Preparation device and method of high-purity landiolol hydrochloride

Abstract

The application relates to the technical field of medicine preparation, in particular to a preparation device and method of high-purity landiolol hydrochloride, which comprises a water bath heating tank, a filtering structure communicated with the lower part of the water bath heating tank through a valve assembly, a cooling liquid storage tank communicated with the lower part of the filtering structure, a semiconductor refrigeration device installed on the outside of the cooling liquid storage tank, a first heat exchange unit installed on the outside of the water bath heating tank, and a second heat exchange unit communicated with the first heat exchange unit and installed on the outside of the semiconductor refrigeration device; from adding a crude solution, heating, filtering, cooling crystallization to equipment resetting, a coherent production process is formed; when a batch of purification is finished, the water bath heating tank is communicated with the cooling liquid storage tank, and the filtering assembly is reset, so that the next batch of production can be immediately started without long-time waiting for equipment adjustment, the production cycle is greatly shortened, the demand for continuity in large-scale industrial production is met, and the yield is significantly improved compared with a traditional intermittent production mode.

Description

Technical Field

[0001] This invention relates to the field of drug preparation technology, specifically to an apparatus and method for preparing high-purity landilol hydrochloride. Background Technology

[0002] Landilol hydrochloride is an ultra-short-acting β1-receptor blocker, mainly used to treat tachyarrhythmias. It can effectively reduce heart rate and reduce cardiac load, playing a key role in the emergency treatment of cardiovascular diseases such as acute myocardial infarction and unstable angina.

[0003] Currently, in the preparation of brandylol hydrochloride, the purification stage is the key link that determines product quality and production efficiency. Traditional purification processes often use recrystallization, which typically involves several steps: preparing a hot saturated solution, hot filtration, and cooling crystallization. Traditional purification methods are inefficient and consume a lot of production equipment operating time during the purification process, making it difficult to improve production efficiency. This cannot meet the urgent need for efficient and continuous preparation of high-purity brandylol hydrochloride in large-scale industrial production. Therefore, a high-purity brandylol hydrochloride preparation device and method are proposed to improve the purification efficiency of brandylol hydrochloride and achieve continuous production. Summary of the Invention

[0004] To address the problems in the prior art, this invention provides an apparatus and method for preparing high-purity brandylol hydrochloride, thereby improving the purification efficiency of brandylol hydrochloride and enabling continuous production.

[0005] The technical solution adopted by the present invention to solve its technical problem is a preparation device and method for high-purity brandylol hydrochloride, including a water bath heating tank and a filter structure connected to the lower part of the water bath heating tank through a valve assembly. The lower part of the filter structure is connected to a cooling liquid storage tank. A semiconductor refrigeration device is installed on the outside of the cooling liquid storage tank. A first heat exchange unit is installed on the outside of the water bath heating tank. A second heat exchange unit connected to the first heat exchange unit is installed on the outside of the semiconductor refrigeration device.

[0006] Specifically, the filter assembly includes a frame connecting the valve assembly and the coolant reservoir. Both sides of the frame are connected to the protective shell via grooves. Inside the protective shell, filter frames with upward openings are slidably sealed. The bottom of the filter frames is provided with filter holes. The front and rear sides of the filter frames are slidably sealed to the inner wall of the frame. Springs are connected between the two sets of filter frames on the opposite sides and the protective shell. Filter plates are inserted into the sides of the filter frames.

[0007] Specifically, the filter frame has a mounting groove on one side that slides with the filter plate, the filter plate is located at the bottom inside the filter frame, and the protective shell has an opening on the side corresponding to the mounting groove.

[0008] Specifically, the filter plate has an embedding groove at the bottom of the inner side of the filter frame, and an expansion pad that expands and presses the upper edge of the filter plate.

[0009] Specifically, the valve assembly includes a valve whose upper end is connected to the flange of the water bath heating tank, and the lower end of the valve is fixedly connected to the upper surface of the frame through a flange connector.

[0010] Specifically, the bottom of the cooling liquid storage tank is fixedly connected to the first drive motor, and the output shaft of the first drive motor is provided with several sets of circumferentially distributed primary stirring blades. The lower part of the cooling liquid storage tank is connected to the discharge pipe. The semiconductor refrigeration device includes several sets of semiconductor refrigeration chips connected to the outside of the cooling liquid storage tank. A negative pressure pump is connected to the cooling liquid storage tank.

[0011] Specifically, the first heat exchange unit includes several sets of arc-shaped heat exchange plates arranged on the outside of the water bath heating tank. Each arc-shaped heat exchange plate is provided with a first circulation channel. The upper end of the first circulation channel is connected to a first liquid inlet connector, and the lower end of the first circulation channel is connected to a first liquid outlet connector.

[0012] The second heat exchange unit includes several sets of planar heat exchange plates disposed on one side of the semiconductor cooling chip. The planar heat exchange plates correspond to the arc-shaped heat exchange plates. Each planar heat exchange plate is provided with a second circulation channel. The upper end of the second circulation channel is connected to the second liquid outlet connector. The second liquid outlet connector is connected to the first liquid inlet connector through a pipeline. The lower end of the second circulation channel is connected to the second liquid inlet connector. The first liquid outlet connector is connected to the second liquid inlet connector through a pipeline.

[0013] Specifically, the upper surface of the water bath heating tank is connected to a first connector and a second connector. A second drive motor is installed on the upper part of the water bath heating tank. The output shaft of the second drive motor is equipped with several sets of circumferentially distributed secondary stirring blades. A pressure relief valve is connected to the upper surface of the water bath heating tank.

[0014] Specifically, a reinforced support structure is fixedly connected between the upper surface of the water bath heating tank and the cooling liquid storage tank 2; several sets of vertically arranged support legs are fixedly connected to the lower end of the cooling liquid storage tank.

[0015] The beneficial effects of this invention are:

[0016] The apparatus for preparing high-purity brandylol hydrochloride described in this invention forms a continuous production process, from adding crude solution, heating, filtering, cooling and crystallizing, to equipment reset. When one batch of purification is completed, the heating tank and cooling storage tank are connected, the filter components are reset, and the next batch of production can be started immediately without waiting for a long time for equipment adjustment, which greatly shortens the production cycle and meets the continuous production requirements of large-scale industrial production. Compared with the traditional intermittent production method, the output is significantly increased.

[0017] The apparatus for preparing high-purity brandylol hydrochloride described in this invention utilizes the negative pressure generated by the cooling storage tank, combined with gravity, to accelerate the passage of the hot saturated solution through the filtration structure. The negative pressure generates suction, which, together with gravity, enhances the driving force of the hot saturated solution. Simultaneously, it alters the pressure distribution of the solution on the filter plate, allowing the solution to be more evenly distributed on the filter plate surface, reducing filtration time and improving overall production efficiency.

[0018] The present invention discloses a device for preparing high-purity brandylol hydrochloride, wherein the first heat exchange unit and the second heat exchange unit are interconnected to form a liquid circulation system, and the liquid circulation is driven by the semiconductor refrigeration device during refrigeration, thereby achieving the heating effect on the water bath heating tank.

[0019] The apparatus for preparing high-purity brandylol hydrochloride described in this invention features an opening on the side of the protective shell that facilitates the installation and removal of the filter plate. It also allows for indirect monitoring of the liquid transport within the water bath heating tank by observing the movement of the filter frame. Under normal circumstances, when the water bath heating tank contains a hot saturated solution, the negative pressure of the cooling storage tank keeps the filter frame in its moved position for filtration. Once the solution transport is complete, the filter frame resets under spring action. Operators can then promptly assess the production progress and perform subsequent operations such as cleaning the filter plate and preparing the next batch of solution, thus improving the convenience and accuracy of production management. Attached Figure Description

[0020] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0021] Figure 1 This is an isometric view of the present invention;

[0022] Figure 2 This is a partial cross-sectional schematic diagram of the arc-shaped heat exchange plate and the planar heat exchange plate of the present invention;

[0023] Figure 3 for Figure 2 Enlarged view of region A;

[0024] Figure 4 for Figure 2 Enlarged view of region B;

[0025] Figure 5 This is a schematic diagram of the internal structure of the water bath heating tank of the present invention;

[0026] Figure 6 This is a schematic diagram of the internal structure of the cooling liquid storage tank of the present invention;

[0027] Figure 7 This is a schematic diagram of the internal structure of the frame of the present invention;

[0028] Figure 8 This is a schematic cross-sectional view of the frame structure of the present invention;

[0029] Figure 9 for Figure 8 Enlarged view of region D;

[0030] Figure 10 for Figure 8 Enlarged view of region E;

[0031] In the diagram: 1. Water bath heating tank; 2. Cooling liquid storage tank; 3. Frame; 4. Slide groove; 5. Protective shell; 6. Filter frame; 7. Filter hole; 8. Spring; 9. Filter plate; 10. Mounting groove; 11. Opening; 12. Embedded groove; 13. Expansion pad; 14. Valve; 15. First drive motor; 16. First stage stirring blade; 17. Discharge pipe; 18. Semiconductor refrigeration chip; 19. Arc-shaped heat exchange plate; 20. First circulation channel; 21. First liquid inlet connector; 22. First liquid outlet connector; 23. Flat heat exchange plate; 24. Second circulation channel; 25. Second liquid outlet connector; 26. Second liquid inlet connector; 27. First connector; 28. Second connector; 29. ​​Second drive motor; 30. Second stage stirring blade; 31. Pressure relief valve; 32. Reinforced support structure; 33. Support leg; 34. Negative pressure pump. Detailed Implementation

[0032] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0033] To improve the purification efficiency of brandylol hydrochloride and achieve continuous production, as one embodiment of the present invention, such as... Figure 1 , Figure 2 As shown, the apparatus and method for preparing high-purity brandylol hydrochloride according to the present invention includes a water bath heating tank 1 and a filter structure connected to the lower part of the water bath heating tank 1 via a valve assembly. The lower part of the filter structure is connected to a cooling liquid storage tank 2. A semiconductor refrigeration device is installed on the outside of the cooling liquid storage tank 2. A first heat exchange unit is installed on the outside of the water bath heating tank 1, and a second heat exchange unit connected to the first heat exchange unit is installed on the outside of the semiconductor refrigeration device.

[0034] When using this device to prepare high-purity brandylol hydrochloride, the crude solution containing brandylol hydrochloride and the recrystallization solvent are first transported to the water bath heating tank 1 in a certain proportion.

[0035] After the semiconductor refrigeration device is put into operation, it transfers the heat from the cooling liquid storage tank 2 to the second heat exchange unit, thereby cooling the cooling liquid storage tank 2 and heating the second heat exchange unit. After being heated, the liquid inside the second heat exchange unit expands and moves upward, thus promoting liquid circulation. At the same time, the liquid moves upward and enters the first heat exchange unit, which heats the water bath heating tank 1. The temperature of the liquid decreases after passing through the first heat exchange unit, causing the liquid to begin to move downward, thereby further facilitating liquid circulation.

[0036] After the water bath heating tank 1 is heated, the crude solution of brandylol hydrochloride and the recrystallization solvent in the tank are heated. When preparing high-purity brandylol hydrochloride, there are a variety of impurities in the crude solution. Heating increases the solubility of brandylol hydrochloride in the solution, which makes subsequent filtration and crystallization separation more convenient.

[0037] As the semiconductor refrigeration device continuously cools the cooling liquid tank 2, the temperature inside the cooling liquid tank 2 continues to drop. The air inside the tank contracts when it gets cold, thus generating negative pressure. Since the lower part of the filter structure is connected to the cooling liquid tank 2, the components in the filter structure will move under the action of negative pressure. When the filter structure moves to a certain position, it is convenient to perform subsequent filtration operations on the hot saturated solution in the water bath heating tank 1 after heating.

[0038] When the valve assembly is opened, the hot saturated solution in the water bath heating tank 1 flows into the filter structure through the valve assembly under the combined action of gravity and the negative pressure of the cooling storage tank 2. The filter structure filters the hot saturated solution, reducing the filtration time and improving the overall production efficiency.

[0039] The filtered solution flows smoothly into the cooling storage tank 2 through the lower part of the filter structure. The filtrate entering the cooling storage tank 2 begins to cool and crystallize under the low-temperature environment created by the continuous cooling of the semiconductor refrigeration device. The solubility of brandylol hydrochloride decreases at low temperatures, and it gradually precipitates out of the solution in the form of crystals. After the crystallization process is completed, the mixture containing crystals in the cooling storage tank 2 is discharged. After discharge, the crystals are separated from the mother liquor by a separation device, and then the crystals are dried to obtain dry, high-purity brandylol hydrochloride crystals.

[0040] After the liquid in the heating tank is discharged, the air in the heating tank enters the cooling liquid storage tank 2, and the air pressure in the cooling liquid storage tank 2 rises rapidly. At this time, the filter assembly automatically resets and moves to its initial state, which can be used to clean the filter assembly and facilitate the subsequent filtration of the next batch of hot saturated solution. After the purification of one batch is completed, the filter assembly resets and the valve assembly can be closed, and then the next batch of production can be quickly put into operation. From adding crude solution, heating, filtering, cooling and crystallization, to equipment reset, a continuous production process is formed, which meets the continuous production requirements of large-scale industrial production and improves production efficiency and output.

[0041] To improve filtration speed, for example, such as Figure 1 , Figure 2 , Figure 7 , Figure 8 , Figure 9 , Figure 10 As shown, the present invention also includes a filter assembly comprising a frame 3 connecting the valve assembly and the cooling liquid tank 2. Both sides of the frame 3 are connected to a protective shell 5 via a sliding groove 4. Filter frames 6 with upward openings are respectively sealed and slidably connected inside the protective shell 5. Filter frames 6 have filter holes 7 at their bottom. The front and rear sides of the filter frames 6 are sealed and slidably connected to the inner wall of the frame 3. Springs 8 are connected between the two sets of filter frames 6 on opposite sides and the protective shell 5. Filter plates 9 are inserted into the sides of the filter frames 6.

[0042] When in use, before the filter assembly is activated, insert the filter plate 9 into the side of the filter frame 6 to ensure the overall sealing of the filter frame 6. When the cooling liquid tank 2 generates negative pressure, since the lower part of the filter assembly is connected to the cooling liquid tank 2, under the action of negative pressure, the filter frame 6 will overcome the elastic force of the spring 8 and slide along the sliding grooves 4 on both sides of the frame 3 towards the cooling liquid tank 2, so that the two sets of filter frames 6 are close to each other, which is convenient for filtering the heated saturated solution after heating.

[0043] When the valve assembly is opened, the hot saturated solution in the water bath heating tank 1 will flow downward naturally under the action of gravity, while the cooling liquid tank 2 will generate negative pressure under the continuous cooling of the semiconductor refrigeration device. Since the lower part of the filter structure is connected to the cooling liquid tank 2, the hot saturated solution is subjected to a stronger driving force under the combined action of gravity and negative pressure, which accelerates the flow towards the filter structure and increases the feeding speed.

[0044] When the hot saturated solution flows into the frame 3 from the valve assembly, various impurities in the solution are intercepted by the filter plate 9 as the hot saturated solution passes through the filter plate 9, thus initially achieving solid-liquid separation. During normal gravity filtration, the filter plate 9 will generate a certain resistance to the filtration of the solution, affecting the feeding speed. However, the presence of negative pressure causes the pressure distribution of the solution on the filter plate 9 to change. The suction force generated by the negative pressure makes the solution more evenly distributed on the surface of the filter plate 9, further improving the filtration speed.

[0045] To facilitate cleaning of filter plate 9, for example, such as Figure 7 , Figure 8 , Figure 9 , Figure 10 As shown, the present invention also includes a mounting groove 10 on one side of the filter frame 6 that is slidably connected to the filter plate 9, the filter plate 9 being located at the bottom inside the filter frame 6, and an opening 11 corresponding to the mounting groove 10 on the side of the protective shell 5.

[0046] When in use, the filter plate 9 can be inserted along the mounting groove 10 on one side of the filter frame 6. When the device is running, the cooling liquid storage tank 2 generates negative pressure, which drives the filter frame 6 to move, making it easier to filter the solution later.

[0047] After the solution in the water bath heating tank 1 is delivered, the cooling liquid storage tank 2 is connected to the water bath heating tank 1. At this time, the air pressure in the cooling liquid storage tank 2 rises rapidly. The filter frame 6 is reset and moved to the initial state by the spring 8. At this time, the filter plate 9 can be slid out along the mounting groove 10 from the opening 11 on the side of the protective shell 5 to clean the filter plate 9.

[0048] The opening 11 on the side of the protective shell 5 is not only used for the installation and removal of the filter plate 9, but also provides convenience for observing the status of the filter frame 6. The movement of the filter frame 6 can be used to indirectly detect the liquid delivery status in the water bath heating tank 1. Under normal circumstances, when there is a hot saturated solution in the water bath heating tank 1, the negative pressure of the cooling liquid storage tank 2 will keep the filter frame 6 in the moved position for filtration. Once the solution delivery in the water bath heating tank 1 is completed, the cooling liquid storage tank 2 is connected to the water bath heating tank 1, and the filter frame 6 will reset and move to the initial state under the action of the spring 8. Therefore, the operator can judge whether the liquid delivery in the water bath heating tank 1 is completed by observing whether the filter frame 6 has reset. This method provides an intuitive reference indicator for monitoring the entire preparation process, which helps the operator to perform subsequent operations in a timely manner, such as cleaning the filter plate 9 and preparing the next batch of solution, thereby improving production efficiency.

[0049] To ensure the stability of filter plate 9 during the filtration process, for example, such as... Figure 8 , Figure 10 As shown, the present invention also includes an embedding groove 12 provided above the filter plate 9 and located at the bottom of the inner side of the filter frame 6, and an expansion pad 13 provided in the embedding groove 12 to expand and press the upper edge of the filter plate 9.

[0050] When in use, the filter plate 9 is inserted into the mounting groove 10 on the side of the filter frame 6. At this time, the expansion pad 13 is in an unexpanded state. When the cooling liquid tank 2 generates negative pressure, the filter frame 6 slides along the sliding grooves 4 on both sides of the frame 3 under the negative pressure. At the same time, the expansion pad 13 expands under the negative pressure environment. The expanded expansion pad 13 will squeeze the upper edge of the filter plate 9 and fix the filter plate 9 tightly in the filter frame 6. This not only ensures the stability of the filter plate 9 during the filtration process, but also enhances the sealing between the filter plate 9 and the filter frame 6. This prevents the hot saturated solution from directly entering the cooling liquid tank 2 through the gap without being filtered by the filter plate 9, ensuring the accuracy and effect of filtration and helping to obtain higher purity brandylol hydrochloride products.

[0051] For example, such as Figure 2 As shown, the present invention also includes a valve assembly comprising a valve 14 whose upper end is connected to a flange of the water bath heating tank 1, and the lower end of the valve 14 is fixedly connected to the upper surface of the frame 3 via a flange connector.

[0052] When in use, valve 14 is opened, and the hot saturated solution flows into the frame 3 for filtration under the action of gravity and the negative pressure of the cooling storage tank 2.

[0053] To improve the quality and purity of crystals, for example, such as Figure 1 , Figure 3 , Figure 6 As shown, the present invention also includes a first drive motor 15 fixedly connected to the bottom of the cooling liquid storage tank 2, a plurality of circumferentially distributed first-stage stirring blades 16 on the output shaft of the first drive motor 15, a discharge pipe 17 connected to the lower part of the cooling liquid storage tank 2, a semiconductor refrigeration device including a plurality of semiconductor refrigeration chips 18 connected to the outside of the cooling liquid storage tank 2, and a negative pressure pump 34 connected to the cooling liquid storage tank 2.

[0054] When in use, after the solution containing landilol hydrochloride flows into the cooling storage tank 2 through filtration, the first drive motor 15 is started and the output shaft of the first drive motor 15 starts to rotate, driving the first stage stirring blade 16 to rotate synchronously. At the same time, the semiconductor cooling chip 18 cools the cooling storage tank 2. After the solution is cooled and crystallized, the discharge pipe 17 is opened to discharge the mixture containing crystals.

[0055] The primary stirring blade 16 rotates under the drive of the first drive motor 15, which can make the solution in the cooling storage tank 2 evenly mixed. During the cooling crystallization process, stirring can make the hydrochloric acid brandylol molecules in the solution come into contact with the low temperature environment more evenly, avoid local overcooling or overheating, promote more uniform crystal precipitation, and improve the quality and purity of crystallization.

[0056] The negative pressure pump 34 can quickly extract gas from the cooling liquid storage tank 2, rapidly forming a stronger negative pressure, further providing a stable and powerful negative pressure environment, and ensuring the negative pressure effect of the cooling liquid storage tank 2.

[0057] To improve energy efficiency, for example, such as Figure 1 , Figure 2 , Figure 3 , Figure 4 As shown, the present invention also includes a first heat exchange unit comprising a plurality of arc-shaped heat exchange plates 19 disposed on the outside of the water bath heating tank 1, each arc-shaped heat exchange plate 19 being provided with a first circulation channel 20, the upper end of the first circulation channel 20 being connected to a first liquid inlet connector 21, and the lower end of the first circulation channel 20 being connected to a first liquid outlet connector 22.

[0058] The second heat exchange unit includes several sets of planar heat exchange plates 23 disposed on one side of the semiconductor cooling chip 18. The planar heat exchange plates 23 correspond to the arc-shaped heat exchange plates 19. Each planar heat exchange plate 23 is provided with a second circulation channel 24. The upper end of the second circulation channel 24 is connected to the second liquid outlet connector 25. The second liquid outlet connector 25 is connected to the first liquid inlet connector 21 through a pipeline. The lower end of the second circulation channel 24 is connected to the second liquid inlet connector 26. The first liquid outlet connector 22 is connected to the second liquid inlet connector 26 through a pipeline.

[0059] During use, in the preparation process, as the semiconductor refrigeration chip 18 operates, the cooling liquid tank 2 is cooled, while the flat heat exchange plate 23 is heated by the semiconductor refrigeration chip 18. After being heated, the liquid in the flat heat exchange plate 23 automatically moves upward and enters the first liquid inlet 21 of the arc-shaped heat exchange plate 19 through the second liquid outlet 25. It can then pass through the arc-shaped heat exchange plate 19 and heat the water bath heating tank 1. The temperature of the liquid drops after passing through the arc-shaped heat exchange plate 19, which further facilitates the downward movement of the liquid. After the liquid in the arc-shaped heat exchange plate 19 moves downward, it is discharged through the first liquid outlet 22 and enters the second liquid inlet 26, thereby promoting the circulation of the liquid between the first heat exchange unit and the second heat exchange unit.

[0060] The interconnected design of the first circulation channel 20 and the second circulation channel 24 enables the liquid to circulate between the two heat exchange units. On the one hand, the heat transported by the semiconductor cooling chip 18 allows the liquid in the second heat exchange unit to flow, ensuring that heat can be continuously transferred to the first heat exchange unit. On the other hand, after the liquid in the first heat exchange unit cools down, the liquid flows back to the second heat exchange unit, so that the heat is recycled and the energy utilization rate is improved.

[0061] It should be noted that the first circulation channel 20 of the present invention includes several sets of arc-shaped channels distributed vertically and arranged horizontally, and adjacent first channels are connected by arc-shaped channels. The second circulation channel 24 includes several sets of heat exchange tubes distributed vertically and arranged horizontally, and adjacent heat exchange tubes are connected by elbows.

[0062] For example, such as Figure 1 , Figure 5 As shown, the present invention also includes a first connector 27 and a second connector 28 connected to the upper surface of the water bath heating tank 1, a second drive motor 29 installed on the upper part of the water bath heating tank 1, a plurality of circumferentially distributed secondary stirring blades 30 provided on the output shaft of the second drive motor 29, and a pressure relief valve 31 connected to the upper surface of the water bath heating tank 1.

[0063] When using it, in the preparation of high-purity brandylol hydrochloride, crude solution and recrystallization solvent and other raw materials are added into the water bath heating tank 1 through the first connector 27 and the second connector 28. The second drive motor 29 is started, and the output shaft drives the secondary stirring blade 30 to rotate, stirring the added solution and making the various solutions added into the water bath heating tank 1 fully mixed. The uniform solution helps to improve the effect of subsequent reaction and crystallization, making the solution uniformly mixed.

[0064] After the solution is mixed, the water bath heating tank 1 is heated to raise the temperature of the solution and form a hot saturated solution. During the heating process, the second drive motor 29 is continuously turned on to ensure that the secondary stirring blades 30 continuously stir and maintain the uniformity of the solution.

[0065] During the heating process, the pressure inside the water bath heating tank 1 will rise as the temperature increases. When the pressure inside the tank exceeds the set safety value, the pressure relief valve 31 will automatically open to release the excess pressure and ensure that the pressure inside the tank is within the safe range. When the pressure drops below the safety value, the pressure relief valve 31 will automatically close.

[0066] For example, such as Figure 1 , Figure 2 As shown, the present invention also includes a reinforced support structure 32 fixedly connected between the upper surfaces of the water bath heating tank 1 and the cooling liquid storage tank 2; and a number of vertically arranged support legs 33 fixedly connected to the lower end of the cooling liquid storage tank 2.

[0067] During use, the reinforced support structure 32 connects the water bath heating tank 1 and the cooling liquid storage tank 2, effectively enhancing the connection stability between the two; several sets of vertical support legs 33 at the lower end of the cooling liquid storage tank 2 provide stable support for the cooling liquid storage tank 2.

[0068] In use, the present invention delivers a crude solution containing brandylol hydrochloride and a recrystallization solvent into the water bath heating tank 1 in a certain proportion through the first connector 27 and the second connector 28. The second drive motor 29 on the upper part of the water bath heating tank 1 is started, and its output shaft drives the secondary stirring blade 30 to rotate, stirring the added solution and making the various solutions fully mixed and uniform.

[0069] When the semiconductor cooling device is turned on, the semiconductor cooling chip 18 starts working. As the semiconductor cooling chip 18 works, the cooling liquid tank 2 is cooled, while the flat heat exchange plate 23 is heated by the semiconductor cooling chip 18. The liquid in the flat heat exchange plate 23 automatically moves upward after being heated, and enters the first liquid inlet 21 of the arc-shaped heat exchange plate 19 through the second liquid outlet 25. It can then pass through the arc-shaped heat exchange plate 19 and heat the water bath heating tank 1. The temperature of the liquid drops after passing through the arc-shaped heat exchange plate 19, which further facilitates the downward movement of the liquid. After the liquid in the arc-shaped heat exchange plate 19 moves downward, it is discharged through the first liquid outlet 22 and enters the second liquid inlet 26, thereby promoting the circulation of the liquid between the first heat exchange unit and the second heat exchange unit.

[0070] During the heating process, as the temperature rises, the pressure inside the water bath heating tank 1 will gradually increase. When the pressure exceeds the preset safety value, the pressure relief valve 31 will automatically open to release the excess pressure and ensure equipment safety. When the pressure drops below the safety value, the pressure relief valve 31 will automatically close to maintain a stable pressure environment inside the tank.

[0071] The semiconductor refrigeration device continuously cools the cooling liquid tank 2. The air inside the tank contracts upon cooling, creating a negative pressure. This negative pressure acts on the filter assembly, causing the filter frame 6 to overcome the elastic force of the spring 8 and slide along the sliding grooves 4 on both sides of the frame 3 towards the cooling liquid tank 2. The two sets of filter frames 6 approach each other, ready for filtration. At the same time, the expansion pad 13 expands under the negative pressure environment. The expanded expansion pad 13 will squeeze the upper edge of the filter plate 9, tightly fixing the filter plate 9 inside the filter frame 6. This not only ensures the stability of the filter plate 9 during the filtration process but also enhances the sealing between the filter plate 9 and the filter frame 6. This prevents the hot saturated solution from directly entering the cooling liquid tank 2 through the gaps without being filtered by the filter plate 9, ensuring the accuracy and effect of filtration and helping to obtain a higher purity brandylol hydrochloride product.

[0072] When the valve assembly is opened, the hot saturated solution in the water bath heating tank 1 will flow downward naturally under the action of gravity, while the cooling liquid tank 2 will generate negative pressure under the continuous cooling of the semiconductor refrigeration device. Since the lower part of the filter structure is connected to the cooling liquid tank 2, the hot saturated solution is subjected to a stronger driving force under the combined action of gravity and negative pressure, which accelerates the flow towards the filter structure and increases the feeding speed.

[0073] When the hot saturated solution flows into the frame 3 from the valve assembly, various impurities in the solution are intercepted by the filter plate 9 as the hot saturated solution passes through the filter plate 9, thus initially achieving solid-liquid separation. During normal gravity filtration, the filter plate 9 will generate a certain resistance to the filtration of the solution, affecting the feeding speed. However, the presence of negative pressure causes the pressure distribution of the solution on the filter plate 9 to change. The suction force generated by the negative pressure makes the solution more evenly distributed on the surface of the filter plate 9, further improving the filtration speed.

[0074] When the solution containing brandylol hydrochloride flows into the cooling storage tank 2 after filtration, the first drive motor 15 is started. The output shaft of the first drive motor 15 starts to rotate, driving the first-stage stirring blade 16 to rotate synchronously. This ensures that the solution in the cooling storage tank 2 is mixed evenly, avoiding local overcooling or overheating, and promoting more uniform crystal precipitation. At the same time, the semiconductor cooling chip 18 cools the cooling storage tank 2. After the solution has cooled and crystallized, the discharge pipe 17 is opened to discharge the mixture containing crystals. After discharge, the crystals are separated from the mother liquor by a separation device. Then, the crystals are dried to obtain dry, high-purity brandylol hydrochloride crystals.

[0075] After the solution in the water bath heating tank 1 is delivered, the cooling liquid storage tank 2 is connected to the water bath heating tank 1. At this time, the air pressure in the cooling liquid storage tank 2 rises rapidly. The filter frame 6 is reset and moved to the initial state by the spring 8. At this time, the filter plate 9 can be slid out along the mounting groove 10 from the opening 11 on the side of the protective shell 5 to clean the filter plate 9.

[0076] Meanwhile, the movement of the filter frame 6 can indirectly detect the liquid delivery status in the water bath heating tank 1. Under normal circumstances, when there is a hot saturated solution in the water bath heating tank 1, the negative pressure of the cooling liquid storage tank 2 will keep the filter frame 6 in the moved position for filtration. Once the solution delivery in the water bath heating tank 1 is completed, the cooling liquid storage tank 2 is connected to the water bath heating tank 1, and the filter frame 6 will reset and move to the initial state under the action of the spring 8. Therefore, the operator can determine whether the liquid delivery in the water bath heating tank 1 is completed by observing whether the filter frame 6 has reset. This method provides an intuitive reference indicator for monitoring the entire preparation process, which helps the operator to perform subsequent operations in a timely manner, such as cleaning the filter plate 9 and preparing the next batch of solution, thereby improving production efficiency.

[0077] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of protection claimed by the present invention. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. An apparatus for preparing high-purity brandylol hydrochloride, characterized in that, It includes a water bath heating tank (1) and a filter structure connected to the lower part of the water bath heating tank (1) via a valve (14) assembly. The lower part of the filter structure is connected to a cooling liquid storage tank (2). A semiconductor refrigeration device is installed on the outside of the cooling liquid storage tank (2). A first heat exchange unit is installed on the outside of the water bath heating tank (1). A second heat exchange unit connected to the first heat exchange unit is installed on the outside of the semiconductor refrigeration device. The filter structure includes a frame (3) connecting the valve (14) assembly and the cooling liquid tank (2). Both sides of the frame (3) are connected to the protective shell (5) through the sliding groove (4). The protective shell (5) is sealed and slidably connected to the filter frame (6) with the opening facing upward. The bottom of the filter frame (6) is provided with a filter hole (7). The front and rear sides of the filter frame (6) are sealed and slidably connected to the inner wall of the frame (3). The two sets of filter frames (6) are connected to the protective shell (5) by a spring (8) on the side away from each other. The filter frame (6) has a filter plate (9) inserted into the side. The filter frame (6) has an installation groove (10) that is slidably connected to the filter plate (9) on one side. The filter plate (9) is located at the bottom inside the filter frame (6). The protective shell (5) has an opening (11) corresponding to the installation groove (10) on the side. As the semiconductor refrigeration device continuously cools the cooling liquid tank (2), the temperature inside the cooling liquid tank (2) continuously decreases. The air inside the tank contracts when it gets cold, thus generating negative pressure. Under the action of negative pressure, the components in the filter structure move. When the filter structure moves to a certain position, it is convenient to filter the hot saturated solution in the water bath heating tank (1) after heating. When the valve assembly is opened, the hot saturated solution in the water bath heating tank (1) flows into the filter structure through the valve assembly under the dual action of gravity and the negative pressure of the cooling liquid tank (2). The filter structure filters the hot saturated solution. When the liquid in the heating tank is discharged, the air in the heating tank enters the cooling liquid tank (2), and the air pressure in the cooling liquid tank (2) rises rapidly. At this time, the filter structure automatically resets and moves to the initial state. The filter plate (9) is provided with an embedding groove (12) at the bottom of the inner side of the filter frame (6), and an expansion pad (13) is provided in the embedding groove (12) to press the upper edge of the filter plate (9) after expansion.

2. The apparatus for preparing high-purity brandylol hydrochloride according to claim 1, characterized in that, The valve (14) assembly includes a valve (14) whose upper end is connected to the flange of the water bath heating tank (1), and the lower end of the valve (14) is fixedly connected to the upper surface of the frame (3) through a flange connector.

3. The apparatus for preparing high-purity brandylol hydrochloride according to claim 2, characterized in that, The bottom of the cooling liquid storage tank (2) is fixedly connected to the first drive motor (15). The output shaft of the first drive motor (15) is provided with several sets of circumferentially distributed first-stage stirring blades (16). The lower part of the cooling liquid storage tank (2) is connected to the discharge pipe (17). The semiconductor refrigeration device includes several sets of semiconductor refrigeration chips (18) connected to the outside of the cooling liquid storage tank (2). A negative pressure pump (34) is connected to the cooling liquid storage tank (2).

4. The apparatus for preparing high-purity brandylol hydrochloride according to claim 3, characterized in that, The first heat exchange unit includes several sets of arc-shaped heat exchange plates (19) arranged on the outside of the water bath heating tank (1). Each arc-shaped heat exchange plate (19) is provided with a first circulation channel (20). The upper end of the first circulation channel (20) is connected to the first liquid inlet connector (21), and the lower end of the first circulation channel (20) is connected to the first liquid outlet connector (22). The second heat exchange unit includes several sets of planar heat exchange plates (23) disposed on one side of the semiconductor cooling chip (18). The planar heat exchange plates (23) correspond to the arc-shaped heat exchange plates (19). Each planar heat exchange plate (23) is provided with a second circulation channel (24). The upper end of the second circulation channel (24) is connected to the second liquid outlet connector (25). The second liquid outlet connector (25) is connected to the first liquid inlet connector (21) through a pipeline. The lower end of the second circulation channel (24) is connected to the second liquid inlet connector (26). The first liquid outlet connector (22) is connected to the second liquid inlet connector (26) through a pipeline.

5. The apparatus for preparing high-purity brandylol hydrochloride according to claim 4, characterized in that, The upper surface of the water bath heating tank (1) is connected to the first connector (27) and the second connector (28). The upper part of the water bath heating tank (1) is equipped with a second drive motor (29). The output shaft of the second drive motor (29) is provided with several sets of circumferentially distributed secondary stirring blades (30). The upper surface of the water bath heating tank (1) is connected to a pressure relief valve (31).

6. The apparatus for preparing high-purity brandylol hydrochloride according to claim 5, characterized in that, A reinforced support structure (32) is fixedly connected between the upper surface of the water bath heating tank (1) and the cooling liquid storage tank (2); a number of vertically arranged support legs (33) are fixedly connected to the lower end of the cooling liquid storage tank (2).

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