Crystallization reaction kettle for medicine preparation

The inert gas-driven movable tube and scraper assembly, combined with the air guide duct and detachable connection design, solves the problems of low crystal scraping efficiency and wear in scraper-type reactors, and achieves efficient and stable crystal scraping and equipment maintenance.

CN120662249AInactive Publication Date: 2025-09-19YANGZHOU TONGDA CHEM PHARM EQUIP FACTORY

Patent Information

Application Number
CN202510955412.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-11
Publication Date
2025-09-19
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing scraper-type crystallization reactor has the problem of secondary deposition and wear during the process of scraping crystals, which leads to a decrease in fit, affecting heat transfer efficiency and product quality.

Method used

An inert gas supply assembly is used to drive the movable tube and scraper group. An air pressure propulsion mechanism is used to efficiently scrape away crystals. The scraper blade surface is flushed through the guide air channel to avoid secondary deposition. The elastic sealing assembly ensures that the scraper group fits tightly against the inner wall. A detachable connecting pipe is designed for easy replacement.

Benefits of technology

It achieves efficient scraping of crystals, avoids secondary deposition, solves the problem of decreased fit due to wear, improves the maintainability and production efficiency of the equipment, and ensures the stable operation of the reactor and product quality.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120662249A_ABST
    Figure CN120662249A_ABST
Patent Text Reader

Abstract

The invention discloses a crystallization reaction kettle for medicine preparation, and relates to the technical field of medicine preparation, and the crystallization reaction kettle is technically characterized by comprising a reaction kettle body and a stirring mechanism, the stirring mechanism comprises a rotation driving assembly arranged at one end of the reaction kettle body, and an output shaft of the rotation driving assembly extends into the kettle and is connected with a stirring center pipe; the other end of the stirring central pipe communicates with an inert gas supply assembly; the side wall of the stirring central pipe is communicated with a stirring branch pipe; a scraper group is arranged at the end part of the movable pipe and comprises a plurality of scraper blades; an elastic sealing assembly is arranged and comprises a V-shaped sealing plate, and the two ends of the V-shaped sealing plate are connected with the end face of the movable pipe through elastic connecting pieces; during gas supply, inert gas passes through all parts and exhaust gaps, air pressure enables the movable pipe to abut against the kettle wall, the sealing plate is jacked up to form a flow guide gas channel, and the gas is guided to be exhausted and scour the scraper blade; according to the method, crystals can be efficiently scraped, secondary deposition can be avoided, and the problem that the fitting degree is reduced due to abrasion can be solved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of medicine preparation, in particular to a crystallization reaction kettle for medicine preparation. Background Art

[0002] In the field of pharmaceutical preparation, crystallization reaction is one of the key links in drug synthesis and purification. It controls the parameters such as the supersaturation of the solution, temperature and stirring conditions to precipitate the target product in the form of crystals, thereby obtaining high-purity and high-stability active pharmaceutical ingredients. The efficiency of the crystallization reaction and the quality of the product are directly subject to the structural design and operating performance of the reaction equipment. Especially in large-scale production, the problem of crystal deposition on the inner wall of the reactor is particularly prominent. The deposited crystals will not only reduce the heat transfer efficiency and affect the uniformity of the reaction system, but may also lead to local supersaturation out of control, thereby causing crystal form variation or impurity enrichment, and ultimately affecting the safety and effectiveness of the drug. Therefore, how to effectively inhibit the deposition of crystals on the inner wall of the reactor has become an important research direction for improving the stability of the crystallization process.

[0003] In response to the above problems, a variety of solutions have been proposed in the prior art. For example, the utility model patent with Chinese patent application number CN202222244988.9 discloses a metronidazole crystallization reactor, the core design of which is to provide a rotatable scraper device inside the reactor, and utilize the relative movement of the scraper and the inner wall of the reactor to scrape off the deposited crystals in real time. This technology significantly reduces the accumulation of crystals on the inner wall by mechanical scraping, improves the heat transfer efficiency and the uniformity of the reaction system, and thus improves the controllability of the crystallization process to a certain extent. Although this solution has positive significance in suppressing the deposition of crystals, its technical implementation still has limitations that have not been fully resolved.

[0004] Specifically, the technical deficiencies of existing scraper-type crystallization reactors primarily manifest themselves in two aspects: First, as the scraper removes crystals, some adhere to the scraper surface due to mechanical forces, forming secondary deposits. This causes scraping efficiency to gradually decrease with extended use. Second, the scraper's long-term frictional contact with the reactor's inner wall inevitably causes wear, which gradually reduces the scraper's fit with the inner wall, weakening the scraping effect and even causing localized accumulation of crystals in the gap between the scraper and the inner wall. These issues not only shorten the equipment's maintenance cycle and increase production costs, but can also affect product quality due to uncontrolled crystal deposition. Summary of the Invention

[0005] In order to solve the above technical problems, the purpose of the present invention is to provide a crystallization reactor for pharmaceutical preparation, which can not only efficiently scrape off crystals and avoid secondary deposition, but also solve the problem of decreased fit due to wear.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A crystallization reactor for pharmaceutical preparation, comprising:

[0008] A reactor body, wherein the top of the reactor body is connected to a feed pipe and the bottom is connected to a discharge pipe, and the discharge pipe is provided with a valve assembly;

[0009] A stirring mechanism, the stirring mechanism comprising a rotary drive assembly disposed at one end of the reactor body, the output shaft of the rotary drive assembly penetrating and extending into the reactor body and fixedly connected to a stirring central tube, the other end of the stirring central tube being connected to an inert gas supply assembly, the gas outlet of the inert gas supply assembly being rotatably connected to the end of the stirring central tube;

[0010] At least one stirring branch pipe is fixedly connected to the side wall of the stirring central pipe, and a movable pipe is slidably connected to the stirring branch pipe, and the cross-sections of the stirring branch pipe and the movable pipe are non-circular; a scraper assembly is provided at the other end of the movable pipe, and the scraper assembly includes a plurality of parallel scraper blades fixedly provided at the end of the movable pipe, and the cross-section of the scraper blade is V-shaped;

[0011] The gaps between the scraper blades and the gap between the scraper blades and the movable tube are both set as exhaust gaps. An elastic sealing component is provided at each exhaust gap. The elastic sealing component includes a sealing plate for sealing the exhaust gap. Both ends of the sealing plate are connected to the end surface of the movable tube through elastic connectors. The cross section of the sealing plate is set to be V-shaped.

[0012] When the inert gas supply assembly supplies gas, the inert gas passes through the stirring central tube, the stirring branch tube, the movable tube and the exhaust gap in sequence; under the action of air pressure, the movable tube moves toward and abuts the inner wall of the reactor body, and the closing plate is lifted up to form a guide air channel between the closing plate and the scraper blade, and the guide air channel is used to guide the inert gas to discharge and flush the surface of the scraper blade.

[0013] Preferably, the elastic connecting member is configured to be in the shape of a flat strap, and the material of the elastic connecting member is one of polyurethane elastomer, silicone rubber or thermoplastic elastomer.

[0014] Preferably, guide plates are provided at both ends of the closing plate, and the guide plates are set to be equilateral trapezoids, and the working surfaces of the guide plates slide in contact with the side edges of the scraper blades; the guide air duct formed when the closing plate is lifted by air pressure is presented as a circumferential closed pipeline composed of the closing plate, the scraper blade and the two guide plates, and the elastic connecting piece is connected to the outer wall of the guide plate.

[0015] Preferably, the size of each exhaust gap and the adjacent spacing distance are the same, and the size of each elastic sealing component and the adjacent spacing distance are the same.

[0016] Preferably, the cross-sections of the stirring branch pipe and the movable pipe are set to be rectangular, the end of the movable pipe facing the inner wall of the reactor is set to be a detachable connecting pipe, the scraper group and the elastic sealing component are both arranged on the detachable connecting pipe, the inner wall of the detachable connecting pipe is provided with a clamping ring, the outer wall of the clamping ring is clamped and adapted to the inner wall of the movable pipe, the outer wall of the detachable connecting pipe is provided with multiple connecting plates, the inner wall of the connecting plate is adapted to the outer wall of the movable pipe and is fixedly connected by bolts.

[0017] Preferably, the inert gas supply assembly includes an inert gas generating device, the gas outlet of the inert gas generating device is connected to a gas supply pipe, a first air pump and a check valve are installed on the gas supply pipe, and the gas outlet of the gas supply pipe is rotatably connected to and communicated with the stirring center pipe.

[0018] Preferably, the outer wall of the reactor body is connected to the rotation drive assembly through a lifting assembly, and the lifting assembly includes a lifting frame fixedly arranged on the outer wall of the reactor body, and a lifting hydraulic cylinder is fixedly arranged on the lifting frame, and the movable part of the lifting hydraulic cylinder is fixedly connected to the rotation drive assembly, and the output shaft of the rotation drive assembly is slidably connected to the reactor body, and the stirring center tube is connected to the air supply pipe through a sliding telescopic tube, and the sliding telescopic tube and the air supply pipe are rotatably connected through an annular bearing, and the sliding telescopic tube consists of two sliding tubes that are slidably fitted and nested.

[0019] Preferably, a closed cover is movably connected to the top of the feed pipe, and a return air hole is provided on the top of the reactor body; the return air hole is connected to a return air pipe, and the return air pipe is connected to one end of the air supply pipe close to the inert gas generating device; a second air pump is provided on the return air pipe, and multiple layers of activated carbon adsorption layers are provided in the return air pipe, and a gas-liquid filter is provided at the return air hole.

[0020] Preferably, the valve assembly is configured as an electromagnetic control valve, and the rotation drive assembly is configured as a servo motor or a stepper motor.

[0021] The present invention has the following beneficial effects:

[0022] 1. Efficiently scrape away crystals; the crystallization reactor used for pharmaceutical preparation has the function of efficiently scraping away crystals. The side wall of the stirring center tube is connected to a stirring branch tube, and a movable tube is slidably connected inside the stirring branch tube. A scraper group is provided at the other end of the movable tube, and the scraper group includes multiple parallel scraper blades. When the inert gas supply assembly supplies gas, the inert gas passes through the stirring center tube, the stirring branch tube, the movable tube and the exhaust gap in turn. Under the action of air pressure, the movable tube moves toward and abuts the inner wall of the reactor body. At this time, the scraper blade is in close contact with the inner wall of the reactor and can directly scrape away the crystals attached to the inner wall. Compared with the traditional method, this method of using air pressure to push the movable tube to drive the scraper blade to scrape away crystals has a stronger scraping force and a larger scraping area. It can more efficiently remove crystals from the inner wall of the reactor, ensure the cleanliness of the interior of the reactor, and is conducive to the subsequent reaction.

[0023] 2. Avoid secondary deposition: The reactor can effectively avoid secondary deposition of crystals. The gaps between the scraper blades and the gaps between the scraper blades and the movable tube are set as exhaust gaps. An elastic sealing component is provided at the exhaust gap. The elastic sealing component includes a closing plate. The two ends of the closing plate are connected to the end face of the movable tube through elastic connectors. The cross section of the closing plate is set to V-shaped. When the inert gas supply assembly supplies gas, the closing plate is lifted up and forms a guide airway between the scraper blade and the scraper blade. The guide airway is used to guide the inert gas to discharge and flush the scraper blade surface. In the process of scraping off the crystals, the scraped crystals may adhere to the scraper blade surface, and the inert gas flushes the scraper blade surface through the guide airway, which can wash away the crystals attached to the scraper blade surface in time and prevent the crystals from being deposited on the scraper blade again, thereby avoiding the problem of secondary deposition and ensuring the effect of scraping off the crystals.

[0024] 3. Addressing the Problem of Loss of Fit Due to Wear: This reactor utilizes a unique air pressure propulsion mechanism to effectively address the issue of loss of fit between the scraper assembly and the reactor's inner wall due to wear. During reactor operation, the inert gas supply assembly continuously supplies air, which passes through the central stirring tube, branch stirring tubes, movable tubes, and exhaust gaps. Driven by air pressure, the movable tubes move toward the inner wall of the reactor body and abut against it, thereby driving the scraper assembly to adhere tightly to the reactor's inner wall. Over time, the scraper blades gradually wear and become thinner as they rub against the inner wall to remove crystals. Without a corresponding compensation mechanism, the fit between the scraper blades and the reactor's inner wall would gradually decrease, resulting in poor scraping performance. However, in this reactor, air pressure is constantly present and acting on the movable tubes. Even when the scraper blades become thinner due to wear, the air pressure can still propel the movable tubes toward the inner wall, ensuring that the scraper assembly maintains a tight fit. This use of air pressure to propel the movable tubes creates an automatic compensation mechanism. Regardless of how the degree of wear of the scraper blade changes, the air pressure can ensure that the scraper group maintains sufficient fit with the inner wall of the reactor, thereby ensuring that the effect of scraping off the crystals is not affected. This effectively solves the problem of decreased fit caused by wear and ensures the stable operation of the reactor and the high efficiency of crystal scraping.

[0025] 4. Easy equipment maintenance and replacement: The cross-sections of the stirring branch pipe and the movable pipe are designed to be rectangular. The end of the movable pipe facing the inner wall of the reactor is designed as a detachable connecting pipe. The scraper group and the elastic sealing component are both installed on the detachable connecting pipe. The inner wall of the detachable connecting pipe is provided with a snap ring, and the outer wall is provided with multiple connecting plates. The outer wall of the snap ring is snap-fitted with the inner wall of the movable pipe, and the inner wall of the connecting plate is adapted to the outer wall of the movable pipe and fixedly connected with bolts, making the detachable connecting pipe easy to install and remove. When the scraper group or the elastic sealing component becomes worn or damaged, the detachable connecting pipe can be quickly replaced without disassembling the entire stirring mechanism, which greatly shortens the time for equipment maintenance and replacement and improves the maintainability and production efficiency of the equipment.

[0026] 5. Optimize the supply and utilization of inert gas: The gas outlet of the inert gas supply assembly is rotatably connected to the end of the stirring center tube. When the inert gas supply assembly supplies gas, the inert gas passes through the stirring center tube, the stirring branch tube, the movable tube, and the exhaust gap in sequence. Under the action of air pressure, the movable tube moves toward and abuts the inner wall of the reactor body. The closing plate is lifted up and forms a guide airway between the scraper blade. The guide airway is used to guide the inert gas to discharge and flush the scraper blade surface. This method can not only evenly disperse the inert gas into the reaction system, provide a good inert environment for the crystallization reaction, and prevent adverse reactions such as material oxidation, but also clean the scraper blade surface to avoid material crystallization on the scraper blade, ensure the normal operation of the scraper blade, and improve the utilization efficiency of the inert gas and the stability of the reaction.

[0027] 6. Ensure a stable and safe inert gas supply: The inert gas supply assembly includes an inert gas generator. The outlet of the generator is connected to a gas supply pipe, which is equipped with a first air pump and a check valve. The first air pump provides power for the inert gas supply, ensuring a stable delivery of inert gas to the reactor. The check valve prevents gases or materials in the reaction system from flowing back into the inert gas generator, preventing contamination of the generator and affecting the purity of the inert gas, thereby ensuring a stable and safe inert gas supply.

[0028] 7. Adapting to Different Reaction Requirements and Improving Equipment Flexibility: The outer wall of the reactor body is connected to the rotary drive assembly via a lifting assembly, which includes a lifting frame, a lifting cylinder, and other components. The movable portion of the lifting cylinder drives the rotary drive assembly up and down, allowing the stirring center tube of the stirring mechanism to move up and down, thereby adjusting the stirring mechanism's position within the reactor. Simultaneously, the stirring center tube is connected to the air supply pipe via a sliding telescopic tube. The sliding telescopic tube consists of two sliding tubes that slide, fit, and nest together, accommodating the up and down movement of the stirring center tube. This design allows the reactor to adapt to the needs of different reaction materials and reaction conditions, improving the equipment's flexibility and versatility.

[0029] 8. Achieve gas recycling and environmental protection: A closed cover plate is flexibly connected to the top of the feed pipe. A return air hole is provided at the top of the reactor body, connected to a return air pipe. This return air pipe is connected to the end of the gas supply pipe near the inert gas generator. A second air pump is installed on the return air pipe, which is equipped with multiple layers of activated carbon adsorption layers. A vapor-liquid filter is installed at the return air hole. During the reaction process, gas from the reactor can enter the return air pipe through the return air hole. The vapor-liquid filter removes liquid droplets and impurities from the gas. After the multiple layers of activated carbon adsorption layers absorb harmful gases, the gas is transported back to the gas supply pipe by the second air pump, achieving inert gas recycling. This not only reduces the cost of inert gas use but also reduces environmental pollution, complying with environmental protection requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying any creative work.

[0031] Figure 1 It is a cross-sectional view of the first embodiment of the present invention.

[0032] Figure 2 This is a cross-sectional view from a top view of the movable tube according to the first embodiment of the present invention.

[0033] Figure 3 This is a schematic diagram of the three-dimensional structure of the detachable connecting pipe according to the first embodiment of the present invention.

[0034] Figure 4 It is a cross-sectional view of a second embodiment of the present invention.

[0035] Figure 5 It is a cross-sectional view of a third embodiment of the present invention.

[0036] Figure 6 This is a partial cross-sectional view of the return air pipe of the third embodiment of the present invention.

[0037] In the figure: 1. Reactor body; 101. Feed pipe; 102. Discharge pipe; 103. Valve assembly; 104. Closing cover; 201. Rotating drive assembly; 202. Stirring center pipe; 203. Stirring branch pipe; 204. Movable pipe; 241. Removable connecting pipe; 242. Snap ring; 243. Connecting plate; 251. Scraper blade; 261. Closing plate; 262. Elastic connector; 263. Guide plate; 271. Inert gas generating device; 272. Air supply pipe; 273. First air pump; 274. Check valve; 275. Lifting frame; 276. Lifting cylinder; 277. Sliding telescopic tube; 278. Annular bearing; 281. Return air hole; 282. Return air pipe; 283. Second air pump; 284. Activated carbon adsorption layer; 285. Vapor-liquid filter. DETAILED DESCRIPTION

[0038] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making any creative efforts shall fall within the scope of protection of the present invention.

[0039] First embodiment

[0040] like Figures 1 to 3 As shown, a crystallization reactor for pharmaceutical preparation comprises a reactor body 1, with a feed pipe 101 connected to the top and a discharge pipe 102 connected to the bottom. Discharge pipe 102 is provided with a valve assembly 103. Feed pipe 101 at the top of reactor body 1 is used to feed raw materials required for pharmaceutical preparation into the reactor, while discharge pipe 102 at the bottom and valve assembly 103 provided on discharge pipe 102 control the output of materials after the reaction is completed. To add materials, feed pipe 101 is opened to add the materials to the reactor. After the reaction is complete, valve assembly 103 is opened to discharge the materials through discharge pipe 102.

[0041] The stirring mechanism includes a rotating drive component 201 arranged at one end of the reactor body 1. The output shaft of the rotating drive component 201 passes through and extends into the reactor body 1 and is fixedly connected to a stirring center tube 202. The other end of the stirring center tube 202 is connected to an inert gas supply component. The gas outlet of the inert gas supply component is rotatably connected to the end of the stirring center tube 202. The rotating drive component 201 of the stirring mechanism drives the stirring center tube 202 to rotate, and the stirring branch tube 203 connected to the side wall of the stirring center tube 202 rotates accordingly, thereby driving the movable tube 204 and the scraper group to rotate, thereby stirring the material in the reactor and promoting the reaction.

[0042] At least one stirring branch pipe 203 is fixedly connected to the side wall of the central stirring pipe 202. A movable pipe 204 is slidably connected to the inner side of the stirring branch pipe 203. The cross-sections of the stirring branch pipe 203 and the movable pipe 204 are non-circular. A scraper assembly is provided at the other end of the movable pipe 204. The scraper assembly includes multiple parallel scraper blades 251 fixedly mounted at the end of the movable pipe 204. The scraper blades 251 have a V-shaped cross-section. At the same time, an inert gas supply assembly supplies gas to the central stirring pipe 202. The inert gas passes through the central stirring pipe 202, the stirring branch pipe 203, the movable pipe 204, and the exhaust gap in sequence. Because the cross-sections of the stirring branch pipe 203 and the movable pipe 204 are non-circular, the movable pipe 204 can slide within the stirring branch pipe 203 without rotating, ensuring that the scraper assembly can stably perform stirring and scraping operations. Under the action of air pressure, the movable tube 204 moves toward and abuts against the inner wall of the reactor body 1 , so that the scraper assembly can fit closely against the inner wall of the reactor and scrape off the crystals attached to the inner wall.

[0043] The gaps between the scraper blades 251 and the gap between the scraper blades 251 and the movable tube 204 are designed as exhaust gaps. Each exhaust gap is equipped with an elastic sealing assembly, which includes a sealing plate 261 for sealing the exhaust gap. Both ends of the sealing plate 261 are connected to the end surface of the movable tube 204 via elastic connectors 262. The cross-section of the sealing plate 261 is designed to be V-shaped. When no air is supplied, the sealing plate 261, under the action of the elastic connectors 262, seals the exhaust gap, preventing material from entering the movable tube 204. When the inert gas supply assembly is supplying air, the air pressure lifts the sealing plate 261, forming a guide airway between the sealing plate 261 and the scraper blades 251.

[0044] The air duct is used to guide the discharge of inert gas, which flushes the surface of scraper blade 251 during the discharge process. On the one hand, the flushing effect can promptly flush away crystals attached to the surface of scraper blade 251, preventing crystals from re-depositing on scraper blade 251 and ensuring the scraping effect of scraper blade 251. On the other hand, the presence of inert gas can also protect the reaction environment, preventing unnecessary reactions between reactants and components in the air, which could affect the quality of pharmaceutical preparation. As the reactor is used for a long time, scraper blade 251 will gradually wear and become thinner due to continuous friction with the inner wall of the reactor to scrape away crystals. However, because the inert gas supply assembly continuously supplies gas, air pressure is always present and continuously acts on movable tube 204. When scraper blade 251 becomes thinner due to wear, the air pressure can still push movable tube 204 to continue moving toward the inner wall of the reactor, allowing the scraper assembly to always fit tightly against the inner wall of the reactor, ensuring that the crystal scraping effect is not affected, and solving the problem of reduced fit caused by wear.

[0045] like Figures 1 to 3 As shown, elastic connector 262 is configured as a flat band, made of a polyurethane elastomer, silicone rubber, or thermoplastic elastomer. These materials have excellent elastic properties. When no air is supplied, elastic connector 262 uses its own elasticity to tighten closing plate 261, tightly fitting it against the end face of movable tube 204, thereby sealing the exhaust gap and preventing material within the reactor from entering the interior of movable tube 204, thereby preventing contamination or damage to the internal structure of movable tube 204 and ensuring the normal operation of the reactor. When the inert gas supply assembly supplies air and the air pressure lifts closing plate 261, elastic connector 262 is stretched and elastically deformed. When the air supply stops or the air pressure changes, elastic connector 262 uses its elastic recovery force to pull closing plate 261 back into place, resealing the exhaust gap and achieving a dynamic balance between closed and open.

[0046] like Figures 1 to 3As shown, guide plates 263 are provided at both ends of the closing plate 261. The guide plates 263 are configured as equilateral trapezoids, and the working surfaces of the guide plates 263 slide and fit against the side edges of the scraper blades 251. The guide airway formed when the closing plate 261 is lifted by air pressure is a circumferential closed conduit consisting of the closing plate 261, the scraper blades 251, and the two guide plates 263. The elastic connectors 262 are connected to the outer walls of the guide plates 263. The equilateral trapezoidal guide plates 263 provided at both ends of the closing plate 261 have working surfaces that slide and fit against the side edges of the scraper blades 251. When the inert gas does not lift up the closing plate 261, the guide plates 263 serve to guide and position the closing plate 261, ensuring that the closing plate 261 can be accurately reset and tightly seal the exhaust gap. When the inert gas supply assembly supplies gas and the air pressure lifts the closing plate 261, due to the presence of the guide plate 263, the guide airway formed when the closing plate 261 is lifted appears as a circumferential closed pipeline composed of the closing plate 261, the scraper blade 251, and the two guide plates 263. This closed pipeline structure can guide the inert gas to be discharged along a specific path, so that the inert gas can be concentrated and effectively flushed on the surface of the scraper blade 251, improving the flushing effect, promptly removing crystals attached to the surface of the scraper blade 251, preventing secondary deposition of crystals, and ensuring the scraping performance of the scraper blade 251. At the same time, the elastic connector 262 is connected to the outer wall of the guide plate 263. During the process of lifting and resetting the closing plate 261, the elastic connector 262 can better control the movement of the closing plate 261 through the guide plate 263, ensuring the formation of the guide airway and the stability of the closure.

[0047] like Figures 1 to 3 As shown, the dimensions and adjacent spacings of each exhaust gap are identical, as are the dimensions and adjacent spacings of each elastic sealing assembly. This uniform design ensures that the inert gas is evenly distributed and flows through each exhaust gap and elastic sealing assembly. During the gas supply process, the inert gas can evenly act on each movable tube 204 and sealing plate 261, ensuring that each scraper assembly receives a similar air pressure driving force. This ensures that each scraper assembly maintains a consistent fit with the inner wall of the reactor, resulting in a more uniform scraping action on the inner wall of the reactor, improving the overall effectiveness of crystal scraping and avoiding the impact on reactor performance and product quality due to incomplete local scraping.

[0048] like Figures 1 to 3As shown, the cross-sections of the stirring branch pipe 203 and the movable pipe 204 are rectangular. The end of the movable pipe 204 facing the inner wall of the reactor is provided with a detachable connecting pipe 241. The scraper assembly and the elastic sealing component are both mounted on the detachable connecting pipe 241. The inner wall of the detachable connecting pipe 241 is provided with a snap ring 242, the outer wall of which snaps and fits with the inner wall of the movable pipe 204. The outer wall of the detachable connecting pipe 241 is provided with multiple connecting plates 243, the inner walls of which fit with the outer wall of the movable pipe 204 and are fixedly connected by bolts. During the long-term operation of the reactor, the scraper blade 251 will gradually wear due to friction with the inner wall of the reactor, resulting in a decrease in scraping effectiveness. In this regard, the design of the detachable connecting pipe 241 plays an important role. With the snap ring 242 on the inner wall of the detachable connecting tube 241 snapping in with the inner wall of the movable tube 204, and the multiple connecting plates 243 on the outer wall of the detachable connecting tube 241 being bolted to the outer wall of the movable tube 204, the operator can easily remove the bolts, remove the detachable connecting tube 241, and replace it with a new detachable connecting tube 241 with a scraper assembly and elastic sealing assembly. This detachable and replaceable method eliminates the need for large-scale disassembly and replacement of the entire movable tube 204 and stirring branch tube 203, reducing maintenance costs and difficulty, improving maintenance efficiency, and ensuring that the reactor can quickly resume normal operation and continue to efficiently scrape crystals.

[0049] like Figures 1 to 3As shown, the inert gas supply assembly is mainly composed of an inert gas generator 271, an air supply pipe 272, a first air pump 273 and a check valve 274. The inert gas generator 271 is used to generate inert gas to provide the required inert gas environment for the reactor. The generated inert gas enters the air supply pipe 272 through the gas outlet. The first air pump 273 installed on the air supply pipe 272 plays the role of conveying gas. It can provide power for the inert gas to flow in the air supply pipe 272 according to a certain pressure and flow rate. By adjusting the power and other parameters of the first air pump 273, the supply speed and pressure of the inert gas can be accurately controlled to meet the demand for the amount of inert gas in different reaction stages. The check valve 274 has the function of preventing gas backflow. During the operation of the reactor, pressure fluctuations may occur within the gas supply pipe 272. The check valve 274 effectively prevents the inert gas from flowing back into the inert gas generator 271, ensuring the stability and safety of the inert gas supply. It also prevents materials or gases within the reactor from flowing back into the gas supply pipe 272, thereby preventing contamination or damage to the inert gas generator 271. The gas outlet of the gas supply pipe 272 is rotatably connected and communicates with the central stirring pipe 202. This allows the gas supply pipe 272 to continue to stably deliver inert gas to the central stirring pipe 202 as the central stirring pipe 202 rotates with the rotary drive assembly 201. After entering the central stirring pipe 202, the inert gas passes through the stirring branch pipe 203, the movable pipe 204, and the exhaust gap, pushing the movable pipe 204 toward the inner wall of the reactor body 1. This allows the scraper assembly to closely adhere to the inner wall of the reactor to perform scraping operations. Simultaneously, a guide air channel is formed to flush the surface of the scraper blade 251, preventing secondary crystal deposition.

[0050] Valve assembly 103 is configured as a solenoid-controlled valve, which features fast response and high control accuracy. During the reactor's operation, the opening and closing of the solenoid-controlled valve can be precisely controlled by an electrical control system. When material needs to be discharged from the reactor, the control system issues a signal, causing the solenoid-controlled valve to open, allowing the material to be smoothly discharged from discharge pipe 102. Once the material is discharged, the control system issues another signal, causing the solenoid-controlled valve to close, preventing further material outflow. This enables precise control of material discharge, ensuring the normal operation of the reactor and the stability of the reaction process.

[0051] The rotation drive assembly 201 is configured as a servo motor or a stepper motor. A servo motor has high precision, high response speed, and good speed regulation performance. It can accurately control the speed and direction of the output shaft according to the instructions of the control system, thereby driving the central stirring tube 202, the stirring branch tube 203, the movable tube 204, and the scraper assembly to rotate stably, achieving uniform stirring of the materials in the reactor and promoting the reaction. At the same time, the servo motor can also adjust the speed in real time according to the different stages and requirements of the reaction to meet various complex reaction conditions. A stepper motor has the advantages of high positioning accuracy and simple control. It can convert electrical pulse signals into angular displacement or linear displacement. By controlling the number and frequency of pulses, the rotation angle and speed of the stepper motor can be precisely controlled. In the reactor, the stepper motor can accurately control the rotation of the stirring mechanism according to a preset program, ensuring the stability and repeatability of the stirring process, which is conducive to improving the quality and efficiency of pharmaceutical preparation.

[0052] Second embodiment

[0053] like Figure 4 As shown, the outer wall of the reactor body 1 is connected to the rotation drive assembly 201 through a lifting assembly, and the lifting assembly includes a lifting frame 275 fixedly arranged on the outer wall of the reactor body 1, and a lifting liquid cylinder 276 is fixedly arranged on the lifting frame 275. The movable part of the lifting liquid cylinder 276 is fixedly connected to the rotation drive assembly 201, and the output shaft of the rotation drive assembly 201 is slidingly connected to the reactor body 1. The stirring center tube 202 is connected to the air supply pipe 272 through a sliding telescopic tube 277. The sliding telescopic tube 277 and the air supply pipe 272 are rotatably connected through an annular bearing 278. The sliding telescopic tube 277 consists of two sliding tubes that are slidably fitted and nested.

[0054] like Figure 4As shown, the lifting assembly is mainly composed of a lifting frame 275 fixed to the outer wall of the reactor body 1 and a lifting cylinder 276, and the movable part of the lifting cylinder 276 is fixedly connected to the rotation drive assembly 201. When it is necessary to adjust the rotation drive assembly 201 and then adjust the relative position of the stirring mechanism and the reactor body 1, the lifting cylinder 276 comes into play. By controlling the hydraulic system of the lifting cylinder 276, the movable part of the lifting cylinder 276 is made to perform telescopic movement. This lifting and adjusting function has multiple practical significances. During the installation or later maintenance of the reactor, if the stirring mechanism conflicts with other components inside the reactor body 1 in terms of installation position, or if the stirring mechanism needs to be inspected or parts replaced, the lifting assembly can be used to lift the rotation drive assembly 201 together with the stirring mechanism as a whole, thereby providing the operator with sufficient operating space to facilitate related operations. In some special pharmaceutical preparation reactions, it may be necessary to change the contact depth or stirring position between the stirring mechanism and the material in the reactor to obtain a better reaction effect. The position of the rotary drive assembly 201 is adjusted by the lifting assembly, thereby changing the position of the stirring central tube 202 in the reactor, thereby meeting the stirring condition requirements of different reaction processes.

[0055] like Figure 4 As shown, the output shaft of the rotary drive assembly 201 is slidably connected to the reactor body 1. This design facilitates the lifting and lowering motion of the lifting assembly. As the lifting assembly drives the rotary drive assembly 201 up and down, the output shaft slides correspondingly on the reactor body 1 without affecting the rotary drive assembly 201's ability to drive the central stirring tube 202. This sliding connection ensures that the central stirring tube 202 can continue to rotate normally even when the stirring mechanism is adjusted, stirring the materials within the reactor and ensuring the continuity and stability of the reaction.

[0056] like Figure 4As shown, the mixing center tube 202 is connected to the air supply tube 272 via a sliding telescopic tube 277. The sliding telescopic tube 277 and the air supply tube 272 are rotatably connected via an annular bearing 278. The sliding telescopic tube 277 consists of two sliding tubes that slide and fit together. Because the lifting assembly drives the rotation drive assembly 201 and the mixing center tube 202 up and down, the two sliding tubes of the sliding telescopic tube 277 can slide relative to each other, thereby adapting to changes in the distance between the mixing center tube 202 and the air supply tube 272. When the mixing center tube 202 rises, the two sliding tubes slide relative to each other and extend; when the mixing center tube 202 descends, the two sliding tubes slide relative to each other and shorten, ensuring that the inert gas is consistently delivered from the air supply tube 272 to the mixing center tube 202, ensuring a continuous inert gas supply. The sliding telescopic tube 277 and the air supply tube 272 are rotatably connected via an annular bearing 278. This allows the sliding telescopic tube 277 to rotate with the mixing center tube 202 as it rotates, while also ensuring a tight seal between the two. The presence of the annular bearing 278 reduces the friction during rotation, making the rotation of the stirring center tube 202 smoother, and also prevents the leakage of inert gas at the connection, ensuring the stability of the inert gas environment in the reactor and ensuring the normal progress of the reaction.

[0057] Third embodiment

[0058] like Figures 5 to 6 As shown, a sealing cover 104 movably connected to the top of the feed tube 101 is used to seal the feed tube 101 during normal operation of the reactor. When material needs to be added to the reactor, the sealing cover 104 is opened, and the material enters the reactor through the feed tube 101. After the addition is completed, the sealing cover 104 is closed to prevent the gas, heat, and material in the reactor from leaking into the external environment, maintaining stable reaction conditions inside the reactor and ensuring the normal progress of the reaction. It also prevents external impurities from entering the reactor and affecting the quality of the pharmaceutical preparation.

[0059] like Figures 5 to 6As shown, the return air hole 281 opened at the top of the reactor body 1 is connected to the return air pipe 282, and the return air pipe 282 is connected to one end of the air supply pipe 272 near the inert gas generator 271, and a second air pump 283 is provided on the return air pipe 282. During the reaction process, some gas will be generated in the reactor. If these gases cannot be discharged in time, the pressure in the reactor will increase, affecting the progress of the reaction and may even cause a safety accident. By providing the return air hole 281 and the return air pipe 282, the gas in the reactor can enter the return air pipe 282 through the return air hole 281. The function of the second air pump 283 is to provide power for the circulation of the gas. It pumps the gas in the return air pipe 282 back to one end of the air supply pipe 272 near the inert gas generator 271, so that the gas re-enters the inert gas supply system, realizing the recycling of the gas. This recycling method can not only reduce the consumption of inert gas and reduce production costs, but also maintain the stability of the inert gas environment in the reactor, which is conducive to the progress of the reaction.

[0060] The multi-layer activated carbon adsorption layer 284 within the return air pipe 282 primarily purifies the circulating gas. During the reaction process, the gas generated within the reactor may contain harmful substances, odor molecules, or tiny particulate impurities. When the gas passes through the activated carbon adsorption layer 284, the activated carbon, with its numerous microporous structures, can adsorb harmful substances, odor molecules, and particulate impurities in the gas, thereby purifying the gas. The purified gas is then pumped back into the inert gas supply system and into the reactor, preventing the accumulation of harmful substances within the reactor, ensuring a clean reaction environment and the quality of pharmaceutical preparation. The vapor-liquid filter 285 located at the return air hole 281 prevents liquid or solid particles from entering the return air pipe 282 along with the gas. During the reaction process, liquid may splash or solid particles may become suspended within the reactor. Without the vapor-liquid filter 285, these liquids and solid particles would enter the return air pipe 282, potentially blocking it, affecting the normal circulation of the gas, and even damaging equipment such as the second air pump 283. The gas-liquid filter 285 can intercept liquid and solid particles and only allow gas to pass through, thereby ensuring the smooth flow of the return gas pipe 282 and the normal operation of the gas circulation system.

[0061] The above are only specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions, or modifications based on the present invention to solve substantially the same technical problems and achieve substantially the same technical effects are all within the scope of protection of the present invention.

Claims

1. A crystallization reactor for pharmaceutical preparation, characterized in that: include: A reactor body (1), wherein the top of the reactor body (1) is connected to a feed pipe (101) and the bottom is connected to a discharge pipe (102), and a valve assembly (103) is provided on the discharge pipe (102); A stirring mechanism, the stirring mechanism comprising a rotation drive assembly (201) arranged at one end of the reactor body (1), an output shaft of the rotation drive assembly (201) passing through and extending into the reactor body (1) and fixedly connected to a stirring central tube (202), the other end of the stirring central tube (202) being connected to an inert gas supply assembly, and a gas outlet of the inert gas supply assembly being rotationally connected to the end of the stirring central tube (202); The side wall of the central stirring tube (202) is fixedly connected to at least one stirring branch tube (203), and a movable tube (204) is slidably connected to the inside of the stirring branch tube (203), and the cross sections of the stirring branch tube (203) and the movable tube (204) are configured to be non-circular; a scraper assembly is provided at the other end of the movable tube (204), and the scraper assembly includes a plurality of parallel scraper blades (251) fixedly provided at the end of the movable tube (204), and the cross sections of the scraper blades (251) are configured to be V-shaped; The gaps between the scraper blades (251) and the gap between the scraper blades (251) and the movable tube (204) are all set as exhaust gaps, and an elastic sealing component is provided at each exhaust gap. The elastic sealing component includes a sealing plate (261) for sealing the exhaust gap, and both ends of the sealing plate (261) are connected to the end surface of the movable tube (204) through an elastic connecting piece (262). The cross section of the sealing plate (261) is set to be V-shaped; When the inert gas supply assembly supplies gas, the inert gas passes through the stirring central tube (202), the stirring branch tube (203), the movable tube (204) and the exhaust gap in sequence; under the action of air pressure, the movable tube (204) moves toward and abuts against the inner wall of the reactor body (1), and the closing plate (261) is lifted up to form a guide air channel with the scraper blade (251), and the guide air channel is used to guide the inert gas to be discharged and flush the surface of the scraper blade (251).

2. The crystallization reactor for pharmaceutical preparation according to claim 1, characterized in that: The elastic connecting member (262) is configured as a flat strap, and the material of the elastic connecting member (262) is one of polyurethane elastomer, silicone rubber or thermoplastic elastomer.

3. The crystallization reactor for pharmaceutical preparation according to claim 2, characterized in that: Guide plates (263) are provided at both ends of the closing plate (261), and the guide plates (263) are configured as equilateral trapezoids. The working surfaces of the guide plates (263) are slidably fitted with the side edges of the scraper blades (251). The guide air channel formed when the closing plate (261) is lifted by air pressure is a circumferential closed pipeline consisting of the closing plate (261), the scraper blades (251) and the two guide plates (263). The elastic connector (262) is connected to the outer wall of the guide plate (263).

4. The crystallization reactor for pharmaceutical preparation according to claim 3, characterized in that: The size of each exhaust gap and the adjacent spacing distance are the same, and the size of each elastic sealing component and the adjacent spacing distance are the same.

5. The crystallization reactor for pharmaceutical preparation according to claim 4, characterized in that: The cross sections of the stirring branch pipe (203) and the movable pipe (204) are rectangular. The end of the movable pipe (204) facing the inner wall of the reactor is provided as a detachable connecting pipe (241). The scraper assembly and the elastic sealing component are both provided on the detachable connecting pipe (241). The inner wall of the detachable connecting pipe (241) is provided with a clamping ring (242). The outer wall of the clamping ring (242) is clamped and adapted to the inner wall of the movable pipe (204). The outer wall of the detachable connecting pipe (241) is provided with a plurality of connecting plates (243). The inner walls of the connecting plates (243) are adapted to the outer wall of the movable pipe (204) and are fixedly connected by bolts.

6. The crystallization reactor for pharmaceutical preparation according to claim 1, characterized in that: The inert gas supply assembly comprises an inert gas generating device (271), the gas outlet of the inert gas generating device (271) is connected to a gas supply pipe (272), a first air pump (273) and a check valve (274) are installed on the gas supply pipe (272), and the gas outlet of the gas supply pipe (272) is rotatably connected to and communicates with the stirring center pipe (202).

7. The crystallization reactor for pharmaceutical preparation according to claim 6, characterized in that: The outer wall of the reactor body (1) is connected to the rotation drive assembly (201) through a lifting assembly, the lifting assembly comprising a lifting frame (275) fixedly arranged on the outer wall of the reactor body (1), a lifting liquid cylinder (276) fixedly arranged on the lifting frame (275), a movable portion of the lifting liquid cylinder (276) fixedly connected to the rotation drive assembly (201), an output shaft of the rotation drive assembly (201) slidingly connected to the reactor body (1), the stirring center tube (202) being connected to the air supply pipe (272) through a sliding telescopic tube (277), the sliding telescopic tube (277) being rotationally connected to the air supply pipe (272) through an annular bearing (278), and the sliding telescopic tube (277) consisting of two sliding tubes that are slidably fitted and nested.

8. The crystallization reactor for pharmaceutical preparation according to claim 6, characterized in that: The top of the feed pipe (101) is movably connected to a closed cover plate (104), and the top of the reactor body (1) is provided with a return air hole (281); the return air hole (281) is connected to a return air pipe (282), and the return air pipe (282) is connected to one end of the air supply pipe (272) close to the inert gas generating device (271); a second air pump (283) is provided on the return air pipe (282), and multiple layers of activated carbon adsorption layers (284) are provided in the return air pipe (282), and a gas-liquid filter (285) is provided at the return air hole (281).

9. The crystallization reactor for pharmaceutical preparation according to claim 1, characterized in that: The valve assembly (103) is configured as an electromagnetic control valve, and the rotation drive assembly (201) is configured as a servo motor or a stepping motor.

Citation Information

Patent Citations

  • Metronidazole crystallization reaction kettle

    CN218307932U

Cited By

  • Vacuum stirring type material preparation device

    CN122057412A

  • A vacuum-stirred material preparation device

    CN122057412B