Online PAT continuous crystallization device

Abstract

The utility model provides an on-line PAT continuous crystallization device, which belongs to the technical field of crystal production, and comprises a plurality of groups of crystallization tanks, the crystallization tanks are connected in series through a series mechanism, the series mechanism comprises an electromagnetic valve, a connecting hose and a peristaltic pump, the crystallizing tanks in the first group are connected with a feeding tank through the serial connection mechanism, a discharging opening is formed in the bottom end of each crystallizing tank, the discharging opening in the bottom end of the crystallizing tank in the last group is connected with a product tank through a discharging pipe, and a centrifugal pump is arranged on the discharging pipe and used for supplying materials into the product tank. A PAT instrument is installed on the crystallizing tank, the size of the connecting hose is matched with that of the discharging port, and a stirring mechanism is arranged in the crystallizing tank; according to the utility model, the problem of unstable product quality caused by lack of detection of real-time process parameters (such as granularity, particle morphology and the like) can be solved.

Description

Technical Field

[0001] The utility model belongs to the technical field of crystal production, and specifically relates to an online PAT continuous crystallization device. Background Art

[0002] In industries such as food, pharmaceuticals, and chemicals, crystallization is an essential process for producing crystalline products and a key factor in controlling their quality. Existing crystallizers mostly use a batch crystallization process, which typically requires manual feeding, resulting in low production efficiency and poor product quality stability. To address these issues, a continuous crystallization device—one that can achieve continuous feeding and discharging—is needed.

[0003] Currently, parameters such as crystal morphology, size, and solution supersaturation in crystallization equipment are not collected in real time. Therefore, the quality control of the final crystallized product still lags behind that of products produced by crystallization technology in advanced countries. The application of process analytical technologies (PAT) is key to this process. Utility Model Content

[0004] In view of this, the utility model provides an online PAT continuous crystallization device, which can monitor crystal processing parameters in real time and achieve stable continuous crystallization production, solving the problem of unstable product quality caused by the lack of real-time process parameter detection (such as particle size, particle morphology, etc.).

[0005] The utility model is achieved in this way:

[0006] The utility model provides an online PAT continuous crystallization device, which comprises a plurality of groups of crystallization tanks, wherein the crystallization tanks are connected in series through a series mechanism, the series mechanism comprises a solenoid valve, a connecting hose and a peristaltic pump, the first group of crystallization tanks are connected to a feed tank through the series mechanism, a discharge port is provided at the bottom end of the crystallization tank, the discharge port at the bottom end of the crystallization tank of the last group is connected to a product tank through a discharge pipe, a centrifugal pump is provided on the discharge pipe for feeding the interior of the product tank, a PAT instrument is installed on the crystallization tank, the size of the connecting hose is adapted to the discharge port, a stirring mechanism is provided inside the crystallization tank, and a separate temperature control system is provided in the crystallization tank, the feed tank and the product tank.

[0007] Wherein, the discharge port at the bottom end of the crystallization tank of the last group is also provided with a solenoid valve.

[0008] The technical effects of an online PAT continuous crystallization device provided by the utility model are as follows: by setting a series mechanism for connecting multiple groups of crystallization tanks in series, continuous feeding, continuous crystallization and discharging can be achieved, and by installing a corresponding PAT instrument on the crystallization tank, important parameters in the crystallization process, including particle size, turbidity, concentration, solid content and other preparation parameters, can be monitored online in real time, thereby strictly regulating the production process and ensuring the stability and consistency of the quality of the crystallized product. By setting a stirring mechanism and a temperature control system, a crystallization environment in the crystallization tank can be constructed.

[0009] On the basis of the above technical solution, the online PAT continuous crystallization device of the present invention can also be improved as follows:

[0010] Wherein, the crystallization tank is provided with a feed port, and the size of the feed port is the same as that of the discharge port.

[0011] The beneficial effect of adopting the above-mentioned improvement scheme is as follows: the feed port is provided to be connected to the discharge port of the adjacent crystallization tank via a connecting hose.

[0012] Furthermore, when connected in series, the two adjacent groups of crystallizers are connected in series through the discharge port at the bottom end of the crystallizer at the front end, the corresponding connection solenoid valve, the connecting hose, and the peristaltic pump to the feed port of the crystallizer at the rear end;

[0013] Furthermore, the crystallization tanks can be placed at different heights, and the material can be transported by gravity. This method is energy-saving and easier to control.

[0014] The beneficial effects of adopting the above-mentioned improvement scheme are: by connecting the crystallization tanks in series, further continuous crystallization can be achieved, and the crystallization environment inside each crystallization tank is guaranteed, making the output quality more stable.

[0015] Furthermore, the stirring mechanism includes a stirring motor, a stirring rod and a stirring blade.

[0016] The beneficial effect of adopting the above-mentioned improvement scheme is: the stirring motor is used to drive the stirring rod and the stirring blades to rotate to achieve a stirring effect, thereby helping crystallization.

[0017] Furthermore, the output end of the stirring motor is fixedly connected to one end of the stirring rod, and the stirring blade is arranged on the surface of the stirring rod.

[0018] Furthermore, the temperature control system includes a heating unit, a refrigeration unit, a circulation pipeline and a temperature sensor.

[0019] The beneficial effect of adopting the above-mentioned improvement scheme is: by setting up a temperature control system, it is used to control the temperature inside the crystallization tank.

[0020] Furthermore, a plurality of PAT instrument installation ports are provided on the top of the crystallization tank, and covers are detachably mounted on the PAT instrument installation ports.

[0021] Furthermore, the PAT instrument includes a probe-type online imaging particle shape and size analyzer, a probe-type turbidity meter, an infrared concentration meter and an ultrasonic solid content meter.

[0022] The beneficial effects of adopting the above-mentioned improvement scheme are: by setting up a probe-type online imaging particle shape and size analyzer, it is used to realize the measurement of crystal nucleation and growth particle shape and size; by setting up a probe-type turbidity meter, it is used to realize the measurement of nucleation point, solubility and metastable zone width; by setting up an infrared concentration meter, it is used to realize the measurement of solution concentration and supersaturation; by setting up an ultrasonic solid content meter, it is used to realize the measurement of solid content concentration.

[0023] Furthermore, the probes of the PAT instrument are extended into the interior of the crystallization tank through positions corresponding to the installation ports of the PAT instrument, and the number of the crystallization tanks is two groups.

[0024] Furthermore, the probes of the PAT instrument are electrically connected to the device host through a connecting line, and are electrically connected to the computer through a connecting line, and the computer is electrically connected to the DCS system terminal through a connecting line.

[0025] The beneficial effect of adopting the above-mentioned improvement scheme is that by electrically connecting the PAT instrument with the computer and the DCS system terminal, real-time monitoring of important parameters in the crystallization process can be achieved.

[0026] Compared with the prior art, the beneficial effects of an online PAT continuous crystallization device provided by the utility model are as follows: by setting a series mechanism for connecting multiple groups of crystallization tanks in series, continuous feeding, continuous crystallization and discharging can be achieved, and by installing a corresponding PAT instrument on the crystallization tank, important parameters in the crystallization process, including particle size, turbidity, concentration, solid content and other preparation parameters, can be monitored online in real time, thereby strictly regulating the production process and ensuring the stability and consistency of the quality of the crystallized product. By setting a stirring mechanism and a temperature control system, a crystallization environment is constructed in the crystallization tank; by connecting the crystallization tanks in series, further continuous crystallization can be achieved, and the crystallization environment inside each crystallization tank is guaranteed, making the output quality more stable. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] 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 description of the embodiments of the present invention. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0028] Figure 1 It is a structural schematic diagram of an online PAT continuous crystallization device;

[0029] Figure 2 A schematic diagram of a PAT instrument for an online PAT continuous crystallization device;

[0030] In the accompanying drawings, the components represented by the reference numerals are as follows:

[0031] 10. Crystallization tank; 11. Series mechanism; 12. Connecting hose; 13. Peristaltic pump; 14. PAT instrument; 15. Feed tank; 16. Discharge port; 17. Discharge pipe; 18. Product tank; 19. Stirring motor; 20. Stirring rod; 21. Stirring blade; 22. PAT instrument installation port; 23. Cover; 24. Computer; 25. DCS system terminal; 26. Centrifugal pump. DETAILED DESCRIPTION

[0032] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention.

[0033] like Figure 1 , shown in Figure 2, is an embodiment of an online PAT continuous crystallization device provided by the utility model. In this embodiment, it includes multiple groups of crystallizers 10, which are connected in series through 11. The series mechanism 11 includes a solenoid valve connecting hose 12 and a peristaltic pump 13. The first group of crystallizers 10 is connected to the feed tank 15 through the series mechanism 11. A discharge port 16 is provided at the bottom end of the crystallizer 10. The discharge port 16 at the bottom end of the crystallizer 10 of the last group is connected to the product tank 18 through a discharge pipe 17. A centrifugal pump 26 is provided on the discharge pipe 17 for feeding the inside of the product tank 18, and a PAT instrument 14 is installed on the crystallizer 10. The size of the connecting hose 12 is adapted to the discharge port 16. A stirring mechanism is provided inside the crystallizer 10, and a separate temperature control system is provided in the crystallizer 10, the feed tank 15 and the product tank 18.

[0034] During use, supersaturated solution is imported in feed tank 15, feed tank 15 is made constant at a given temperature, and the solute inside is completely dissolved, and now, feed tank 15 should be settled solution; The connecting hose 12 of the first crystallizer 10 (by the first crystallizer of material flow direction) connecting feed tank 15 is opened, and the settled solution in feed tank 15 is squeezed in the first crystallizer 10, and the constant temperature value of the first crystallizer is set by temperature control system; After the temperature sensor monitors that the solution temperature in the first crystallizer 10 is down to a given temperature, the connecting hose 12 connecting between the first crystallizer 10 and the second crystallizer 10 is opened, and the settled solution in the first crystallizer 10 is squeezed into the second crystallizer 10 Then set the temperature value in the second crystallizer 10; at this time, there is solution in both the first and second crystallizers 10, and close all connecting hoses 12; turn on the stirring motor 19 and continue stirring for a period of time. When nucleation begins in the second crystallizer 10, all connecting hoses 12 are opened at the same time, and the continuous crystallization process starts to run; insert the probe of the PAT instrument 14 into the second crystallizer 10 corresponding to the position of the PAT instrument installation port 22, and monitor the concentration, supersaturation, turbidity, morphology, and particle size distribution changes in the tank in real time; it is suitable for evaporation crystallization, cooling crystallization, antisolvent, etc. When the parameters of the crystal reach the preset value, it can be extracted from the crystallizer 10 by the centrifugal pump 26 in conjunction with the discharge pipe 17 and transferred to the product tank 18 for storage.

[0035] In the above technical solution, a feed port is provided on the crystallization tank 10 , and the size of the feed port is the same as that of the discharge port 16 .

[0036] Furthermore, in the above technical solution, when connected in series, the two adjacent groups of crystallization tanks 10 are connected in series through the discharge port 16 at the bottom end of the front crystallization tank 10, and the connecting hose 12 and the peristaltic pump 13 are connected in series with the feed port of the rear crystallization tank 10.

[0037] Furthermore, in the above technical solution, the stirring mechanism includes a stirring motor 19 , a stirring rod 20 and a stirring blade 21 .

[0038] Furthermore, in the above technical solution, the output end of the stirring motor 19 is fixedly connected to one end of the stirring rod 20 , and the stirring blade 21 is provided on the surface of the stirring rod 20 .

[0039] Furthermore, in the above technical solution, the temperature control system includes a heating unit, a refrigeration unit, a circulation pipeline and a temperature sensor.

[0040] Furthermore, in the above technical solution, a plurality of PAT instrument installation ports 22 are provided on the top of the crystallization tank 10 , and a cover 23 is detachably mounted on the PAT instrument installation port 22 .

[0041] Furthermore, in the above technical solution, the PAT instrument 14 includes a probe-type online imaging particle shape and size analyzer, a probe-type turbidity meter, an infrared concentration meter, and an ultrasonic solid content meter.

[0042] Furthermore, in the above technical solution, the probes of the PAT instrument 14 are all extended into the interior of the crystallization tank 10 through positions corresponding to the PAT instrument installation ports 22 , and the number of crystallization tanks 10 is two groups.

[0043] Furthermore, in the above technical solution, the probes of the PAT instrument 14 are electrically connected to the device host through a connecting line, and are electrically connected to the computer 24 through a connecting line, and the computer 24 is electrically connected to the DCS system terminal 25 through a connecting line.

[0044] Specifically, the principle of the present invention is: during use, the supersaturated solution is imported into the feed tank 15, the feed tank 15 is constant at a given temperature, the solute inside is completely dissolved, and now the feed tank 15 should be a clear solution; the connecting hose 12 of the first crystallizer 10 (the first crystallizer in the material flow direction) connected to the feed tank 15 is opened, and the clear solution in the feed tank 15 is squeezed into the first crystallizer 10, and the constant temperature value of the first crystallizer is set by the temperature control system; after the temperature sensor monitors that the solution temperature in the first crystallizer 10 drops to a given temperature, the connecting hose 12 connected between the first crystallizer 10 and the second crystallizer 10 is opened, and the clear solution in the first crystallizer 10 is squeezed into the first crystallizer 10. two crystallizers 10, and then set the temperature value in the second crystallizer 10; at this time, there is solution in both the first and second crystallizers 10, and all connecting hoses 12 are closed; turn on the stirring motor 19 and continue stirring for a period of time. When nucleation begins in the second crystallizer 10, all connecting hoses 12 are opened at the same time, and the continuous crystallization process starts to run; the probe of the PAT instrument 14 is inserted into the second crystallizer 10 corresponding to the position of the PAT instrument installation port 22, and the concentration, supersaturation, turbidity, morphology, and particle size distribution changes in the tank are monitored in real time; it is suitable for evaporative crystallization, cooling crystallization, antisolvent, etc. When the parameters of the crystal reach the preset value, it can be extracted from the crystallizer 10 through the centrifugal pump 26 in conjunction with the discharge pipe 17 and transferred to the product tank 18 for storage.

Claims

1. An online PAT continuous crystallization device, characterized in that: The invention comprises a plurality of groups of crystallization tanks (10), wherein the crystallization tanks (10) are connected in series via a series mechanism (11), wherein the series mechanism (11) comprises a solenoid valve, a connecting hose (12) and a peristaltic pump (13), wherein the first group of crystallization tanks (10) is connected to a feed tank (15) via the series mechanism (11), and a discharge port (16) is provided at the bottom end of the crystallization tank (10), and the discharge port (16) at the bottom end of the crystallization tank (10) of the last group is connected via a discharge pipe (17). The crystallizer (10) is connected to the product tank (18), the discharge pipe (17) is provided with a centrifugal pump (26) for feeding the inside of the product tank (18), and the crystallizer (10) is installed with a PAT instrument (14), the size of the connecting hose (12) is adapted to the discharge port (16), the crystallizer (10) is provided with a stirring mechanism, and the crystallizer (10), the feed tank (15) and the product tank (18) are all provided with separate temperature control systems.

2. An online PAT continuous crystallization device according to claim 1, characterized in that, The crystallization tank (10) is provided with a feed port, and the size of the feed port is the same as that of the discharge port (16).

3. An online PAT continuous crystallization device according to claim 2, characterized in that, When connected in series, the two adjacent groups of crystallization tanks (10) are connected in series via the discharge port (16) at the bottom end of the front crystallization tank (10), and the corresponding electromagnetic valve, the connecting hose (12), and the peristaltic pump (13) are connected in series with the feed port of the rear crystallization tank (10).

4. An online PAT continuous crystallization device according to claim 3, characterized in that, The stirring mechanism comprises a stirring motor (19), a stirring rod (20) and a stirring blade (21).

5. An online PAT continuous crystallization device according to claim 4, characterized in that, The output end of the stirring motor (19) is fixedly connected to one end of the stirring rod (20), and the stirring blade (21) is arranged on the surface of the stirring rod (20).

6. An online PAT continuous crystallization device according to claim 5, characterized in that: The temperature control system includes a heating unit, a refrigeration unit, a circulation pipeline and a temperature sensor.

7. An online PAT continuous crystallization device according to claim 6, characterized in that: The top of the crystallization tank (10) is provided with a plurality of PAT instrument installation ports (22), and a cover (23) is detachably mounted on the PAT instrument installation port (22).

8. An online PAT continuous crystallization device according to claim 7, characterized in that: The PAT instrument (14) includes a probe-type online imaging particle shape and size analyzer, a probe-type turbidity meter, an infrared concentration meter, and an ultrasonic solid content meter.

9. An online PAT continuous crystallization device according to claim 8, characterized in that: The probes of the PAT instrument (14) are extended into the interior of the crystallization tank (10) through positions corresponding to the PAT instrument installation ports (22), and the number of the crystallization tanks (10) is two groups.

10. The online PAT continuous crystallization device according to claim 9, characterized in that: The probes of the PAT instrument (14) are electrically connected to the device host through a connecting line, and are electrically connected to the computer (24) through a connecting line. The computer (24) is electrically connected to the DCS system terminal (25) through a connecting line.

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