Efficient reaction device based on raw material dropwise adding device
By using raw material droppers and protective gas input devices in a closed reactor to control the reaction temperature and atmosphere, the problems of low yield and safety hazards in the preparation of di(diethylamino)silane are solved, and an efficient and safe chemical reaction process is achieved.
Patent Information
- Application Number
- CN202422334788.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-25
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2034-09-25
AI Technical Summary
In the prior art, the preparation yield of di(diethylamino)silane is low and the volatile raw materials have safety hazards in an open environment, making it easy to form explosive mixtures.
A closed reactor is used to combine a raw material dropper and a protective gas input device to control the reaction temperature through a constant temperature water bath. The raw material dropper is used to add the same temperature raw material to the protection gas input device to input the same temperature protection gas to ensure that the reaction is carried out in a closed environment.
The reaction efficiency and product yield of di(diethylamino)silane are improved, the escape of volatile chemicals is avoided, and the safety and stability of the reaction are ensured.
Smart Images
Figure CN223082784U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of reactors, in particular to a reactor for efficiently preparing bis(diethylamino)silane based on a raw material dropper. Background Art
[0002] Bis(diethylamino)silane (BDEAS) is one of the popular organic amino-silane precursors used in various deposition processes in the semiconductor field to manufacture silicon-containing thin films. The preparation of bis(diethylamino)silane has also become the focus of research by technicians. Currently, bis(diethylamino)silane is usually prepared by reacting chlorosilane with alkylamine, but the reaction yield is relatively low in actual industrial production. Moreover, diethylamine, one of the raw materials used to prepare alkylamine, is an organic compound that is extremely volatile, with strong irritation and corrosiveness.
[0003] In an open environment, diethylamine will quickly volatilize into the air, which will not only cause loss of reactants, but may also pose hazards to the environment and operators. And hexane is also an easily volatile organic solvent, whose volatility may be slightly lower than that of diethylamine, but it will still quickly diffuse in an open environment. The vapors of diethylamine and hexane dispersed in the air can both form explosive mixtures with oxygen in the air, posing an explosion risk.
[0004] Therefore, in order to ensure the safety of the reaction and better control the reaction conditions, diethylamine and hexane need to be placed in a closed container during the reaction process. At the same time, a raw material dropping device and a device for replacing the gas in the closed container are provided on the closed container. This will be more conducive to improving the preparation efficiency of bis(diethylamino)silane, thereby obtaining a higher yield. Summary of the Invention
[0005] In order to solve the above problems, the utility model proposes an efficient reaction device, adopting the following technical solutions.
[0006] An efficient reaction device based on a raw material dropper, comprising a closed reactor arranged in a constant temperature water bath. The closed reactor is configured with a stirring device and a plurality of interfaces.
[0007] The closed reactor is equipped with a raw material dropper and a protective gas input device. The raw material dropper includes a tube layer and a shell layer sleeved on the outer wall of the tube layer. A cavity filled with flowing cooling medium is formed between the tube layer and the shell layer. The protective gas input device includes an inner tube and an outer tube sleeved on the outer wall of the inner tube. A cavity filled with flowing cooling medium is formed between the inner tube and the outer tube. The upper end of the tube layer is configured as a feed hopper with a stopcock. A stopcock valve is arranged in the middle at the lower end of the tube layer. The joint of the tube layer below the stopcock valve is hermetically connected to the interface of the closed reactor.
[0008] A constant pressure pipe is provided on the side wall of the pipe layer. Both ends of the constant pressure pipe are communicated with the side wall of the pipe layer, and the stopcock valve is located on the pipe layer between the constant pressure pipes;
[0009] The upper port of the inner pipe is communicated with the gas generating device, and the lower end of the inner pipe is hermetically connected to the interface of the closed reactor; water inlets and outlets are provided at both ends of the shell layer and both ends of the outer pipe. The water inlets are connected to the constant temperature water bath through a pump body, and the outlets are connected to the constant temperature water bath through a pipeline; the stirring paddle of the stirring device is located inside the closed reactor.
[0010] Further, the closed reactor is in the shape of a square box. The interfaces communicated with the raw material dropping device and the protective gas input device are both opened on the upper end surface of the closed reactor. Third interfaces are opened on the upper end surface and the side wall of the closed reactor for preloading the initial reaction raw materials.
[0011] Further, the constant temperature water bath is in the shape of a semi-open box. The closed reactor can be placed inside the constant temperature water bath, and there is a space reserved between the closed reactor and the side wall of the constant temperature water bath. A stopcock valve is installed at the interface of the closed reactor.
[0012] Further, when only one stopcock valve is provided at the joint at the lower end of the pipe layer, one end of the constant pressure pipe is connected to the pipe wall of the pipe layer below the feed hopper, and the other end is connected to the pipe wall of the joint below the stopcock valve. When two stopcock valves are provided on the joint at the lower end of the pipe layer in sequence from top to bottom, one end of the constant pressure pipe is connected to the pipe wall of the pipe layer below the feed hopper, and the other end is connected to the pipe wall between the two stopcock valves of the joint.
[0013] Further, the gas generating device includes a gas storage cylinder, a first gas distribution pipe, a second gas distribution pipe, a first valve, a dryer, which are sequentially communicated with the outlet of the gas storage cylinder through a pipeline. The outlet end of the dryer is communicated with the first gas distribution pipe through a gas transmission pipe. The first gas distribution pipe and the second gas distribution pipe are both equidistantly arranged with an equal number of corresponding branch pipes along the length direction. A pair of branch pipes of the first gas distribution pipe and the second gas distribution pipe form a group and are respectively communicated with two interfaces of a three-way valve. The other interface of the three-way valve is communicated with the upper end of the inner pipe of the protective gas input device. The second gas distribution pipe is also communicated with an air pump, and the first gas distribution pipe is also communicated with a bubbling device.
[0014] Further, a thermometer and a pressure gauge are installed inside the closed reactor.
[0015] Further, the outer wall surface of the constant temperature water bath is wrapped with heat insulating material.
[0016] Compared with the prior art, the beneficial effects of the present utility model are as follows: Through the comprehensive reaction device of the present utility model, a balanced and efficient chemical reaction process can be achieved. On the one hand, a low-temperature raw material at the same temperature is dropped into the reaction material through the raw material dropper, and on the other hand, a low-temperature protective gas at the same temperature is input into the reaction vessel through the protective gas input device. This can avoid the escape of volatile chemical substances, evenly drop the reaction raw materials, and at the same time enable the chemical reaction to proceed continuously in an environment filled with the protective gas, improving the reaction efficiency and product yield. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 is a schematic diagram of the overall reaction device;
[0018] Figure 2 is a schematic diagram of the structure of the raw material dropper;
[0019] Figure 3 is a schematic diagram of the structure of the raw material dropper;
[0020] Figure 4 is a schematic diagram of the structure of the protective gas input device;
[0021] Figure 5 is a schematic diagram of the gas generation device. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0022] The drawings are only for illustrative purposes and should not be construed as limiting the present invention; For a better illustration of this embodiment, some components in the drawings will be omitted, enlarged or reduced, which do not represent the dimensions of the actual product; For those skilled in the art, it is understandable that some well-known structures and their descriptions in the drawings may be omitted; The positional relationships described in the drawings are only for illustrative purposes and should not be construed as limiting the present invention. The following further describes the present invention in detail with specific embodiments.
[0023] As Figure 1 shown, it is a schematic diagram of a comprehensive reaction device for efficiently preparing bis(diethylamino)silane proposed by the present utility model, including a constant temperature water bath 1 and a closed reactor 2 located in the constant temperature water bath 1. A raw material feeding port, two raw material droppers 4, a protective gas input device 5 and a stirring device 3 are provided on the closed reactor 2. The raw material feeding port is used to add the initial reaction raw materials to the closed reactor 2. The raw material dropper 4 is used to drop the reaction raw materials into the closed reactor 2 drop by drop. The protective gas input device 5 is connected to the gas generation device 6. Bis(diethylamino)silane is prepared in the closed reactor 2.
[0024] As Figure 1As shown in the figure, the closed reactor 2 is box-shaped, and there are multiple interfaces at its upper end, including two first interfaces connected to two raw material droppers 4, a second interface connected to a protective gas input device 5, and a third interface for inserting a thermometer 7. Among them, the first interface, the second interface, and the third interface are all opened on the upper end surface of the closed reactor 2, so that the raw material droppers 4 and the protective gas input device 5 can be vertically installed on the closed reactor 2. A stirring device 3 is also centrally arranged on the upper end surface of the closed reactor 2. The stirring rod of the stirring device 3 passes through the opening on the upper end surface of the closed reactor 2, and a stirring paddle is arranged at its lower end, and its upper end is coaxially connected to the output shaft of the stirring motor. Starting the stirring motor can drive the stirring paddle located inside the closed reactor 2 to rotate, so that the liquid materials inside the closed reactor 2 are evenly mixed.
[0025] The constant temperature water bath 1 is in the shape of a semi-open box. The closed reactor 2 can be placed inside the constant temperature water bath 1, and there is a space reserved between it and the side wall of the constant temperature water bath 1. Ice-water mixture is pre-stored in the constant temperature water bath 1 as the medium for the water bath. Mixing an appropriate amount of ice cubes and cold water in the constant temperature water bath 1 can provide a stable environment of 0 °C. As the reaction progresses, the ice cubes may melt, and ice cubes need to be added regularly to keep the reaction temperature of the closed reactor 2 stable. Outside the constant temperature water bath 1, the outer wall surface of the constant temperature water bath 1 is wrapped with heat-insulating materials (such as foam, insulating cotton, etc.) to reduce heat dissipation or absorption. A thermometer is set in the constant temperature water bath 1 to monitor the temperature of the water bath. If the water bath temperature deviates from 0 °C, the temperature can be restored by adding ice cubes.
[0026] As Figure 2As shown in the figure, it is a schematic structural diagram of the raw material dropper 4, including a tube layer 41 and a shell layer 42. The tube layer 41 is used to hold the raw materials for the reaction, and a cooling medium flows in the shell layer 42, so that the dropped reaction raw materials are maintained at a constant temperature. The tube layer 41 is in the shape of a slender tube. Its upper end is provided with a feed hopper 47 and is equipped with a cock. The lower end is provided with a stop valve 46. Below the stop valve 46 is the discharge port. The discharge port of the tube layer 41 can be connected and matched with the first interface of the closed reactor 2. By controlling the rotation angle of the stop valve 46, the dropping speed of the raw materials in the tube layer 41 can be controlled. A constant pressure tube 45 is provided on the side wall of the tube layer 41. One end of the constant pressure tube 45 is connected to the tube layer 41 below the feed hopper 47, and the other end passes through the shell layer 42 and is connected to the tube layer 41 below the stop valve 46. When the reaction raw materials are filled in the tube layer 41 and the feed hopper 47 is blocked by the cock, in order to facilitate the smooth dropping of the raw materials, the constant pressure tube 45 is provided, so that the air pressure balance in the tube layer 41 is maintained, which is conducive to the smooth dropping of the raw materials. The shell layer 42 is also in the shape of a slender tube. The shell layer 42 is sleeved on the outer periphery of the tube layer 41. The length of the shell layer 42 is less than that of the tube layer 41. The upper edge of the shell layer 42 is closed and connected to the tube wall of the tube layer 41 below the feed hopper 47, and the lower edge of the shell layer 42 is closed and connected to the tube wall of the tube layer 41 above the stop valve 46, so that a closed cavity is formed between the shell layer 42 and the tube layer 41; water inlet 1 43 and water outlet 1 44 are respectively opened on the side walls at both ends of the shell layer 42. The water inlet 1 43 is located below the water outlet 1 44. The water inlet 1 43 is connected to the constant temperature water bath 1 through a water pump, and the water outlet 1 43 transports the cooling water back to the constant temperature water bath 1 through a pipeline. In this way, it can be ensured that the dropped reaction raw materials and the reactants in the closed reactor 2 are at the same temperature, which can promote the reaction process and improve the reaction efficiency.
[0027] As Figure 4 shown in the figure, it is a schematic structural diagram of the protective gas input device 5, including an inner tube 51 and an outer tube 52. The upper port of the inner tube 51 is connected to the gas generating device 6, and the lower port of the inner tube 51 can be connected and matched with the second interface of the closed reactor 2; an outer tube 52 is sleeved on the outer wall of the inner tube 52. The length of the outer tube 52 is less than that of the inner tube 51, and the upper edge and the lower edge of the outer tube 52 are respectively closed and connected to the tube wall of the inner tube 51, so that a closed cavity is formed between the outer tube 52 and the inner tube 51; water inlet 2 53 and water outlet 2 54 are opened on the side walls at both ends of the outer tube 52. The water inlet 2 53 is located below the water outlet 2 54. The water inlet 2 53 is connected to the constant temperature water bath 1 through a water pump, and the water outlet 2 54 transports the cooling water back to the constant temperature water bath 1 through a pipeline. In this way, it can be ensured that when the protective gas is input into the closed reactor 2, the volatile organic substances in the closed reactor 2 are condensed and refluxed.
[0028] Optionally, both the raw material dropper 4 and the protective gas input device 5 are made of transparent materials, and a scale is provided on the side wall of the raw material dropper 4 to monitor the dosage of the reaction raw materials in real time.
[0029] As Figure 5 shown, it is a schematic diagram of the gas generation device 6, including a gas storage cylinder 61, a dryer 64, a three-way valve 69, two gas distribution pipes, a gas pump 67 and a bubbling device 68. The first gas distribution pipe 70 and the second gas distribution pipe 71 are both equidistantly arranged with an equal number of corresponding branch pipes along the length direction. A pair of branch pipes of the first gas distribution pipe 70 and the second gas distribution pipe 71 form a group, and each group of branch pipes communicates with two interfaces of the three-way valve 69. Among them, the third interface of the three-way valve 69 communicates with the upper end of the inner pipe 51 of the protective gas input device 5. Specifically, the gas storage cylinder 61 stores an inert gas such as nitrogen or argon. The gas storage cylinder 61 is connected to the dryer 64 through a valve 62. A flow meter 63 is arranged between the valve 62 and the dryer 64 to monitor the gas flow rate and timely adjust the opening of the valve 62 to adjust the gas delivery volume. The outlet end of the dryer 64 is connected to the first gas distribution pipe 70 through a gas delivery pipe 66. The second gas distribution pipe 71 is also connected to the gas pump 67, and the first gas distribution pipe 70 is also connected to the bubbling device 68.
[0030] According to the reaction requirements, multiple gas storage cylinders can be set to communicate with the first gas distribution pipe 70, so as to input different types of gases into the closed reactor. By adjusting the valve 62 of each gas storage cylinder 61 of the gas, the gas flow rate delivered to the protective gas input device 5 and the closed reactor 2 can be adjusted, thereby adjusting the gas composition ratio.
[0031] The usage process of this device is as follows. Before the reaction starts, the constant temperature water bath 1 is not in use. The solvent is loaded into the sealed reactor 2. The protective gas inlet 5 is installed at the second interface of the sealed reactor 2. The first interface of the sealed reactor 2 is sealed with a film. The protective gas inlet 5 is connected to the gas generating device. First step, evacuate the gas in the reaction device. Close the rotary three-way valve 69, so that the sealed reactor 2 is connected to the air pump 67 through the second gas pipe 71, and at the same time, the sealed reactor 2 is disconnected from the first gas pipe 70. Start the air pump 67 and use the air pump 67 to evacuate the gas in the sealed reactor 2. Second step, fill the reaction device with gas. Rotate the rotary three-way valve 69 so that the sealed reactor 2 is disconnected from the second gas pipe 71, and at the same time, the sealed reactor 2 is connected to the gas storage bottle 61 and the bubbling device 68 through the first gas pipe 70, and fill the sealed reactor 2 with gas until the bubbling device 68 starts to bubble. Repeat the steps of the first step and the second step, and repeat the gas displacement operation until the gas in the sealed reactor 2 and the connecting pipes is replaced. Third step, keep the gas storage bottle 61 inputting the protective gas into the sealed reactor 2, and observe the bubbles emerging from the bubbling device 68. Start the constant temperature water bath body and keep the temperature at 0 degrees Celsius. At the same time, insert the interface of the raw material dropper 4 filled with the reaction raw materials into the first interface of the sealed reactor 2, open the plug of the feed hopper of the raw material dropper 4, and connect the feed hopper of the raw material dropper 4 to the bubbling device 68 through a hose. Continue to input the protective gas to displace the gas in the raw material dropper 4. Finally, clamp the hose with a clip, and then open the stopcock valve 46 of the raw material dropper 4 and drip the reaction raw materials into the pipe layer 41 of the raw material dropper 4 to carry out the reaction.
[0032] Further, as Figure 3 shown is an improved raw material dropper 4. The part of the pipe layer 41 below the lower end of the shell layer 42 is successively provided with two stopcock valves 46 from top to bottom. One end of the constant pressure pipe 45 is connected to the pipe layer 41 below the feed hopper 47, and the other end passes through the shell layer 42 and is connected to the pipe layer 41 between the two stopcock valves 46. The other structures of the raw material dropper 4 are the same as Figure 2 . When using the raw material dropper 4 Figure 3 , directly insert the lower end of the raw material dropper 4 filled with the reaction raw materials and with the upper end of the feed hopper sealed into the first interface of the sealed reactor 2, and then open the two stopcock valves 46 in sequence to drip the reaction raw materials, saving the step of displacing the gas.
[0033] Figure 3 and Figure 2 both set a stopcock valve 46 above the connection part of the constant pressure pipe 45 and the pipe layer 41 in the raw material dropper 4, avoiding the problem that after the reaction raw materials are injected into the raw material dropper 4, a U-shaped connection is formed in the pipe layer 41 and the constant pressure pipe 45, resulting in the liquid reaction raw materials being unable to drip into the sealed reactor due to the influence of pressure.
[0034] In this embodiment, the raw material dropper 4 injects raw materials inside an operating box with air isolation, and the raw material dropper 4 does not introduce air and water.
[0035] In this embodiment of Figure 5 the first gas distribution pipe 70 and the second gas distribution pipe 71 are provided with multiple pairs of branch pipes for facilitating the connection of multiple sealed reactors 2 through three-way valves and intermittent operation at the same time to increase the output.
[0036] In this embodiment, two raw material droppers 4 are respectively used to drip SiH2Cl2 and (C2H5)2NH into the sealed reactor 2, and Si[(C2H5)2N]2H2 is generated by reaction in the sealed reactor 2. Air and water are not introduced during the whole reaction process.
[0037] Through the comprehensive reaction device of the present utility model, a balanced and efficient chemical reaction process can be realized. On the one hand, low-temperature raw materials at the same temperature are dripped into the reaction materials through the raw material dropper, and on the other hand, low-temperature protective gas at the same temperature is input into the reaction vessel through the protective gas input device. This can avoid the escape of volatile chemical substances, balance the dripping of reaction raw materials, and at the same time enable the chemical reaction to proceed continuously in an environment filled with protective gas, improving the reaction efficiency and product yield.
Claims
1. An efficient reaction device based on a raw material dropping device, comprising a closed reactor (2) arranged in a constant temperature water bath tank (1), wherein the closed reactor (2) is configured with a stirring device (7) and a plurality of interfaces, and is characterized in that, The closed reactor (2) is equipped with at least one: a raw material dropping device (4) and a protective gas inlet device (5). The raw material dropping device (4) includes a tube layer (41) and a shell layer (42) sleeved on the outer wall of the tube layer (41). A cavity filled with flowing cooling medium is formed between the tube layer (41) and the shell layer (42). The upper end of the tube layer (41) extending out of the shell layer (42) is configured as a feed hopper (47) with a stopcock. A stopcock valve (46) is arranged in the middle of the lower end of the tube layer (41) extending out of the shell layer (42). The joint of the tube layer (41) below the stopcock valve (46) is used for sealing connection with the interface of the closed reactor (2). One end of a constant pressure tube (45) passes through the shell layer (42) and communicates with the side wall of the tube layer (41). The other end of the constant pressure tube (45) communicates with the side wall of the joint of the tube layer (41) below the stopcock valve (46). The protective gas inlet device (5) includes an inner tube (51) and an outer tube (52) sleeved on the outer wall of the inner tube (51). A cavity filled with flowing cooling medium is formed between the inner tube (51) and the outer tube (52). The upper port of the inner tube (51) communicates with a gas generating device (6). The lower end of the inner tube (51) is hermetically connected to the interface of the closed reactor (2). Both ends of the shell layer (42) and both ends of the outer tube (52) are provided with water inlets and water outlets. The water inlets are connected to a constant temperature water bath (1) through a pump body, and the water outlets are connected to the constant temperature water bath (1) through a pipeline. The stirring paddle of the stirring device (7) is located inside the closed reactor (2).
2. The high-efficiency reaction device based on a raw material dropper according to claim 1, wherein The interfaces communicating with the raw material dropping device (4) and the interfaces communicating with the protective gas inlet device (5) are all opened on the upper end face of the closed reactor (2).
3. The high-efficiency reaction device based on a raw material dropper according to claim 1, characterized in that, A stopcock valve is installed at the interface of the closed reactor (2).
4. The high-efficiency reaction device based on a raw material dropper according to claim 1, characterized in that, Two stopcock valves (46) are successively arranged on the joint from top to bottom.
5. The high-efficiency reaction device based on a raw material dropper according to claim 1, wherein One end of the constant pressure tube (45) passes through the shell layer (42) and is connected to the tube wall of the tube layer (41) below the feed hopper (47), and the other end is connected to the tube wall of the joint below the stopcock valve (46).
6. The high-efficiency reaction device based on a raw material dropper according to claim 4, characterized in that, One end of the constant pressure tube (45) is connected to the tube wall of the tube layer (41) below the feed hopper (47), and the other end is connected to the tube wall between the two stopcock valves (46) of the joint.
7. The high-efficiency reaction device based on a raw material dropper according to claim 1, characterized in that, The gas generating device (6) includes a gas storage cylinder (61), a first gas distribution pipe (70), a second gas distribution pipe (71), and a first valve (62), a dryer (64) that are successively connected through pipelines to the outlet of the gas storage cylinder (61). The outlet end of the dryer (64) is communicated with the first gas distribution pipe (70) through a gas transmission pipe (66). The first gas distribution pipe (70) and the second gas distribution pipe (71) are both equidistantly arranged with an equal number of corresponding branch pipes along the length direction. A pair of branch pipes of the first gas distribution pipe (70) and the second gas distribution pipe (71) form a group and are respectively communicated with two interfaces of a three-way valve (69). The other interface of the three-way valve (69) is communicated with the upper end of the inner tube (51) of the protective gas inlet device (5). The second gas distribution pipe (71) is also communicated with an air pump (67). The first gas distribution pipe (70) is also communicated with a bubbling device (68).
8. The high-efficiency reaction device based on a raw material dropper according to claim 1, characterized in that, A thermometer and a pressure gauge are installed inside the closed reactor (2).
9. The high-efficiency reaction device based on a raw material dropper according to claim 1, characterized in that, The outer wall surface of the constant temperature water bath (1) is wrapped with heat-insulating material.