A pharmaceutical magnesium chloride cooling crystallization device

Abstract

This utility model belongs to the technical field of cooling crystallization devices, and particularly relates to a cooling crystallization device for pharmaceutical-grade magnesium chloride. It includes a reaction vessel, a side-wall detection structure, and a cooling structure. The side-wall detection structure is sealed and installed on an assembly port on the side wall of the reaction vessel via a sealed mounting structure. The side-wall detection structure includes a protective sleeve and a detection element disposed within the protective sleeve. The sealed mounting structure includes a sealing support body, a sealing support outer plate, and a displacement monitoring structure disposed between the two. The cooling structure includes a cooling jacket, a cooling serpentine tube, or a combination of both, wrapped around the outside of the reaction vessel. A regulating valve is installed on the coolant inlet pipe. This utility model adopts a closed-loop heat exchange method, which avoids introducing impurities into the system, eliminating impurities at the source and ensuring product purity. Through temperature control interlocking, the cooling crystallization rate is precisely adjusted to achieve stable and uniform crystal particles with concentrated particle size distribution, effectively improving product quality.

Description

Technical Field

[0001] This utility model belongs to the technical field of cooling crystallization devices, and in particular relates to a cooling crystallization device for pharmaceutical magnesium chloride. Background Technology

[0002] The pharmacopoeia specifies magnesium chloride with the chemical formula MgCl2·6H2O, and a content requirement of 98.0%–101.0%, with even more detailed regulations on other impurities. Cooling crystallization is a common operation in magnesium chloride production. To meet the high-quality requirements of pharmaceutical-grade magnesium chloride, the cooling method and cooling rate of the equipment need to be designed and optimized. In recent years, cooling gas has been commonly used to cool and crystallize the material. However, because the gas directly contacts the crystallizing liquid, it easily introduces impurities, reducing the quality of pharmaceutical-grade magnesium chloride and affecting the normal use by downstream customers.

[0003] Currently, cooling crystallization devices used in the production of pharmaceutical-grade magnesium chloride often suffer from the following drawbacks: ① Gas cooling easily introduces impurities, leading to a decline in the quality and poor uniformity of the pharmaceutical-grade magnesium chloride product; ② The top-mounted temperature measuring device is too long and has poor heat transfer performance, resulting in reduced accuracy in temperature measurement of the pharmaceutical-grade magnesium chloride product; ③ Detecting particle size after crystallization is also cumbersome. Therefore, designing a cooling crystallization device for pharmaceutical-grade magnesium chloride that can overcome these shortcomings is a pressing technical problem to be solved in this field. Utility Model Content

[0004] In order to solve the problems existing in the prior art, this utility model provides a pharmaceutical magnesium chloride cooling crystallization device.

[0005] The technical solution adopted by this utility model to solve this problem is:

[0006] A pharmaceutical-grade magnesium chloride cooling crystallization apparatus includes a reaction vessel, a feed pipe and a stirring motor installed at the top of the reaction vessel, and a discharge pipe installed at the bottom of the reaction vessel. It also includes:

[0007] A side-wall type detection structure is sealed and installed on an assembly port on the side wall of a reactor via a sealed mounting structure. The side-wall type detection structure includes a protective sleeve and a detection element disposed within the protective sleeve. One end of the protective sleeve is a closed end, and the other end is an open end. The sealed mounting structure includes a sealing support body, a sealing support outer plate, and a displacement monitoring structure disposed between the two. The open end of the protective sleeve is fixedly connected to the sealing support body. The sealing support body is interference-fitted onto the assembly port via a sealing element and fixed with bolts. The support outer plate is bolted onto the assembly port.

[0008] The cooling structure includes a cooling jacket, a cooling serpentine tube, or a combination of both, wrapped around the outside of the reactor. Both the cooling jacket and the cooling serpentine tube are equipped with a coolant inlet pipe and a coolant outlet pipe, and a regulating valve is provided on the coolant inlet pipe.

[0009] In the above technical solution, the protective sleeve is a straight tube sleeve, and the open end of the protective sleeve has an arc transition and is fixedly connected to the sealing support.

[0010] In the above technical solution, the sealing support body includes an integrally connected tapered reducing support body and a polygonal support plate, wherein the diameter of the tapered reducing support body at the end near the protective sleeve is smaller than the diameter of the end away from the protective sleeve.

[0011] In the above technical solution, the assembly port includes: a tapered inner hole section adapted to the shape of the tapered differential support body, a polygonal middle hole section adapted to the shape of the polygonal support plate, and a cylindrical outer hole section adapted to the shape of the sealing support outer plate.

[0012] In the above technical solution, the tapered differential support body is interference-fitted to the tapered inner hole section through a sealing element, the polygonal support plate is interference-fitted to the polygonal middle hole section through a sealing element and fixed with bolts, and the outer support plate is interference-fitted to the cylindrical outer hole section through a sealing element and fixed with bolts.

[0013] In the above technical solution, the displacement monitoring structure includes:

[0014] At least two displacement rods are fixedly mounted on a polygonal support plate, and permanent magnets are provided on the displacement rods.

[0015] The number of sliding holes is the same as the number of displacement rods, and they are correspondingly opened on the outer plate of the sealing support. Electromagnets and magnetic sensors are installed in the sliding holes.

[0016] The displacement rods are inserted into the sliding holes one by one. After the sealing support body and the sealing support outer plate are sealed and installed on the assembly port on the side wall of the reactor, the permanent magnet and the electromagnet are attracted by magnetism.

[0017] In the above technical solution, the detection element is a thermocouple, and the protective sleeve is a titanium sleeve.

[0018] In the above technical solution, the detection element is a particle size detection camera, and the protective sleeve is a tempered glass sleeve.

[0019] In the above technical solution, the reactor is equipped with a stirrer, which includes a stirring rod, a U-shaped stirring paddle mounted on the stirring rod, and several turbine stirring paddles mounted on the stirring rod.

[0020] In the above technical solution, the turbine agitator includes an agitator disk and arc-shaped agitators arranged in pairs symmetrically at the upper and lower ends of the agitator disk. The arc-shaped agitators are distributed in a ring array around the central axis of the agitator disk.

[0021] The advantages and positive effects of this utility model are:

[0022] 1. In this utility model, in view of the characteristics of high viscosity and low pH value of the crystallization liquid, the reaction vessel adopts a composite material, such as titanium-plated carbon steel. The use of composite materials can improve hardness and corrosion resistance at the same time, significantly extend the service life of the device, reduce maintenance costs, and effectively ensure the efficiency, stability and economy of the magnesium chloride crystallization process.

[0023] 2. In this utility model, the cooling method adopts a cooling jacket, a cooling serpentine tube, or a combination of both cooling structures. The closed heat exchange method can avoid introducing impurities into the system, eliminate the introduction of impurities into the system from the source, and ensure product purity.

[0024] 3. In this utility model, the regulating valve can be interlocked with the temperature detection element. The opening and closing size of the regulating valve can be controlled according to the temperature, thereby accurately controlling the rate of temperature drop of the crystallizing liquid. By precisely adjusting the cooling crystallization rate through temperature control interlock, stable and uniform crystallized particles and concentrated particle size distribution can be achieved, effectively improving product quality.

[0025] 4. In this utility model, when the bolts of the sealing support outer plate become loose, the electromagnet and permanent magnet in the electromagnet displacement monitoring structure will physically separate, and then an alarm will be triggered. The staff can promptly detect this and tighten the sealing support outer plate to prevent further loosening and avoid gaps between the responsiveness and the side wall detection structure, which could lead to leakage. Attached Figure Description

[0026] The technical solution of this utility model will be further described in detail below with reference to the accompanying drawings and embodiments. However, it should be understood that these drawings are designed for illustrative purposes only and are not intended to limit the scope of this utility model. In addition, unless otherwise specified, these drawings are intended only to conceptually illustrate the structural construction described herein and are not necessarily drawn to scale.

[0027] Figure 1 This is a schematic diagram of the structure of this utility model. Figure 1 ;

[0028] Figure 2 yes Figure 1 The main view;

[0029] Figure 3 yes Figure 1 A schematic diagram of a half-section structure;

[0030] Figure 4 yes Figure 3 The main view;

[0031] Figure 5 yes Figure 3 Schematic diagram of the structure of the stirrer;

[0032] Figure 6 yes Figure 5 Top view;

[0033] Figure 7 yes Figure 3 Exploded view of the middle sidewall detection structure and the sealed installation structure;

[0034] Figure 8 yes Figure 7 Enlarged view of section A in the middle;

[0035] Figure 9 yes Figure 3 A structural diagram from another angle;

[0036] Figure 10 yes Figure 9 Enlarged view of section B;

[0037] Figure 11 yes Figure 9 Schematic diagram of the structure of the stirrer;

[0038] Figure 12 yes Figure 7 The main view;

[0039] Figure 13 yes Figure 12 Enlarged view of section C;

[0040] Figure 14 This is a half-section diagram of the side-wall detection structure and the sealed installation structure in their assembled state.

[0041] Figure 15 yes Figure 14 A structural diagram from another angle;

[0042] Figure 16 yes Figure 15 The main view;

[0043] Figure 17 This is a schematic diagram of the structure of this utility model. Figure 2 ;

[0044] Figure 18 yes Figure 17 The main view.

[0045] In the diagram: 1-Reaction vessel; 2-Feed pipe; 3-Stirring motor; 4-Discharge pipe; 5-Assembly port; 501-Conical inner hole section; 502-Polygonal central hole section; 503-Cylindrical outer hole section; 6-Protective sleeve; 7-Detection element; 8-Sealing support outer plate; 9-Seal; 10-Cooling jacket; 11-Cooling serpentine pipe; 12-Coolant inlet pipe; 13-Coolant outlet pipe; 14-Regulating valve; 15-Conical reducing support body; 16-Polygonal support plate; 17-Displacement rod; 18-Permanent magnet; 19-Sliding hole; 20-Electromagnet and magnetic control sensor; 21-Stirring rod; 22-U-shaped stirring paddle; 23-Stirring disc; 24-Arc-shaped stirring paddle. Detailed Implementation

[0046] First, it should be noted that the specific structure, features, and advantages of this utility model will be described in detail below by way of examples. However, all descriptions are for illustrative purposes only and should not be construed as limiting the utility model in any way. Furthermore, any single technical feature described or implied in the embodiments mentioned herein, or any single technical feature shown or implied in the accompanying drawings, can still be arbitrarily combined or deleted among these technical features (or their equivalents) to obtain more other embodiments of this utility model that may not be directly mentioned herein. Additionally, for the sake of simplifying the drawings, the same or similar technical features may be indicated only in one place in the same drawing.

[0047] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "setting," "connection," "fixing," and "screw-on" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; 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; they can refer to the internal communication of two components or the interaction between two components. Unless otherwise explicitly limited, those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances. The utility model will now be described in detail with reference to the accompanying drawings.

[0048] Example 1:

[0049] A pharmaceutical-grade magnesium chloride cooling crystallization apparatus includes a reaction vessel 1, with a feed pipe 2 and a stirring motor 3 installed at the top of the reaction vessel 1, and a discharge pipe 4 installed at the bottom of the reaction vessel 1. It also includes:

[0050] A side-wall type detection structure is sealed and installed on the assembly port 5 on the side wall of the reactor 1 through a sealing installation structure. The side-wall type detection structure includes a protective sleeve 6 and a detection element 7 disposed in the protective sleeve 6. One end of the protective sleeve 6 is a closed end and the other end is an open end. The sealing installation structure includes a sealing support body, a sealing support outer plate 8, and a displacement monitoring structure disposed between the two. The open end of the protective sleeve 6 is fixedly connected to the sealing support body. The sealing support body is interference-fitted onto the assembly port 5 through a sealing element 9 and fixed with bolts. The support outer plate 8 is installed onto the assembly port 5 with bolts.

[0051] The cooling structure includes a cooling jacket 10, a cooling serpentine tube 11, or a combination of both, wrapped around the outside of the reactor. Both the cooling jacket 10 and the cooling serpentine tube 11 are provided with a coolant inlet pipe 12 and a coolant outlet pipe 13. A regulating valve 14 is provided on the coolant inlet pipe 12.

[0052] In this embodiment, considering the high viscosity and low pH of the crystallization liquid, the reactor 1 is made of composite materials, such as titanium-plated carbon steel. Using composite materials improves hardness while also providing corrosion resistance, significantly extending the lifespan of the device, reducing maintenance costs, and effectively ensuring the efficiency, stability, and economy of the magnesium chloride crystallization process. The cooling method employs a cooling jacket 10, a cooling serpentine tube 11, or a combination of both, using a closed-loop heat exchange system to avoid introducing impurities into the system, thus preventing impurities from entering the system at the source and ensuring product purity. The regulating valve 14 can be interlocked with the temperature detection element, controlling the opening and closing of the valve according to the temperature, thereby precisely controlling the rate of temperature decrease of the crystallization liquid. Through temperature control interlocking, the cooling crystallization rate is precisely adjusted, achieving stable and uniform crystal particles with a concentrated particle size distribution, effectively improving product quality.

[0053] At least one assembly port 5 is provided on the side wall of the reactor 1. A side-wall detection structure is sealed and installed on the assembly port through a sealing installation structure. The side-wall detection structure includes a protective sleeve 6 and a detection element 7 set inside the protective sleeve 6. The detection element can be, but is not limited to, a temperature detection element or a crystal size detection element. The detection element is inserted into the protective sleeve through the open end of the protective sleeve. The protective sleeve is then sealed and installed inside the assembly port through the sealing installation structure. The protective sleeve protects and supports the detection element. When the internal element is a temperature detection element, the protective sleeve is made of titanium material, which provides high temperature measurement accuracy. When the internal element is a crystal size detection element, the protective sleeve is made of tempered glass, which provides high visibility. The sealed installation structure includes a sealed support body, a sealed support outer plate 8, and a displacement monitoring structure set between the two. The displacement monitoring structure is preferably an electromagnet-type displacement monitoring structure. When the bolts of the sealed support outer plate become loose, the electromagnet and permanent magnet in the electromagnet-type displacement monitoring structure will physically separate, thereby triggering an alarm. The staff can promptly detect and tighten the sealed support outer plate to prevent further loosening and avoid gaps between the detection structure and the side wall detection structure, which could lead to leakage. The use of an electromagnet-type displacement monitoring structure solves the corrosion problem and enables non-contact displacement monitoring.

[0054] Furthermore, in this embodiment, the protective sleeve 6 can be a straight tube, and a suitable length of protective sleeve can be selected and installed according to the requirements to meet the temperature measurement or particle size detection requirements at different locations. The open end of the protective sleeve 6 has an arc transition and is fixedly connected to the sealing support.

[0055] Furthermore, in this embodiment, the sealing support may include an integrally connected tapered reducing support 15 and polygonal support plate 16, wherein the diameter of the tapered reducing support 15 near the protective sleeve 6 is smaller than the diameter of the end away from the protective sleeve 6.

[0056] Furthermore, in this embodiment, the assembly port 5 may include: a tapered inner hole section 501 adapted to the shape of the tapered support body, a polygonal middle hole section 502 adapted to the shape of the polygonal support plate, and a cylindrical outer hole section 503 adapted to the shape of the sealing support outer plate.

[0057] Furthermore, in this embodiment, the tapered differential support 15 is interference-fitted to the tapered inner hole section 501 via a seal, the polygonal support plate 16 is interference-fitted to the polygonal middle hole section 502 via a seal and fixed with bolts, and the outer support plate 8 is interference-fitted to the cylindrical outer hole section 503 via a seal and fixed with bolts. The above fixing makes the sidewall detection structure sealed on the assembly port 5. The seal can be, but is not limited to, a sealing ring.

[0058] Example 2:

[0059] Embodiment 2 of this utility model is a further improvement on Embodiment 1 in order to fully leverage the technical advantages of the present invention. The following is an illustrative example.

[0060] The displacement monitoring structure includes:

[0061] At least two displacement rods 17 are fixedly installed on the polygonal support plate 16, and permanent magnets 18 are provided on the displacement rods 17.

[0062] The number of sliding holes 19 is the same as the number of displacement rods 17, and they are correspondingly opened on the sealing support outer plate 8. An electromagnet and a magnetic control sensor 20 are installed in the sliding holes 19.

[0063] The displacement rods 17 are inserted into the sliding holes 19 one by one. After the sealing support body and the sealing support outer plate are sealed and installed on the assembly port 5 on the side wall of the reactor 1, the permanent magnet 18 is attracted to the electromagnet.

[0064] In this embodiment, an electromagnet and a magnetic control sensor (reed switch or Hall effect sensor) are installed in the sliding hole of the sealed support outer plate. A permanent magnet is installed on one side of the polygonal support plate via a displacement rod (the position must be aligned with the electromagnet and magnetic control sensor). The magnetic control sensor signal is connected to the alarm circuit (simple series drive or microcontroller input) through a connection circuit. Then, the output of the alarm circuit is connected to the actuator (buzzer, wireless module). The electromagnet, magnetic control sensor, alarm circuit, and actuator are all connected to a power source. When the permanent magnet and the electromagnet are magnetically attracted, the buzzer should be silent; when the permanent magnet and the electromagnet are physically separated, the buzzer is immediately triggered.

[0065] It should be noted that by precisely setting the relative position and distance between the permanent magnet, the electromagnet, and the magnetic control sensor, it is ensured that the sensor can be reliably triggered (reed switch closed / Hall sensor output effective level) when the magnet is engaged, and can be reliably reset when the magnet is disengaged.

[0066] Furthermore, in this embodiment, the detection element 7 can be a thermocouple, and the protective sleeve 6 can be a titanium sleeve. The titanium sleeve can be surface modified or coated with a composite coating, such as a polytetrafluoroethylene (PTFE) coating, to further improve corrosion resistance without affecting thermal conductivity.

[0067] Furthermore, in this embodiment, the detection element 7 can be a particle size detection camera, and the protective sleeve 6 can be a tempered glass sleeve.

[0068] Furthermore, in this embodiment, a stirrer can be installed inside the reactor 1. Due to the high viscosity and low pH of magnesium chloride crystallizing liquid, the stirrer material needs to be a composite material, such as titanium-plated carbon steel, which can improve hardness while also having corrosion resistance, thus greatly extending the life of the device.

[0069] Furthermore, in this embodiment, the stirrer may include a stirring rod 21, a U-shaped stirring paddle 22 disposed on the stirring rod 21, and a plurality of turbine stirring paddles disposed on the stirring rod 21.

[0070] Furthermore, in this embodiment, the turbine agitator includes an agitator disk 23 and arc-shaped agitator blades 24 arranged symmetrically at the upper and lower ends of the agitator disk 23. The arc-shaped agitator blades 24 are arranged in a ring array around the central axis of the agitator disk 23. When the arc-shaped agitator blades rotate, they can drive the material to generate vortices, which, in conjunction with the U-shaped agitator blades, can further improve the agitation effect.

[0071] The above embodiments have provided a detailed description of the present invention, but the content described is only a preferred embodiment of the present invention and should not be considered as limiting the scope of the present invention. All equivalent changes and improvements made in accordance with the claims of the present invention should still fall within the patent coverage of the present invention.

Claims

1. A pharmaceutical-grade magnesium chloride cooling crystallization apparatus, comprising a reaction vessel, wherein a feed pipe and a stirring motor are provided at the top of the reaction vessel, and a discharge pipe is provided at the bottom of the reaction vessel, characterized in that: Also includes: A side-wall type detection structure is sealed and installed on an assembly port on the side wall of a reactor via a sealed mounting structure. The side-wall type detection structure includes a protective sleeve and a detection element disposed within the protective sleeve. One end of the protective sleeve is a closed end, and the other end is an open end. The sealed mounting structure includes a sealing support body, a sealing support outer plate, and a displacement monitoring structure disposed between the two. The open end of the protective sleeve is fixedly connected to the sealing support body. The sealing support body is interference-fitted onto the assembly port via a sealing element and fixed with bolts. The support outer plate is bolted onto the assembly port. The cooling structure includes a cooling jacket, a cooling serpentine tube, or a combination of both, wrapped around the outside of the reactor. Both the cooling jacket and the cooling serpentine tube are equipped with a coolant inlet pipe and a coolant outlet pipe, and a regulating valve is provided on the coolant inlet pipe.

2. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as claimed in claim 1, wherein: The protective sleeve is a straight tube, and the open end of the protective sleeve has an arc transition and is fixedly connected to the sealing support.

3. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as defined in claim 2, wherein: The sealing support body includes an integrally connected tapered reducing support body and a polygonal support plate, wherein the diameter of the tapered reducing support body at the end near the protective sleeve is smaller than the diameter of the end away from the protective sleeve.

4. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as defined in claim 3, wherein: The assembly port includes: a tapered inner hole section adapted to the shape of the tapered differential support body, a polygonal middle hole section adapted to the shape of the polygonal support plate, and a cylindrical outer hole section adapted to the shape of the sealing support outer plate.

5. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as defined in claim 4, wherein: The tapered support body is interference-fitted to the tapered inner hole section via a sealing element, the polygonal support plate is interference-fitted to the polygonal middle hole section via a sealing element and fixed with bolts, and the outer support plate is interference-fitted to the cylindrical outer hole section via a sealing element and fixed with bolts.

6. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as defined in claim 3, wherein: The displacement monitoring structure includes: At least two displacement rods are fixedly mounted on a polygonal support plate, and permanent magnets are provided on the displacement rods. The number of sliding holes is the same as the number of displacement rods, and they are correspondingly opened on the outer plate of the sealing support. Electromagnets and magnetic sensors are installed in the sliding holes. The displacement rods are inserted into the sliding holes one by one. After the sealing support body and the sealing support outer plate are sealed and installed on the assembly port on the side wall of the reactor, the permanent magnet and the electromagnet are attracted by magnetism.

7. A pharmaceutical magnesium chloride cooling crystallization apparatus according to any one of claims 2-6, characterized in that: The detection element is a thermocouple, and the protective sleeve is a titanium sleeve.

8. A pharmaceutical magnesium chloride cooling crystallization apparatus according to any one of claims 2-6, characterized in that: The detection element is a particle size detection camera, and the protective sleeve is a tempered glass sleeve.

9. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as defined in claim 1, wherein: The reactor is equipped with a stirrer, which includes a stirring rod, a U-shaped stirring paddle mounted on the stirring rod, and several turbine stirring paddles mounted on the stirring rod.

10. A pharmaceutical grade magnesium chloride cooling crystallization apparatus as defined in claim 9, wherein: The turbine impeller includes an impeller disk and two arc-shaped impellers arranged symmetrically at the upper and lower ends of the impeller disk. The arc-shaped impellers are arranged in a ring array around the central axis of the impeller disk.

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