A continuous preparation method of an organic metal reagent
By using steel balls and stirring shafts in a dynamic continuous microreactor to remove the oxide layer on the metal surface, the problem of induction period in the preparation of organometallic reagents is solved, and the continuous and stable progress of the reaction and the improvement of product quality are achieved.
Patent Information
- Application Number
- CN202411962451.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-30
- Publication Date
- 2025-04-01
AI Technical Summary
The preparation of organometallic reagents has a long induction period, which leads to uncertainty in the occurrence of reactions, prolongs the reaction process time or even does not react, and there is a safety hazard.
Under a nitrogen atmosphere, the metal is continuously transported into a dynamic continuous microreactor, and halogenated alkanes and organic solvents are continuously passed into contact reactions. By setting a steel ball and a stirring shaft in the reactor, the oxide layer on the metal surface is removed, the fresh surface area is increased, and the induction period is eliminated.
Effectively eliminate the reaction induction period, so that the reaction can be carried out smoothly and continuously and stably, avoiding problems such as difficult to start the reaction and out of control of subsequent reaction rates due to the induction period, and improving reaction efficiency and product quality.
Smart Images
Figure CN119733457A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of organometallic reagents, and in particular to a continuous preparation method of organometallic reagents. Background Art
[0002] Grignard reagent is a type of alkylating reagent and is widely used in organic synthesis processes. The preparation of Grignard reagent is carried out by reacting alkyl halide with metallic magnesium (magnesium chips, magnesium particles) in an ether solvent. There is an induction period in the preparation of Grignard reagent. This is because a dense oxide film forms a passivation layer on the solid surface of the magnesium chips. The reaction is not easy to occur in the initial stage of material mixing. Once the reaction occurs, the reaction rate is very fast and generates huge heat, which is difficult to effectively control and is prone to loss of control and explosion accidents.
[0003] Alkyl aluminum sesquioxide is prepared by the reaction of aluminum metal powder and halogenated alkane in saturated alkane, especially methyl aluminum sesquioxide, which is synthesized by methyl chloride and aluminum powder and is an intermediate for the preparation of trimethyl aluminum.
[0004] Trimethylaluminum is widely used as a precursor material for integrated circuit chip manufacturing, high-efficiency battery manufacturing, display packaging, and alkylating agent for organic synthesis. Trimethylaluminum is a key raw material for the preparation of olefin polymerization cocatalyst methylaluminoxane and modified methylaluminoxane cocatalyst, such as metallocene polyolefins, synthetic lubricants, POE elastic materials, and α-olefins. Alkyl aluminum can also be directly used in IC chip aluminum oxide film deposition materials, such as (CH3)3Al2Cl3.
[0005] Alkyl lithium reagent is an alkylating reagent prepared by the reaction of metallic lithium (powder, granules, ribbons) and alkyl halides in saturated hydrocarbon solvents or ether solvents. Since the surface reaction process also has an induction period, the reaction time is difficult to effectively control, which can easily cause temperature runaway and pose a safety hazard.
[0006] The preparation of organometallic reagents has a long induction period, which leads to uncertainty in the reaction, prolongs the reaction process time or even causes no reaction. Therefore, how to eliminate the induction period in the reaction process, make the reaction safer, the reaction process smoother, the reaction process more efficient and the cost lower is an important direction for chemical process research. Summary of the invention
[0007] In order to solve the problems mentioned in the above background technology, the present invention provides a continuous preparation method of an organic metal reagent.
[0008] In order to achieve the above object, the present invention adopts the following technical solutions: A continuous preparation method of an organic metal reagent, in a nitrogen atmosphere, continuously transporting a metal into a dynamic continuous microreactor, and simultaneously continuously introducing a halogenated alkane and an organic solvent for contact reaction to generate an organic metal reagent; The metal is selected from any one of aluminum, magnesium or lithium; The dynamic continuous microreactor comprises a reactor shell, a jacket is arranged outside the reactor shell, and a solid feed inlet, a first liquid feed inlet and a second liquid feed inlet are arranged on one side of the top end of the reactor shell; A premixer is provided on one side of the reactor shell near the solid feed inlet; A stirring shaft is rotatably installed inside the reactor shell, and multiple partitions are fixed outside the stirring shaft. A gap is left between the partition and the inner wall of the reactor shell for materials to flow through. The partition divides the inside of the reactor shell into multiple reaction chambers. Steel balls are arranged in the reaction chambers between adjacent partitions. A stirring plate is fixed outside the stirring shaft between adjacent partitions, and plate holes are opened on the stirring plate.
[0009] Preferably, the aluminum is aluminum particles or aluminum powder; the magnesium is selected from any one of magnesium bars, magnesium particles or magnesium powder; and the lithium is selected from any one of lithium bars, lithium particles or lithium powder.
[0010] Preferably, the halogenated alkane is selected from any one of methyl chloride, methyl bromide, ethyl chloride, ethyl bromide, butyl chloride, butyl bromide, 1-chlorohexane, benzyl chloride and cyclopentane bromide.
[0011] Preferably, when the metal is aluminum, an initiator is also introduced into the dynamic continuous microreactor, and the initiator is selected from any one of methyl sesquialuminum, iodine and methyl iodide.
[0012] Preferably, when the metal is aluminum, the organic solvent is selected from any one or more of octane, decanane, dodecane, hexadecane and liquid alkanes with a higher carbon content; When the metal is magnesium or lithium, the organic solvent is selected from any one of ethyl ether, propyl ether, isopropyl ether, butyl ether, isobutyl ether, n-pentyl ether, diisopentyl ether, toluene, pentane, hexane, octane, decane, dodecane, hexadecane and tetrahydrofuran.
[0013] Preferably, the reaction temperature in the dynamic continuous microreactor is controlled at 20-150°C.
[0014] Preferably, a propeller agitator is provided on one side of the reactor shell near the solid feed port, the propeller agitator is fixedly mounted on the outside of the shaft sleeve, and the shaft sleeve is rotatably sleeved on the outside of the agitator shaft.
[0015] Preferably, a drive box is fixed to the outside of the reactor shell, and one end of the shaft sleeve and the stirring shaft both extend into the drive box. The drive box drives the shaft sleeve to rotate continuously, and the drive box drives the stirring shaft to rotate intermittently.
[0016] Preferably, a rotating motor is fixed inside the driving box, a first gear is fixed to the output shaft of the rotating motor, a second gear is fixed to the outside of the sleeve, and the first gear is meshed with the second gear.
[0017] Preferably, one end of the stirring shaft is connected to the third gear via a one-way transmission, a hydraulic cylinder is fixed in the driving box, a bracket is fixed to the output shaft of the hydraulic cylinder, a rack is fixed on the bracket, and the rack is meshed with the third gear.
[0018] Preferably, a guide rail is fixed in the driving box, a slider is fixed on the bracket, and the slider is slidably mounted on the guide rail.
[0019] Preferably, the premixer comprises an annular fixed cover and an annular rotating container, and the annular rotating container is fixed to the outside of the stirring shaft through a connecting rod.
[0020] Preferably, a first liquid distribution ring pipe and a second liquid distribution ring pipe are respectively provided on both sides of the annular rotating container, and the first liquid distribution ring pipe and the second liquid distribution ring pipe are respectively fixed and connected to the first liquid feed port and the second liquid feed port, and a plurality of first liquid distribution tubes and second liquid distribution tubes are respectively fixed on the side where the first liquid distribution ring pipe and the second liquid distribution ring pipe are close to each other, and the first liquid distribution tubes and the second liquid distribution tubes are fixedly connected to both sides of the annular fixed cover.
[0021] Preferably, the positions of the first dispensing tube and the second dispensing tube correspond one to one, an annular baffle is fixed on the inner side of the annular fixed cover, a mesh hole is provided on the annular baffle, the bottom end of the solid feed port is fixed and connected to the annular fixed cover, and the bottom end of the solid feed port directly passes through the annular baffle, and a plurality of discharge pipes are provided on the side of the annular rotating container close to the partition.
[0022] Preferably, an extrusion screw is rotatably installed inside the discharge pipe, a fourth gear is fixed to one end of the extrusion screw, a gear ring is fixed to the first distribution liquid distribution ring tube, and a plurality of fourth gears are all meshed with the gear ring.
[0023] Compared with the prior art, the present invention has the following beneficial effects: 1. Eliminate the induction period: By setting steel balls between adjacent partitions in the dynamic continuous microreactor, when the stirring shaft rotates, the steel balls roll and collide due to gravity, grinding the solid metal particles (such as aluminum particles, magnesium particles, and lithium particles), removing their surface oxide layer, and transforming the metal materials from particles to flakes, increasing the fresh surface area of the solid metal, effectively eliminating the reaction induction period, allowing the reaction to proceed smoothly, continuously and stably, and avoiding problems such as difficulty in starting the reaction and loss of control of the subsequent reaction rate due to the induction period.
[0024] 2. Improve grinding efficiency: The stirring shaft is driven by the drive box to rotate intermittently. The steel balls obtain a large acceleration at the beginning of rotation and gather on one side of the reaction chamber to generate a strong impact force. After the rotation ends, they collide and rub against the stationary stirring plate and the inner wall of the reactor due to inertia. The collision effect produced by this intermittent motion causes the solid metal particles to quickly turn into ultra-thin flaky debris, increasing the fresh surface area of the solid metal, significantly improving the reaction activity, facilitating the smooth progress of the reaction, and improving product production efficiency and product quality.
[0025] 3. Promote the propulsion and mixing of heterogeneous materials: The propulsion agitator on the sleeve can not only stir the reactants but also give thrust to the reactants when it rotates continuously, promoting the materials to react through each reaction chamber in turn to ensure a smooth reaction process. In the premixer, two different liquid raw materials enter the annular fixed cover through the corresponding distribution ring pipe and the liquid separation pipe for the first mixing, and then enter the annular rotating container after the second mixing through the obstruction of the annular baffle and the flow effect of the mesh. The solid material directly enters the annular rotating container and is evenly distributed and mixed with the liquid with the help of the barrier mesh during its rotation. After that, the mixed liquid is ejected under the action of pressure, achieving efficient premixing and greatly improving the reaction efficiency.
[0026] 4. Prevent discharge blockage: When the extrusion screw in the discharge pipe rotates in the annular rotating container, the fourth gear and the gear ring mesh and rotate automatically, which can effectively prevent the liquid material from being mixed with solid The discharge pipe is blocked to ensure the continuity and stability of the reaction. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 It is a process flow chart of the present invention; Figure 2 is a three-dimensional cross-sectional view of the present invention; Figure 3 A perspective view of the present invention; Figure 4 It is a cross-sectional view from the main perspective of the present invention; Figure 5 It is a schematic diagram of the internal structure of the drive box of the present invention from a first viewing angle; Figure 6 A schematic diagram of the internal structure of the drive box of the present invention from a second viewing angle; Figure 7 is a stereoscopic diagram of a premixer of the present invention; Figure 8 This is an exploded view of the premixer of the present invention from a first perspective; Fig. 9 This is an exploded view of the premixer of the present invention from a second perspective; Fig.10 A cross-sectional view of an annular rotating container of the present invention; Fig.11 It is a cross-sectional view of the one-way transmission of the present invention.
[0028] In the figure: 1. Reactor shell; 101. Solid feed port; 102. First liquid feed port; 1021. First liquid distribution ring; 1022. First liquid distribution pipe; 1023. Gear ring; 103. Second liquid feed port; 1031. Second liquid distribution ring; 1032. Second liquid distribution pipe; 104. Product outlet; 2. Jacket; 201. Cold and hot medium outlet; 202. Cold and hot medium inlet; 3. Drive box; 301. Rotating motor; 302. First gear; 303. Second gear; 4. Stirring shaft; 401. Partition plate; 402. Stirring plate; 402 1. Plate hole; 403. Steel ball; 404. One-way transmission; 4041. Transmission housing; 4042. Ratchet; 4043. Ratchet; 405. Third gear; 406. Hydraulic cylinder; 407. Bracket; 4071. Guide rail; 4072. Slider; 408. Rack; 409. Connecting rod; 5. Premixer; 501. Propeller agitator; 502. Second gear; 6. Annular fixed cover; 601. Annular rotating container; 602. Annular baffle; 603. Annular rotating container; 605. Discharge pipe; 606. Extrusion screw; 6061. Fourth gear. DETAILED DESCRIPTION Example 1
[0029] Reference Figure 1-11 , a continuous preparation method of an organic metal reagent, in which a metal is continuously transported into a dynamic continuous microreactor under a nitrogen atmosphere, and a halogenated alkane and an organic solvent are continuously introduced for contact reaction to generate an organic metal reagent; (1) Preparation of methyl magnesium bromide diisoamyl ether solution Dry diisoamyl ether (water content ≤ 80ppm) was added to the first liquid feed port of the dynamic continuous microreactor through metering pump-1, and the feeding rate was set to 350g / min; monobromomethane was added to the second liquid feed port of the dynamic continuous microreactor through metering pump-2, and the feeding rate was set to 200g / min (2.1mol / min); magnesium chips were added through the solid feeder connected to the solid feed port, and the feeding rate was 58g / min (2.4mol / min). The temperature of the heat transfer oil in the reactor jacket was set between 40-60℃. The reaction system was carried out under the protection of inert gas, including the product receiving tank.
[0030] First, turn on the heating and cooling circulator and set the temperature to 50°C. When the temperature of the microreactor jacket reaches 50°C, turn on the material feed pump. The Grignard reaction occurs continuously in the microreactor to generate methyl magnesium bromide diisoamyl ether solution, which is collected in the product receiving tank. The solution concentration can be calibrated by titration.
[0031] (2) Preparation of 2.0 mol / L n-butylmagnesium chloride tetrahydrofuran solution Dry tetrahydrofuran (water content ≤ 60ppm) is connected to the first liquid feed port of the dynamic continuous microreactor through metering pump-1 for feeding, and the feeding rate is set to 728g / min; 1-chlorohexane is connected to the second liquid feed port of the dynamic continuous microreactor through metering pump-2 for feeding, and the feeding rate is set to 186g / min (2.01mol / min); magnesium chips are connected to the solid feed port through the solid feeder for feeding, and the feeding rate is 48.5g / min (2.02mol / min). The temperature of the heat transfer oil in the reactor jacket is set between 40-60℃. The reaction system is carried out under the protection of inert gas, including the product receiving tank.
[0032] First, turn on the heating and cooling circulator and set the temperature to 40°C. When the temperature of the microreactor jacket reaches 40°C, turn on the material feed pump. The Grignard reaction is carried out continuously in the microreactor. The concentration of the generated n-butylmagnesium chloride Grignard reagent tetrahydrofuran solution is about 2.0 mol / L. The accurate concentration of the solution needs to be calibrated by titration.
[0033] (3) Preparation of 1.0 mol / L methyl lithium ether solution Anhydrous ether (water content ≤ 50ppm) was added through metering pump-1 connected to the first liquid feed port of the dynamic continuous microreactor, and the feeding rate was set to 828g / min; monobromomethane was added through metering pump-2 connected to the second liquid feed port of the dynamic continuous microreactor, and the feeding rate was set to 92.6g / min (1.0 mol / min); lithium chips were added through the solid feeder connected to the solid feed port, and the feeding rate was 13.9g / min (2.0 mol / min). The temperature of the thermal oil in the reactor jacket was set between -10 and 0°C. The reaction system was carried out under inert gas protection, including the product receiving tank.
[0034] Turn on the heating and cooling circulator and set the temperature to 0°C. When the temperature of the microreactor jacket reaches 0°C, turn on the material feed pump. The material reacts continuously in the microreactor to generate methyl lithium ether solution and lithium bromide solid. The reaction solution is filtered to remove lithium bromide solid to obtain a 1.0 mol / L solution, and the accurate concentration needs to be calibrated by titration.
[0035] (4) Preparation of 2.0 mol / L n-butyllithium hexane solution Dry n-hexane (water content ≤ 50ppm) was added to the first liquid feed port of the dynamic continuous microreactor through metering pump-1, and the feeding rate was set to 572g / min; 1-chlorobutane was added to the second liquid feed port of the dynamic continuous microreactor through metering pump-2, and the feeding rate was set to 185.2g / min (2.0 mol / min); lithium chips were added through the solid feeder connected to the solid feed port, and the feeding rate was 38.6g / min (4.0 mol / min). The temperature of the heat transfer oil in the reactor jacket was set between 50-60℃. The reaction system was carried out under inert gas protection, including the product receiving tank.
[0036] Turn on the heating and cooling circulator and set the temperature to 55°C. When the temperature of the microreactor jacket reaches 30°C, turn on the material feed pump. The material reacts continuously in the microreactor to generate methyl lithium ether solution and lithium bromide solid. The reaction solution is filtered to remove lithium chloride solid to obtain a 2.0 mol / L solution, and the accurate concentration needs to be calibrated by titration.
[0037] (5) Dynamic continuous preparation of alkyl aluminum sesquihydrate In a nitrogen atmosphere, aluminum particles are continuously transported into a dynamic continuous microreactor, and iodomethane, hexadecane and methyl chloride are continuously introduced for contact reaction to generate alkyl sesquialuminum; The molar ratio of the reaction materials is: Al / CH3Cl=1.1 / 1.5, and the volume ratio of the solvent to the materials is 5~10 / 1; iodomethane is used as an inducing agent, and the molar amount is 1% of the amount of CH3Cl, which is mixed with the solvent and added together.
[0038] Among them, the feeding speed of aluminum particles is: 100 g / min; Hexadecane feed rate: 2L / min; The feeding rate of methyl chloride is: 255 g / min; The reaction temperature is controlled at 100-130°C; The dynamic continuous microreactor comprises a reactor shell 1, a jacket 2 is provided on the outside of the reactor shell 1, a cold medium inlet 202 and a cold medium outlet 201 are respectively installed on the jacket 2, a solid feed inlet 101, a first liquid feed inlet 102 and a second liquid feed inlet 103 are installed on one side of the top of the reactor shell 1, and a product outlet 104 is provided at one end of the reactor shell 1 away from the solid feed inlet 101; A premixer 5 is provided on one side of the reactor shell 1 near the solid feed port 101; A stirring shaft 4 is rotatably mounted inside the reactor shell 1, and a plurality of partitions 401 are fixed outside the stirring shaft 4. A gap for materials to flow through is left between the partitions 401 and the inner wall of the reactor shell 1. The partitions 401 divide the inside of the reactor shell 1 into a plurality of reaction chambers. Steel balls 403 are arranged in the reaction chambers between adjacent partitions 401. A stirring plate 402 is fixed outside the stirring shaft 4 and located between adjacent partitions 401. The stirring plate 402 is provided with plate holes 4021. The first cavity is a feed cavity, and the last cavity is a discharge cavity. The reactor shell 1 is a pipeline structure, the partition 401 is disc-shaped, and the stirring plate 402 is rectangular, which divides each reaction cavity into two parts. After the reactants are put into the first cavity, they are premixed by the premixer 5, and then enter each reaction cavity in turn to react in each reaction cavity. The diameter of the steel ball 403 is about 20 mm (larger than the gap between the partition 401 and the inner wall of the reactor shell 1). When the stirring shaft 4 rotates, it can drive the stirring plate 402 to stir the material to promote the reaction. The steel ball 403 will continuously roll and collide in the reaction cavity due to gravity, and can grind solid metal particles. Using this continuous dynamic continuous microreactor, halogenated alkanes and metals are reacted in an organic solvent, and the metal is ground by the steel ball 403 to remove the oxide layer and eliminate the induction period, thereby realizing continuous and stable preparation of organic metal reagents, effectively controlling the reaction rate and heat release, and improving safety and product quality stability.
[0039] A propeller agitator 501 is provided on one side of the reactor shell 1 near the solid feed port 101. The propeller agitator 501 is fixedly mounted on the outside of the shaft sleeve 5. The shaft sleeve 5 is rotatably sleeved on the outside of the stirring shaft 4. When the propulsion agitator 501 rotates, it can give thrust to the reaction materials while stirring the reactants, thereby promoting the materials to react through each reaction chamber, and finally the finished product flows out from the product outlet 104. Example 2
[0040] Reference Figure 1-11 The difference between this embodiment and embodiment 1 is that a driving box 3 is fixed to the outside of the reactor housing 1, and one end of the shaft sleeve 5 and the stirring shaft 4 both extend into the driving box 3, and the driving box 3 drives the shaft sleeve 5 to rotate continuously, and the driving box 3 drives the stirring shaft 4 to rotate intermittently; Since the driving stirring shaft 4 rotates intermittently, the intermittent rotation can make the steel balls 403 have a better grinding effect when grinding solid metal particles. When the stirring shaft rotates intermittently, the steel balls 403 will obtain a large acceleration at the moment of starting to rotate, gather on one side of the reaction chamber and generate a strong impact force. After the rotation ends, the steel balls will continue to move due to inertia, and collide and rub with the stationary stirring plate 402 and the inner wall of the reactor shell 1, so as to grind the solid metal particles more fully. The collision effect generated by this intermittent motion can improve the grinding efficiency, make the particle size distribution of the solid metal particles narrower, and facilitate the reaction. Example 3
[0041] Reference Figure 1-11 The difference between this embodiment and embodiment 2 is that a rotating motor 301 is fixed inside the driving box 3, a first gear 302 is fixed to the output shaft of the rotating motor 301, a second gear 502 is fixed to the outside of the sleeve 5, and the first gear 302 meshes with the second gear 502; When the driving box 3 is turned on, the first gear 302 is meshed with the second gear 502 to drive the shaft sleeve 5 to rotate continuously, thereby driving the propulsion agitator 501 to rotate continuously and push the material forward.
[0042] Among them, one end of the stirring shaft 4 is connected to the third gear 405 through a one-way transmission 404, a hydraulic cylinder 406 is fixed in the driving box 3, the output shaft of the hydraulic cylinder 406 is fixed with a bracket 407, a rack 408 is fixed on the bracket 407, the rack 408 is meshed with the third gear 405, a guide rail 4071 is fixed in the driving box 3, a slider 4072 is fixed on the bracket 407, and the slider 4072 is slidably installed on the guide rail 4071; The one-way transmission 404 includes a transmission housing 4041 and a ratchet 4042, which are rotatably matched. The ratchet 4042 is fixed to the stirring shaft 4, and the transmission housing 4041 is fixed to the third gear 405. The transmission housing 4041 is elastically rotatably installed with multiple ratchets 4043 through torsion springs and pin shafts, which can clamp the ratchet 4042 in one direction. Therefore, when the hydraulic cylinder 406 reciprocates and extends and drives the rack 408 to move back and forth, it can drive the stirring shaft 4 to rotate intermittently in one direction. Example 4
[0043] Reference Figure 1-11 The difference between this embodiment and embodiment 3 is that the premixer 5 includes an annular fixed cover 601 and an annular rotating container 603, the annular rotating container 603 is fixed to the outside of the stirring shaft 4 by a connecting rod 409, and the two sides of the annular rotating container 603 are respectively provided with a first distribution liquid distribution ring pipe 1021 and a second liquid distribution ring pipe 1031, the first distribution liquid distribution ring pipe 1021 and the second liquid distribution ring pipe 1031 are respectively fixed and connected to the first liquid feed port 102 and the second liquid feed port 103, and the first distribution liquid distribution ring pipe 1021 and the second liquid distribution ring pipe 1031 are close to each other. A plurality of first liquid dispensing tubes 1022 and a second liquid dispensing tube 1031 are fixed on the sides thereof, the first liquid dispensing tube 1022 and the second liquid dispensing tube 1031 are fixedly connected to both sides of the annular fixed cover 601, the positions of the first liquid dispensing tube 1022 and the second liquid dispensing tube 1031 correspond one to one, an annular baffle plate 602 is fixed on the inner side of the annular fixed cover 601, mesh holes are provided on the annular baffle plate 602, the bottom end of the solid feed port 101 is fixed and connected to the annular fixed cover 601, and the bottom end of the solid feed port 101 directly passes through the annular baffle plate 602, and a plurality of discharge pipes 605 are provided on one side of the annular rotating container 603 close to the partition plate 401; When adding materials, metal is added through the solid feed port 101, and halogenated alkane and organic solvent are added through the first liquid feed port 102 and the second liquid feed port 103. Different liquids first enter the first liquid distribution ring pipe 1021 and the second liquid distribution ring pipe 1031, and then flow into the annular fixed cover 601 through each first liquid distribution pipe 1022 and the second liquid distribution pipe 1031. Since the positions of the first liquid distribution pipe 1022 and the second liquid distribution pipe 1031 correspond one to one, different liquid raw materials will be offset, thereby performing the first mixing. Then, the initially mixed liquid is blocked by the annular baffle 602 and passes through the annular baffle 603. The blocking and bypass effects of the mesh holes on 02 allow the mixed particles to enter the annular rotating container 603 for the second time, and the solid materials directly enter the annular rotating container 603. Since the annular rotating container 603 is rotating, a plurality of barrier mesh plates 604 are fixed in the annular rotating container 603. As the annular rotating container 603 rotates, the solid particles will fall into the gaps between different barrier mesh plates 604, thereby ensuring that the solid particles are more evenly distributed in the annular rotating container 603 and mixed with the liquid. After mixing, due to the pressure of the liquid, the mixed liquid will be ejected from the discharge pipe 605, thereby achieving an efficient pre-mixing effect and improving the reaction efficiency.
[0044] The discharge pipe 605 is internally rotatably mounted with an extrusion screw 606, one end of which is fixed with a fourth gear 6061, and the first liquid distribution ring pipe 1021 is fixed with a gear ring 1023, and the plurality of fourth gears 6061 are all meshed with the gear ring 1023; When the annular rotating container 603 rotates along with the stirring shaft 4 , the fourth gear 6061 moves along the gear ring 1023 , thereby driving the extrusion screw 606 to rotate, thereby promoting the discharge of materials and preventing the solid materials from clogging the discharge pipe 605 .
[0045] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field. The present invention is mainly used to protect mechanical devices, so the present invention will no longer explain the control method and circuit connection in detail.
[0046] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. A continuous preparation method of an organometallic reagent, characterized in that: In a nitrogen atmosphere, the metal is continuously transported into a dynamic continuous microreactor, and at the same time, halogenated alkanes and organic solvents are continuously introduced for contact reaction to generate an organic metal reagent; The metal is selected from any one of aluminum, magnesium or lithium; The dynamic continuous microreactor comprises a reactor shell (1), a jacket (2) is provided on the outside of the reactor shell (1), and a solid feed inlet (101), a first liquid feed inlet (102) and a second liquid feed inlet (103) are installed on one side of the top end of the reactor shell (1); A premixer (5) is provided on one side of the reactor shell (1) close to the solid feed inlet (101); A stirring shaft (4) is rotatably mounted inside the reactor shell (1), a plurality of partitions (401) are fixed outside the stirring shaft (4), a gap for materials to flow through is left between the partitions (401) and the inner wall of the reactor shell (1), the partitions (401) divide the inside of the reactor shell (1) into a plurality of reaction chambers, steel balls (403) are arranged in the reaction chambers between adjacent partitions (401), and a stirring plate (402) is fixed outside the stirring shaft (4) between adjacent partitions (401), and a plate hole (4021) is opened on the stirring plate (402).
2. The method for continuously preparing an organometallic reagent according to claim 1, characterized in that: The aluminum is aluminum particles or aluminum powder; the magnesium is selected from any one of magnesium bars, magnesium particles or magnesium powder; the lithium is selected from any one of lithium bars, lithium particles or lithium powder.
3. The method for continuously preparing an organometallic reagent according to claim 1, characterized in that: The halogenated alkane is selected from any one of methyl chloride, methyl bromide, ethyl chloride, ethyl bromide, butyl chloride, butyl bromide, 1-chlorohexane, benzyl chloride and cyclopentane bromide.
4. The method for continuously preparing an organometallic reagent according to claim 1, characterized in that: When the metal is aluminum, an initiator is also introduced into the dynamic continuous microreactor, and the initiator is selected from any one of methyl sesquialuminum, iodine, and methyl iodide.
5. The method for continuously preparing an organometallic reagent according to claim 1, characterized in that: When the metal is aluminum, the organic solvent is selected from any one or more of octane, decanane, dodecane, hexadecane and liquid alkanes with a higher carbon content; When the metal is magnesium or lithium, the organic solvent is selected from any one of ethyl ether, propyl ether, isopropyl ether, butyl ether, isobutyl ether, n-pentyl ether, diisopentyl ether, toluene, pentane, hexane, octane, decane, dodecane, hexadecane and tetrahydrofuran.
6. The method for continuously preparing an organometallic reagent according to claim 1, characterized in that: The reaction temperature in the dynamic continuous microreactor is controlled at 20-150°C.
7. The method for continuously preparing an organometallic reagent according to claim 1, characterized in that: A propeller agitator (501) is provided on one side of the reactor shell (1) near the solid feed port (101), and the propeller agitator (501) is fixedly mounted on the outside of a shaft sleeve (5), and the shaft sleeve (5) is rotatably sleeved on the outside of the agitator shaft (4).
8. The method for continuously preparing an organometallic reagent according to claim 7, characterized in that: A drive box (3) is fixed to the outside of the reactor shell (1); one end of the shaft sleeve (5) and the stirring shaft (4) both extend into the drive box (3); the drive box (3) drives the shaft sleeve (5) to rotate continuously, and the drive box (3) drives the stirring shaft (4) to rotate intermittently.
9. The method for continuously preparing an organometallic reagent according to claim 8, characterized in that: A rotating motor (301) is fixed inside the driving box (3), a first gear (302) is fixed to the output shaft of the rotating motor (301), a second gear (502) is fixed to the outside of the shaft sleeve (5), and the first gear (302) is meshed with the second gear (502).
10. The method for continuously preparing an organometallic reagent according to claim 7, characterized in that: One end of the stirring shaft (4) is connected to a third gear (405) via a one-way transmission (404); a hydraulic cylinder (406) is fixed in the driving box (3); a bracket (407) is fixed to the output shaft of the hydraulic cylinder (406); a rack (408) is fixed to the bracket (407); and the rack (408) is meshed with the third gear (405).