reaction vessel, rotating rod lower end is installed with stirring plate, two feed pipes that penetrate shell are connected and communicated with the reaction vessel top, discharge pipe that penetrates shell is connected and communicated with the reaction vessel bottom, first valve is installed on discharge pipe, gas outlet pipe that penetrates shell is connected and communicated with the reaction vessel top, still including flowmeter, second valve, temperature detector, electric heating module, control panel and control knob, flowmeter is installed in the end of feed pipe close to shell, second valve is installed in the end of feed pipe away from shell, temperature detector for detecting the temperature of reaction vessel is installed on shell, electric heating module is arranged between the gap of shell and reaction vessel, control panel is installed on one side of shell, control knob is installed on control panel.
[0007] In one of the embodiments, the signal output end of the temperature detector is electrically connected with the signal input end of the control panel, the signal input end of the electric heating module is electrically connected with the signal output end of the control knob, and the signal output end of the flowmeter is electrically connected with the signal input end of the control panel.
[0008] In one of the embodiments, the utility model further includes a first bevel gear, a support frame, a rotating shaft, a second bevel gear, a third bevel gear, a connecting ring and a stirring frame, the first bevel gear is fixedly connected to the rotating rod, the support frame is installed in the shell, the connecting ring is rotatably arranged on the support frame, the third bevel gear is fixedly connected to the top of the connecting ring, the stirring frame is fixedly connected to the bottom of the connecting ring, the rotating rod penetrates the support frame, the connecting ring and the stirring frame, the rotating shaft is rotatably arranged on both sides of the shell, the second bevel gear is fixedly connected to one end of the rotating shaft close to the rotating rod, and the first bevel gear and the third bevel gear are meshed and driven by the two second bevel gears.
[0009] In one of the embodiments, the utility model further includes a liquid storage tank, a liquid adding pipe, an air guide pipe and a third valve, the liquid storage tank is installed on one side of the shell, the liquid adding pipe is connected and communicated with the top of the liquid storage tank, the air guide pipe is connected and communicated with the gas outlet pipe, the air guide pipe penetrates the liquid storage tank, and the third valve is connected and communicated with one side of the liquid storage tank away from the shell.
[0010] In one of the embodiments, the utility model further includes an observation glass, and the observation glass is embeddedly installed on the shell and the reaction vessel.
[0011] In one of the embodiments, the utility model further includes a foot pad, and the foot pad is installed on one side of the support seat away from the shell.
[0012] In one of the embodiments, a sealing cover is further included, and the sealing cover is slidably arranged on the liquid adding pipe.
[0013] The beneficial effects are: 1. The dosages of raw materials added into the reaction container are accurately controlled through the feeding pipe, the flow meter and the second valve, and the temperature of the reaction container is adjusted through the electric heating module, so that the reaction is not out of control due to excessive one-time addition of hexamethyldisilazane.
[0014] 2. The stirring plate and the first bevel gear are driven to rotate through the rotating rod, the stirring frame is driven to rotate reversely through the connecting ring, so that the hexamethyldisilazane and the deionized water in the reaction container are stirred from two different directions, so that the hexamethyldisilazane and the deionized water are fully contacted and rapidly hydrolyzed, and the efficiency of the hydrolysis reaction is improved.
[0015] 3. In the process of the hydrolysis reaction, the ammonia gas generated is introduced into the liquid storage tank, and the water in the liquid storage tank absorbs the ammonia gas to generate ammonia water, so that the ammonia gas is prevented from diffusing into the air to cause air pollution. BRIEF DESCRIPTION OF DRAWINGS
[0016] Figure 1 It is a three-dimensional structure schematic view of the utility model.
[0017] Figure 2 It is a three-dimensional sectional structure schematic view of the shell, the reaction container and the rotating rod of the utility model.
[0018] Figure 3 It is a three-dimensional sectional structure schematic view of the shell, the stirring plate and the support frame of the utility model.
[0019] Figure 4 It is a three-dimensional structure schematic view of the rotating rod, the rotating shaft and the stirring frame of the utility model.
[0020] Figure 5 It is an explosion view of the support frame, the connecting ring and the stirring frame of the utility model.
[0021] Figure 6 It is a three-dimensional sectional structure schematic view of the shell, the liquid storage tank and the air guide pipe of the utility model.
[0022] In the drawings, 1 is a support seat, 2 is a shell, 201 is a temperature detector, 3 is a reaction container, 4 is a motor, 5 is a rotating rod, 6 is a stirring plate, 7 is a discharge pipe, 8 is a first valve, 9 is a feeding pipe, 10 is a flow meter, 11 is a second valve, 12 is an electric heating module, 13 is a control panel, 14 is a control knob, 15 is an air outlet pipe, 16 is a first bevel gear, 1601 is a support frame, 17 is a rotating shaft, 18 is a second bevel gear, 19 is a third bevel gear, 20 is a connecting ring, 21 is a stirring frame, 22 is a liquid storage tank, 23 is a liquid adding pipe, 24 is an air guide pipe, 25 is a third valve, 26 is an observation glass, 27 is a foot pad, and 28 is a sealing cover. Detailed Implementation
[0023] The embodiments of this utility model will now be described in detail with reference to the accompanying drawings.
[0024] Example 1: A raw material hydrolysis reactor for the preparation of hexamethyldisiloxane, see reference. Figures 1-4 As shown, the system includes a support base 1, an outer shell 2, a reaction vessel 3, a motor 4, a rotating rod 5, a stirring plate 6, a feed pipe 9, a discharge pipe 7, a first valve 8, and a vent pipe 15. Three support bases 1 are bolted together at the lower part of the outer shell 2. Foot pads 27 are installed at the bottom of each support base 1 to increase friction between the support base 1 and the ground, improving the stability of the outer shell 2. The reaction vessel 3 is housed inside the outer shell 2. Both the outer shell 2 and the reaction vessel 3 have embedded observation glass 26, allowing real-time observation of the reaction within the reaction vessel 3 for timely control of the raw material hydrolysis. A motor 4 is bolted to the top of the outer shell 2. A rotating rod 5 is connected to the output shaft of the motor 4 via a coupling. The rotating rod 5 passes through the outer shell 2 and the reaction vessel 3. A stirring plate 6 is bolted to the lower end of the rotating rod 5. Two feed pipes 9, penetrating the outer shell 2, are connected and connected to the top of the reaction vessel 3. The bottom of the reaction vessel 3 is connected to and communicates with a discharge pipe 7 that penetrates the outer shell 2. A first valve 8 is installed on the discharge pipe 7. The top of the reaction vessel 3 is connected to and communicates with an exhaust pipe 15 that penetrates the outer shell 2. It also includes a flow meter 10, a second valve 11, a temperature detector 201, an electric heating module 12, a control panel 13, and a control knob 14. A flow meter 10 is installed at the lower end of the feed pipe 9, and a second valve 11 is installed at the upper end of the feed pipe 9. A temperature detector 201 for detecting the temperature of the reaction vessel 3 is installed on the outer shell 2. An electric heating module 12 is disposed between the outer shell 2 and the reaction vessel 3. A control panel 13 is installed on the rear side of the outer shell 2. A control knob 14 is installed on the control panel 13. The signal output terminal of the temperature detector 201 is electrically connected to the signal input terminal of the control panel 13. The signal input terminal of the electric heating module 12 is electrically connected to the signal output terminal of the control knob 14. The signal output terminal of the flow meter 10 is electrically connected to the signal input terminal of the control panel 13.
[0025] When preparing hexamethyldisiloxane, the left feeding pipe 9 is connected with the hexamethyldisilazane feeding pipe, the right feeding pipe 9 is connected with the deionized water feeding pipe, then the second valve 11 on the right feeding pipe 9 is opened, the deionized water is added into the reaction container 3, the flow meter 10 on the right feeding pipe 9 measures the dosage of the added deionized water, then the motor 4 is started, the motor 4 drives the rotating rod 5 to stir the deionized water in the reaction container 3, the electric heating module 12 is started, the heating power of the electric heating module 12 is adjusted through the control knob 14, so that the temperature of the reaction container 3 is adjusted, the temperature detector 201 detects the temperature of the reaction container 3, so that the temperature of the reaction container 3 is maintained at 40-60℃, then the second valve 11 on the left feeding pipe 9 is opened, and the feeding speed of the feeding pipe 9 is controlled, so that the hexamethyldisilazane slowly enters the reaction container 3, the flow meter 10 on the left feeding pipe 9 measures the dosage of the added hexamethyldisilazane, the flow meter 10 feeds back the dosages of the deionized water and the hexamethyldisilazane to the control panel 13 for display, so that the dosages and the speeds of the added deionized water and the hexamethyldisilazane are accurately controlled, so as to avoid that too much hexamethyldisilazane is added at one time, causing the reaction to be out of control, the rotating rod 5 stirs and mixes the deionized water and the hexamethyldisilazane in the reaction container 3, so that the deionized water and the hexamethyldisilazane are hydrolyzed, the generated nitrogen gas passes through the gas outlet pipe 15, and the generated hexamethyldisiloxane remains in the reaction container 3, after the hydrolysis reaction is completed, the first valve 8 is turned, so that the hexamethyldisiloxane and the remaining materials in the reaction container 3 are discharged through the discharge pipe 7.
[0026] Example 2: Based on example 1, refer to Figures 3-5 As shown in the figure, it also includes a first bevel gear 16, a support frame 1601, a rotating shaft 17, a second bevel gear 18, a third bevel gear 19, a connecting ring 20 and a stirring frame 21, the first bevel gear 16 is fixedly connected to the rotating rod 5 by key connection, the support frame 1601 is installed inside the shell 2, the connecting ring 20 is rotatably arranged on the support frame 1601, the third bevel gear 19 is fixedly connected to the top of the connecting ring 20 by welding, the stirring frame 21 is fixedly connected to the bottom of the connecting ring 20, the rotating rod 5 penetrates through the support frame 1601, the connecting ring 20 and the stirring frame 21, the rotating shaft 17 is rotatably arranged on both sides of the shell 2, the second bevel gear 18 is fixedly connected to one end of the rotating shaft 17 close to the rotating rod 5 by key connection, and the first bevel gear 16 and the third bevel gear 19 are meshed and driven by the two second bevel gears 18.
[0027] When the hexamethyldisilazane and deionized water in the reaction container 3 are stirred, the rotating rod 5 drives the stirring plate 6 and the first bevel gear 16 to rotate, the first bevel gear 16 drives the second bevel gear 18 to rotate, the second bevel gear 18 drives the third bevel gear 19 to rotate reversely, the third bevel gear 19 drives the stirring frame 21 to rotate reversely through the connecting ring 20, so that the hexamethyldisilazane and deionized water in the reaction container 3 are stirred from two different directions, the hexamethyldisilazane and deionized water are fully contacted and rapidly hydrolyzed.
[0028] Referring to Figs. 1-3, Figure 1 and Figure 6 The shell 2 is provided with a liquid storage tank 22, a liquid adding pipe 23, an air guide pipe 24 and a third valve 25. The liquid storage tank 22 is mounted on the left side of the shell 2 by means of bolts. The liquid adding pipe 23 is connected to the top of the liquid storage tank 22. The air guide pipe 24 is connected to the air outlet pipe 15 and penetrates the liquid storage tank 22. The third valve 25 is connected to the left side of the liquid storage tank 22. A sealing cover 28 is slidably arranged on the liquid adding pipe 23. The sealing cover 28 is used to seal the liquid storage tank 22 to prevent ammonia gas from overflowing through the liquid adding pipe 23 when absorbing ammonia gas.
[0029] Before preparing hexamethyldisiloxane, the sealing cover 28 is slid upward to open the liquid adding pipe 23, and then water is added into the liquid storage tank 22 through the liquid adding pipe 23. During the hydrolysis reaction, ammonia gas generated is introduced into the liquid storage tank 22 through the air outlet pipe 15 and the air guide pipe 24. The water in the liquid storage tank 22 absorbs the ammonia gas to generate ammonia water, thereby preventing the ammonia gas from diffusing into the air to cause air pollution. After the hydrolysis reaction is completed, the third valve 25 is rotated to discharge the ammonia water in the liquid storage tank 22 through the third valve 25, thereby facilitating the recycling of the ammonia water.
[0030] The above embodiments are provided for those skilled in the art to implement or use the present application, and those skilled in the art can make various modifications or changes to the above embodiments without departing from the inventive concept of the present application. Therefore, the protection scope of the present application should not be limited by the above embodiments, but should be the maximum scope of the innovative features mentioned in the claims.
Claims
1. A hexamethyldisiloxane preparation raw material hydrolysis reactor, comprising support seats (1), an outer shell (2), a reaction container (3), a motor (4), a rotating rod (5), a stirring plate (6), a feed pipe (9), a discharge pipe (7), a first valve (8) and an exhaust pipe (15), a plurality of support seats (1) are mounted on the lower part of the outer shell (2), the reaction container (3) is arranged in the inner part of the outer shell (2), the motor (4) is mounted on the top of the outer shell (2), a rotating rod (5) is connected to the output shaft of the motor (4) through a shaft coupling, the rotating rod (5) penetrates the outer shell (2) and the reaction container (3), the stirring plate (6) is mounted on the lower end of the rotating rod (5), two feed pipes (9) penetrating the outer shell (2) are connected and communicated with the top of the reaction container (3), the discharge pipe (7) penetrating the outer shell (2) is connected and communicated with the bottom of the reaction container (3), the first valve (8) is mounted on the discharge pipe (7), the exhaust pipe (15) penetrating the outer shell (2) is connected and communicated with the top of the reaction container (3), characterized in that: The utility model also includes a flowmeter (10), a second valve (11), a temperature detector (201), an electric heating module (12), a control panel (13) and a control knob (14), the flowmeter (10) is installed on the one end of the feed pipe (9) close to the shell (2), the second valve (11) is installed on the one end of the feed pipe (9) away from the shell (2), the temperature detector (201) for detecting the temperature of the reaction container (3) is installed on the shell (2), the electric heating module (12) is arranged between the gap between the shell (2) and the reaction container (3), the control panel (13) is installed on the one side of the shell (2), and the control knob (14) is installed on the control panel (13).
2. The raw material hydrolysis reactor for preparing hexamethyldisiloxane according to claim 1, characterized in that: The signal output end of the temperature detector (201) is electrically connected with the signal input end of the control panel (13), the signal input end of the electric heating module (12) is electrically connected with the signal output end of the control knob (14), and the signal output end of the flowmeter (10) is electrically connected with the signal input end of the control panel (13).
3. The hydrolysis reactor for raw material of hexamethyldisiloxane production according to claim 2, characterized in that: The utility model also includes a first bevel gear (16), a support frame (1601), a rotating shaft (17), a second bevel gear (18), a third bevel gear (19), a connecting ring (20) and a stirring frame (21), the first bevel gear (16) is fixedly connected on the rotating rod (5), the support frame (1601) is installed in the shell (2), the connecting ring (20) is rotatably arranged on the support frame (1601), the third bevel gear (19) is fixedly connected on the top of the connecting ring (20), the stirring frame (21) is fixedly connected on the bottom of the connecting ring (20), the rotating rod (5) penetrates through the support frame (1601), the connecting ring (20) and the stirring frame (21), the rotating shaft (17) is rotatably arranged on the both sides in the shell (2), the second bevel gear (18) is fixedly connected on the one end of the rotating shaft (17) close to the rotating rod (5), and the first bevel gear (16) and the third bevel gear (19) are meshed and driven through the two second bevel gears (18).
4. The hydrolysis reactor for raw material of hexamethyldisiloxane production according to claim 3, characterized in that: The utility model also includes a liquid storage tank (22), a liquid adding pipe (23), an air guide pipe (24) and a third valve (25), the liquid storage tank (22) is installed on the one side of the shell (2), the liquid adding pipe (23) is connected and communicated on the top of the liquid storage tank (22), the air guide pipe (24) is connected and communicated on the air outlet pipe (15), the air guide pipe (24) penetrates through the liquid storage tank (22), and the third valve (25) is connected and communicated on the one side of the liquid storage tank (22) away from the shell (2).
5. The hexamethyldisiloxane production raw material hydrolysis reactor of claim 4, wherein: the reactor is a continuous stirred tank reactor. The utility model also includes an observation glass (26), and the observation glass (26) is embeddedly installed on the shell (2) and the reaction container (3).
6. The hydrolysis reactor for raw material of hexamethyldisiloxane production according to claim 5, characterized in that: The utility model also includes a foot pad (27), and the foot pad (27) is installed on the one side of the support base (1) away from the shell (2).
7. The hydrolysis reactor for raw material of hexamethyldisiloxane production according to claim 6, characterized in that: The utility model also includes a sealing cover (28), and the sealing cover (28) is slidably arranged on the liquid adding pipe (23).
Citation Information
Patent Citations
Hydrolysis device for producing hexamethyldisiloxane
CN212017796U