Efficient separation and purification device for preparing agomelatine raw material medicine
By using a pretreatment filter and a biaxial stirring system in the preparation of agomelatine API, the problems of uneven solvent mixing and the influence of small particulate matter were solved, thereby improving the uniformity of crystal particle size and the purification effect.
Patent Information
- Application Number
- CN202511730873.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-24
- Publication Date
- 2026-02-24
AI Technical Summary
In the existing technology, uneven solvent mixing during agomelatine crystallization leads to uneven crystal particle size, and the small particulate matter in the crude solvent affects the purification and crystallization effect.
The system employs a pretreatment filter cartridge and a dual-shaft stirring system. The pretreatment filter cartridge filters out fine particles in the crude solvent, and the propeller and anchor impellers are used to achieve thorough mixing of the solvent within the reactor, ensuring uniform crystal particle size.
This method achieves uniformity of agomelatine crystal particle size and improves purification effect, avoids filter cloth clogging and crystal particle size differences, and improves crystallization efficiency.
Smart Images

Figure CN121550702A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of pharmaceutical production technology, and specifically relates to a high-efficiency separation and purification device for the preparation of agomelatine raw material. Background Technology
[0002] Agomelatine is a novel antidepressant that acts as both a melatonin (MT) receptor agonist and a serotonin (5-HT) 2C receptor antagonist. Agomelatine is effective in treating adult depression, particularly major depressive disorder (MMD), and can effectively improve sleep parameters and maintain sexual function. It can also improve sleep rhythm disorders associated with depression. Agomelatine raw material is the active ingredient in the drug formulation, providing the material basis for its therapeutic effect. After undergoing rigorous quality control and approval processes, it is used to produce the final drug for patients, such as agomelatine tablets.
[0003] When the crude agomelatine is prepared and the corresponding crystal form of agomelatine is needed, the crude agomelatine solvent is added dropwise to the corresponding solvent for dissolution. After stirring and crystallization, the corresponding crystal form of agomelatine is obtained. Crystallization is the key step in determining the crystal form (such as crystal form I, V) and purity of agomelatine. In this process, stirring the mixed solvent with a stirring paddle can accelerate the crystallization efficiency. However, in the existing technology, the solvent is usually stirred with a flat paddle. During the stirring process of the flat paddle, it is easy to cause uneven local mixing of the solvent, resulting in uneven crystal particle size and large differences in crystal size after crystallization, which causes filter cloth blockage. At the same time, during the addition of crude agomelatine solvent, due to the lack of pre-filtration, the small particles in the crude product can also easily cause uneven crystal particle size after crystallization. Summary of the Invention
[0004] The purpose of this invention is to provide a high-efficiency separation and purification device for the preparation of agomelatine raw material. Its advantages are that it can fully agitate the solvent, enhance the material circulation near the vessel wall, and ensure uniform crystal particle size after crystallization. At the same time, during the addition of crude solvent, it can pre-filter the crude solvent to avoid the small particulate matter in the crude solvent from affecting the subsequent purification and crystallization, thus avoiding uneven crystal particle size.
[0005] The above-mentioned technical objective of the present invention is achieved through the following technical solution: a high-efficiency separation and purification device for preparing agomelatine raw material, comprising a vessel body, wherein a crude product feed pipe is provided on one side of the top of the vessel body, and a pretreatment filtration component is provided inside the crude product feed pipe; The pretreatment filtration assembly includes an installation cylinder and a cylindrical pretreatment filter element. The installation cylinder is placed inside the coarse product feed pipe. A fixing plate that rests on the top of the coarse product feed pipe is integrally connected to the top of the installation cylinder. The pretreatment filter element is placed inside the installation cylinder. The installation cylinder is detachably connected to a connecting plate whose top rests on the fixing plate. A pressure cylinder whose bottom end presses against the pretreatment filter element is fixedly connected to the bottom of the connecting plate. The bottom of the pressure cylinder has through holes that are arranged in a ring around the top of the pretreatment filter element. The bottom of the installation cylinder is connected to a base, and the base has a drain hole that communicates with the pretreatment filter element.
[0006] The inner cavity of the vessel is also rotatably connected to a first stirring shaft, on which a propulsion stirring paddle is fixedly sleeved. A second stirring shaft with both ends passing through the first stirring shaft is rotatably connected inside the first stirring shaft, and an anchor stirring paddle is connected to the bottom of the second stirring shaft.
[0007] Using the above technical solution: the mounting cylinder is placed on the crude product feed pipe by a fixed plate, and when the bottom end of the pressure cylinder presses down on the pretreatment filter element, its top connecting plate is placed on the fixed plate, so that the pressure cylinder is placed in the inner cavity of the mounting cylinder. During the process of adding crude product solvent, the crude product solvent is added into the pressure cylinder with the top opening. Then the crude product solvent can fall down through the through hole. The crude product solvent accumulated in the inner cavity of the mounting cylinder will then enter the inner cavity of the pretreatment filter element and be filtered. The filtered crude product solvent will enter the inner cavity of the reactor body through the drain hole.
[0008] During the purification and crystallization process of the filtered crude solvent, the first and second stirring shafts are driven to rotate, which in turn drives the propeller-type and anchor-type stirring paddles to rotate. The anchor-type stirring paddle generates radial flow, closely adhering to the vessel wall, ensuring effective mixing of the vessel wall and bottom corners. Meanwhile, the propeller-type stirring paddle generates strong axial flow, promoting the circulation of materials up and down. The two working together enable the solvent to have strong radial and axial flow, achieving seamless mixing of the solvent inside the vessel, avoiding stratification and dead zones, and ensuring the overall mixing effect.
[0009] The present invention is further configured such that a flow guide cylinder, which is frustoconical in shape and surrounds a through hole, is fixedly connected to the bottom end of the pressure cylinder, the bottom end of the flow guide cylinder is open, and the top end of the pretreatment filter element extends into the inner cavity of the flow guide cylinder.
[0010] The above technical solution is adopted: the guide tube is used to receive the crude solvent falling down through the through hole. The guide tube is wider at the top and narrower at the bottom, and the whole is a frustum device. When the crude solvent falls into the guide tube, the crude solvent can flow along the inclined inner wall of the guide tube and be guided to fall on the outer wall of the pretreatment filter element, so that the crude solvent can be filtered by the pretreatment filter element and enter the inner cavity of the pretreatment filter element.
[0011] The invention is further configured such that notches are provided on both sides of the fixed plate, and limiting connecting rods are connected to both outer walls of the mounting cylinder. The outer diameter of the connecting plate is smaller than the outer diameter of the fixed plate. Grooves are provided on both sides of the top of the connecting plate. L-shaped pressure plates are provided on both sides of the inner cavity of the pressure cylinder. One end of the pressure plate presses on the groove. An L-shaped limiting block is provided on the top of the pressure plate. The end of the limiting connecting rod passes through the notch and rests on the groove. A limiting hole is provided on the limiting connecting rod to be engaged with the limiting block.
[0012] The above technical solution is adopted: the pressure plates on both sides of the inner cavity of the pressure cylinder are connected by a connecting rod. When the pressure cylinder presses down on the pretreatment filter element, the connecting plate rests on the fixed plate. At this time, one end of the pressure plate is pressed on the groove, and the other end of the pressure plate extends into the inner cavity of the pressure cylinder, which can limit the pressure cylinder. When the limiting connecting rod passes through the notch, and the limiting hole on the limiting connecting rod is passed through the limiting block on the pressure plate, the inner wall of the L-shaped limiting block abuts against the inner wall of one side of the notch, so that the limiting connecting rod and the pressure plate are limited, thereby ensuring that the pressure cylinder and the connecting plate can be stably limited on the mounting cylinder.
[0013] The invention is further configured such that the pretreatment filter element is cylindrical with an opening at the bottom, a block extending into the inner cavity of the pretreatment filter element is fixedly connected to the top of the base, the drain hole penetrates the block, a flushing pipe penetrating the block and the base is provided on the block, a water distribution pipe communicating with its inner cavity is connected to the top side of the flushing pipe, an annular pipe communicating with its inner cavity is connected to the end of the water distribution pipe, a nozzle distributed in a ring is provided at the top of the annular pipe, and a drain pipe communicating with its inner cavity and located above the block is installed on one side of the mounting cylinder.
[0014] The above technical solution is as follows: When the crude solvent is filtered by the pretreatment filter element and enters the inner cavity of the pretreatment filter element, the filtered crude solvent will pass through the drain hole and enter the inner cavity of the reactor body. Therefore, the tiny particulate impurities contained in the crude solvent are left on the outer wall of the pretreatment filter element. When the crude solvent is purified and crystallized and removed from the reactor body, the inner cavity of the reactor body is cleaned. The flushing pipe can supply water to the annular pipe through the water distribution pipe, so that the nozzle at the top of the annular pipe can spray cleaning liquid onto the inner wall of the pretreatment filter element, thereby playing the role of backwashing and cleaning. The cleaning liquid during cleaning accumulates in the installation cylinder and can be discharged through the drain pipe.
[0015] The present invention is further configured such that a flushing water inlet pipe with an end penetrating through the crude product feed pipe is installed in the inner cavity of the crude product feed pipe, and the bottom end of the flushing pipe is inserted into the flushing water inlet pipe.
[0016] The above technical solution is adopted: the bottom end of the flushing pipe is integrally connected to an insert with an outer diameter smaller than that of the flushing pipe. The outer wall of the insert is equipped with at least two O-ring seals. When the installation cylinder is placed in the inner cavity of the coarse product feed pipe, the insert is inserted into the flushing water inlet pipe, so that the flushing water inlet pipe and the flushing pipe are connected together.
[0017] The present invention is further configured such that the propulsion agitator has two agitator blades, and the propulsion agitator is located in the inner cavity of the anchor agitator.
[0018] With the above technical solution, when the propeller-type agitator and the anchor-type agitator rotate, they will not come into contact and interfere with each other.
[0019] The present invention is further configured such that a mounting frame is fixedly connected to the top of the vessel body, a drive motor is mounted on the top of the mounting frame, the top ends of the first stirring shaft and the second stirring shaft both penetrate the vessel body, and the output shaft of the drive motor penetrates the mounting frame and is connected to the second stirring shaft.
[0020] The above technical solution is adopted: the drive motor is used to drive the second stirring shaft to rotate, so as to drive the anchor-type stirring paddle to carry out stirring work.
[0021] The present invention is further configured such that the top end of the first stirring shaft penetrates the vessel body and is movably fitted with a sleeve, the top end of the sleeve is fixedly connected to a lower clutch sleeve, the top end of the second stirring shaft penetrates the vessel body and passes through the lower clutch sleeve, and an upper clutch sleeve located above the lower clutch sleeve is fixedly fitted on the second stirring shaft, and the lower clutch sleeve can be connected to or separated from the upper clutch sleeve.
[0022] The above technical solution is adopted: when the upper clutch sleeve is separated from the lower clutch sleeve, the first stirring shaft and the second stirring shaft do not rotate synchronously; when the lower clutch sleeve is connected to the upper clutch sleeve, the first stirring shaft and the second stirring shaft rotate synchronously.
[0023] The present invention is further configured such that the bottom of the upper clutch sleeve is provided with a toothed groove, the top of the lower clutch sleeve is integrally connected with a toothed block that mates with the toothed groove, the bottom of the lower sleeve is fixedly connected with a lifting plate that is movably penetrated by the first stirring shaft, the top of the vessel body is equipped with an electric push rod that is connected to the lifting plate and the output shaft, and a spring sleeved on the first stirring shaft is provided between the bottom end of the lifting plate and the vessel body.
[0024] Using the above technical solution: the electric actuator drives the lifting plate to move up and down, so that the lower clutch sleeve at the top of the lower sleeve can move relative to the upper clutch sleeve, so that the lower clutch sleeve can connect or separate from the upper clutch sleeve. When the lower clutch sleeve connects with the upper clutch sleeve, the toothed block is inserted into the toothed slot.
[0025] The present invention is further configured such that a guide groove is provided on the inner wall of the sleeve, and a guide key that slides in cooperation with the guide groove is installed on the outer wall of the first stirring shaft.
[0026] The above technical solution is adopted: when the sleeve and the lower clutch sleeve move relative to the upper clutch sleeve, the guide groove on the inner wall of the sleeve can move relative to the guide key, which can ensure that the first stirring shaft and the second stirring shaft rotate synchronously when the lower clutch sleeve is connected to the upper clutch sleeve.
[0027] In summary, the present invention has the following beneficial effects: 1. By setting up an installation cylinder and a pretreatment filter element, this invention can filter out tiny particles in the crude solvent of agomelatine raw material before adding it to the reactor for purification and crystallization, thus ensuring uniform crystal particle size after subsequent crystallization.
[0028] 2. The present invention presses one end of the pressure plate onto the groove and connects the limiting hole on the limiting connecting rod with the limiting block on the pressure plate, so that the pressure plate can stably limit the pressure cylinder, so that the pretreatment filter element is limited. The connection between the limiting connecting rod and the pressure plate can also be easily released, thereby facilitating the removal and replacement of the pretreatment filter element.
[0029] 3. This invention, through the synergistic cooperation of propulsion-type agitator and anchor-type agitator, can ensure that the corners of the vessel wall and bottom are effectively agitated, achieving seamless mixing of the solvent inside the vessel, avoiding stratification and dead zones, so as to ensure uniform crystal particle size after crystallization. Attached Figure Description
[0030] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a cross-sectional schematic diagram of the propulsion impeller of the present invention; Figure 3 This is a cross-sectional structural schematic diagram of the anchor-type mixing impeller of the present invention; Figure 4 This is a schematic diagram of the structure of the propulsion agitator of the present invention when it has multiple blades; Figure 5 This is a schematic diagram of the pretreatment filtration assembly of the present invention; Figure 6 For the present invention Figure 5 Enlarged diagram of point A in the diagram; Figure 7 This is a schematic diagram of the pretreatment filtration component of the present invention in a separated state; Figure 8 This is a schematic diagram of the structure of the pressure cylinder of the present invention; Figure 9 This is a schematic diagram of the base of the present invention; Figure 10 This is a schematic diagram of the structure of the first and second stirring shafts of the present invention; Figure 11 This is a schematic diagram of the upper clutch sleeve and lower clutch sleeve of the present invention; Figure 12 For the present invention Figure 11 Enlarged diagram of point B in the diagram; Figure 13 This is a schematic diagram of the planar structure of the mounting cylinder of the present invention.
[0031] Reference numerals: 1. Reactor body; 2. Crude product feed pipe; 3. Pretreatment filter assembly; 31. Mounting cylinder; 311. Drain pipe; 32. Fixing plate; 321. Notch; 33. Pretreatment filter element; 34. Pressure cylinder; 341. Through hole; 342. Guide cylinder; 35. Connecting plate; 351. Groove; 36. Limiting connecting rod; 361. Limiting rod; 362. Limiting hole; 37. Pressure plate; 371. Limiting block; 38. Connecting rod; 39. Base; 391. Block; 392. Drain 393. Flushing pipe; 394. Insertion pipe; 395. Water distribution pipe; 396. Annular pipe; 397. Nozzle; 4. Flushing inlet pipe; 5. Mounting bracket; 6. Drive motor; 7. First stirring shaft; 71. Propeller-type stirring paddle; 72. Sleeve; 73. Lower clutch sleeve; 74. Toothed insert; 75. Guide groove; 76. Guide key; 8. Second stirring shaft; 81. Anchor-type stirring paddle; 82. Upper clutch sleeve; 83. Toothed insert groove; 9. Lifting plate; 10. Spring; 11. Electric actuator. Detailed Implementation
[0032] The present invention will be further described in detail below with reference to the accompanying drawings.
[0033] Example 1: refer to Figures 1-9 A high-efficiency separation and purification device for preparing agomelatine raw material includes a vessel body 1. A crude product feed pipe 2 is provided on one side of the top of the vessel body 1. A pretreatment filter assembly 3 is provided inside the crude product feed pipe 2. The pretreatment filter assembly 3 includes a mounting cylinder 31 and a cylindrical pretreatment filter element 33. The mounting cylinder 31 is placed inside the cavity of the crude product feed pipe 2. A fixing plate 32 that rests on the top of the crude product feed pipe 2 is integrally connected to the top of the mounting cylinder 31. The pretreatment filter element 33 is placed inside the cavity of the mounting cylinder 31. The mounting cylinder 31 is detachably connected to a connecting plate 35 whose top rests on a fixed plate 32. The bottom of the connecting plate 35 is fixedly connected to a pressure cylinder 34 whose bottom end presses against the pretreatment filter element 33. The pressure cylinder 34 seals the top of the pretreatment filter element 33. The bottom of the pressure cylinder 34 has through holes 341 that surround the top of the pretreatment filter element 33 and are distributed in a ring. The bottom of the mounting cylinder 31 is connected to a base 39. The base 39 has a drain hole 392 that communicates with the pretreatment filter element 33.
[0034] The mounting cylinder 31 is placed on the crude product feed pipe 2 via the fixing plate 32. When the bottom end of the pressure cylinder 34 presses down on the pretreatment filter element 33, its top connecting plate 35 rests on the fixing plate 32, so that the pressure cylinder 34 is placed in the inner cavity of the mounting cylinder 31. During the addition of crude product solvent, the crude product solvent is added into the pressure cylinder 34 with the top opening. Then, the crude product solvent can pass through the through hole 341 and fall downward. The crude product solvent accumulated in the inner cavity of the mounting cylinder 31 will then enter the inner cavity of the pretreatment filter element 33 and be filtered. The filtered crude product solvent will enter the inner cavity of the vessel body 1 through the drain hole 392. The pretreatment filter element 33 is made of 0.22μm PES and has a porous rigid skeleton. That is, the PES filter membrane is hot-melt welded to the inner cavity of the porous rigid skeleton made of polypropylene material, which can effectively filter the small particles in the crude product solvent. The vessel body 1 has a heat exchange jacket and a discharge pipe at the bottom of the vessel body 1, which are conventional components of existing technology and will not be described in detail in this invention.
[0035] When the feed pipe 2 is connected to the corresponding crude solvent input pipe, the crude solvent input pipe may have an insertion head that can be inserted into the inner cavity of the pressure cylinder 34 so that the crude solvent can enter the inner cavity of the pressure cylinder 34. At the same time, when the crude solvent is input, a slow feeding method is adopted to slow down the flow rate of the crude solvent input and prevent the crude solvent from overflowing after entering the pressure cylinder 34.
[0036] refer to Figure 7 The bottom end of the pressure cylinder 34 is fixedly connected to a guide cylinder 342 that is shaped like a frustum and surrounds the through hole 341. The bottom end of the guide cylinder 342 is open, and the top end of the pretreatment filter element 33 extends into the inner cavity of the guide cylinder 342.
[0037] The pressure cylinder 34 and the guide cylinder 342 are integrally set. When the top of the pretreatment filter element 33 extends into the inner cavity of the guide cylinder 342, there is a gap between the outer wall of the pretreatment filter element 33 and the inner wall of the guide cylinder 342. The guide cylinder 342 is used to receive the crude solvent falling down through the through hole 341. The guide cylinder 342 is wider at the top and narrower at the bottom, and is in the shape of a frustum. When the crude solvent falls into the guide cylinder 342, the crude solvent can flow along the inclined inner wall of the guide cylinder 342 and be guided to fall on the outer wall of the pretreatment filter element 33 so that the crude solvent can be filtered by the pretreatment filter element 33 and enter the inner cavity of the pretreatment filter element 33.
[0038] refer to Figure 5 and Figure 6The fixed plate 32 has notches 321 on both sides. The outer walls of the mounting cylinder 31 are connected by limiting connecting rods 36. The outer diameter of the connecting plate 35 is smaller than the outer diameter of the fixed plate 32. The top of the connecting plate 35 has grooves 351 on both sides. The inner cavity of the pressure cylinder 34 has L-shaped pressure plates 37 on both sides. One end of the pressure plate 37 presses on the groove 351. The top of the pressure plate 37 has an L-shaped limiting block 371. The end of the limiting connecting rod 36 passes through the notch 321 and rests on the groove 351. The top of the limiting connecting rod 36 has a limiting rod 361 that is rotatably connected to it. The limiting rod 361 has a limiting hole 362 that is locked in the limiting block 371.
[0039] The pressure plates 37 on both sides of the inner cavity of the pressure cylinder 34 are connected by connecting rods 38. When the pressure cylinder 34 presses down on the pre-treatment filter element 33, the connecting plate 35 rests on the fixed plate 32. At this time, one end of the pressure plate 37 is pressed onto the groove 351, and the other end of the pressure plate 37 extends into the inner cavity of the pressure cylinder 34, which can limit the pressure cylinder 34. The limiting rod 361 and the limiting connecting rod 36 can be rotated through a fold or through a hinge. The limiting rod 361 and the limiting connecting rod 36 can be folded into an L-shape. When the limiting connecting rod 36 passes through the notch 321, and the limiting rod 36... When the limiting hole 362 on the pressure plate 37 passes through the limiting block 371 on the pressure plate 37, the inner wall of the L-shaped limiting block 371 abuts against the inner wall of one side of the notch 321, so that the limiting connecting rod 36 and the pressure plate 37 are limited, thereby ensuring that the pressure cylinder 34 and the connecting plate 35 can be stably limited on the mounting cylinder 31. When the flange is connected to the crude product feed pipe 2, the fixing plate 32 rests on the flange of the crude product feed pipe 2. At the same time, the fixing plate 32 is surrounded by the annularly distributed mounting holes on the flange of the crude product feed pipe 2, without affecting the connection between the flange of the crude product feed pipe 2 and other pipes.
[0040] refer to Figure 5 , Figure 7 , Figure 9 , Figure 13 The pretreatment filter element 33 is cylindrical with an opening at the bottom. A block 391 extending into the inner cavity of the pretreatment filter element 33 is fixedly connected to the top of the base 39. A drain hole 392 passes through the block 391. A flushing pipe 393 is provided on the block 391. The flushing pipe 393 passes through the block 391 and the base 39. A water distribution pipe 395 communicating with its inner cavity is connected to the top side of the flushing pipe 393. An annular pipe 396 communicating with its inner cavity is connected to the end of the water distribution pipe 395. A ring-shaped nozzle 397 is provided at the top of the annular pipe 396. A drain pipe 311 communicating with its inner cavity and located above the block 391 is installed on one side of the mounting cylinder 31. A flushing water inlet pipe 4 with its end penetrating through the coarse product feed pipe 2 is installed in the inner cavity of the coarse product feed pipe 2. The flushing water inlet pipe 4 is inserted into the bottom end of the flushing pipe 393.
[0041] The flushing inlet pipe 4 is L-shaped, with one end located inside the crude product inlet pipe 2 and the other end located outside the crude product inlet pipe 2. The bottom end of the flushing pipe 393 is integrally connected to an insert pipe 394 with an outer diameter smaller than the flushing pipe 393. The outer wall of the insert pipe 394 is fitted with at least two O-ring seals. When the mounting cylinder 31 is placed inside the crude product inlet pipe 2, the insert pipe 394 is interference-fitted into the flushing inlet pipe 4, thus connecting the flushing inlet pipe 4 and the flushing pipe 393 together. When the crude solvent is filtered by the pretreatment filter element 33 and enters the inner cavity of the pretreatment filter element 33, the filtered crude solvent passes through the drain hole 392 and enters the inner cavity of the vessel body 1. Impurities in the crude solvent are blocked by the pretreatment filter element 33, thus the small particulate impurities contained in the crude solvent are eliminated. The crude solvent is retained on the outer wall of the pretreatment filter element 33. When the crude solvent is purified and crystallized, it is removed from the vessel body 1. While the inner cavity of the vessel body 1 is being cleaned, the rinsing pipe 393 can supply water to the annular pipe 396 through the water distribution pipe 395, so that the nozzle 397 at the top of the annular pipe 396 can spray cleaning liquid onto the inner wall of the pretreatment filter element 33, thereby cleaning the inner wall of the pretreatment filter element 33. During this process, a portion of the cleaning liquid can pass through the pretreatment filter element 33 and flow to the outside of the pretreatment filter element 33, and flow downward along the pretreatment filter element 33, so that the outer wall of the pretreatment filter element 33 can be cleaned to a certain extent. The cleaning liquid during cleaning accumulates in the mounting cylinder 31 and can be discharged into the vessel body 1 through the drain pipe 311 and the drain hole 392.
[0042] Of course, in addition to rinsing by flushing water through the inlet pipe 4, a corresponding cleaning solution can also be added to the pressure cylinder 34. The cleaning solution flows downward and rinses the outer wall of the pretreatment filter element 33, which can wash away the impurities attached to the outer wall of the pretreatment filter element 33. Alternatively, the entire pretreatment filter assembly 3 can be removed from the coarse product feed pipe 2, and then the connection between the pressure plate 37 and the limiting connecting rod 36 can be released. The pressure cylinder 34 and the pretreatment filter element 33 can then be removed as a whole, and the pretreatment filter element 33 can be rinsed afterward.
[0043] Brief description of the process: Before the crude solvent purification and crystallization of agomelatine raw material, crude solvent is added to the vessel 1. During the addition process, the crude solvent is added into the pressure cylinder 34 with the top opening. Then, the crude solvent can pass through the through hole 341 and fall into the guide cylinder 342. After that, the crude solvent can flow along the inclined inner wall of the guide cylinder 342 and be guided onto the outer wall of the pretreatment filter element 33 so that the crude solvent can be filtered by the pretreatment filter element 33 and enter the inner cavity of the pretreatment filter element 33, so that the micro particles are separated by the pretreatment filter element 33. The crude solvent that has been pretreated and filtered will enter the inner cavity of the vessel 1 through the drain hole 392 for subsequent purification and crystallization.
[0044] Example 2: Based on Example 1, and referring to Figure 3 and Figure 4 , Figures 10-12 A high-efficiency separation and purification device for preparing agomelatine raw material includes a first stirring shaft 7 and a second stirring shaft 8. The inner cavity of the vessel body 1 is rotatably connected to the first stirring shaft 7. A propeller-type stirring paddle 71 is fixedly sleeved on the first stirring shaft 7. The interior of the first stirring shaft 7 is rotatably connected to a second stirring shaft 8 with both ends passing through the first stirring shaft 7. An anchor-type stirring paddle 81 is connected to the bottom of the second stirring shaft 8. A mounting frame 5 is fixedly connected to the top of the vessel body 1. A drive motor 6 is installed on the top of the mounting frame 5. The top ends of the first stirring shaft 7 and the second stirring shaft 8 both pass through the vessel body 1. The output shaft of the drive motor 6 passes through the mounting frame 5 and is connected to the second stirring shaft 8.
[0045] The drive motor 6 is used to drive the second stirring shaft 8 to rotate, so as to drive the push-anchor type stirring paddle 81 to rotate. When the first stirring shaft 7 and the second stirring shaft 8 rotate synchronously, the anchor type stirring paddle 81 generates radial flow, closely adhering to the vessel wall, ensuring that the corners of the vessel wall and bottom of the vessel body 1 can be effectively stirred. Meanwhile, the push-anchor type stirring paddle 71 generates strong axial flow, promoting the circulation of materials up and down. The two work together to enable the solvent to have strong radial and axial flow, achieving no dead corners in the solvent inside the vessel body 1, avoiding stratification and dead zones, and ensuring the overall mixing effect.
[0046] refer to Figure 3 and Figure 4 The propulsion agitator 71 has two agitator blades and is located inside the anchor agitator 81.
[0047] The propulsion agitator 71 can also have three, four or more agitator blades, and is not limited to two agitator blades.
[0048] refer to Figures 10-12 The top end of the first stirring shaft 7 passes through the vessel body 1 and is movably fitted with a sleeve 72. The top end of the sleeve 72 is fixedly connected to a lower clutch sleeve 73. The top end of the second stirring shaft 8 passes through the vessel body 1 and passes through the lower clutch sleeve 73. An upper clutch sleeve 82 located above the lower clutch sleeve 73 is fixedly fitted on the second stirring shaft 8. The lower clutch sleeve 73 can be connected or separated from the upper clutch sleeve 82. A toothed groove 83 is opened at the bottom of the upper clutch sleeve 82. A toothed block 74 that mates with the toothed groove 83 is integrally connected to the top of the lower clutch sleeve 73. A lifting plate 9 that is movably passed through by the first stirring shaft 7 is fixedly connected to the bottom of the lower sleeve 72. An electric push rod 11 connected to the lifting plate 9 and an output shaft is installed on the top of the vessel body 1. A spring 10 fitted on the first stirring shaft 7 is provided between the bottom end of the lifting plate 9 and the vessel body 1. A guide groove 75 is opened on the inner wall of the sleeve 72. A guide key 76 that slides with the guide groove 75 is installed on the outer wall of the first stirring shaft 7.
[0049] When the electric actuator 11 drives the lifting plate 9 to rise and fall, the lower clutch sleeve 73 at the top of the lower sleeve 72 can move relative to the upper clutch sleeve 82, so that the lower clutch sleeve 73 and the upper clutch sleeve 82 can be connected or separated. When the lower clutch sleeve 73 and the upper clutch sleeve 82 are connected, the jaw insert 74 is engaged in the jaw insert groove 83, and the guide groove 75 on the inner wall of the sleeve 72 can move relative to the guide key 76, so as to ensure that the first stirring shaft 7 and the second stirring shaft 8 rotate synchronously when the lower clutch sleeve 73 and the upper clutch sleeve 82 are connected. Brief description of the usage process: When the lower clutch sleeve 73 is separated from the upper clutch sleeve 82, the drive motor 6 drives the second stirring shaft 8 to rotate. The second stirring shaft 8 drives the anchor stirring paddle 81 to rotate independently. The anchor stirring paddle 81 pushes the material to circulate as a whole. Meanwhile, the propeller stirring paddle 71 connected to the first stirring shaft 7 is pushed by the material. At the same time, the propeller stirring paddle 71 acts like a series of obstacles, cutting and dispersing the material flowing through it, generating a large number of local eddies and turbulences. When the lower clutch sleeve 73 is connected to the upper clutch sleeve 82, the anchor stirring paddle 81 and the propeller stirring paddle 71 can work together. The anchor stirring paddle 81 generates radial flow, and the propeller stirring paddle 71 generates strong axial flow, promoting the up and down circulation of the material. The two work together to enable the solvent to have strong radial and axial flow, achieving no dead angle mixing of the solvent inside the vessel 1.
[0050] It should be noted that parts have a lifespan and can be replaced during regular maintenance when they no longer meet performance requirements. Deterioration in performance due to prolonged use of parts is not a design defect of this application.
[0051] This specific embodiment is merely an explanation of the present invention and is not intended to limit the invention. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they are within the scope of the claims of the present invention.
Claims
1. A high-efficiency separation and purification device for the preparation of agomelatine raw material, comprising a vessel body (1), characterized in that: The top side of the vessel body (1) is provided with a crude product feed pipe (2), and a pretreatment filter assembly (3) is provided inside the crude product feed pipe (2). The pretreatment filter assembly (3) includes an installation cylinder (31) and a cylindrical pretreatment filter element (33). The installation cylinder (31) is placed inside the coarse product feed pipe (2). The top of the installation cylinder (31) is integrally connected to a fixing plate (32) that rests on the top of the coarse product feed pipe (2). The pretreatment filter element (33) is placed inside the installation cylinder (31). The installation cylinder (31) is detachably connected to a connecting plate (35) whose top rests on the fixing plate (32). The bottom of the connecting plate (35) is fixedly connected to a pressure cylinder (34) whose bottom end presses against the pretreatment filter element (33). The bottom of the pressure cylinder (34) has through holes (341) that surround the top of the pretreatment filter element (33) and are distributed in a ring. The bottom of the installation cylinder (31) is connected to a base (39). The base (39) has a drain hole (392) that communicates with the pretreatment filter element (33). The inner cavity of the vessel body (1) is also rotatably connected to a first stirring shaft (7), and a propulsion stirring paddle (71) is fixedly sleeved on the first stirring shaft (7). The inner cavity of the first stirring shaft (7) is rotatably connected to a second stirring shaft (8) with both ends passing through the first stirring shaft (7), and an anchor stirring paddle (81) is connected to the bottom of the second stirring shaft (8).
2. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 1, characterized in that: The bottom end of the pressure cylinder (34) is fixedly connected to a flow guide cylinder (342) which is shaped like a frustum and surrounds the through hole (341). The bottom end of the flow guide cylinder (342) is open, and the top end of the pretreatment filter element (33) extends into the inner cavity of the flow guide cylinder (342).
3. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 1, characterized in that: The fixed plate (32) has notches (321) on both sides. The outer walls of the mounting cylinder (31) are connected by limiting connecting rods (36). The outer diameter of the connecting plate (35) is smaller than that of the fixed plate (32). The top of the connecting plate (35) has grooves (351) on both sides. The inner cavity of the pressure cylinder (34) has L-shaped pressure plates (37) on both sides. One end of the pressure plate (37) presses on the groove (351). The top of the pressure plate (37) has an L-shaped limiting block (371). The end of the limiting connecting rod (36) passes through the notch (321) and rests on the groove (351). The top of the limiting connecting rod (36) has a limiting rod (361) that is rotatably connected to it. The limiting rod (361) has a limiting hole (362) that is locked in the limiting block (371).
4. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 1, characterized in that: The pretreatment filter element (33) is cylindrical with an opening at the bottom. The top of the base (39) is fixedly connected to a block (391) that extends into the inner cavity of the pretreatment filter element (33). The drain hole (392) penetrates the block (391). The block (391) is provided with a flushing pipe (393) that penetrates the block (391) and the base (39). The top side of the flushing pipe (393) is connected to a water distribution pipe (395) that communicates with its inner cavity. The end of the water distribution pipe (395) is connected to an annular pipe (396) that communicates with its inner cavity. The top of the annular pipe (396) is provided with nozzles (397) arranged in a ring. The side of the mounting cylinder (31) is equipped with a drain pipe (311) that communicates with its inner cavity and is located above the block (391).
5. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 4, characterized in that: The inner cavity of the crude product feed pipe (2) is equipped with a flushing water inlet pipe (4) with its end penetrating through the crude product feed pipe (2), and the bottom end of the flushing pipe (393) is inserted into the flushing water inlet pipe (4).
6. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 1, characterized in that: The propulsion agitator (71) has two agitator blades and is located inside the anchor agitator (81).
7. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 1, characterized in that: The top of the vessel body (1) is fixedly connected to a mounting bracket (5), and a drive motor (6) is installed on the top of the mounting bracket (5). The top ends of the first stirring shaft (7) and the second stirring shaft (8) both penetrate the vessel body (1). The output shaft of the drive motor (6) penetrates the mounting bracket (5) and is connected to the second stirring shaft (8).
8. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 1, characterized in that: The top end of the first stirring shaft (7) passes through the vessel body (1) and is movably fitted with a sleeve (72). The top end of the sleeve (72) is fixedly connected to a lower clutch sleeve (73). The top end of the second stirring shaft (8) passes through the vessel body (1) and passes through the lower clutch sleeve (73). An upper clutch sleeve (82) is fixedly fitted on the second stirring shaft (8) above the lower clutch sleeve (73). The lower clutch sleeve (73) can be connected to or separated from the upper clutch sleeve (82).
9. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 8, characterized in that: The bottom of the upper clutch sleeve (82) is provided with a toothed groove (83), the top of the lower clutch sleeve (73) is integrally connected with a toothed block (74) that cooperates with the toothed groove (83), the bottom of the lower sleeve (72) is fixedly connected with a lifting plate (9) that is movably penetrated by the first stirring shaft (7), the top of the vessel body (1) is equipped with an electric push rod (11) whose output shaft is connected to the lifting plate (9), and a spring (10) is provided between the bottom end of the lifting plate (9) and the vessel body (1) and sleeved on the first stirring shaft (7).
10. The high-efficiency separation and purification device for preparing agomelatine raw material according to claim 8, characterized in that: The inner wall of the sleeve (72) is provided with a guide groove (75), and the outer wall of the first stirring shaft (7) is provided with a guide key (76) that slides in cooperation with the guide groove (75).
Citation Information
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