Reaction device for preparing lithium bis(trimethylsilyl)amide

Abstract

A reaction device for preparing lithium bis(trimethylsilyl)amide, comprising a placement table (1), a reaction kettle (2) being fixedly connected to the middle portion of the placement table (1) by means of side supports distributed in an array, and a stirring device (3) being provided at the middle portion of the top end of the reaction kettle (2). A liquid dropping assembly (4) and a feeding pipe (10) are separately provided at eccentric positions of the top end of the reaction kettle (2). The bottom portion of the reaction kettle (2) is connected to a filter cylinder (12) by means of a discharge pipe, a liquid transfer filter assembly (8) is provided inside the filter cylinder (12), and, by means of a liquid transfer pipe (13), the liquid transfer filter assembly (8) is connected to a liquid discharge assembly (5) provided at the bottom portion of the placement table. The reaction device for preparing lithium bis(trimethylsilyl)amide can perform liquid dropping adding operation for a mixed liquid in the kettle, and allows the liquid dropping rate to be regulated according to actual requirements; moreover, a liquid beating frame is used to perform high-speed beating on the dropping added liquid, such that the liquid drops fall in a scattered manner into the mixed liquid, thereby improving the contact effect between the added liquid and the mixed liquid, and accelerating a reaction process.

Description

A reaction device for preparing lithium bis(trimethylsilyl)amide Technical Field

[0001] The present invention relates to the technical field of chemical production, in particular to a reaction device for preparing bis(trimethylsilyl)lithium amide. Background Art

[0002] Lithium bis(trimethylsilyl)amide is a chemical substance and an important organolithium reagent. It has the advantages of low toxicity, high reactivity, and easy operation. It is widely used in the field of organic synthesis. It appears as white crystals or crystalline powder and can be dissolved in organic solvents such as ether, chloroform, and tetrahydrofuran, but is insoluble in water.

[0003] The Chinese patent application number CN202210736409.4 discloses a process for preparing lithium bis(trimethylsilyl)amide. Under an inert atmosphere, hexamethyldisilazane, tetrahydrofuran and metallic lithium are added to a reaction flask, and a mixture of styrene and tetrahydrofuran is added dropwise to react to generate lithium bis(trimethylsilyl)amide. In the reaction process, the use of metallic lithium ingots to replace metallic lithium particles greatly reduces production costs and reduces the introduction of unnecessary impurities. Moreover, since the surface area of ​​metallic lithium ingots of equal mass in contact with the external atmosphere is much smaller than that of metallic lithium particles, the side reactions caused by the contact of metallic lithium with the external atmosphere can be greatly reduced, thereby improving the purity of the product.

[0004] Although the above-mentioned document can greatly reduce the side reactions caused by the contact between metallic lithium and the external atmosphere and improve the purity of the product, in the process of preparing lithium bis(trimethylsilyl)amide, it is necessary to drip and add unsaturated conjugated olefin electron carriers to the mixed liquid in the preparation container. However, the current dripping device has a simple structure and only has a simple dripping function. After the added liquid falls, it directly contacts the mixed liquid. The local reaction rate does not meet the requirements, and the added droplets cannot react completely, resulting in precipitation. Summary of the Invention

[0005] The present invention discloses a reaction device for preparing lithium bis(trimethylsilyl)amide, which aims to solve the technical problem in the background art that the added liquid directly contacts the mixed liquid after falling, the local reaction rate does not meet the requirement, the added liquid droplets cannot react completely, and precipitation occurs.

[0006] The present invention proposes a reaction device for preparing lithium bis(trimethylsilyl)amide, comprising a placement table, the middle portion of which is fixedly connected to a reactor via an array of side supports, and a stirring device is provided at the middle portion of the top of the reactor. A drip assembly and a feeding pipe are provided at eccentric positions at the top of the reactor. The bottom of the reactor is connected to a filter cartridge via a discharge pipe, and a liquid transfer filter assembly is provided inside the filter cartridge. The liquid transfer filter assembly is connected to a liquid discharge assembly provided at the bottom of the placement table via a liquid transfer pipe.

[0007] The cam is connected to the first supporting plate and the second supporting plate is connected to the supporting plate by the cam, and the cam is connected to the first supporting plate by the cam.

[0008] Preferably, the liquid pumping assembly includes a first pressure plate fixedly connected to the bottom of the movable column and a second pressure plate fixedly connected to the top of the rotating column. A hollow expansion piece is provided between the first pressure plate and the second pressure plate. The top of the hollow expansion piece is connected to the first hard connecting tube fixedly connected to the movable column through a first through groove, and the bottom of the hollow expansion piece is connected to the second hard connecting tube fixedly connected to the rotating column through a second through groove.

[0009] A first electromagnetic valve is provided inside the first through groove, and a second electromagnetic valve is provided inside the second through groove.

[0010] Preferably, the hollow expansion member includes a corrugated portion fixedly connected to the first pressing plate and the second pressing plate, expansion portions are provided at both ends of the corrugated portion, and flexible convex strips distributed in an array are provided on the surface of the expansion portion.

[0011] Preferably, the telescopic assembly includes a first disc rotatably connected to the top of the reactor, the bottom of the first disc is fixedly connected to an electric push rod, and the telescopic end of the electric push rod is fixedly connected to a second disc fixedly connected to the top of the movable column.

[0012] Preferably, the interior of the diverter plate is provided with an annular cone portion, the middle portion and the outer periphery of the diverter plate are both provided with mesh plates, and the diverter plate is connected to the bottom of the reactor through the mesh plates.

[0013] Preferably, the dripping assembly includes a liquid adding cylinder arranged on the top of the reactor, a liquid dropping tube penetrating into the interior of the reactor is provided at the bottom of the liquid adding cylinder, a splash guard is provided at the bottom of the liquid dropping tube, a liquid beating rack is provided below the splash guard, and the liquid beating rack is fixedly connected to the output shaft of the dispersion motor arranged on the side wall of the reactor.

[0014] The anti-splash plate is provided with a photoelectric sensor for detecting the number of liquid droplets splashed on the anti-splash plate.

[0015] Preferably, the end of the first hard connecting tube away from the liquid pumping component is directed toward the bottom of the splash plate.

[0016] Preferably, the liquid transfer and filtration assembly includes a central seat arranged on the filter cylinder, a liquid expansion tube connected to the liquid transfer tube is provided inside the central seat, a driving motor is fixedly connected to the outside of the central seat, the output end of the driving motor passes through the inner cavity of the liquid expansion tube and is movably connected to the inner wall of the other side of the central seat, and a cam is fixedly connected to the outside of the output end of the driving motor, and the cam is located in the inner cavity of the liquid transfer tube.

[0017] Preferably, the bottom of the expansion tube is fixedly connected to an expansion tube, the interior of the expansion tube is movably connected to a filter box, the interior of the filter box is provided with a double-layer filter screen, the top of the filter box is fixedly connected to a plurality of circumferentially equidistant return springs, the other end of the return spring is fixedly connected to the top inner wall of the expansion tube, the upper side of the filter box is fixedly connected to a main shaft, the top end of the main shaft is fixedly connected to a contact, and the contact is in contact with a cam.

[0018] Preferably, the drainage assembly includes a liquid pump arranged on the side of the filter cartridge, a liquid suction pipe is fixedly connected to the top of the liquid pump, the liquid suction pipe is fixedly connected to the liquid transfer pipe, and a drainage pipe is provided on the side of the liquid pump.

[0019] Technical effects and advantages of the present invention:

[0020] 1. The present invention provides a reaction apparatus for preparing lithium bis(trimethylsilyl)amide, which is capable of performing a dropwise addition operation on a mixed liquid in a kettle. The dropwise addition rate can be adjusted according to actual needs. At the same time, a liquid beating rod is used to strike the dripping added liquid at high speed, causing the droplets to scatter and fall into the mixed liquid, thereby improving the contact effect between the added liquid and the mixed liquid and accelerating the reaction process.

[0021] 2. The present invention provides a hollow expansion member and a diverter plate so that the dispersed n-butyl lithium solution can be evenly distributed on the diverter plate. At the same time, by contacting tetrahydrofuran and hexamethyldisilazane with the n-butyl lithium solution in advance, on the one hand, it avoids the droplets from being large or concentrated together during the dripping process, causing uneven reaction or regional reaction, which affects the reaction effect; on the other hand, it avoids the generation of violent splashing or bubble formation when the n-butyl lithium solution is dripped into the reactor.

[0022] 3. The present invention sets a hollow expansion piece and a photoelectric sensor for detection. When the control system detects that the deformation of the hollow expansion piece is too small, the photoelectric sensor set on the splash guard detects the number of droplets adhering to the splash guard. If the number of droplets is greater than the set value, the electric push rod is controlled to reciprocate and extend, and the frequency of the reciprocating extension and contraction is increased, so that the basic solution can be sprayed out from the top of the first hard connecting tube to rinse the droplets adhering to the splash guard. After rinsing, the basic solution falls on the diverter plate and flows to the bottom of the reactor through the diverter plate, so that the droplets adhering to the splash guard can be fully mixed with the basic solution at the bottom of the reactor. If the number of droplets is less than the set value, the control system controls the electric push rod to extend, controls the first through slot and the first hard tube to be in a non-connected state, and controls the second through slot and the second hard tube to be in a non-connected state. When the electric push rod extends, the first pressure plate squeezes the hollow expansion piece, so that the corrugated part of the hollow expansion piece is compressed and folded, and the expansion part of the hollow expansion piece is compressed and expanded, and finally the middle part of the hollow expansion piece becomes narrower and the two ends become larger, forming a shape similar to a dumbbell. As the rotating column rotates, the expansion part of the hollow expansion piece synchronously stirs the basic solution in the reactor to improve the mixing degree of the basic solution and the added solution. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] FIG1 is a schematic diagram of the main structure of the present invention.

[0024] FIG2 is a schematic diagram of the cross-sectional structure of the reactor of the present invention.

[0025] FIG3 is an enlarged view of point A in FIG2 of the present invention.

[0026] FIG4 is an enlarged view of point B in FIG2 of the present invention.

[0027] FIG5 is a schematic structural diagram of the diverter plate of the present invention.

[0028] FIG6 is a schematic structural diagram of the hollow expansion member of the present invention.

[0029] FIG7 is a schematic structural diagram of the hollow expansion member of the present invention after being squeezed.

[0030] FIG8 is a schematic structural diagram of the filter cartridge of the present invention.

[0031] FIG9 is a schematic diagram of the internal structure of the filter cartridge of the present invention.

[0032] FIG10 is a schematic structural diagram of the liquid transfer and filtration assembly of the present invention.

[0033] In the figure: 1. Placement table; 2. Reactor; 3. Stirring device; 301. Mixing motor; 302. First prism; 303. Movable column; 304. First prism groove; 305. Diverter plate; 306. First rigid connecting pipe; 307. Second prism; 308. Rotating column; 309. Second prism groove; 310. Second rigid connecting pipe; 311. Leakage trough; 4. Dropping assembly; 401. Liquid adding cylinder; 402. Dropping pipe; 403. Splash guard; 404. Liquid mixing stand; 405. Dispersion motor; 5. Drainage assembly; 501. Liquid pump; 502. Suction pipe; 503. Drainage pipe; 6. Telescopic assembly; 601. First disc; 602. Electric push rod; 603, second disc; 7, liquid extraction assembly; 701, first pressure plate; 702, second pressure plate; 703, hollow expansion member; 704, first through groove; 705, second through groove; 7031, corrugated portion; 7032, expansion portion; 7033, flexible ridge; 8, liquid transfer and filtration assembly; 801, center seat; 802, liquid expansion pipe; 803, drive motor; 804, cam; 805, expansion pipe; 806, filter box; 807, double-layer filter screen; 808, return spring; 809, main shaft; 810, contact; 9, side support; 10, feeding pipe; 11, discharge pipe; 12, filter cartridge; 13, liquid transfer pipe; 14, annular cone; 15, mesh plate. Implementation Method

[0034] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Example

[0035] 1 to 10 , a reaction apparatus for preparing lithium bis(trimethylsilyl)amide comprises a placement table 1, a reactor 2 being fixedly connected to the middle of the placement table 1 via an array of side supports 9, a stirring device 3 being provided at the middle of the top of the reactor 2; a drip assembly 4 and a feeding pipe 10 being provided at eccentric positions at the top of the reactor 2; a filter cartridge 12 being connected to the bottom of the reactor 2 via a discharge pipe 11, a liquid transfer filter assembly 8 being provided inside the filter cartridge 12, and the liquid transfer filter assembly 8 being connected to a drain assembly 5 provided at the bottom of the placement table 1 via a liquid transfer pipe 13;

[0036] Specifically, before the reaction, the raw materials are added into the reactor 2 through the feeding pipe 10 . During the reaction, the control system controls the stirring device 3 to mix and stir the raw materials in the reactor 2 .

[0037] An observation window is provided on the filter cartridge 12. After the reaction is completed, the prepared solution enters the filter cartridge 12 from the discharge pipe 11 (a control valve is provided on the discharge pipe 11). The filter cartridge 12 serves as a transfer device for the discharge of the prepared liquid and can be disassembled to facilitate cleaning when excessive sediment accumulates inside. The observation window is made of corrosion-resistant tempered glass, which can observe the situation inside the filter cartridge 12 in real time.

[0038] Specifically, the dripping assembly 4 includes a liquid adding cylinder 401 arranged on the top of the reactor 2, a liquid dropping tube 402 penetrating into the interior of the reactor 2 is provided at the bottom of the liquid adding cylinder 401, a splash plate 403 is provided at the bottom of the liquid dropping tube 402, and a liquid beating rack 404 is provided below the splash plate 403. The liquid beating rack 404 is fixedly connected to the output shaft of the dispersion motor 405 arranged on the side wall of the reactor 2.

[0039] During specific use, when dripping liquid into the reactor 2, the dropper 402 drops the added liquid in the liquid adding cylinder 401 into the reactor 2 (the liquid adding cylinder 401 is provided with a control valve, which can adjust the dripping speed of the dropper 402). When the dispersion motor 405 is in working state, it drives the liquid beating rack 404 to rotate, and the liquid beating rack 404 breaks up the dripping added liquid and disperses it to fall.

[0040] In a specific application scenario, the dripping component 4 is suitable for the step of adding additive liquid to the mixed liquid during the reaction process, that is, the dripping component 4 can perform a dripping and adding operation on the mixed liquid in the reactor 2, and the dripping rate can be adjusted according to actual needs. At the same time, the liquid beating rack 404 is used to hit the dripping additive liquid at high speed, so that the droplets fly into the mixed liquid, thereby improving the contact effect between the additive liquid and the mixed liquid and accelerating the reaction process; the splash plate 403 can block the scattered additive liquid from the top to prevent the additive liquid from splashing and adhering to the inner wall of the reactor 2 after being scattered.

[0041] Specifically, the bottom of the expansion tube 802 is fixedly connected to the expansion tube 805, the interior of the expansion tube 805 is movably connected to the filter box 806, the interior of the filter box 806 is provided with a double-layer filter screen 807, the top of the filter box 806 is fixedly connected to a plurality of circumferentially equidistant return springs 808, the other end of the return spring 808 is fixedly connected to the top inner wall of the expansion tube 805, the upper side of the filter box 806 is fixedly connected to the main shaft 809, the top of the main shaft 809 is fixedly connected to the contact 810, and the contact 810 is in contact with the cam 804.

[0042] Specifically, after the prepared liquid completes the transfer in the filter cartridge 12, the solution will be discharged through the transfer tube 13. During this process, the drive motor 803 is started to drive the cam 804 to rotate, and the cam 804 rotates to push the contact 810 (under the elastic force of the return spring 808, the contact 810 is always in contact with the cam 804). The filter box 806 is in a high-frequency vibration state under the elastic force of the return spring 808. The solution enters the transfer tube 13 through the double-layer filter mesh 807, and the solid precipitation remains in the filter cartridge 12.

[0043] In a specific application scenario, the liquid transfer and filtration component 8 is suitable for the solid-liquid separation operation of the solution in the filter cartridge 12, that is, the liquid transfer and filtration component 8 can be used to separate the solid and liquid of the solution in the filter cartridge 12, and the prepared solution is discharged from the liquid transfer tube 13 for collection, while the solid precipitate remains in the filter cartridge 12 for subsequent centralized treatment; the drive motor 803 is used to drive the filter box 806 to vibrate at high frequency, which can avoid the occurrence of solid precipitates adhering to the filter net while filtering the double-layer filter net 807, thereby affecting the filtration effect.

[0044] Specifically, the drainage component 5 includes a liquid pump 501 arranged on the side of the filter cylinder 12, a liquid suction pipe 502 is fixedly connected to the top of the liquid pump 501, the liquid suction pipe 502 is fixedly connected to the liquid transfer pipe 13, and a drainage pipe 503 is provided on the side of the liquid pump 501.

[0045] Specifically, when the transfer tube 13 is discharging liquid, the liquid pump 501 works and applies suction to the transfer tube 13 through the suction tube 502. The solution in the filter cartridge 12 is sucked into the transfer tube 13, and the solution entering the suction tube 502 will be discharged from the discharge tube 503 for collection; the liquid pump 501 applies power to the transfer tube 13 to assist it in performing the liquid transfer and discharge operation.

[0046] During use, before the reaction, the raw materials are added to the reactor 2 from the feeding tube 10. During the reaction, the raw materials in the reactor 2 are mixed and stirred by controlling the stirring device 3. When the liquid is dripped into the reactor 2, the dropper 402 drops the additive liquid in the liquid adding cylinder 401 into the reactor 2 (the liquid adding cylinder 401 is provided with a control valve, which can adjust the dripping speed of the dropper 402). The dispersion motor 405 is in working state, driving the liquid beating rack 404 to rotate, and the liquid beating rack 404 breaks up the dripping additive liquid and disperses it to fall.

[0047] After the reaction is completed, the prepared solution enters the filter cartridge 12 from the discharge pipe 11 (a control valve is provided on the discharge pipe 11). After the prepared solution completes the transfer in the filter cartridge 12, the solution will be discharged through the transfer pipe 13. During this process, the drive motor 803 starts to drive the cam 804 to rotate, and the cam 804 rotates to push the contact 810 (under the elastic force of the return spring 808, the contact 810 is always in contact with the cam 804). The filter box 806 is in a high-frequency vibration state under the elastic force of the return spring 808. The solution passes through the double-layer filter mesh 807 and enters the transfer pipe 13, and the solid precipitate remains in the filter cartridge 12. When the transfer pipe 13 is draining, the liquid pump 501 works to apply suction to the transfer pipe 13 through the suction pipe 502. The solution in the filter cartridge 12 is sucked into the transfer pipe 13, and the solution entering the suction pipe 502 will be discharged from the discharge pipe 503 for collection. Example

[0048] While the above embodiment can somewhat alleviate the distribution of droplets in the solution, the dripping rate and droplet size must be controlled within a certain range during the dripping operation to avoid safety issues or unsatisfactory reaction effects caused by excessive or insufficient pressure fluctuations. Furthermore, the dripping assembly 4 must be adjusted accordingly based on the pressure fluctuations within the reactor 2. Furthermore, when the droplets are dripped into the reactor 2, violent splashing or bubble formation should be avoided to ensure smooth operation. In view of this, the technical solution based on Example 1 has been modified as follows.

[0049] 1 to 10 , a reaction apparatus for preparing lithium bis(trimethylsilyl)amide comprises a placement table 1, the middle portion of the placement table 1 is fixedly connected to a reactor 2 via an array of side supports 9, a stirring device 3 is provided at the middle portion of the top of the reactor 2; a drip assembly 4 and a feeding pipe 10 are provided at eccentric positions at the top of the reactor 2; a filter cartridge 12 is connected to the bottom of the reactor 2 via a discharge pipe 11, a liquid transfer filter assembly 8 is provided inside the filter cartridge 12, and the liquid transfer filter assembly 8 is connected to a discharge assembly 5 provided at the bottom of the placement table 1 via a liquid transfer pipe 13.

[0050] The stirring device 3 includes a mixing motor 301 arranged at the top of the reactor 2. The output shaft of the mixing motor 301 penetrates into the interior of the reactor 2 and is fixedly connected to a first prism 302. The first prism 302 is axially slidably connected to a movable column 303 arranged inside the reactor 2. A first prism groove 304 is provided inside the movable column 303 and is slidably connected to the first prism 302. The top of the movable column 303 is rotatably connected to the inner top of the reactor 2 through a telescopic component 6. A diverter plate 305 for carrying droplets is provided in the middle of the movable column 303. The diverter plate 305 is provided with a first hard connecting pipe 3 distributed in an array. 06. One end of the first hard connecting tube 306 away from the diversion plate 305 is connected to the liquid pumping component 7 arranged at the bottom of the movable column 303. The interior of the liquid pumping component 7 is provided with a second prism 307 fixedly connected to the movable column 303. The second prism 307 is axially slidably connected to the rotating column 308 arranged inside the reactor 2. A second prism groove 309 slidably connected to the second prism 307 is provided inside the rotating column 308. The middle part of the rotating column 308 is fixedly connected with a second hard connecting tube 310 distributed in an array. The bottom circumference of the rotating column 308 is provided with a leakage groove 311 connected to the discharge pipe 11.

[0051] Specifically, the liquid pumping component 7 includes a first pressure plate 701 fixedly connected to the bottom of the movable column 303 and a second pressure plate 702 fixedly connected to the top of the rotating column 308. A hollow expansion piece 703 is provided between the first pressure plate 701 and the second pressure plate 702. The top of the hollow expansion piece 703 is connected to the first hard connecting tube 306 fixedly connected to the movable column 303 through the first through groove 704, and the bottom of the hollow expansion piece 703 is connected to the second hard connecting tube 310 fixedly connected to the rotating column 308 through the second through groove 705.

[0052] A first solenoid valve is disposed inside the first through groove 704 , and a second solenoid valve is disposed inside the second through groove 705 .

[0053] Specifically, the hollow expansion member 703 includes a corrugated portion 7031 fixedly connected to the first pressing plate 701 and the second pressing plate 702 , an expansion portion 7032 is provided at both ends of the corrugated portion 7031 , and a surface of the expansion portion 7032 is provided with flexible ridges 7033 distributed in an array.

[0054] Specifically, the telescopic assembly 6 includes a first disc 601 rotatably connected to the top of the reactor 2, an electric push rod 602 is fixedly connected to the bottom of the first disc 601, and the telescopic end of the electric push rod 602 is fixedly connected to the second disc 603 fixedly connected to the top of the movable column 303.

[0055] Specifically, the interior of the diverter plate 305 is provided with an annular cone 14 , the middle portion and the outer periphery of the diverter plate 305 are both provided with mesh plates 15 , and the diverter plate 305 is connected to the bottom of the reactor 2 through the mesh plates 15 .

[0056] Specifically, the dripping assembly 4 includes a liquid adding cylinder 401 arranged on the top of the reactor 2, a liquid dropping tube 402 penetrating into the interior of the reactor 2 is provided at the bottom of the liquid adding cylinder 401, a splash plate 403 is provided at the bottom of the liquid dropping tube 402, and a liquid beating rack 404 is provided below the splash plate 403. The liquid beating rack 404 is fixedly connected to the output shaft of the dispersion motor 405 arranged on the side wall of the reactor 2.

[0057] The anti-splash plate 403 is provided with a photoelectric sensor for detecting the number of liquid droplets splashed on the anti-splash plate 403 .

[0058] Specifically, one end of the first hard connecting tube 306 away from the liquid pumping assembly 7 faces the bottom of the splash plate 403 .

[0059] Lithium bis(trimethylsilyl)amide is also known as lithium hexamethyldisilazide. The preparation method of lithium hexamethyldisilazide is generally as follows: in a crystallized and dried reactor 2, replace the reactor 2 with argon, add tetrahydrofuran and hexamethyldisilazane (hereinafter collectively referred to as the basic solution) to the reactor 2 through an overhead tank, reduce the temperature to -15°C ± 5°C, maintain this temperature, open the control valve in the dropper 402, and add n-butyllithium solution dropwise (hereinafter collectively referred to as the added solution after contact), raise the temperature to 10°C after the addition is completed, and maintain the temperature for 1 hour to obtain the lithium hexamethyldisilazide solution.

[0060] The first rigid connecting tube is connected to the hollow expansion member 703 via the first through slot 704 , and the second rigid connecting tube is connected to the hollow expansion member 703 via the second through slot 705 . A pressure sensor for detecting the deformation of the hollow expansion member 703 is provided on the hollow expansion member 703 .

[0061] In the initial state, the first solenoid valve inside the first through groove 704 is in a closed state (i.e., the first through groove 704 and the first hard connecting tube 306 are in a connected state), and the second solenoid valve inside the second through groove 705 is in an open state (i.e., the second through groove 705 and the second hard connecting tube 310 are in a non-connected state); the electric push rod 602 is in a contracted state; and there is no liquid inside the hollow expansion member 703.

[0062] During use, the basic solution is first added to the interior of the reactor 2 through the feeding tube 10. After entering the reactor 2, the basic solution flows to the bottom of the reactor 2 through the mesh plate 15 on the diverter disk 305, and finally makes the basic solution flush with the top of the second pressure plate 702 in the reactor 2. Then the control system controls the mixing motor 301 to operate. During the operation of the mixing motor 301, the output shaft of the mixing motor 301 drives the movable column 303 to rotate through the first prism 302. Since the top of the movable column 303 is fixedly connected to the first disc 601 through the electric push rod 602, and the first disc 601 is rotatably connected to the inner top of the reactor 2, when the first prism 302 drives the movable column 303 to rotate, the movable column 303 is clamped by the electric push rod 602 and will not fall down.

[0063] During the rotation of the movable column 303, the middle part of the movable column 303 synchronously drives the diverter plate 305 to rotate through the first hard connecting tube 306, and the bottom of the movable column 303 synchronously drives the rotating column 308 to rotate through the cooperation of the second prism 307 and the second prism groove 309. The rotating column 308 drives the second hard connecting tube 310 to rotate, and the rotating second hard connecting tube 310 stirs the solution inside the reactor 2.

[0064] While the second hard connecting tube 310 is stirring the basic solution in the reactor 2, the liquid adding cylinder 401 drips the added solution into the reactor 2 through the dripping tube 402. The speed and time of dripping the added solution are controlled by the control system (that is, within unit time, the control system controls the range of opening of the control valve provided on the dripping tube 402, thereby controlling the dripping speed of the dripping tube 402). During the process of dripping the added solution, the control system controls the dispersion motor 405 to drive the liquid beating rack 404 to rotate, and the liquid beating rack 404 breaks up the droplets of the added solution. As shown in Figure 2, the diverter plate 305 is located below the liquid beating rack 404, and the diverter plate 305 is constantly rotating under the influence of the mixing motor 301, so that the droplets of the added solution will fall evenly on the surface of the annular cone 14 on the diverter plate 305 after being broken up by the liquid beating rack 404.

[0065] After a drop of added solution drips from the dropper 402, the control system controls the electric push rod 602 to extend, so that the telescopic end of the electric push rod 602 squeezes the movable column 303 downward through the second disc 603, and the first pressure plate 701 on the movable column 303 squeezes the hollow expansion member 703 on the second pressure plate 702, so that the air inside the hollow expansion member 703 is discharged along the first through groove 704 and the first hard connecting tube 306, and then controls the first solenoid valve inside the first through groove 704 to open (that is, the first through groove 704 and the first hard connecting tube 306 are in a non-connected state), and the second solenoid valve inside the second through groove 705 to close (that is, the second through groove 705 and the second hard connecting tube 310 are in a connected state), and controls the electric push rod 602 to contract, and the electric push rod 602 drives the hollow expansion member 703 to extend through the first pressure plate 701, so that negative pressure is generated inside the hollow expansion member 703, and the hollow expansion member 703 is in a non-connected state. 310 , and the hollow expansion member 703 is connected to the first through-groove 704 by the first solenoid valve 602.

[0066] The basic solution squeezed above the diverter disk 305 comes into contact with the additive solution distributed on the annular cone 14 in advance (after the basic solution and the additive solution come into contact, a reactant solution is generated). Under the influence of the annular cone 14, the reactant solution moves toward the circumference of the diverter disk 305 and the middle of the diverter disk 305 respectively, and flows to the basic solution at the bottom of the reactor 2 through the mesh plates 15 provided on the circumference and middle of the diverter disk 305. The reactant solution flowing out of the mesh plates 15 provided on the circumference of the diverter disk 305 flows along the inner wall of the reactor 2 to the circumference of the inner bottom of the reactor 2. The reactant solution flowing out of the mesh plates 15 provided in the middle of the diverter disk 305 flows along the outer walls of the movable column 303 and the rotating column 308 to the middle of the inner bottom of the reactor 2. As the mixing motor 301 continues to operate, the reactant solution falling in the middle and circumference of the inner bottom of the reactor 2 is fully mixed with the basic solution inside the reactor 2. By providing the hollow expansion member 703 and the diverter plate 305, the dispersed n-butyl lithium solution can be evenly distributed on the diverter plate 305. At the same time, by bringing tetrahydrofuran and hexamethyldisilazane into contact with the n-butyl lithium solution in advance, on the one hand, it is avoided that the droplets during the dripping process are large or concentrated together, resulting in uneven reaction or regional reaction, which affects the reaction effect; on the other hand, it is avoided that the n-butyl lithium solution is splashed violently or bubbles are formed when it is dripped into the reactor 2.

[0067] After the basic solution and the additive solution are mixed, an exothermic reaction will occur, causing the internal pressure in the reactor 2 to gradually increase. After the basic solution inside the hollow expansion member 703 is squeezed to the top of the diverter disk 305, the electric push rod 602 drives the hollow expansion member 703 to return to its initial state through the first pressure plate 701. At this time, the increased internal pressure in the reactor 2 will gradually squeeze the hollow expansion member 703, causing it to deform. Therefore, the control system can detect the internal pressure of the reactor 2 through the pressure sensor provided inside the hollow expansion member 703 before the next drop of additive solution drips; the greater the internal pressure in the reactor 2, the greater the deformation of the hollow expansion member 703, and the smaller the internal pressure in the reactor 2, the smaller the deformation of the hollow expansion member 703.

[0068] When the control system detects that the deformation of the hollow expansion member 703 is too large during this time period, it indicates that the exothermic reaction generated after the basic solution and the additive solution are mixed in the reactor 2 is too large, that is, the content of the additive solution in the basic solution is too much. At this time, the control system controls the opening range of the control valve set on the drip tube 402, and the opening range of the control valve becomes smaller, thereby controlling the size and speed of the droplets dripping from the drip tube 402, thereby avoiding excessive mixing of the basic solution and the additive solution in the reactor 2, thereby avoiding safety problems caused by excessive pressure changes or unsatisfactory reaction effects.

[0069] When the control system detects that the deformation of the hollow expansion member 703 is too small during this time period, it indicates that the exothermic reaction generated after the basic solution and the added solution are mixed in the reactor 2 is too small, that is, the content of the added solution in the basic solution is too little. Since the amount of the added solution dripping into the basic solution is controlled by the control valve in the dripping pipe 402 controlled by the control system, that is, the amount of the added solution dripping into the basic solution will not be a problem, there are only two possibilities. The first possibility is that the dispersion motor 405 drives the liquid-beating rack 404 to disperse the droplets of the added solution. When the liquid droplets are dispersed, too much of them splash onto the anti-splash plate 403, so that only a small part of the droplets pass through the diverter plate 305 to mix with the basic solution at the bottom of the reactor 2; the second situation is that the droplets smoothly pass through the liquid-beating rack 404 and fall onto the diverter plate 305, so that when the droplets mix with the basic solution at the bottom of the reactor 2, only a local reaction occurs, and the added droplets cannot react completely; at this time, the photoelectric sensor set on the anti-splash plate 403 detects the number of droplets attached to the anti-splash plate 403. If the number of droplets is greater than the set value, it indicates that this situation is the first situation. In this case, the control system controls the electric push rod 602 to reciprocate and extend. During the reciprocating extension and retraction process of the electric push rod 602, the first solenoid valve in the first slot 704 and the second solenoid valve in the second slot 705 are switched on and off alternately, so that the basic solution at the bottom of the reactor 2 is continuously pumped toward the diverter plate 305. By increasing the reciprocating extension and retraction frequency of the electric push rod 602, the basic solution at the bottom of the reactor 2 is ejected from the top of the first hard connecting pipe 306. At the same time, since the first hard connecting pipe 306 is away from the liquid extraction group One end of each component 7 is directed toward the bottom of the splash plate 403, so that the basic solution sprayed from the first hard connecting tube 306 can rinse the droplets adhering to the splash plate 403. After rinsing, the basic solution falls on the diverter plate 305 and moves toward the circumferential side of the diverter plate 305 and the middle of the diverter plate 305 through the annular cone portion 14 on the diverter plate 305, and finally flows to the bottom of the reactor 2 through the mesh plate 15 on the diverter plate 305, so that the droplets adhering to the splash plate 403 can be fully mixed with the basic solution at the bottom of the reactor 2.

[0070] If the number of droplets is less than the set value, it indicates that this situation is the second situation. At this time, the control system controls the electric push rod 602 to extend, and at the same time controls the first solenoid valve in the first through groove 704 and the second solenoid valve in the second through groove 705 to start at the same time, so that the first through groove 704 and the first hard tube are in a non-connected state, and the second through groove 705 and the second hard tube are in a non-connected state, so that the hollow expansion part 7032 at this time is similar to an airbag.

[0071] As the electric push rod 602 extends, the first pressure plate 701 on the movable column 303 squeezes the hollow expansion member 703, causing the corrugated portion 7031 of the hollow expansion member 703 to fold under pressure (a limit block is provided on the outside of the corrugated portion 7031 for limiting the expansion of the corrugated portion 7031. The limit block limits the corrugated portion 7031 so that it can only fold and cannot expand when the first pressure plate 701 squeezes the hollow expansion member 703). The expansion portion 7032 of the hollow expansion member 703 is compressed and expanded, and finally the hollow expansion member 703 is compressed and expanded. The middle part of the hollow expansion member 703 becomes narrower and the two ends become larger, forming a shape similar to a dumbbell (as shown in Figure 10). Since the expansion part 7032 is provided with an array of flexible ridges 7033, and the basic solution is flush with the top of the second pressure plate 702 in the reactor 2, when the mixing motor 301 rotates, the expansion part 7032 of the hollow expansion member 703 synchronously stirs the basic solution in the reactor 2 through the flexible ridges 7033, thereby improving the stirring effect and enhancing the mixing degree of the basic solution and the added solution.

[0072] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A reaction device for preparing bis(trimethylsilyl) lithium amide, comprising a placement table, characterized in that: The middle part of the placing table is fixedly connected with a reactor through an array of side supports, and a stirring device is provided in the middle of the top of the reactor; a drip assembly and a feeding pipe are respectively provided at the eccentric position of the top of the reactor; the bottom of the reactor is connected with a filter cartridge through a feed pipe, and a liquid transfer filter assembly is provided inside the filter cartridge, and the liquid transfer filter assembly is connected to a liquid discharge assembly provided at the bottom of the placing table through a liquid transfer pipe; The stirring device includes a mixing motor arranged at the top of the reactor, the output shaft of the mixing motor penetrates into the reactor and is fixedly connected to the first prism, the first prism is axially slidably connected to a movable column arranged inside the reactor, a first prism groove is provided in the movable column and is slidably connected to the first prism, the top of the movable column is rotatably connected to the inner top of the reactor through a telescopic component, the middle part of the movable column is provided with a diverter plate for carrying droplets, the diverter plate is provided with a first hard connecting pipe distributed in an array, the first hard connecting pipe is connected to a liquid pumping component arranged at the bottom of the movable column at one end away from the diverter plate, the liquid pumping component is provided with a second prism fixedly connected to the movable column, the second prism is axially slidably connected to a rotating column arranged inside the reactor, a second prism groove is provided in the rotating column and is slidably connected to the second prism, the middle part of the rotating column is fixedly connected to a second hard connecting pipe distributed in an array, and a leakage groove connected to the discharge pipe is provided on the bottom circumferential side of the rotating column.

2. A reaction device for preparing bis(trimethylsilyl)lithium amide according to claim 1, characterized in that: The liquid pumping assembly includes a first pressing plate fixedly connected to the bottom of the movable column and a second pressing plate fixedly connected to the top of the rotating column, a hollow expansion piece is provided between the first pressing plate and the second pressing plate, the top of the hollow expansion piece is connected to the first hard connecting pipe fixedly connected to the movable column through a first through groove, and the bottom of the hollow expansion piece is connected to the second hard connecting pipe fixedly connected to the rotating column through a second through groove; A first electromagnetic valve is disposed inside the first through groove, and a second electromagnetic valve is disposed inside the second through groove.

3. A reaction device for preparing bis(trimethylsilyl)lithium amide according to claim 2, characterized in that: The hollow expansion member comprises a corrugated portion fixedly connected to the first pressing plate and the second pressing plate, expansion portions are arranged at both ends of the corrugated portion, and flexible convex strips distributed in an array are arranged on the surface of the expansion portion.

4. A reaction device for preparing bis(trimethylsilyl) lithium amide according to claim 1, characterized in that: The telescopic assembly includes a first disc rotatably connected to the top of the reactor, an electric push rod is fixedly connected to the bottom of the first disc, and a telescopic end of the electric push rod is fixedly connected to a second disc fixedly connected to the top of the movable column.

5. A reaction device for preparing bis(trimethylsilyl)lithium amide according to claim 1, characterized in that: The interior of the diverter plate is provided with an annular cone portion, the middle portion of the diverter plate and the outer periphery of the diverter plate are both provided with mesh plates, and the diverter plate is connected with the bottom of the reaction kettle through the mesh plates.

6. A reaction device for preparing bis(trimethylsilyl) lithium amide according to claim 1, characterized in that: The liquid dripping assembly comprises a liquid adding cylinder arranged on the top of the reactor, a liquid dripping tube penetrating into the reactor is arranged at the bottom of the liquid adding cylinder, a splash plate is arranged at the bottom of the liquid dripping tube, a liquid beating rack is arranged below the splash plate, and the liquid beating rack is fixedly connected to the output shaft of the dispersion motor arranged on the side wall of the reactor; The splash plate is provided with a photoelectric sensor for detecting the number of liquid droplets splashed on the splash plate.

7. A reaction device for preparing bis(trimethylsilyl)lithium amide according to claim 6, characterized in that: One end of the first hard connecting tube away from the liquid pumping assembly faces the bottom of the splash plate.

8. A reaction device for preparing bis(trimethylsilyl) lithium amide according to claim 1, characterized in that: The liquid transfer and filtration assembly includes a central seat arranged on the filtration cylinder, a liquid expansion tube connected to the liquid transfer tube is arranged inside the central seat, a driving motor is fixedly connected to the outside of the central seat, the output end of the driving motor passes through the inner cavity of the liquid expansion tube and is movably connected to the inner wall of the other side of the central seat, and a cam is fixedly connected to the outside of the output end of the driving motor, and the cam is located in the inner cavity of the liquid transfer tube.

9. A reaction device for preparing bis(trimethylsilyl)lithium amide according to claim 8, characterized in that: The bottom of the expansion tube is fixedly connected to an expansion tube, the interior of the expansion tube is movably connected to a filter box, the interior of the filter box is provided with a double-layer filter screen, the top of the filter box is fixedly connected to a plurality of circumferentially equidistant return springs, the other end of the return spring is fixedly connected to the top inner wall of the expansion tube, the upper side of the filter box is fixedly connected to a main shaft, the top end of the main shaft is fixedly connected to a contact, and the contact is in contact with a cam.

10. A reaction device for preparing bis(trimethylsilyl) lithium amide according to claim 1, characterized in that: The liquid discharge assembly comprises a liquid pump arranged on the side of the filter cartridge, a liquid suction pipe is fixedly connected to the top of the liquid pump, the liquid suction pipe is fixedly connected to the liquid transfer pipe, and a liquid discharge pipe is arranged on the side of the liquid pump.

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