Reaction kettle for preparing phosphorane gas
By introducing a vacuum pump, a nitrogen tank and an oxygen detector into the reaction kettle for preparation of phosphane gas, the complete replacement of oxygen in the reaction kettle and real-time monitoring is achieved, and the problems of affected reactions and safety hazards in the prior art are solved, and the yield and reaction safety are improved.
Patent Information
- Application Number
- CN202420680257.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-03
- Publication Date
- 2025-04-18
- Estimated Expiration
- 2034-04-03
AI Technical Summary
In the prior art, when producing phosphane gas, it is difficult to achieve oxygen-free and air-free conditions in the reactor, resulting in an impact on the reaction, a decrease in yield and even an explosion may occur.
A system including the reactor body, a vacuum pump, a nitrogen tank and an oxygen measuring instrument was designed. Through the cooperation of the nitrogen tank and a vacuum pump, the oxygen content in the reactor is completely replaced, and the oxygen content is monitored in real time through the oxygen measuring instrument to ensure the safety of the reaction.
It effectively ensures the safety of chemical reactions in the reactor, improves nitrogen replacement efficiency, shortens the replacement time, and ensures the reliability and safety of the reaction process.
Smart Images
Figure CN222766253U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical equipment, in particular to a reaction kettle for preparing phosphine gas. Background Art
[0002] A reactor is a container used for physical mixing or chemical reactions. It is mainly used to mix materials and provide chemical reactions. It is often used in the production of chemical products such as coatings, surfactants, and water treatment agents.
[0003] Phosphine (PH3) is a very important electronic gas. As an n-type dopant, it plays a very key role in epitaxial GaP materials and ion implantation processes. It is also an important raw material for synthesizing compound semiconductor gallium arsenide phosphide (GaAsP). It is also widely used in solar cells, grain fumigation and other fields. At present, most industries use yellow phosphorus and alkali to react to produce sodium hypophosphite, which produces a large amount of phosphine gas as a by-product. During the reaction of yellow phosphorus and alkali, the reactor is required to be isolated from air as much as possible. Therefore, if the reactor cannot be oxygen-free and air-isolated, the reaction will be affected, the yield will decrease, and even explosion may occur if improper operation is encountered. Utility Model Content
[0004] The utility model aims to provide a reaction kettle for preparing phosphine gas to solve the problems raised in the above background technology.
[0005] To achieve the above-mentioned purpose, the utility model provides the following technical solutions: a reactor for preparing phosphine gas, comprising a reactor body, a vacuum pump, a nitrogen tank and an oxygen meter, a driving motor is installed in the center of the upper part of the reactor body, the output end of the driving motor is arranged downward and fixedly connected to a rotating shaft, the rotating shaft is arranged inside the reactor body, and a stirring blade and a spiral heating plate are fixed on the rotating shaft; a control circuit of the spiral heating plate is connected to a temperature controller, the temperature controller is fixed on the outer wall of the reactor body, a temperature sensor is arranged in the reactor body, and a signal output line of the temperature sensor is connected to a signal input end of the temperature controller; the vacuum pump is connected to the connecting main pipe, one end of the connecting main pipe is respectively connected to a first connecting branch pipe and a second connecting branch pipe, the first connecting branch pipe is connected to the nitrogen tank, and the second connecting branch pipe is connected to the reactor body; the oxygen meter is connected to a first oxygen measuring pipeline and a second oxygen measuring pipeline, the first oxygen measuring pipeline is connected to the reactor body, and the second oxygen measuring pipeline is connected to the nitrogen tank.
[0006] Preferably, a feeding device is provided at the top of the reactor body, and an observation device is provided at one side of the reactor body. The observation device includes a temperature display and a barometer, and the temperature display displays the sensed temperature of the temperature sensor.
[0007] Preferably, one side of the reactor body is connected to an exhaust pipe, an exhaust valve is arranged in the middle of the exhaust pipe, a discharge pipe is fixedly arranged at the bottom end of the reactor body, and a discharge valve is arranged in the middle of the discharge pipe.
[0008] Preferably, a nitrogen inlet pipe connected to a nitrogen source is provided on one side of the nitrogen tank.
[0009] Preferably, the middle sections of the nitrogen inlet pipe, the connecting main pipe, the first connecting branch pipe, and the second connecting branch pipe are all provided with solenoid valves.
[0010] Compared with the prior art, the utility model has the following beneficial effects: the utility model is provided with a nitrogen tank and a vacuum pump, so that the oxygen in the reactor body is replaced as completely as possible, thereby ensuring the safety of the chemical reaction in the reactor; since the nitrogen tank can store a certain amount of nitrogen, the reactor body can be quickly replaced, thereby improving the replacement efficiency and shortening the time required for nitrogen replacement; the utility model can measure the oxygen content of the oxygen tank and the reactor to be tested in real time by providing an oxygen meter, and use the actual measured value to feed back the replacement effect, so that the result is more reliable and the safety of the reaction process is ensured; the utility model can rotate under the drive of the drive motor during the reaction by providing a rotating shaft and a stirring blade, so that the material reaction is more sufficient. BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Figure 1 It is a schematic diagram of the structure of the utility model.
[0012] In the figure: 1. Reactor body; 2. Drive motor; 3. Rotating shaft; 4. Stirring blade; 5. Spiral heating plate; 6. Feeding device; 7. Temperature controller; 8. Temperature sensor; 9. Observation device; 10. Discharge pipe; 1001. Discharge valve; 11. Exhaust pipe; 1101. Exhaust valve; 12. Nitrogen tank; 13. Vacuum pump; 14. Connecting main pipe; 1401. First connecting branch pipe; 1402. Second connecting branch pipe; 15. Oxygen meter; 16. First oxygen measuring pipeline; 17. Second oxygen measuring pipeline; 18. Solenoid valve. DETAILED DESCRIPTION
[0013] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.
[0014] In the description of the present invention, it should be noted that the terms "vertical", "up", "down", "horizontal", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.
[0015] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set", "install", "connect", and "connect" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0016] See also Figure 1 The utility model provides a technical solution: a reactor for preparing phosphine gas, comprising a reactor body 1, a vacuum pump 13, a nitrogen tank 12 and an oxygen meter 15, a driving motor 2 is installed in the upper center of the reactor body 1, the output end of the driving motor 2 is arranged downward and fixedly connected to a rotating shaft 3, the rotating shaft 3 is arranged inside the reactor body 1, and a stirring blade 4 and a spiral heating plate 5 are fixed on the rotating shaft 3; the control circuit of the spiral heating plate 5 is connected to a temperature controller 7, the temperature controller 7 is fixed on the outer wall of the reactor body 1, a temperature sensor 8 is arranged in the reactor body 1, and the temperature sensor 8 is arranged in the reactor body 1. The signal output line of the temperature sensor 8 is connected to the signal input end of the temperature controller 7; the vacuum pump 13 is connected to the connecting main pipe 14, one end of the connecting main pipe 14 is respectively connected to the first connecting branch pipe 1401 and the second connecting branch pipe 1402, the first connecting branch pipe 1401 is connected to the nitrogen tank 12, and the second connecting branch pipe 1402 is connected to the reactor body 1; the oxygen meter 15 is connected to the first oxygen measuring pipeline 16 and the second oxygen measuring pipeline 17, the first oxygen measuring pipeline 16 is connected to the reactor body 1, and the second oxygen measuring pipeline 17 is connected to the nitrogen tank 12.
[0017] Furthermore, a feeding device 6 is provided at the top of the reactor body 1 , and an observation device 9 is provided at one side of the reactor body 1 . The observation device 9 includes a temperature display and a barometer. The temperature display displays the sensed temperature of the temperature sensor 8 .
[0018] Furthermore, one side of the reactor body 1 is connected to an exhaust pipe 11, an exhaust valve 1101 is arranged in the middle of the exhaust pipe 11, and a discharge pipe 10 is fixedly arranged at the bottom end of the reactor body 1, a discharge valve 1001 is arranged in the middle of the discharge pipe 10.
[0019] Furthermore, a nitrogen inlet pipe 1201 connected to a nitrogen source is provided on one side of the nitrogen tank 12 .
[0020] Furthermore, the middle sections of the nitrogen inlet pipe 1201 , the connecting main pipe 14 , the first connecting branch pipe 1401 , and the second connecting branch pipe 1402 are all provided with solenoid valves 18 .
[0021] Working principle: The utility model provides a reactor for preparing phosphine gas. When it is used, firstly, the reaction materials are added into the reactor body 1 from the feeding device 6, and the reaction materials are yellow phosphorus and C1-C5 low-carbon alcohol solution. Then, the vacuum pump 13 and the oxygen meter 15 are turned on, and the electromagnetic valve 18 on the second connecting branch pipe 1402 and the nitrogen inlet pipe 1201 is closed. The electromagnetic valve 18 on the first connecting branch pipe 1401 and the connecting main pipe 14 is opened to evacuate the gas in the nitrogen tank 12 so that the nitrogen tank 12 is in a vacuum state. Then, the electromagnetic valve 18 on the first connecting branch pipe 1401 is closed, and the electromagnetic valve 18 on the nitrogen inlet pipe 1201 is opened to fill the nitrogen tank 12 with nitrogen. At this time, the oxygen meter 15 monitors the oxygen content in the nitrogen tank 12. If the oxygen content is less than 0.5%, it is qualified. Otherwise, the above operation needs to be repeated. Then, the electromagnetic valve 18 on the second connecting branch pipe 1402 is adjusted to control the replacement pressure in the reactor body 1. The observation device 9 The barometer displays the internal pressure of the reactor body 1. The first connecting branch 1401 is closed, and the electromagnetic valves 18 on the connecting main pipe 14 and the second connecting branch 1402 are opened. The reactor body 1 begins to be evacuated. After the barometer value stabilizes, the electromagnetic valve 18 on the connecting main pipe 14 is closed, and the electromagnetic valves 18 on the first connecting branch 1401 and the nitrogen inlet pipe 1201 are opened. Nitrogen is filled into the reactor body 1. The oxygen meter 15 is observed. After it is full, the first connecting branch is closed, and the electromagnetic valve 18 on the connecting main pipe 14 is opened. The vacuum replacement is performed again until it is stable, and then the electromagnetic valve 18 on the second connecting branch 1402 is closed to complete the nitrogen replacement in the reactor body 1. Then, the spiral heating plate 5 is started through the thermostat 7 to control the temperature in the reactor body 1 to be constant at 25-60°C. Then, sodium hydroxide solution is added dropwise through the feeding device 6, and the drive motor 2 is turned on. Stirring is continued for 4-8 hours, and the generated phosphine gas is discharged from the exhaust pipe 11.
[0022] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A reaction kettle for preparing phosphine gas, characterized in that: The invention comprises a reactor body (1), a vacuum pump (13), a nitrogen tank (12) and an oxygen meter (15), wherein a driving motor (2) is installed in the center of the upper part of the reactor body (1), the output end of the driving motor (2) is arranged downward and fixedly connected to a rotating shaft (3), the rotating shaft (3) is arranged inside the reactor body (1), and a stirring blade (4) and a spiral heating plate (5) are fixed on the rotating shaft (3); the control circuit of the spiral heating plate (5) is connected to a temperature controller (7), the temperature controller (7) is fixed on the outer wall of the reactor body (1), a temperature sensor (8) is arranged inside the reactor body (1), and the signal output of the temperature sensor (8) is The vacuum pump (13) is connected to a connecting main pipe (14), one end of which is respectively connected to a first connecting branch pipe (1401) and a second connecting branch pipe (1402), the first connecting branch pipe (1401) is connected to the nitrogen tank (12), and the second connecting branch pipe (1402) is connected to the reactor body (1); the oxygen meter (15) is connected to a first oxygen measuring pipeline (16) and a second oxygen measuring pipeline (17), the first oxygen measuring pipeline (16) is connected to the reactor body (1), and the second oxygen measuring pipeline (17) is connected to the nitrogen tank (12).
2. The reaction kettle for preparing phosphine gas according to claim 1, characterized in that: A feeding device (6) is provided at the top of the reactor body (1), and an observation device (9) is provided on one side of the reactor body (1). The observation device (9) includes a temperature display and a barometer. The temperature display displays the sensed temperature of the temperature sensor (8).
3. The reaction kettle for preparing phosphine gas according to claim 1, characterized in that: One side of the reactor body (1) is connected to an exhaust pipe (11), an exhaust valve (1101) is arranged in the middle of the exhaust pipe (11), and a discharge pipe (10) is fixedly arranged at the bottom end of the reactor body (1), and a discharge valve (1001) is arranged in the middle of the discharge pipe (10).
4. The reaction kettle for preparing phosphine gas according to claim 1, characterized in that: A nitrogen inlet pipe (1201) connected to a nitrogen source is provided on one side of the nitrogen tank (12).
5. The reaction kettle for preparing phosphine gas according to claim 4, characterized in that: The middle sections of the nitrogen inlet pipe (1201), the connecting main pipe (14), the first connecting branch pipe (1401) and the second connecting branch pipe (1402) are all provided with solenoid valves (18).