Preparation device of diethyl zinc

Abstract

The utility model relates to a diethyl zinc preparation device which comprises a reaction kettle, adding devices are arranged on the left side and the right side of the reaction kettle, the adding device for adding raw materials into the reaction kettle is arranged on the left side of the reaction kettle, the adding device for adding solvents into the reaction kettle is arranged on the right side of the reaction kettle, and a microcontroller is arranged in the adding device on the left side. A plurality of through holes are formed in the side face of the reaction kettle, the adding device is connected with the through holes in the side face of the reaction kettle through a conveying pipe, the conveying pipe is arranged in a downward inclined mode, a temperature control assembly capable of adjusting the temperature in the reaction kettle is arranged below the reaction kettle, a vacuum pump is arranged on one side of the reaction kettle, and an air inlet of the vacuum pump is connected with the interior of the reaction kettle. The air outlet is connected with air, and a stirring assembly for rotationally stirring a solution in the reaction kettle is arranged in the reaction kettle. According to the utility model, raw materials and solvents can be automatically and accurately added into the device for stirring and preparation according to a certain amount, so that man-made errors are avoided, and the success rate of preparation is improved.

Description

Technical Field

[0001] The utility model relates to the field of chemical industry, in particular to a preparation device of diethyl zinc. Background Art

[0002] Diethylzinc ((CH3CH2)2Zn) is one of the most important catalyst monomers used in the research and production of carbon dioxide-based fully degradable plastic resins. At the same time, diethylzinc is also an MO source for MOCVD, an important growth method for compound semiconductor thin film materials. It is an important dopant for materials such as gallium arsenide. It can also be used to prepare materials such as ZnSe and ZnS. The purity of diethylzinc is required to be very high in the MOCVD process. If it contains a lot of impurities, it will directly affect the photoelectric properties of the prepared material. It can also be used to protect and repair paper cultural relics and extend the life of books and periodicals; it is used in asymmetric addition, enantioselective addition and stereoselective addition reactions of aldehydes and benzaldehyde. Existing problems: In the preparation process, there are inaccurate additions of raw materials or solvents, which leads to preparation failures and even safety accidents. Utility Model Content

[0003] In view of the above, the utility model provides a preparation device for diethyl zinc, which can automatically add raw materials and solvents into the device according to certain dosages for preparation, thus well solving the above problems.

[0004] According to one aspect of the utility model, a preparation device of diethyl zinc is provided, comprising a reactor, wherein the reactor is provided with adding devices on the left and right sides, wherein the left side of the reactor is an adding device capable of automatically controlling the metering of raw materials into the reactor, and the right side of the reactor is an adding device capable of automatically controlling the metering of solvents into the reactor, a microcontroller is provided in the adding device on the left side, a plurality of through holes are provided on the side of the reactor, the adding device is connected to the through holes on the side of the reactor through a delivery pipe, and the delivery pipe is arranged to be tilted downward, a temperature control component capable of adjusting the temperature in the reactor is provided below the reactor, a vacuum pump is provided on one side of the reactor, an air inlet of the vacuum pump is connected to the reactor, and an air outlet is connected to the air, and a stirring component for rotating and stirring the solution in the reactor is provided in the reactor;

[0005] The adding device comprises a device body, a rotary feed valve capable of controlling the outflow of powdered or granular solids, and a solenoid valve capable of controlling the outflow of liquids. The device body is provided with a plurality of storage chambers, which are connected to the delivery pipe via the rotary feed valve or the solenoid valve, and the output end of the microcontroller is connected to the rotary feed valve and the solenoid valve.

[0006] The temperature control component includes a shell and a semiconductor refrigeration chip, the shell is arranged below the reaction kettle, the semiconductor refrigeration chip is arranged inside the shell, and the semiconductor refrigeration chip is connected to the output end of the microcontroller;

[0007] The stirring assembly includes a fixed frame, a stirring shaft, a driving motor and a stirring blade. The fixed frame is arranged at the center of the top of the reactor, the stirring shaft is vertically arranged below the fixed frame, the driving motor is connected to the top of the stirring shaft, the stirring blade is arranged at the bottom of the stirring shaft, and the driving motor is connected to the output end of the microcontroller.

[0008] Furthermore, the number of the storage chambers is 2 to 6.

[0009] Furthermore, the number of the rotary feed valve and the number of the solenoid valve are at least 1 respectively.

[0010] Furthermore, a power cord is provided on one side of the adding device.

[0011] Furthermore, a large number of small holes are provided at the contact portion between the shell and the reactor.

[0012] Furthermore, a feeding port for adding raw materials or solvents is provided on one side of the storage chamber.

[0013] Furthermore, a start switch is provided on one side of the adding device.

[0014] The beneficial effects of the utility model include being able to automatically and accurately add raw materials and solvents into the device according to certain measurements for stirring and preparation, thus avoiding human errors and improving the success rate of preparation. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a structural schematic diagram of the utility model.

[0016] In the figure, 1-reaction kettle, 2-adding device, 3-start switch, 4-storage chamber, 5-rotary feed valve, 6-conveying pipe, 7-solenoid valve, 8-vacuum pump, 9-microcontroller, 10-fixed frame, 11-stirring shaft, 12-stirring blade, 13-shell, 14-semiconductor refrigeration plate. DETAILED DESCRIPTION

[0017] The utility model is described in detail below with reference to the accompanying drawings and specific embodiments.

[0018] As shown in the figure, a preparation device of diethyl zinc comprises a reactor 1, and an adding device 2 is provided on the left and right sides of the reactor 1, wherein the left side of the reactor 1 is an adding device 2 that can automatically control the metering of raw materials into the reactor 1, and the right side of the reactor 1 is an adding device 2 that can automatically control the metering of solvents into the reactor 1, a microcontroller 9 is fixedly provided in the adding device 2 on the left side, a plurality of through holes are provided on the side of the reactor 1, the adding device 2 is fixedly connected to the through holes on the side of the reactor 1 through a conveying pipe 6, and the conveying pipe 6 is arranged to be tilted downward, a temperature control component that can adjust the temperature in the reactor 1 is fixedly provided below the reactor 1, a vacuum pump 8 is provided on one side of the reactor 1, an air inlet of the vacuum pump 8 is fixedly connected to the reactor 1, and an air outlet is connected to the air, and a stirring component that rotates and stirs the solution in the reactor 1 is fixedly provided in the reactor 1; the vacuum pump 8 is a common prior art in the mechanical field, and will not be described in detail here.

[0019] The adding device 2 includes a device body, a rotary feed valve 5 that can control the outflow of powdered or granular solids, and a solenoid valve 7 that can control the outflow of liquids. The device body is provided with a plurality of storage chambers 4, and the storage chambers 4 are fixedly connected to the delivery pipe 6 through the rotary feed valve 5 or the solenoid valve 7. The output end of the microcontroller 9 is fixedly connected to the rotary feed valve 5 and the solenoid valve 7. When working, the rotary feed valve 5 or the solenoid valve 7 is controlled by the microcontroller 9 to open so that the raw material or solvent flows out. The rotary feed valve 5 and the solenoid valve 7 are both common existing technologies in the mechanical field, and will not be described in detail here.

[0020] The temperature control component includes a shell 13 and a semiconductor refrigeration sheet 14. The shell 13 is fixedly arranged below the reactor 1. The semiconductor refrigeration sheet 14 is fixedly arranged in the shell 13. The semiconductor refrigeration sheet 14 is connected to the output end of the microcontroller 9. The semiconductor refrigeration sheet 14 is started by the microcontroller 9, and then the temperature is transferred to the reactor 1 through the small holes on the shell 13. The semiconductor refrigeration sheet 14 is a common existing technology in the mechanical field and will not be described in detail here.

[0021] The stirring assembly includes a fixed frame 10, a stirring shaft 11, a driving motor and a stirring blade 12. The fixed frame 10 is fixedly arranged at the top center position of the reactor 1, the stirring shaft 11 is vertically fixedly arranged below the fixed frame 10, the driving motor is fixedly connected to the top end of the stirring shaft 11, the stirring blade 12 is fixedly arranged at the bottom end of the stirring shaft 11, and the driving motor is connected to the output end of the microcontroller 9; when working, the driving motor drives the stirring shaft 11 to rotate, thereby rotating the stirring blade 12.

[0022] In this embodiment, the number of the storage chambers 4 is 2 to 6, which is sufficient to add all the raw materials and solvents for preparing diethyl zinc.

[0023] In this embodiment, the number of the rotary feed valve 5 and the electromagnetic valve 7 is at least one, respectively, so as to reasonably allow the solid medium and the liquid medium to flow out through the corresponding valves.

[0024] In this embodiment, the air in the reactor 1 is extracted by the vacuum pump 8 to make the pressure in the reactor 1 lower than that in the storage chamber 4. The raw material or solvent can automatically flow out under the action of the pressure difference by simply opening the rotary feed valve 5 or the solenoid valve 7.

[0025] In this embodiment, the vacuum pump 8 is provided with a separate switch button.

[0026] In this embodiment, the reactor 1 is in a vacuum state throughout the entire process to prevent diethyl zinc from spontaneously igniting when it encounters air.

[0027] In this embodiment, a power line is provided on one side of the adding device 2 to provide power.

[0028] In this embodiment, a feeding port for adding raw materials or solvents which can be manually switched on and off is provided on one side of the storage chamber 4 .

[0029] In this embodiment, a start switch 3 is provided on one side of the adding device 2 , and the start switch 3 is connected to the microcontroller 9 .

[0030] In this embodiment, an opening which can be manually opened and closed for sampling is provided on the top of the reactor 1 .

[0031] In this embodiment, a large number of small holes are provided in the contact portion between the shell 13 and the reactor 1 , and the cooling effect generated by the semiconductor cooling sheet 14 is transmitted to the reactor 1 .

[0032] In this embodiment, the interior of the shell 13 is coated with a polyimide low-temperature resistant material to prevent the shell 13 from being broken due to low temperature.

[0033] During the specific implementation of the utility model, the air in the reactor 1 is firstly extracted by using a vacuum pump 8, and then raw materials ethylmagnesium bromide and zinc chloride are added to the storage chamber 4 in the left adding device 2, and calcium chloride, tetrahydrofuran and dilute acid are added to the storage chamber 4 in the right adding device 2, and then the semiconductor refrigeration sheet 14 is started to control the temperature in the reactor 1 to be lower than zero degrees Celsius, and then the microcontroller 9 controls the adding device 2 to add an appropriate amount of tetrahydrofuran solvent, then zinc chloride is added to the solvent, and the stirring component is started to make it dissolve evenly, and then the ethylmagnesium bromide solution is slowly added dropwise through the adding device 2 to react, and during the reaction process, it is necessary to stir and maintain low temperature control to avoid uncontrolled reaction. After the ethylmagnesium bromide solution is added dropwise, the reaction mixture is continuously stirred by the stirring component, and the low temperature reaction is maintained for 12 hours, and then an appropriate amount of dilute acid is added through the adding device 2 to accelerate the completion of the reaction, and then calcium chloride is added to remove the moisture in the solvent to obtain a pure diethyl zinc product, and finally the diethyl zinc is taken out through a sampling tool.

[0034] It is worth noting that: in the description of the present utility model, the meaning of "multiple" is two or more than two, unless otherwise clearly and specifically defined. In the present utility model, unless otherwise clearly specified and defined, the terms "install", "connect", "connect", "fix" and the like 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; the circuits described in the present utility model are all commonly used circuits in the field, and other related components are all existing commonly used components. For ordinary technicians in the field, the specific meanings of the above terms in the present utility model can be understood according to the specific circumstances.

[0035] It is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive from any point of view, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes that fall within the meaning and scope of the elements of the claims be included in the present invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

[0036] In this embodiment, the control circuit of the utility model is a common circuit in the circuit field. The device of the utility model can be connected to an external power supply or a built-in battery through a power cord to provide power for the device. Technicians in the relevant technical field can implement it and will not be elaborated here.

Claims

1. A preparation device for diethyl zinc, comprising a reaction kettle, characterized in that: The reactor is provided with adding devices on both sides, wherein the left side of the reactor is an adding device capable of automatically controlling the metering of raw materials into the reactor, and the right side of the reactor is an adding device capable of automatically controlling the metering of solvents into the reactor, a microcontroller is arranged in the adding device on the left side, a plurality of through holes are arranged on the side of the reactor, the adding device is connected to the through holes on the side of the reactor through a delivery pipe, and the delivery pipe is arranged to be tilted downward, a temperature control component capable of adjusting the temperature in the reactor is arranged below the reactor, a vacuum pump is arranged on one side of the reactor, an air inlet of the vacuum pump is connected to the reactor, and an air outlet is connected to the air, and a stirring component for rotating and stirring the solution in the reactor is arranged in the reactor; The adding device comprises a device body, a rotary feed valve capable of controlling the outflow of powdered or granular solids, and a solenoid valve capable of controlling the outflow of liquids. The device body is provided with a plurality of storage chambers, which are connected to the delivery pipe via the rotary feed valve or the solenoid valve, and the output end of the microcontroller is connected to the rotary feed valve and the solenoid valve. The temperature control component includes a shell and a semiconductor refrigeration chip, the shell is arranged below the reaction kettle, the semiconductor refrigeration chip is arranged inside the shell, and the semiconductor refrigeration chip is connected to the output end of the microcontroller; The stirring assembly includes a fixed frame, a stirring shaft, a driving motor and a stirring blade, wherein the fixed frame is arranged at the center of the top of the reactor, the stirring shaft is vertically arranged below the fixed frame, the driving motor is connected to the top of the stirring shaft, the stirring blade is arranged at the bottom of the stirring shaft, and the driving motor is connected to the output end of the microcontroller; During operation, the vacuum pump first extracts the air in the reactor, the adding device inputs the raw materials or solvents into the reactor in sequence, and the stirring component stirs to make it react evenly.

2. A preparation device for diethyl zinc according to claim 1, characterized in that: The number of the storage chambers is 2 to 6.

3. A preparation device for diethyl zinc according to claim 1, characterized in that: The number of the rotary feed valve and the number of the solenoid valve are at least 1.

4. A preparation device for diethyl zinc according to claim 1, characterized in that: A power line is arranged on one side of the adding device.

5. A preparation device for diethyl zinc according to claim 1, characterized in that: The contact portion between the shell and the reactor is provided with a large number of small holes.

6. A device for preparing diethyl zinc according to claim 2, characterized in that: A feeding port for adding raw materials or solvents is arranged on one side of the storage chamber.

7. A device for preparing diethyl zinc according to claim 4, characterized in that: A starting switch is arranged on one side of the adding device.

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