A segmented alcoholysis separation apparatus for silicone azeotrope monomers
By designing a segmented alcoholysis separation device for organosilicon azeotropic monomers and utilizing cold water cooling and gas collection technologies, the safety and environmental protection issues in the separation of organosilicon monomer azeotropics were solved, achieving a highly efficient and safe separation process.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- RUNYU NEW MATERIAL TECH (HUBEI) CO LTD
- Filing Date
- 2026-05-09
- Publication Date
- 2026-06-05
AI Technical Summary
Existing technologies are difficult to efficiently separate organosilicon monomer azeotropes. Traditional methods involve large equipment investment, high energy consumption, high complexity, high environmental costs, and safety hazards, as well as the risk of extractant loss and product contamination.
Design a staged alcoholysis separation device for organosilicon azeotropic monomers, including an explosion-proof outer tank, a reaction tank, a water inlet connector, a feeding assembly, and a processing assembly. By injecting cold water and cooling the spiral assembly, combined with the gas collection of the gas outlet and the processing assembly, the device achieves safe control of the alcoholysis reaction and treatment of hydrogen chloride gas.
It effectively reduces the risk of boiling during alcoholysis, reduces raw material splashing, improves reaction safety, and enables efficient collection and treatment of hydrogen chloride gas, reducing energy consumption and environmental costs.
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Figure CN122141592A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of alcoholysis separation technology, specifically to a segmented alcoholysis separation device for organosilicon azeotropic monomers. Background Technology
[0002] In the synthesis and distillation of organosilicon monomers (such as methylchlorosilanes and phenylchlorosilanes), azeotropic mixtures that are difficult to separate using conventional physical methods (such as ordinary distillation) are often formed. A typical example is the azeotrope formed by methyltrichlorosilane (M1) and trimethylchlorosilane (M3), as well as complex azeotropic systems containing dimethyldichlorosilane (M2), high-boiling-point substances, etc. Traditional treatment methods, such as incineration or landfill, not only waste valuable silicon-containing raw materials but also generate pollutants such as hydrogen chloride and silica, which is inconsistent with the development concept of green chemistry. The accumulation of azeotropes occupies storage tank space, and their treatment requires additional energy consumption and environmental costs. To treat these azeotropes, the industry has explored a variety of methods, but all have obvious limitations. This method requires the introduction of a third component (extractant), which increases the complexity of the process flow, and the extractant needs to be separated from the product afterward, resulting in high energy consumption and the risk of extractant loss and product contamination. The solution is to break the azeotropic composition by changing the system pressure. However, this method requires large equipment investment and high operating energy consumption. Furthermore, for some azeotropic substances, the azeotropic composition is not sensitive to pressure changes, resulting in limited separation effects. It is still in the laboratory or pilot stage and has issues such as membrane material stability, flux, selectivity, and cost. It is still far from large-scale industrial application.
[0003] Alcohololysis is a strongly exothermic reaction. Feeding the materials all at once or simply mixing them can lead to an overly vigorous reaction, a rapid increase in temperature, and a risk of accidents such as boiling over or material overflow. Summary of the Invention
[0004] To solve the above technical problems, the present invention is achieved through the following technical solution: a staged alcoholysis separation device for organosilicon azeotropic monomers, comprising an explosion-proof outer tank, a reaction tank body fixedly connected to the bottom of the inner wall of the explosion-proof outer tank via a bracket, a water inlet connector fixedly connected to the top of the reaction tank body, a feeding assembly fixedly connected to the top of the reaction tank body on one side of the water inlet connector, a processing assembly fixedly connected to the center of the top of the reaction tank body, a pumping electric pump penetrating and fixedly connected to the top of the explosion-proof outer tank, a feeding connector penetrating and fixedly connected to the top of the explosion-proof outer tank body on one side of the pumping electric pump, the bottom of the processing assembly communicating with the top of the reaction tank body, the top of the reaction tank body communicating with the bottom of the feeding connector, and the top of the processing assembly communicating with the bottom of the pumping electric pump.
[0005] The reaction vessel includes a protective outer shell. A reaction tank is fixedly connected to the inner wall of the protective outer shell via a bracket. An air outlet is provided at the top of the protective outer shell. Anti-impact blades are fixedly connected to the top of the inner wall of the reaction tank. A heat dissipation assembly is fixedly connected to the inner wall of the reaction tank below the anti-impact blades. A spiral assembly is fixedly connected to the bottom of the inner wall of the reaction tank. The top of the spiral assembly is connected to the bottom of the heat dissipation assembly, and a feeding assembly is connected to inject raw materials. The raw materials are mixed and undergo alcoholysis reaction inside the reaction tank. Cold water is injected through a water inlet connector. At the same time as water is injected, the water flows along the heat dissipation assembly into the spiral assembly, thereby dissipating heat from the inside of the raw materials. This helps to reduce the boiling reaction during the raw material reaction. The cold water is guided by the reaction tank and the heat dissipation assembly to remove heat. At the same time, the air outlet reduces splashing during the raw material reaction. The gas enters the processing assembly for collection, thereby facilitating the collection of hydrogen chloride gas. The feeding connector is used to introduce raw materials, and the extraction pump is used to extract raw materials and stir them during extraction.
[0006] Preferably, the heat dissipation assembly includes a multi-pipe connector, the top of which is connected to a cooling pipe, and an anti-impact plate is fixedly connected to the side of the cooling pipe. The end of the anti-impact plate away from the multi-pipe connector is fixedly connected to the inner wall side of the reaction tank, and the bottom of the multi-pipe connector is connected to the top of the spiral assembly.
[0007] Preferably, the spiral assembly includes a fixed base plate, the top of which is connected to a conical tube. A spiral blade is fixedly connected to the inner wall of the conical tube. The bottom of the fixed base plate is fixedly connected to the bottom of the inner wall of the reaction tank. Water flows through the inlet connector into the area between the protective shell and the reaction tank, and then flows along the inner wall of the cooling pipe into the multi-pipe connector. The water, guided by the spiral blades, continuously cools the conical tube, thereby reducing the large amount of heat generated during the alcoholysis reaction. The anti-splatter plate also blocks the raw materials, suppressing splashing and reducing the probability of splashing.
[0008] Preferably, the feeding assembly includes an annular splitter pipe, the top of which is connected to a feeding connector, the bottom of which is connected to a guide pipe, and the end of the guide pipe away from the annular splitter pipe is connected to a spraying assembly. The feeding connector passes through the top of the protective shell and is fixedly connected to the protective shell. The guide pipe passes through the side of the reaction tank and is fixedly connected to the reaction tank. The spraying assembly is located on one side of the conical tube.
[0009] Preferably, the spraying assembly includes a connecting pipe, the top of which is connected to a conical nozzle. A guide vane is fixedly connected to the inner wall of the conical nozzle, and a discharge hole is provided on the side of the guide vane. The end of the connecting pipe away from the conical nozzle is connected to the bottom of the feed pipe and connected to the feed connector. The feed connector introduces the raw material, which flows along the feed pipe and is discharged along the connecting pipe. The raw material is sprayed out along the conical nozzle, and under pressure, it is spirally sprayed out along the guide vane and directly sprayed out under the action of the discharge hole. The direction of the conical nozzle is set along the tangential direction of the conical pipe, so that the raw material is self-mixed while being introduced, thereby accelerating the reaction rate.
[0010] Preferably, the processing component includes an air guide pipe, the top of which is connected to a cold water connector, the bottom of which is connected to a drain pipe, an air guide assembly fixedly connected to the inner side of the air guide pipe, the bottom of which is connected to the top of the protective shell, and the side of which is fixedly connected to the side of the mounting bracket.
[0011] Preferably, the gas guiding assembly includes a gas supply pipe, the side of which is connected to a curved ventilation pipe. The curved ventilation pipe has an outlet hole on its side. The side of the gas supply pipe is fixedly connected to the inner wall of the gas guiding pipe. Hydrogen chloride gas generated during the alcoholysis process is introduced along the bottom of the gas guiding pipe. A cold water connector is connected, allowing water to flow in. The hydrogen chloride gas enters the curved ventilation pipe along the gas supply pipe and is sprayed into the water along the tangential direction of the gas supply pipe, facilitating the mixing and dissolution of the hydrogen chloride gas with the water. This treats the hydrogen chloride gas, and the liquid hydrogen chloride is discharged through a drain pipe.
[0012] This invention provides a staged alcoholysis separation device for organosilicon azeotropic monomers. It has the following beneficial effects: 1. This staged alcoholysis separation device for organosilicon azeotropic monomers is equipped with a reaction tank connected to a feeding assembly for injecting raw materials. The raw materials are mixed and undergo alcoholysis reaction inside the reaction tank. Cold water is injected through a water inlet connector. Simultaneously, the water flows along the heat dissipation assembly into the spiral assembly, thereby dissipating heat from the inside of the raw materials. This helps to reduce the boiling reaction during the raw material reaction. The cold water is guided by the reaction tank and the heat dissipation assembly to remove heat. At the same time, the gas outlet is designed to reduce splashing during the raw material reaction. Meanwhile, the gas enters the processing assembly for collection, which facilitates the collection of hydrogen chloride gas. The feeding connector is used to introduce the raw materials, and the extraction pump is used to extract the raw materials, while stirring the raw materials during extraction.
[0013] 2. The staged alcoholysis separation equipment for organosilicon azeotropic monomers is equipped with a conical tube. Water flows through the inlet connector into the area between the protective shell and the reaction tank, and then flows along the inner wall of the cooling pipe into the interior of the multi-pipe connector. The water flow into the conical tube is continuously cooled by the guiding action of the spiral blades, thereby reducing the large amount of heat generated in the alcoholysis reaction. The anti-splatter plate blocks the raw material, thereby suppressing splashing and reducing the probability of raw material splashing.
[0014] 3. The staged alcoholysis separation equipment for organosilicon azeotropic monomers is equipped with a feed inlet. When the feed inlet is connected, the feed inlet introduces the raw material, which flows along the feed pipe and is discharged along the connecting pipe. The raw material is sprayed out along the conical nozzle, and under the action of pressure, it is spirally sprayed out along the guide vanes and directly sprayed out under the action of the discharge hole. The direction of the conical nozzle is set along the tangential direction of the conical pipe, so that the raw material is self-mixed while being introduced, thereby accelerating the reaction rate.
[0015] 4. The staged alcoholysis separation device for organosilicon azeotropic monomers is equipped with a gas guide pipe. During the alcoholysis process, the hydrogen chloride gas generated by the reaction is introduced along the bottom of the gas guide pipe. The cold water connector is connected to introduce water flow. The hydrogen chloride gas enters the interior of the curved ventilation pipe along the gas delivery pipe and is sprayed into the water along the tangential direction of the gas delivery pipe, thereby facilitating the mixing and dissolution of hydrogen chloride gas with water, thus treating the hydrogen chloride gas. The hydrogen chloride liquid is then discharged through the drain pipe. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the segmented alcoholysis separation device for organosilicon azeotropic monomers of the present invention; Figure 2 This is a schematic diagram of the internal structure of the staged alcoholysis separation device for organosilicon azeotropic monomers of the present invention. Figure 3 This is a schematic diagram of the reaction vessel structure of the present invention; Figure 4 This is a schematic diagram of the heat dissipation component structure of the present invention; Figure 5 This is a schematic diagram of the spiral component structure of the present invention; Figure 6 This is a schematic diagram of the feeding assembly structure of the present invention; Figure 7 This is a schematic diagram of the spray assembly structure of the present invention; Figure 8 This is a schematic diagram of the processing component structure of the present invention; Figure 9 This is a schematic diagram of the air guiding component structure of the present invention.
[0017] In the diagram: 1. Explosion-proof outer tank; 2. Reaction tank body; 3. Water inlet connector; 4. Feeding assembly; 6. Processing assembly; 7. Feeding interface; 8. Extraction pump; 201. Protective outer shell; 202. Reaction tank; 203. Gas outlet; 204. Anti-impact blades; 205. Heat dissipation assembly; 206. Spiral assembly; 2051. Multi-pipe connector; 2052. Cooling pipe; 2053. Anti-impact plate; 2061. Fixed base plate; 2062. Conical shape Pipe; 2063, Spiral blade; 401, Annular splitter pipe; 402, Feed connector; 403, Guide pipe; 404, Spray assembly; 4041, Connecting pipe; 4042, Conical nozzle; 4043, Guide vane; 4044, Discharge hole; 601, Air guide pipe; 602, Cold water connector; 603, Drain pipe; 604, Air guide assembly; 6041, Air supply pipe; 6042, Curved ventilation pipe; 6043, Air outlet. Detailed Implementation
[0018] 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.
[0019] For the first embodiment, please refer to... Figures 1-3 This invention provides a technical solution: a segmented alcoholysis separation device for organosilicon azeotropic monomers, comprising an explosion-proof outer tank 1, a reaction tank 2 fixedly connected to the bottom of the inner wall of the explosion-proof outer tank 1 via a bracket, a water inlet connector 3 fixedly connected to the top of the reaction tank 2, a feeding assembly 4 fixedly connected to the top of the reaction tank 2 on one side of the water inlet connector 3, a processing assembly 6 fixedly connected to the center of the top of the reaction tank 2, a pump 8 penetrating and fixedly connected to the top of the explosion-proof outer tank 1, a feeding interface 7 penetrating and fixedly connected to the top of the explosion-proof outer tank 1 on one side of the pump 8, the bottom of the processing assembly 6 communicating with the top of the reaction tank 2, the top of the reaction tank 2 communicating with the bottom of the feeding interface 7, and the top of the processing assembly 6 communicating with the bottom of the pump 8.
[0020] The reaction vessel 2 includes a protective shell 201. A reaction tank 202 is fixedly connected to the inner wall side of the protective shell 201 via a bracket. An air outlet 203 is provided on the top of the protective shell 201. An anti-impact blade 204 is fixedly connected to the top of the inner wall of the reaction tank 202. A heat dissipation assembly 205 is fixedly connected to the inner wall side of the reaction tank 202 below the anti-impact blade 204. A spiral assembly 206 is fixedly connected to the bottom of the inner wall of the reaction tank 202. The top of the spiral assembly 206 communicates with the bottom of the heat dissipation assembly 205.
[0021] The feed assembly 4 is connected to inject raw materials, which are mixed and undergo alcoholysis reaction inside the reaction tank 202. Cold water is injected through the water inlet 3. At the same time, the water flows along the heat dissipation assembly 205 into the spiral assembly 206 to dissipate heat from inside the raw materials, thereby reducing the boiling reaction during the reaction. The cold water is guided by the reaction tank 202 and the heat dissipation assembly 205 to remove heat. At the same time, the gas outlet 203 reduces splashing during the reaction. The gas enters the processing assembly 6 for collection, which facilitates the collection of hydrogen chloride gas. The feed inlet 7 is used to introduce raw materials, and the extraction pump 8 is used to extract raw materials and stir them at the same time.
[0022] Second embodiment, please refer to Figures 1-5 Based on the first embodiment, the present invention provides a technical solution: the heat dissipation component 205 includes a multi-pipe connector 2051, the top of the multi-pipe connector 2051 is connected to a cooling pipe 2052, the side of the cooling pipe 2052 is fixedly connected to an anti-impact plate 2053, the end of the anti-impact plate 2053 away from the multi-pipe connector 2051 is fixedly connected to the inner wall side of the reaction tank 202, and the bottom of the multi-pipe connector 2051 is connected to the top of the spiral component 206.
[0023] The spiral assembly 206 includes a fixed base plate 2061, the top of which is connected to a tapered tube 2062, the inner wall of which is fixedly connected to a spiral blade 2063, and the bottom of the fixed base plate 2061 is fixedly connected to the bottom of the inner wall of the reaction tank 202.
[0024] Water flows through the inlet connector 3 into the space between the protective shell 201 and the reaction tank 202, and flows along the inner wall of the cooling pipe 2052 into the multi-pipe connector 2051. The water then enters the conical pipe 2062 and is continuously cooled by the spiral blades 2063, thereby reducing the heat generated in the alcoholysis reaction. The anti-splatter plate 2053 blocks the raw materials, thereby suppressing splashing and reducing the probability of raw material splashing.
[0025] Third embodiment, please refer to Figures 1-7Based on the second embodiment, the present invention provides a technical solution: the feeding assembly 4 includes an annular diverter pipe 401, the top of the annular diverter pipe 401 is connected to a feeding connector 402, the bottom of the annular diverter pipe 401 is connected to a guide pipe 403, the end of the guide pipe 403 away from the annular diverter pipe 401 is connected to a spraying assembly 404, the feeding connector 402 penetrates the top of the protective shell 201 and is fixedly connected to the protective shell 201, the guide pipe 403 penetrates the side of the reaction tank 202 and is fixedly connected to the reaction tank 202, and the spraying assembly 404 is located on one side of the conical tube 2062.
[0026] The spraying assembly 404 includes a connecting pipe 4041, the top of which is connected to a conical nozzle 4042. A guide vane 4043 is fixedly connected to the inner wall of the conical nozzle 4042. A discharge hole 4044 is provided on the side of the guide vane 4043. The end of the connecting pipe 4041 away from the conical nozzle 4042 is connected to the bottom of the guide pipe 403.
[0027] When the feed connector 402 is connected, the feed connector 402 introduces the raw material, which flows along the guide pipe 403 and is discharged along the connecting pipe 4041. The raw material is sprayed out along the conical nozzle 4042, and under the action of pressure, it is spirally sprayed out along the guide vane 4043 and directly sprayed out under the action of the discharge hole 4044. The conical nozzle 4042 is set in the tangential direction of the conical pipe 2062, so that the raw material is self-mixed while being introduced, thereby accelerating the reaction rate.
[0028] For the fourth embodiment, please refer to [link / reference]. Figures 1-9 Based on the third embodiment, the present invention provides a technical solution: the processing component 6 includes a vent pipe 601, the top of the vent pipe 601 is connected to a cold water connector 602, the bottom of the vent pipe 601 is connected to a drain pipe 603, the inner wall side of the vent pipe 601 is fixedly connected to a vent assembly 604, the bottom of the vent pipe 601 is connected to the top of the protective shell 201, and the side of the vent pipe 601 is fixedly connected to the inner wall side of the explosion-proof outer tank 1 through a bracket.
[0029] The air guiding assembly 604 includes an air supply pipe 6041, a curved ventilation pipe 6042 connected to the side of the air supply pipe 6041, an air outlet 6043 opened on the side of the curved ventilation pipe 6042, and the side of the air supply pipe 6041 is fixedly connected to the inner wall side of the air guiding pipe 601.
[0030] During the alcoholysis process, the hydrogen chloride gas produced by the reaction is introduced along the bottom of the gas inlet pipe 601. The cold water connector 602 is then connected, allowing water to flow in. The hydrogen chloride gas enters the interior of the curved ventilation pipe 6042 along the gas inlet pipe 6041 and is sprayed into the water along the tangential direction of the gas inlet pipe 6041. This facilitates the mixing and dissolution of the hydrogen chloride gas with the water, thereby treating the hydrogen chloride gas. The hydrogen chloride liquid is then discharged through the drain pipe 603.
[0031] Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. All other embodiments obtained by those skilled in the art and related fields based on the embodiments of the present invention without inventive effort should fall within the scope of protection of the present invention. Structures, devices, and operating methods not specifically described and explained in the present invention, unless otherwise specified or limited, shall be implemented according to conventional means in the art.
Claims
1. A staged alcoholysis separation device for organosilicon azeotropic monomers, characterized in that: The device includes an explosion-proof outer tank (1), a reaction tank (2) is fixedly connected to the bottom of the inner wall of the explosion-proof outer tank (1) by a bracket, a water inlet connector (3) is fixedly connected to the top of the reaction tank (2), a feeding assembly (4) is fixedly connected to the top of the reaction tank (2) on the side of the water inlet connector (3), a processing assembly (6) is fixedly connected to the center of the top of the reaction tank (2), a pumping electric pump (8) is fixedly connected through the top of the explosion-proof outer tank (1), a feeding interface (7) is fixedly connected through the top of the explosion-proof outer tank (1) on the side of the pumping electric pump (8), the bottom of the processing assembly (6) is connected to the top of the reaction tank (2), the top of the reaction tank (2) is connected to the bottom of the feeding interface (7), and the top of the processing assembly (6) is connected to the bottom of the pumping electric pump (8). The reaction vessel (2) includes a protective shell (201). A reaction tank (202) is fixedly connected to the inner wall side of the protective shell (201) via a bracket. An air outlet (203) is provided at the top of the protective shell (201). An anti-impact blade (204) is fixedly connected to the top of the inner wall of the reaction tank (202). A heat dissipation assembly (205) is fixedly connected to the inner wall side of the reaction tank (202) below the anti-impact blade (204). A spiral assembly (206) is fixedly connected to the bottom of the inner wall of the reaction tank (202). The top of the spiral assembly (206) is connected to the bottom of the heat dissipation assembly (205). The feeding assembly (4) includes an annular splitter pipe (401), the top of which is connected to a feed connector (402), the bottom of which is connected to a guide pipe (403), and the end of the guide pipe (403) away from the annular splitter pipe (401) is connected to a spray assembly (404). The spraying assembly (404) includes a connecting pipe (4041), the top of which is connected to a conical nozzle (4042), and a guide vane (4043) is fixedly connected to the inner wall of the conical nozzle (4042). A discharge hole (4044) is provided on the side of the guide vane (4043), and the end of the connecting pipe (4041) away from the conical nozzle (4042) is connected to the bottom of the guide pipe (403).
2. The staged alcoholysis separation device for organosilicon azeotropic monomers according to claim 1, characterized in that: The heat dissipation assembly (205) includes a multi-pipe connector (2051), the top of which is connected to a cooling pipe (2052), and the side of the cooling pipe (2052) is fixedly connected to an anti-impact plate (2053). The end of the anti-impact plate (2053) away from the multi-pipe connector (2051) is fixedly connected to the inner wall side of the reaction tank (202). The bottom of the multi-pipe connector (2051) is connected to the top of the spiral assembly (206).
3. The staged alcoholysis separation device for organosilicon azeotropic monomers according to claim 1, characterized in that: The spiral assembly (206) includes a fixed base plate (2061), the top of which is connected to a conical tube (2062), the inner wall of which is fixedly connected to a spiral blade (2063), and the bottom of which is fixedly connected to the bottom of the inner wall of the reaction tank (202).
4. The staged alcoholysis separation device for organosilicon azeotropic monomers according to claim 1, characterized in that: The feed connector (402) passes through the top of the protective shell (201) and is fixedly connected to the protective shell (201). The guide pipe (403) passes through the side of the reaction tank (202) and is fixedly connected to the reaction tank (202). The spraying assembly (404) is located on one side of the conical tube (2062).
5. The staged alcoholysis separation device for organosilicon azeotropic monomers according to claim 1, characterized in that: The processing component (6) includes an air guide pipe (601), the top of which is connected to a cold water connector (602), the bottom of which is connected to a drain pipe (603), and an air guide assembly (604) is fixedly connected to the inner wall side of the air guide pipe (601).
6. The staged alcoholysis separation device for organosilicon azeotropic monomers according to claim 5, characterized in that: The bottom of the air guide pipe (601) is connected to the top of the protective shell (201), and the side of the air guide pipe (601) is fixedly connected to the inner wall side of the explosion-proof outer tank (1) through a bracket.
7. The staged alcoholysis separation device for organosilicon azeotropic monomers according to claim 5, characterized in that: The air guiding assembly (604) includes an air supply pipe (6041), the side of which is connected to a curved ventilation pipe (6042), and the side of the curved ventilation pipe (6042) is provided with an air outlet (6043). The side of the air supply pipe (6041) is fixedly connected to the inner wall side of the air guiding pipe (601).