A device for preparing trimethylaluminum with enhanced medium dispersion

Abstract

The utility model discloses a kind of preparation devices of trimethylaluminum of reinforced medium dispersion, including a reactor, gas phase space and liquid phase space are formed after liquid is imported into reactor, reactor is equipped with first ultrasonic generator and a first stirrer with self-suction function, for the gas in the gas phase space of reactor top is inhaled into first stirrer after sending to the bottom liquid phase space of reactor to participate in reaction again;And a drop tank, drop tank is connected with reactor by pipeline, drop tank is equipped with second ultrasonic generator and second stirrer.The utility model makes the reaction gas in reactor circulate between liquid phase space and gas phase space, ensure that material is in turbulent state, improve reaction efficiency, and under ultrasonic vibration, aluminum generated by reaction is hindered to be wrapped on the surface of alkaline earth metal, reduce the input amount of alkaline earth metal, reduce production cost, simultaneously, the dispersion of ultrasonic reinforced medium in solvent is convenient for the uniform addition of suspension liquid in drop tank to participate in reaction.

Description

Technical Field

[0001] This utility model relates to a trimethylaluminum preparation apparatus for enhancing media dispersion. Background Technology

[0002] Trimethylaluminum is a very important chemical raw material with a wide range of applications. It can be used not only to prepare methylaluminoxane as a co-catalyst in the polymerization of high-end α-polyolefins, but also for the deposition and growth of thin film materials for semiconductor, photovoltaic, and LED components and chips, and is receiving increasing attention.

[0003] Currently, the main methods for synthesizing trimethylaluminum include sodium reduction, aluminum reduction, magnesium-aluminum alloy reduction, Grignard reagent method, and alkyl exchange method.

[0004] Sodium reduction is the mainstream industrial production process due to the readily available and inexpensive raw materials and low production costs. However, certain problems still exist in its production process:

[0005] (1) During the reaction process, there is a problem that the aluminum metal generated by the reaction encapsulates the alkaline earth metal, which prevents further reaction. Therefore, it is impossible to accurately control the amount of alkaline earth metal added, and it is difficult to control the occurrence of side reactions. The product yield and purity need to be improved.

[0006] (2) This reaction is a gas-liquid-solid three-phase reaction. Due to the influence of the mass transfer rate, the reaction efficiency needs to be improved. Utility Model Content

[0007] The purpose of this invention is to provide a technical solution for a trimethylaluminum preparation device that enhances media dispersion, addressing the shortcomings of existing technologies. This device allows the reaction gas in the reactor to circulate between the liquid and gas phases, ensuring the material is in a turbulent state and improving reaction efficiency. Furthermore, under ultrasonic vibration, the aluminum generated during the reaction is coated on the surface of the alkaline earth metal, ensuring the smooth progress of the reaction, reducing the amount of alkaline earth metal required, and lowering production costs. Simultaneously, ultrasonic enhancement of the media dispersion in the solvent facilitates the uniform addition of the suspension from the dropping tank to the reactor to participate in the reaction, further improving reaction efficiency.

[0008] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0009] A trimethylaluminum preparation apparatus for enhancing media dispersion, characterized in that: it includes...

[0010] A reactor is provided in which liquid is introduced to form a gas phase space and a liquid phase space. The reactor is equipped with a first ultrasonic generator and a first stirrer with a self-aspirating function, which is used to draw the reaction gas in the gas phase space at the top of the reactor into the first stirrer and send it to the liquid phase space at the bottom of the reactor to re-participate in the reaction.

[0011] A dropper is connected to the reactor via a pipeline. The dropper is equipped with a second ultrasonic generator and a second stirrer.

[0012] The above structural design allows the reactant gas in the reactor to circulate between the liquid and gas phases, ensuring that the material is in a turbulent state and improving reaction efficiency. Furthermore, under ultrasonic vibration, the aluminum generated by the reaction is coated on the surface of the alkaline earth metal, ensuring the smooth progress of the reaction, reducing the amount of alkaline earth metal required, and lowering production costs. At the same time, ultrasonic enhancement can improve the dispersion of the medium in the solvent, facilitating the uniform addition of the suspension in the dropper to the reactor to participate in the reaction and improving reaction efficiency.

[0013] Furthermore, the first stirrer includes a stirring shaft with a hollow internal structure, at least one air inlet located at the upper end of the stirring shaft and connected to the gas phase space, and stirring blades distributed vertically along the stirring shaft. The stirring blades located at the lower end are provided with an air outlet. The air inlet is connected to the air outlet through the stirring shaft, which facilitates the circulation of reaction gases in the gas phase space and liquid phase space and improves reaction efficiency.

[0014] Furthermore, the first agitator also includes reinforcing ribs, which are distributed in a spiral structure on the agitator shaft to improve the stability and reliability of the first agitator and extend its service life.

[0015] Furthermore, the power of the first ultrasonic generator is 500W to 8000W, preferably 800W to 3000W, and the power of the second ultrasonic generator is 100W to 5000W, preferably 400W to 1000W.

[0016] Furthermore, the reactor is equipped with a first liquid feed pipe, a gas phase outlet pipe, a gas feed pipe, and a reaction liquid outlet pipe. The first liquid feed pipe and the gas phase outlet pipe are connected to the gas phase space, and the gas feed pipe and the reaction liquid outlet pipe are connected to the liquid phase space.

[0017] Furthermore, a gas distributor is connected to the outlet end of the gas feed pipe, and the gas distributor is located in the liquid phase space.

[0018] Furthermore, a first jacket is provided on the outside of the reactor for introducing hot or cold fluids to heat or cool the medium inside the reactor.

[0019] Furthermore, the drip tank is equipped with a second liquid inlet pipe for supplying liquid to the drip tank.

[0020] Furthermore, a second jacket is provided on the outside of the dripping tank for introducing hot or cold fluids to heat or cool the medium inside the dripping tank.

[0021] This utility model, by adopting the above-mentioned technical solution, has the following beneficial effects:

[0022] 1. This utility model uses a first stirrer with a self-priming function to draw the reaction gas in the gas phase space above the reactor into the stirring shaft and send it to the liquid phase at the bottom of the reactor. On the one hand, the raw material gas can participate in the reaction again, and on the other hand, the gas that is re-introduced can break the liquid into small droplets, increase the contact area, enhance the mass transfer rate, and thus improve the reaction efficiency.

[0023] 2. Under the dual action of mechanical stirring and ultrasound, this utility model can keep the liquid in the reactor in a turbulent state at all times, ensuring full contact between the gas, liquid and solid phases, while preventing the aluminum generated during the reaction from being coated on the surface of the alkaline earth metal, ensuring the smooth progress of the reaction, reducing the amount of alkaline earth metal to be fed, and lowering production costs.

[0024] 3. This invention can use ultrasound to disperse the strengthening medium in the solvent, which facilitates the uniform addition of the suspension in the dropping tank to the reactor to participate in the reaction and improves the reaction efficiency. Attached image description:

[0025] The present invention will be further described below with reference to the accompanying drawings:

[0026] Figure 1 This is a schematic diagram of the structure of a trimethylaluminum preparation device for enhancing media dispersion according to the present invention;

[0027] Figure 2 This is a schematic diagram of the structure of the first stirrer in this utility model.

[0028] Wherein: 1-reactor; 2-droplet tank; 3-first ultrasonic generator; 4-second ultrasonic generator; 5-first stirrer; 6-second stirrer; 7-first jacket; 8-first liquid feed pipe; 9-gas feed pipe; 10-gas distributor; 11-gas phase outlet pipe; 12-reaction liquid outlet pipe; 13-second jacket; 14-second liquid feed pipe; 15-pipeline; 16-stirring shaft; 17-air inlet; 18-stirring paddle; 19-reinforcing rib; 20-air outlet. Detailed Implementation

[0029] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0030] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. 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 should fall within the protection scope of the present invention.

[0031] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this utility model are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion.

[0032] like Figures 1 to 2 As shown, this utility model discloses a trimethylaluminum preparation device for enhancing media dispersion, which includes a reactor 1 and a dropper 2. The dropper 2 is connected to the reactor 1 through a pipeline 15, and a valve can be installed on the pipeline 15.

[0033] After liquid is introduced into reactor 1, a gas phase space and a liquid phase space are formed. Reactor 1 is equipped with a first ultrasonic generator 3 and a first stirrer 5 with a self-aspirating function, which is used to draw the gas in the gas phase space at the top of reactor 1 into the first stirrer 5 and send it to the liquid phase space at the bottom of reactor 1 to participate in the reaction again.

[0034] The first stirrer 5 includes a stirring shaft 16 with a hollow internal structure, at least one air inlet 17 located at the upper end of the stirring shaft 16 and connected to the gas phase space, and stirring paddles 18 distributed vertically along the stirring shaft 16. The stirring paddles 18 located at the bottom are provided with an air outlet 20. The air inlet 17 is connected to the air outlet 20 through the stirring shaft 16, which facilitates the circulation of reaction gas in the gas phase space and the liquid phase space and improves the reaction efficiency.

[0035] The first agitator 5 also includes reinforcing ribs 19, which are distributed in a spiral structure on the agitator shaft 16 to improve the stability and reliability of the first agitator 5 and extend its service life.

[0036] Reactor 1 is equipped with a first liquid feed pipe 8, a gas phase outlet pipe 11, a gas feed pipe 9, and a reaction liquid outlet pipe 12. The first liquid feed pipe 8 and the gas phase outlet pipe 11 are connected to the gas phase space, and the gas feed pipe 9 and the reaction liquid outlet pipe 12 are connected to the liquid phase space. A valve is installed on the reaction liquid outlet pipe 12.

[0037] The outlet end of the gas feed pipe 9 is connected to a gas distributor 10. The gas distributor 10 is located in the liquid phase space. The gas distributor 10 can be a hollow circular tube with evenly distributed air holes, with the air holes facing the bottom and the air hole diameter being 0.5 to 5 mm.

[0038] The reactor 1 is provided with a first jacket 7 on the outside, which is used to introduce hot or cold fluids to heat or cool the medium inside the reactor 1.

[0039] The dripping tank 2 is equipped with a second ultrasonic generator 4 and a second stirrer 6.

[0040] The power of the first ultrasonic generator 3 is 500W to 8000W, preferably 800W to 3000W, and the power of the second ultrasonic generator 4 is 100W to 5000W, preferably 400W to 1000W.

[0041] The first ultrasonic generator 3 and the second ultrasonic generator 4 in this invention convert 50-60Hz alternating current into 15kHz-40kHz high-frequency power to supply the transducer. The transducer then converts the high-frequency power into mechanical vibration, achieving a hybrid effect. Both the first ultrasonic generator 3 and the second ultrasonic generator 4 adopt existing structures, which will not be described in detail here.

[0042] The first and second agitators also include drive motors, which are connected to the agitator shafts via couplings.

[0043] The drip tank 2 is equipped with a second liquid inlet pipe 14 for supplying liquid to the drip tank 2.

[0044] The outer side of the drip tank 2 is provided with a second jacket 13 for introducing hot or cold fluids to heat or cool the medium inside the drip tank 2.

[0045] The above structural design allows the reactant gas in the reactor to circulate between the liquid and gas phases, ensuring that the material is in a turbulent state and improving reaction efficiency. Furthermore, under ultrasonic vibration, the aluminum generated by the reaction is coated on the surface of the alkaline earth metal, ensuring the smooth progress of the reaction, reducing the amount of alkaline earth metal required, and lowering production costs. At the same time, ultrasonic enhancement can improve the dispersion of the medium in the solvent, facilitating the uniform addition of the suspension in the dropper to the reactor to participate in the reaction and improving reaction efficiency.

[0046] In practical use, this utility model is:

[0047] S1. Add 1363g of sodium-toluene suspension with a mass fraction of 10% to the dripping tank 2. Flow heat transfer oil into the second jacket 13 of the dripping tank 2 to heat the medium in the dripping tank 2 to 105℃, so that the sodium becomes molten. Start the second stirrer 6 and the second ultrasonic generator 4. Control the speed of the second stirrer 6 at 750r / min and the power of the second ultrasonic generator 4 at 500W to fully disperse the molten sodium in the toluene. Set aside for later use.

[0048] S2. Add 200g of methyl sesquialuminum into reactor 1 through the first liquid feed pipe 8. Start the first stirrer 5 and the first ultrasonic generator 3. Control the speed of the first stirrer 5 at 800r / min and the power of the first ultrasonic generator 3 at 1000W. Introduce heat transfer oil into the first jacket 7 of reactor 1 to heat the medium in reactor 1, heating the solution in reactor 1 to 105℃~115℃ and maintaining it. Continuously introduce chloromethane into reactor 1 through the gas feed pipe 9. Gas was introduced, and the pressure inside reactor 1 was maintained at 0.3 MPa. A total of 155 g of chloromethane was introduced after the reaction was completed. While chloromethane was introduced, the suspension prepared in step S1 was slowly dripped into reactor 1, and the dripping rate was controlled at 5 ml / min. After dripping, the mixture was kept at the same temperature and pressure for 2 hours. The residual pressure was then released from the gas phase outlet pipe 11 of reactor 1. After the residual pressure was released, the reaction liquid containing trimethylaluminum was discharged from the reaction liquid outlet pipe 12 at the bottom of reactor 1. After post-processing, 131.5 g of trimethylaluminum was obtained.

[0049] like Figure 2 As shown, during the pressure-holding reaction, due to the rapid rotation of the first stirrer 5, a negative pressure is formed at the bottom of the first stirrer 5, which causes chloromethane gas to be drawn in through the air inlet on the stirring shaft 16, and discharged through the air outlet 20 on the stirring paddle 18 below after passing through the hollow stirring shaft 16. This forces the reaction gas to circulate in the reactor 1 and stirs the liquid, thereby enhancing mass transfer and improving reaction efficiency.

[0050] The above are merely specific embodiments of this utility model, but the technical features of this utility model are not limited thereto. Any simple changes, equivalent substitutions, or modifications made based on this utility model to achieve essentially the same technical effect are all covered within the protection scope of this utility model.

Claims

1. A trimethylaluminum preparation device for enhancing medium dispersion, characterized in that: include A reactor, wherein liquid is introduced into the reactor to form a gas phase space and a liquid phase space, the reactor is equipped with a first ultrasonic generator and a first stirrer with a self-aspirating function, which is used to draw the reaction gas in the gas phase space at the top of the reactor into the first stirrer and send it to the liquid phase space at the bottom of the reactor to re-participate in the reaction. A dropper is provided, which is connected to the reactor via a pipeline, and the dropper is equipped with a second ultrasonic generator and a second stirrer.

2. The trimethylaluminum preparation device for enhancing medium dispersion according to claim 1, wherein: The first stirrer includes a stirring shaft with a hollow internal structure, at least one air inlet located at the upper end of the stirring shaft and connected to the gas phase space, and stirring paddles distributed vertically along the stirring shaft. The stirring paddle located at the lower end has an air outlet, and the air inlet is connected to the air outlet through the stirring shaft.

3. The trimethylaluminum preparation device for enhancing medium dispersion according to claim 2, characterized in that: The first stirrer also includes reinforcing ribs, which are distributed in a spiral structure on the stirring shaft.

4. The trimethylaluminum preparation device for enhancing medium dispersion according to claim 1, wherein: The power of the first ultrasonic generator is 500W to 8000W, and the power of the second ultrasonic generator is 100W to 5000W.

5. A trimethylaluminum preparation device for enhancing medium dispersion according to any one of claims 1 to 4, characterized in that: The reactor is provided with a first liquid feed pipe, a gas phase outlet pipe, a gas feed pipe and a reaction liquid outlet pipe. The first liquid feed pipe and the gas phase outlet pipe are connected to the gas phase space, and the gas feed pipe and the reaction liquid outlet pipe are connected to the liquid phase space.

6. The trimethylaluminum preparation device for enhancing medium dispersion according to claim 5, wherein: The outlet end of the gas feed pipe is connected to a gas distributor, which is located within the liquid phase space.

7. The preparation device of trimethylaluminum for enhancing medium dispersion according to claim 5, wherein: The reactor is provided with a first jacket on the outside for introducing hot or cold fluids to heat or cool the medium inside the reactor.

8. A trimethylaluminum preparation device for enhancing medium dispersion according to any one of claims 1 to 4, characterized in that: The drip tank is equipped with a second liquid inlet pipe for supplying liquid to the drip tank.

9. The apparatus for preparing trimethylaluminum with enhanced media dispersion according to claim 8, characterized in that: The outer side of the dripping tank is provided with a second jacket for introducing hot or cold fluids to heat or cool the medium inside the dripping tank.

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