Online PAT intermittent crystallization device

Abstract

The utility model provides an on-line PAT intermittent crystallization device, which belongs to the technical field of crystallization monitoring, and comprises a feeding tank, the feeding tank is communicated with a crystallization tank through a material conveying system, a temperature control device is arranged outside the crystallization tank, a stirring mechanism is arranged inside the crystallization tank, and the feeding tank is communicated with the crystallization tank through a material conveying system. A PAT equipment set is installed at the top end of the crystallizing tank through a connecting assembly, the stirring mechanism comprises a motor and a stirring paddle, and the bottom end of the crystallizing tank is communicated with the product tank through the material conveying system. The PAT equipment group comprises a probe type on-line imaging particle shape and particle size analyzer, a probe type turbidity meter, an infrared concentration measuring instrument, an ultraviolet concentration measuring instrument, a Raman spectrometer, a pH meter and an ultrasonic solid content instrument, and the PAT equipment can be independently used or used in a combined manner; according to the utility model, the problem of poor product crystallization quality stability caused by manual feeding can be avoided, and harm to human bodies caused by generation of dangerous chemical products can be prevented.

Description

Technical Field

[0001] The utility model belongs to the technical field of crystallization monitoring, and in particular relates to an online PAT intermittent 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 step 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.

[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 the advanced technology of developed countries. The application of Process Analytical Technologies (PAT) is key to this. PAT technology is a system for analyzing and controlling production by means of real-time monitoring (for example, during processing) of the key quality and performance characteristics of raw materials, intermediates, and processes.

[0004] In order to solve the above problems, the present invention proposes a crystallization device with fully automatic feeding and discharging based on Process Analytical Technologies (PAT) technology. Utility Model Content

[0005] In view of this, the utility model provides an online PAT intermittent crystallization device, which can avoid the problem of poor stability of product crystallization quality caused by manual feeding.

[0006] The utility model is achieved in this way:

[0007] The utility model provides an online PAT intermittent crystallization device, which includes a feed tank, which is connected to a crystallization tank through a material conveying system, a temperature control device is provided on the outside of the crystallization tank, a stirring mechanism is provided on the inside of the crystallization tank, a PAT equipment group is installed on the top of the crystallization tank through a connecting assembly, the stirring mechanism includes a motor and a stirring paddle, the bottom of the crystallization tank is connected to a product tank through the material conveying system, the PAT equipment group includes a probe-type online imaging particle shape and size analyzer, a probe-type turbidity meter, an infrared concentration meter, an ultraviolet concentration meter, a Raman spectrometer, a pH meter, and an ultrasonic solid content meter, and the connecting assembly includes multiple groups of connecting sleeves.

[0008] The technical effects of an online PAT intermittent crystallization device provided by the utility model are as follows: by designing a feed tank, a crystallization tank, a temperature control device, a stirring mechanism, and a PAT equipment group, the production process is strictly controlled to achieve stable and uniform product quality; by setting a probe-type online imaging particle shape and size analyzer, it is used to measure crystal nucleation and growth particle shape and size; by setting a probe-type turbidity meter, it is used to measure the nucleation point, solubility and metastable zone width; by setting an infrared concentration meter, it is used to measure the solution concentration and supersaturation; by setting a connecting sleeve, it is used to facilitate the installation of corresponding PAT equipment, and flexibly adjust according to actual conditions to add or reduce PAT equipment.

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

[0010] Wherein, the material conveying system includes a peristaltic pump and a conveying hose, and the input end and the output end of the peristaltic pump are respectively connected to the feed tank and the crystallization tank through the conveying hose.

[0011] Furthermore, the material conveying system also includes a solenoid valve, a centrifugal pump and a conveying pipe. The solenoid valve is arranged at the bottom end of the crystallization tank, and the input end and output end of the centrifugal pump are respectively connected to the bottom end of the crystallization tank and the product tank through the conveying pipe.

[0012] Furthermore, the connecting sleeve is arranged at the top of the crystallization tank, and the inner wall of the connecting sleeve is provided with a fixed lining.

[0013] Furthermore, the surface of the fixed lining is provided with an anti-slip layer.

[0014] Furthermore, the surface of the anti-slip layer is provided with hemispherical silicone protrusions.

[0015] Furthermore, the motor is arranged at the top of the crystallization tank, the stirring paddle is arranged inside the crystallization tank, and the top of the stirring paddle is fixedly connected to the output end of the motor.

[0016] Furthermore, the collection probes of the probe-type online imaging particle shape and size analyzer, the probe-type turbidity meter, the infrared concentration meter and the ultrasonic solid content meter are all inserted into and installed inside the crystallization tank through the connecting sleeve.

[0017] Furthermore, both sides of the probe tube of the acquisition probe are provided with limit blocks, and both sides of the inner wall of the connecting sleeve are provided with limit slots adapted to the limit blocks.

[0018] Furthermore, the PAT equipment group also includes a host computer, and the probe-type online imaging particle shape and size analyzer, probe-type turbidity meter, infrared concentration meter, ultraviolet concentration meter, Raman spectrometer, pH meter, and ultrasonic solid content meter are electrically connected to the host computer respectively.

[0019] Compared with the prior art, the beneficial effects of the online PAT intermittent crystallization device provided by the utility model are: by designing a feed tank, a crystallization tank, a temperature control device, a stirring mechanism, and a PAT equipment group, the production process is strictly controlled to achieve stable and uniform product quality; by setting a probe-type online imaging particle shape and size analyzer, it is used to measure crystal nucleation and growth particle shape and size; by setting a probe-type turbidity meter, it is used to measure the nucleation point, solubility and metastable zone width; by setting an infrared concentration meter, it is used to measure the solution concentration and supersaturation; by setting a connecting sleeve, it is used to facilitate the installation of corresponding PAT equipment, and flexibly adjust according to actual conditions to add or reduce PAT equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] 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.

[0021] Figure 1 Schematic diagram of an online PAT batch crystallization device;

[0022] Figure 2 A schematic diagram of a connecting sleeve of an online PAT batch crystallization device;

[0023] In the accompanying drawings, the components represented by the reference numerals are as follows:

[0024] 1. Feed tank; 10. Probe-type turbidity meter; 11. Infrared concentration meter; 13. Connecting sleeve; 14. Peristaltic pump; 15. Delivery hose; 18. Delivery pipe; 19. Fixed lining; 2. Crystallization tank; 20. Limit block; 21. Limit slot; 3. Temperature control device; 4. Stirring mechanism; 5. PAT equipment group; 6. Motor; 7. Stirring paddle; 8. Product tank; 9. Probe-type online imaging particle shape and size analyzer. DETAILED DESCRIPTION

[0025] 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.

[0026] like Figure 1 2 is an embodiment of an online PAT intermittent crystallization device provided by the utility model. In this embodiment, it includes a feed tank 1, which is connected to the crystallization tank 2 through a material conveying system. A temperature control device 3 is provided on the outside of the crystallization tank 2, and a stirring mechanism 4 is provided inside the crystallization tank 2. The top of the crystallization tank 2 is installed with a PAT equipment group 5 through a connecting component. The stirring mechanism 4 includes a motor 6 and a stirring paddle 7. The bottom end of the crystallization tank 2 is connected to the product tank 8 through the material conveying system. The PAT equipment group 5 includes a probe-type online imaging particle shape and size analyzer 9, a probe-type turbidity meter 10, an infrared concentration meter 11, an ultraviolet concentration meter, a Raman spectrometer, a pH meter, and an ultrasonic solid content meter. The connecting component includes multiple groups of connecting sleeves 13.

[0027] Among them, the PAT device group 5 can add or reduce PAT devices according to actual needs, which is convenient for the individual use or combined use of PAT devices.

[0028] Among them, the feed tank 1 can be a jacketed or single-layer glass, stainless steel, or plastic tank body, which is used for temporary storage of raw materials; the product tank 8 can also be a jacketed or single-layer glass, stainless steel, or plastic tank body, which is used for storage of finished products.

[0029] The temperature control device 3 includes a heating unit and a refrigeration unit, and uses oil, water and other media through a circulation pipeline to achieve temperature control of the feed tank 1, the crystallization tank 2 and the product tank 8.

[0030] During use, a supersaturated solution of a predetermined amount and temperature is prepared and introduced into a feed tank 1. The feed tank 1 is maintained at a temperature set by a temperature control device 3 to completely dissolve the solute, resulting in a clear solution in the feed tank 1. The peristaltic pump 14 connecting the feed tank 1 and the crystallizer 2 is turned on to pump the clarified solution into the crystallizer 2 at a specific flow rate. The interior of the crystallizer 2 is now in a constant temperature state. The motor 6 is turned on to continuously stir the solution for a period of time at a set stirring rate, maintaining the stirring rate and cooling the solution by adjusting the temperature set by the temperature control device 3. A PAT device is installed at the corresponding position of the connecting sleeve 13, and the PAT device probe is inserted into the crystallizer 2 to monitor changes in important parameters within the tank, such as concentration, supersaturation, turbidity, morphology, and particle size distribution, in real time. Furthermore, the closed-loop control software of the host computer helps the operator adjust parameters such as temperature and stirring rate. After a certain period of time, the desired crystals are obtained. The parameters collected by the PAT device during the crystallization process assist the operator in determining whether the crystallization is complete. If the parameters meet the crystallization quality conditions, the user terminates the crystallization process and opens the solenoid valve, and the crystals enter the storage tank (8) through the conveying pipe (18). After that, new materials are input from the feed tank (1) and the cycle continues.

[0031] In the above technical solution, the material conveying system includes a peristaltic pump 14 and a conveying hose 15 , and the input end and the output end of the peristaltic pump 14 are connected to the feed tank 1 and the crystallization tank 2 respectively through the conveying hose 15 .

[0032] Furthermore, in the above technical solution, the material conveying system also includes a solenoid valve, a centrifugal pump and a conveying pipe 18. The solenoid valve is arranged at the bottom end of the crystallization tank 2, and the input end and output end of the centrifugal pump are respectively connected to the bottom end of the crystallization tank 2 and the product tank 8 through the conveying pipe 18.

[0033] Furthermore, in the above technical solution, the connecting sleeve 13 is provided at the top of the crystallization tank 2 , and the inner wall of the connecting sleeve 13 is provided with a fixed lining 19 .

[0034] Furthermore, in the above technical solution, the surface of the fixed lining 19 is provided with an anti-slip layer.

[0035] Furthermore, in the above technical solution, hemispherical silicone protrusions are arranged on the surface of the anti-slip layer.

[0036] Furthermore, in the above technical solution, the motor 6 is arranged at the top of the crystallization tank 2, the stirring paddle 7 is arranged inside the crystallization tank 2, and the top of the stirring paddle 7 is fixedly connected to the output end of the motor 6.

[0037] Furthermore, in the above technical solution, the collection probes of the probe-type online imaging particle shape and size analyzer 9, the probe-type turbidity meter 10, the infrared concentration meter 11 and the ultrasonic solid content meter are all inserted and installed into the crystallization tank 2 through the connecting sleeve 13.

[0038] Furthermore, in the above technical solution, limit blocks 20 are provided on both sides of the probe tube of the acquisition probe, and limit slots 21 adapted to fit the limit blocks 20 are opened on both sides of the inner wall of the connecting sleeve 13 .

[0039] Furthermore, in the above technical solution, the PAT equipment group 5 also includes a host computer, and the probe-type online imaging particle shape and size analyzer 9, the probe-type turbidity meter 10, the infrared concentration meter 11 and the ultrasonic solid content meter are electrically connected to the host computer respectively.

[0040] The host computer is a computer with built-in closed-loop control software for displaying and adjusting parameters such as the temperature inside the crystallization tank 2 and the stirring rate of the motor 6.

[0041] Among them, the model of the probe-type online imaging particle shape and size analyzer 9 is: 2D Vision Probe; the model of the probe-type turbidity meter 10 is: Turbidity probe; the infrared concentration meter 11 uses the probe-type online infrared spectrometer model: JGM ATR FTIR; the ultrasonic solid content meter uses the online ultrasonic solid phase concentration meter model Concert.

[0042] Specifically, the principle of the present invention is as follows: during use, a supersaturated solution of a predetermined amount and a predetermined temperature is prepared and introduced into a feed tank 1; the feed tank 1 is kept constant at a temperature set by a temperature control device 3, so that the solute is completely dissolved, at which point a clear solution should be present in the feed tank 1; the peristaltic pump 14 connecting the feed tank 1 and the crystallizer 2 is turned on, and the clarified solution is pumped into the crystallizer 2 at a specific flow rate. At this point, the interior of the crystallizer 2 is in a constant temperature state; the motor 6 is turned on and stirred for a period of time at a set stirring rate, the stirring rate is maintained, and the temperature is lowered by adjusting the set temperature of the temperature control device 3; a PAT device is installed at the corresponding position of the connecting sleeve 13, and the PAT device probe is inserted into the crystallizer 2 to monitor changes in important parameters within the tank, such as concentration, supersaturation, turbidity, morphology, and particle size distribution, in real time. Furthermore, the closed-loop control software of the host computer helps the operator adjust parameters such as temperature and stirring rate. After a certain period of time, the desired crystals are obtained. The parameters collected by the PAT device during the crystallization process assist the operator in determining whether the crystallization is complete. If the parameters meet the crystallization quality conditions, the user terminates the crystallization process and opens the solenoid valve, and the crystals enter the storage tank (8) through the conveying pipe (18). After that, new materials are input from the feed tank (1) and the cycle continues.

Claims

1. An online PAT intermittent crystallization device, characterized in that: The invention comprises a feed tank (1), wherein the feed tank (1) is connected to a crystallization tank (2) through a material conveying system, a temperature control device (3) is provided on the outside of the crystallization tank (2), a stirring mechanism (4) is provided on the inside of the crystallization tank (2), a PAT equipment group (5) is installed on the top of the crystallization tank (2) through a connecting assembly, the stirring mechanism (4) comprises a motor (6) and a stirring paddle (7), the bottom end of the crystallization tank (2) is connected to a product tank (8) through the material conveying system, the PAT equipment group (5) comprises a probe-type online imaging particle shape and size analyzer (9), a probe-type turbidity meter (10), an infrared concentration meter (11), an ultraviolet concentration meter, a Raman spectrometer, a pH meter and an ultrasonic solid content meter, and the connecting assembly comprises a plurality of connecting sleeves (13).

2. An online PAT intermittent crystallization device according to claim 1, characterized in that, The material conveying system comprises a peristaltic pump (14) and a conveying hose (15), wherein the input end and the output end of the peristaltic pump (14) are respectively connected to the feed tank (1) and the crystallization tank (2) through the conveying hose (15).

3. An online PAT intermittent crystallization device according to claim 2, characterized in that, The material conveying system further comprises a solenoid valve, a centrifugal pump and a conveying pipe (18), wherein the solenoid valve is arranged at the bottom end of the crystallization tank (2), and the input end and the output end of the centrifugal pump are respectively connected to the bottom end of the crystallization tank (2) and the product tank (8) through the conveying pipe (18).

4. An online PAT intermittent crystallization device according to claim 3, characterized in that, The connecting sleeve (13) is arranged at the top end of the crystallization tank (2), and the inner wall of the connecting sleeve (13) is provided with a fixed lining (19).

5. An online PAT intermittent crystallization device according to claim 4, characterized in that, The surface of the fixed lining (19) is provided with an anti-slip layer.

6. An online PAT intermittent crystallization device according to claim 5, characterized in that, The surface of the anti-slip layer is arranged with hemispherical silicone protrusions.

7. An online PAT intermittent crystallization device according to claim 6, characterized in that, The motor (6) is arranged at the top of the crystallization tank (2), the stirring paddle (7) is arranged inside the crystallization tank (2), and the top of the stirring paddle (7) is fixedly connected to the output end of the motor (6).

8. An online PAT intermittent crystallization device according to claim 7, characterized in that, The probe-type online imaging particle shape and size analyzer (9), the probe-type turbidity meter (10), the infrared concentration meter (11), and the collection probes of the ultrasonic solid content meter are all inserted and installed into the crystallization tank (2) through the connecting sleeve (13).

9. An online PAT intermittent crystallization device according to claim 8, characterized in that: Limiting blocks (20) are provided on both sides of the probe tube of the acquisition probe, and limiting slots (21) adapted to the limiting blocks (20) are provided on both sides of the inner wall of the connecting sleeve (13).

10. The online PAT intermittent crystallization device according to claim 9, characterized in that: The PAT equipment group (5) further includes a host computer, and the probe-type online imaging particle shape and size analyzer (9), the probe-type turbidity meter (10), the infrared concentration meter (11) and the ultrasonic solid content meter are electrically connected to the host computer respectively.

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