Xanthine raw material medicine impurity removal device and method
Patent Information
- Application Number
- CN202610880224.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-17
- Publication Date
- 2026-10-09
AI Technical Summary
[0004]本发明实施例提供一种黄嘌呤类原料药除杂装置及除杂方法,旨在能够解决现有的黄嘌呤类原料药生产中杂质无法在线高效分离的问题
[0015]本实现方式中,与现有技术相比,浮游槽板半浸没于液面,其水平槽口能够持续捕获因密度差上浮的杂质与络合物,这些杂质不再随母液进入下一工序,而是经由连接管被转移至杂浆罐,实现了杂质与晶浆的在线分流。由于杂质在结晶阶段即被移出,后续无需通过大量酸碱处理来降解杂质,减少了化学品消耗与废液排放,符合绿色生产要求。振动机构进一步将杂浆分为清液和难溶杂质,清液中含有合格晶浆,可通过回流重新进入结晶釜,提高了整体收率。
Smart Images

Figure CN122874918A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of raw material drug impurity removal technology, specifically relating to a xanthine-based raw material drug impurity removal device. Background Technology
[0002] Impurities are often generated in xanthine raw materials due to factors such as synthesis process, dissolution of metal catalysts, and purity of raw materials. Improper control of reaction conditions such as temperature, pressure, flow rate, stirring method, and rate can also produce corresponding side reaction impurities. Metal catalysts and metal ion impurities in the reaction environment may affect the stability, solubility, and other physicochemical properties of xanthine materials, and may also undergo complexation reactions with materials and impurity components to form insoluble or poorly soluble layered complexes.
[0003] In existing technologies, due to the lack of online impurity separation devices for primary and intermediate products in drug batch quality control and continuous production modes, impurities in primary and intermediate products are often carried into the next production process along with the crystallization and concentration of the mother liquor. This requires the use of more materials to degrade or hydrolyze under acidic or alkaline conditions, resulting in low final yield of finished products, difficulty in filtration and separation, and easy environmental pollution. Summary of the Invention
[0004] This invention provides a xanthine-based raw material impurity removal device and method, which aims to solve the problem that impurities cannot be efficiently separated online in the production of xanthine-based raw materials.
[0005] To achieve the above objectives, the technical solution adopted by the present invention is: to provide a xanthine-based raw material impurity removal device, comprising: A crystallization vessel has a crystallization chamber, which is equipped with a stirrer. The inner wall of the crystallization chamber is connected to a floating trough plate, which is located on the surface of the liquid and is in a semi-submerged state. The floating trough plate is provided with a separation trough with a horizontally set opening. The floating trough plate is also connected to a connecting pipe, which passes through the side wall of the crystallization vessel and extends outward. A slurry tank has a slurry chamber; the slurry chamber is connected to the crystallization chamber via the connecting pipe; A vibration mechanism is connected below the slurry tank and has a clear liquid outlet and an impurity outlet; the clear liquid outlet is connected to a clear liquid return tank; and the impurity outlet is connected to an impurity recovery mechanism.
[0006] In one possible implementation, the floating tank plate is provided with an adjustment bracket, which is disposed on the inner wall of the crystallization chamber. The adjustment bracket can adjust the immersion depth of the floating tank plate in the vertical direction to adapt to the position of the liquid surface during the crystallization process.
[0007] In one possible implementation, the edge of the flotation tank plate is provided with an overflow weir lip, the height of which is 5-15mm lower than the normal operating liquid level of the crystallization vessel, so that the floating slurry can naturally overflow into the separation tank.
[0008] In one possible implementation, one end of the floating tank plate is connected to the inner wall of the crystallization chamber, and the other end extends toward the stirring rod of the stirrer arranged in a vertical direction. The extended end of the floating tank plate is provided with a notch for placing the stirring rod.
[0009] In one possible implementation, the discharge port of the slurry tank is equipped with a weighing sensor for real-time monitoring of the mass of the slurry in the slurry chamber, and the top of the slurry tank is equipped with a breather valve for maintaining the normal pressure environment inside the tank.
[0010] In one possible implementation, the vibration mechanism includes: The vibrating screen is set at an angle relative to the horizontal direction; A backflush nozzle is located below the vibrating screen and is connected to an external compressed air source for timed pulse cleaning of the vibrating screen.
[0011] In one possible implementation, the clear liquid return tank is equipped with a pneumatic stirring device for periodically blowing gas to prevent crystal slurry deposition in the tank, and the bottom of the clear liquid return tank is equipped with a flow aid to assist in material discharge.
[0012] In one possible implementation, the xanthine raw material impurity removal device further includes a reflux pump, one end of which is connected to the outlet of the clear liquid reflux tank, and the other end of which is connected to the reflux port of the crystallization kettle, for transporting the qualified crystal slurry in the clear liquid reflux tank back to the crystallization kettle to continue participating in crystallization.
[0013] In one possible implementation, the impurity recovery mechanism includes: The frame of the ton bag machine is located at the impurity outlet; A ton bag is installed on the frame of the ton bag machine, and the opening of the ton bag is correspondingly set with the impurity outlet; A conveyor belt is installed on the frame of the ton bag machine and located below the ton bag, used to transport the ton bag fully loaded with impurities out of the working area.
[0014] One possible implementation also includes a method for removing impurities from xanthine raw materials, comprising the following steps: S1: The xanthine raw material solution is introduced into the crystallization kettle for cooling and crystallization. The low-density impurities generated in the reaction float to the liquid surface to form a slurry layer. S2: The floating slurry is intercepted by the floating trough plate and introduced into the connecting pipe, and continuously exported to the slurry tank for buffering and metering; S3: When the amount of impurities reaches the set value, the impurities in the impurity tank are discharged into the vibration mechanism and separated into clear liquid containing qualified crystal slurry and insoluble impurities; S4: After entering the clear liquid reflux tank for buffering, the clear liquid is returned to the crystallization kettle via the reflux pump to continue crystallization, while the sparingly soluble impurities enter the impurity recovery mechanism for closed collection and transfer.
[0015] In this implementation, compared to existing technologies, the floating tank plate is partially submerged in the liquid surface. Its horizontal openings continuously capture impurities and complexes that rise due to density differences. These impurities no longer enter the next process with the mother liquor but are transferred to the slurry tank via connecting pipes, achieving online separation of impurities and crystal slurry. Since impurities are removed during the crystallization stage, subsequent large-scale acid and alkali treatment is unnecessary to degrade them, reducing chemical consumption and wastewater discharge, thus meeting green production requirements. The vibration mechanism further separates the slurry into clear liquid and insoluble impurities. The clear liquid contains qualified crystal slurry and can be refluxed back into the crystallization reactor, improving the overall yield. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the xanthine-based raw material impurity removal device provided in an embodiment of the present invention; Figure 2 This is a schematic diagram of the crystallization vessel of the xanthine-based raw material impurity removal device provided in an embodiment of the present invention; Figure 3 A schematic diagram of the impurity tank, vibration mechanism and clear liquid return tank of the xanthine raw material impurity removal device provided in an embodiment of the present invention; Figure 4 This is a schematic diagram of the impurity recovery mechanism of the xanthine raw material impurity removal device provided in an embodiment of the present invention; Figure 5 This is a top view of the floating tank plate of the xanthine-based raw material impurity removal device provided in an embodiment of the present invention; Figure 6 This is a schematic diagram of the main structure of the floating tank plate of the xanthine-based raw material impurity removal device provided in an embodiment of the present invention; Figure 7 This is a side view of the floating tank plate of the xanthine-based raw material impurity removal device provided in an embodiment of the present invention; Figure 8 A schematic diagram of the process steps for removing impurities from xanthine raw materials provided in an embodiment of the present invention; Explanation of reference numerals in the attached figures: 10. Crystallization vessel; 11. Agitator; 12. Floating tank plate; 121. Separation tank; 122. Adjustment support; 123. Overflow weir; 124. Notch; 20. Slurry tank; 21. Weighing sensor; 22. Breathing valve; 30. Vibration mechanism; 40. Clear liquid return tank; 50. Impurity recovery mechanism; 51. Ton bag machine frame; 52. Ton bag; 53. Conveyor belt; 60. Return pump. Detailed Implementation
[0017] To make the technical problems to be solved, the technical solutions, and the beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
[0018] It should be noted that the terms "length", "width", "height", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "head", and "tail" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention.
[0019] It should also be noted that, unless otherwise explicitly specified and limited, terms such as "installation," "connection," "fixing," and "setting" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part of a structure. They can refer to a mechanical connection or an electrical connection. They can refer to a direct connection or an indirect connection through an intermediate medium, or to the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0020] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Additionally, "multiple" and "several" mean two or more, unless otherwise explicitly specified.
[0021] Please refer to the following: Figures 1 to 8The impurity removal device for xanthine raw materials provided by the present invention will now be described. The xanthine raw material impurity removal device includes a crystallization kettle 10, a slurry tank 20, a vibration mechanism 30, a clear liquid return tank 40, and an impurity recovery mechanism 50. The crystallization kettle 10 has a crystallization chamber, within which a stirrer 11 is installed. A floating trough plate 12 is connected to the inner wall of the crystallization chamber, and the floating trough plate 12 is partially submerged at the surface of the drug solution. A separation tank 121 with a horizontally positioned opening is provided on the wall of the floating trough plate 12. The floating trough plate 12 is also connected to a connecting pipe, which penetrates the side wall of the crystallization kettle 10 and extends outward. The slurry tank 20 has a slurry chamber. The slurry chamber is connected to the crystallization chamber via a connecting pipe. The vibration mechanism 30 is connected below the slurry tank and has a clear liquid outlet and an impurity outlet. The clear liquid outlet is connected to the clear liquid return tank 40. The impurity outlet is connected to the impurity recovery mechanism 50.
[0022] The xanthine raw material impurity removal device provided in this embodiment, compared with the prior art, has a floating tank plate 12 that is partially submerged in the liquid surface. Its horizontal opening can continuously capture impurities and complexes that float to the surface due to density differences. These impurities no longer enter the next process with the mother liquor, but are transferred to the slurry tank 20 via connecting pipes, realizing online separation of impurities and crystal slurry. Since the impurities are removed during the crystallization stage, there is no need for subsequent large-scale acid and alkali treatment to degrade the impurities, reducing chemical consumption and waste liquid discharge, which meets the requirements of green production. The vibration mechanism 30 further separates the slurry into clear liquid and insoluble impurities. The clear liquid contains qualified crystal slurry, which can be refluxed back into the crystallization kettle 10, improving the overall yield.
[0023] The position and semi-submerged state of the floating trough plate 12 make the hydrodynamic conditions inside the crystallizer 10 more stable, and the flow field of the agitator 11 will not directly impact the trough opening, thereby reducing the probability of crystal slurry accidentally entering the impurity tank 20. In addition, the transfer of impurities in the closed pipeline reduces the risk of cross-contamination caused by manual operation. This device can be directly embedded into the existing continuous production line without changing the main structure of the crystallizer 10. The floating trough plate 12 can be replaced by a liftable overflow baffle, the connecting pipe can be made of flexible and corrosion-resistant pipe, the impurity tank 20 can be replaced by a buffer tank with a scraper conveyor, and the vibration mechanism 30 can be replaced by a centrifugal screening device, as long as the continuous capture, transfer and separation of floating impurities can be achieved.
[0024] In some embodiments, the above-mentioned floating tank plate 12 can be adopted as follows: Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 7 The structure shown. See also Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 7The floating tank plate 12 is provided with an adjustment bracket 122, which is set on the inner wall of the crystallization chamber. The adjustment bracket 122 can adjust the immersion depth of the floating tank plate 12 in the vertical direction to adapt to the position of the liquid surface during the crystallization process.
[0025] The adjusting bracket 122 is used to adjust the immersion depth of the flotation tank 12 vertically. This directly addresses liquid level changes caused by evaporation, crystal precipitation, or feed replenishment during the crystallization process. By adjusting the tank opening position, it ensures the opening is always in the optimal capture position, preventing impurities from failing to enter the separation tank 121 due to a drop in liquid level, or the tank opening from being completely submerged due to a rise in liquid level, thus losing its separation function. This improves the adaptability and stability of the device, allowing the same equipment to process different batches and formulations of xanthine raw materials without replacing the flotation tank 12.
[0026] The presence of the adjusting bracket 122 makes equipment maintenance more convenient, allowing for fine-tuning of the tank position without shutting down the system, thus reducing downtime. Furthermore, the adjusting bracket 122 can be integrated with an automated control system, automatically adjusting based on feedback from the liquid level sensor to achieve unattended operation. In terms of application, this function is particularly suitable for multi-variety, small-batch raw material pharmaceutical production scenarios, allowing companies to cover the impurity removal needs of multiple products with a single device.
[0027] The adjusting bracket 122 can be a screw lifting mechanism, a pneumatic lifting arm, or a magnetic coupling adjusting device. As long as it can achieve precise adjustment of the height of the floating tank plate 12, it is an equivalent substitution of this claim.
[0028] In some embodiments, the above-mentioned floating tank plate 12 can be adopted as follows: Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 7 The structure shown. See also Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 7 The edge of the floating tank plate 12 is provided with an overflow weir 123. The height of the overflow weir 123 is 5-15mm lower than the normal working liquid level of the crystallization vessel 10, so that the floating slurry can overflow naturally into the separation tank 121.
[0029] An overflow weir 123 is added to the edge of the flotation tank 12, with its height 5-15 mm lower than the normal operating liquid level of the crystallizer 10. This design ensures that the floating slurry can overflow naturally into the separation tank 121 without additional power. Technically, the overflow weir 123 creates a stable liquid level difference, making the flow of the impurity layer smoother and preventing slurry entrainment caused by excessive flow velocity. At the same time, the low height of the weir reduces the accumulation of impurities at the tank opening, lowering the risk of clogging.
[0030] The overflow weir lip 123 also serves as a buffer, absorbing some of the energy of the fluctuations in the liquid level within the crystallization vessel 10, preventing impurities from overflowing. In applications, this design is particularly suitable for scenarios requiring high impurity removal efficiency, such as the production of high-purity pharmaceutical raw materials.
[0031] The overflow weir lip 123 can be made of an adjustable weir plate, and the material can be corrosion-resistant materials such as polytetrafluoroethylene or Hastelloy.
[0032] In some embodiments, the above-mentioned floating tank plate 12 can be adopted as follows: Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 7 The structure shown. See also Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 7 One end of the floating tank plate 12 is connected to the inner wall of the crystallization chamber, and the other end extends toward the stirring rod of the stirrer 11 in a vertical direction. The extended end of the floating tank plate 12 is provided with a notch 124 for placing the stirring rod.
[0033] The extended end of the floating trough plate 12 is provided with a notch 124 for placing the stirring rod. This structure solves the spatial conflict problem between the floating trough plate 12 and the agitator 11. Technically, the notch 124 design allows the floating trough plate 12 to be as close as possible to the stirring center area, which is the main accumulation area for impurities, thereby improving impurity capture efficiency. The notch 124 avoids mechanical interference between the floating trough plate 12 and the stirring rod, ensuring the normal operation of the agitator 11.
[0034] The notch 124 also facilitates the installation and removal of the floating tank plate 12, eliminating the need to remove the agitator 11 during maintenance and reducing maintenance costs. In terms of application, this design is particularly suitable for crystallizing vessels 10 where the agitator 11 is located in the center, maximizing the use of the space inside the vessel.
[0035] The shape of the notch 124 can be customized according to the specific size of the stirring rod, or a detachable notch 124 cover plate can be used, as long as it can avoid and cooperate with the stirring rod.
[0036] In some embodiments, the aforementioned slurry tank 20 may be adopted as follows: Figure 1 , Figure 3 The structure shown. See also Figure 1 , Figure 3 The discharge port of the slurry tank 20 is equipped with a weighing sensor 21, which is used to monitor the quality of the slurry in the slurry chamber in real time. The top of the slurry tank 20 is equipped with a breather valve 22, which is used to maintain the normal pressure environment inside the tank.
[0037] A weighing sensor 21 is installed at the outlet of the slurry tank 20, and a breather valve 22 is installed at the top. The weighing sensor 21 is used to monitor the quality of the slurry in real time. Technically, this allows operators to accurately grasp the accumulation of slurry and arrange subsequent processing in a timely manner, avoiding overflow or blockage caused by excessive slurry. The breather valve 22 is used to maintain the normal pressure inside the tank, preventing pressure fluctuations caused by temperature changes or material entry and exit, and ensuring stable storage of the slurry.
[0038] The combination of weighing data and breather valve 22 also provides a basis for automated control. For example, when the mass of the slurry reaches the set value, the vibration mechanism 30 can be automatically triggered to start, realizing full-process automation.
[0039] The weighing sensor 21 can be replaced with a radar level gauge or a differential pressure level sensor, and the breather valve 22 can be replaced with a combination of a pressure relief valve and a safety valve, as long as it can achieve the monitoring of the quality of the slurry and the pressure balance.
[0040] In some embodiments, the vibration mechanism 30 described above may employ, for example... Figure 1 , Figure 3 The structure shown. See also Figure 1 , Figure 3 The vibration mechanism 30 includes a vibrating screen and a back-blowing nozzle. The vibrating screen is inclined relative to the horizontal direction. The back-blowing nozzle is located below the vibrating screen and is connected to an external compressed air source for timed pulse cleaning of the vibrating screen.
[0041] The vibrating screen uses an inclined angle to automatically transport and separate impurities, while backflushing nozzles periodically remove screen blockages. Technically, this combination significantly improves separation efficiency and screen lifespan, reducing the frequency of manual cleaning. The inclined screen also allows the separated clear liquid to flow naturally to the outlet, eliminating the need for additional pumping.
[0042] The pulse cleaning function of the backflush nozzles also prevents impurities from compacting on the screen, maintaining screening accuracy. In application, this structure is particularly suitable for systems containing sticky impurities and can effectively handle difficult-to-separate materials.
[0043] Vibrating screens can be replaced with ultrasonic screens, and backflushing nozzles can be replaced with mechanical brushing devices, as long as efficient separation and anti-clogging of impurities can be achieved.
[0044] In some embodiments, the aforementioned clear liquid return tank 40 can be adopted as follows: Figure 1 , Figure 3 The structure shown. See also Figure 1 , Figure 3The clear liquid return tank 40 is equipped with a pneumatic stirring device, which is used to periodically spray gas to prevent crystal slurry from depositing in the tank. The bottom of the clear liquid return tank 40 is equipped with a flow aid to assist in the discharge.
[0045] Pneumatic agitation uses periodic gas injection to prevent crystal slurry deposition, while a flow aid assists in material discharge. Technically, this solves the blockage problem caused by crystal slurry settling within the clear liquid return tank 40, ensuring smooth return of the clear liquid. Compared to mechanical agitation, pneumatic agitation is more suitable for flammable and explosive environments, improving safety.
[0046] Pneumatic agitation also provides a certain degree of air lifting, promoting the resuspension of tiny crystals in the clarified liquid and improving the uniformity of the reflux slurry. In application, this design is particularly suitable for crystallization processes that require high uniformity of the slurry. The pneumatic agitator can be replaced with a magnetic agitator or an ultrasonic anti-settling device, and the flow aid can be replaced with a vibrating discharge device, as long as it can prevent slurry deposition and assist in discharge.
[0047] In some embodiments, the above-mentioned xanthine raw material impurity removal device can employ, for example... Figure 1 , Figure 3 The structure shown. See also Figure 1 , Figure 3 The xanthine raw material impurity removal device also includes a reflux pump 60. One end of the reflux pump 60 is connected to the outlet of the clear liquid reflux tank 40, and the other end of the reflux pump 60 is connected to the reflux port of the crystallization kettle 10. It is used to transport the qualified crystal slurry in the clear liquid reflux tank 40 back to the crystallization kettle 10 to continue to participate in crystallization.
[0048] The qualified crystal slurry in the clear liquid reflux tank 40 is transported back to the crystallization kettle 10, which realizes the recycling of crystal slurry, avoids the waste of qualified products, and significantly improves the yield. The reflux pump 60 can also control the reflux speed and flow rate, and optimize the supersaturation distribution in the crystallization process.
[0049] The operation of the reflux pump 60 also promotes mixing within the crystallizer 10, improving mass and heat transfer conditions. In applications, this function is particularly suitable for processes requiring precise control of crystal growth rates. The reflux pump 60 can be replaced by an ejector or a gravity reflux system, as long as reliable reflux of the crystal slurry can be achieved.
[0050] In some embodiments, the impurity recovery mechanism 50 described above may employ, for example... Figure 1 , Figure 4 The structure shown. See also Figure 1 , Figure 4The impurity recovery mechanism 50 includes: a ton bag machine frame 51, a ton bag 52, and a conveyor belt 53. The ton bag machine frame 51 is located at the impurity outlet. The ton bag 52 is mounted on the ton bag machine frame 51, with its opening corresponding to the impurity outlet. The conveyor belt 53 is mounted on the ton bag machine frame 51 and located below the ton bag 52, used to transport the ton bag 52, which is fully loaded with impurities, out of the working area.
[0051] The impurity recovery mechanism 50 includes a ton bag frame 51, ton bags 52, and a conveyor belt 53. Technically, this achieves closed-loop collection and automated transfer of sparingly soluble impurities, reducing the risk of human contact with hazardous substances and facilitating subsequent processing or disposal. The large-capacity design of the ton bags 52 reduces replacement frequency, while the conveyor belt 53 improves transfer efficiency.
[0052] Enclosed collection also prevents impurities from being stirred up and improves the workshop environment. In terms of application, this structure is particularly suitable for solid waste treatment in large-scale continuous production. The ton bag 52 can be replaced with a rigid container, and the conveyor belt 53 can be replaced with a forklift transfer system, as long as the closed collection and transfer of impurities can be achieved.
[0053] In some embodiments, the method for removing impurities from xanthine raw materials can be as follows: Figure 8 The steps are shown. See also... Figure 8 This includes the following steps: S1: The xanthine raw material solution is introduced into the crystallization kettle 10 for cooling and crystallization. The low-density impurities generated in the reaction float to the liquid surface to form a slurry layer.
[0054] S2: The floating slurry is intercepted by the floating trough plate 12 and introduced into the connecting pipe, and continuously exported to the slurry tank 20 for buffering and metering.
[0055] S3: When the amount of impurities reaches the set value, the impurities in the impurity tank 20 are discharged into the vibration mechanism 30 and separated into clear liquid containing qualified crystal pulp and insoluble impurities.
[0056] S4: After entering the clear liquid reflux tank 40 for buffering, the clear liquid is returned to the crystallization kettle 10 via the reflux pump 60 to continue crystallization. Insoluble impurities enter the impurity recovery mechanism 50 for closed collection and transfer.
[0057] This method enables fully online impurity treatment, removing impurities without interrupting production and significantly improving efficiency. By recirculating the clarified liquid, it reduces raw material waste and wastewater discharge, lowering production costs and environmental impact. Furthermore, the method can adapt to the characteristics of different impurities by adjusting parameters in each step (such as crystallization temperature and impurity slurry removal rate), demonstrating strong versatility. In application, this method can be directly applied to the industrial production of existing xanthine-based active pharmaceutical ingredients without major adjustments to the process route. Specific parameters for each step can be adjusted according to actual production conditions, for example, by employing gradient cooling crystallization or a segmented reflux strategy.
[0058] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A device for removing impurities from xanthine-based raw materials, characterized in that, include: A crystallization vessel has a crystallization chamber, which is equipped with a stirrer. The inner wall of the crystallization chamber is connected to a floating trough plate, which is located on the surface of the liquid and is in a semi-submerged state. The floating trough plate is provided with a separation trough with a horizontally set opening. The floating trough plate is also connected to a connecting pipe, which passes through the side wall of the crystallization vessel and extends outward. A slurry tank has a slurry chamber; the slurry chamber is connected to the crystallization chamber via the connecting pipe; A vibration mechanism is connected below the slurry tank and has a clear liquid outlet and an impurity outlet; the clear liquid outlet is connected to a clear liquid return tank; and the impurity outlet is connected to an impurity recovery mechanism.
2. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The floating tank plate is equipped with an adjustment bracket, which is located on the inner wall of the crystallization chamber. The adjustment bracket can adjust the immersion depth of the floating tank plate in the vertical direction to adapt to the position of the liquid surface during the crystallization process.
3. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The floating trough plate has an overflow weir at the edge of the trough opening. The height of the overflow weir is 5-15mm lower than the normal working liquid level of the crystallization vessel, so that the floating slurry can overflow naturally into the separation tank.
4. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, One end of the floating tank plate is connected to the inner wall of the crystallization chamber, and the other end extends toward the stirring rod that is vertically arranged in the stirrer. The extended end of the floating tank plate is provided with a notch for placing the stirring rod.
5. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The discharge port of the slurry tank is equipped with a weighing sensor, which is used to monitor the mass of the slurry in the slurry chamber in real time. The top of the slurry tank is equipped with a breather valve, which is used to maintain the normal pressure environment inside the tank.
6. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The vibration mechanism includes: The vibrating screen is set at an angle relative to the horizontal direction; A backflush nozzle is located below the vibrating screen and is connected to an external compressed air source for timed pulse cleaning of the vibrating screen.
7. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The clear liquid return tank is equipped with a pneumatic stirring device, which is used to periodically spray gas to prevent crystal slurry deposition in the tank. The bottom of the clear liquid return tank is equipped with a flow aid to assist in material discharge.
8. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The xanthine raw material impurity removal device also includes a reflux pump. One end of the reflux pump is connected to the outlet of the clear liquid reflux tank, and the other end of the reflux pump is connected to the reflux port of the crystallization kettle, which is used to transport the qualified crystal slurry in the clear liquid reflux tank back to the crystallization kettle to continue to participate in crystallization.
9. The xanthine-based raw material impurity removal device as described in claim 1, characterized in that, The impurity recovery mechanism includes: The frame of the ton bag machine is located at the impurity outlet; A ton bag is installed on the frame of the ton bag machine, and the opening of the ton bag is correspondingly set with the impurity outlet; A conveyor belt is installed on the frame of the ton bag machine and located below the ton bag, used to transport the ton bag fully loaded with impurities out of the working area.
10. A method for removing impurities from xanthine raw materials, using the xanthine raw material impurity removal device as described in claim 8, characterized in that, Includes the following steps: S1: The xanthine raw material solution is introduced into the crystallization kettle for cooling and crystallization. The low-density impurities generated in the reaction float to the liquid surface to form a slurry layer. S2: The floating slurry is intercepted by the floating trough plate and introduced into the connecting pipe, and continuously exported to the slurry tank for buffering and metering; S3: When the amount of impurities reaches the set value, the impurities in the impurity tank are discharged into the vibration mechanism and separated into clear liquid containing qualified crystal slurry and insoluble impurities; S4: After entering the clear liquid reflux tank for buffering, the clear liquid is returned to the crystallization kettle via the reflux pump to continue crystallization, while the sparingly soluble impurities enter the impurity recovery mechanism for closed collection and transfer.