Apparatus for recrystallization of material

Abstract

The utility model provides a kind of equipment for material recrystallization, the inside of reaction kettle body is located the bottom of reaction kettle body and is equipped with filter element, filter element divides the inside of reaction kettle body into upper chamber and lower chamber, and movable assembly is equipped in lower chamber, movable assembly is set to be able to move towards the direction of close or away from filter element, and movable assembly can prevent liquid in upper chamber from flowing into lower chamber below movable assembly;The middle part of movable assembly is equipped with first through-hole, and first through-hole is equipped with closure mechanism for closing first through-hole, and the below of movable assembly is equipped with ejector rod, and ejector rod is used to prop up closure mechanism to make first through-hole open when movable assembly moves away from filter element direction.The equipment makes that material will not flow into the material to be crystallized after dissolving below filter element before crystallization, so it not only can avoid material waste, but also can avoid some incomplete dissolution material in melting process into the cavity below filter element.

Description

Technical Field

[0001] This utility model relates to a device for recrystallizing materials. Background Technology

[0002] In chemical and pharmaceutical synthesis, material purification and drying processes are common. Recrystallization is a frequently used method for purifying materials, especially pharmaceutical intermediates, and often requires multiple recrystallizations to obtain high-purity products. Single recrystallizations are relatively easy to achieve in production. This involves heating and cooling the reaction vessel, allowing crystals to precipitate, removing the solvent by centrifugation or filtration, and then repeatedly returning the material to the reaction vessel. Finally, the material is dried. This process is complex and often requires human intervention. Furthermore, the solvents used for recrystallization are often volatile, posing environmental pollution or health risks. Therefore, achieving multiple crystallizations within the same container is of great significance in chemical and pharmaceutical production.

[0003] Commonly available equipment combines washing, filtering, and drying in one unit. However, in practical use, a gap has been found between the filter plate and the liquid outlet, making it more suitable for washing solid materials. The recrystallization process requires heating and dissolving the material before cooling to precipitate the solids. After dissolving, the material passes through the filter plate and enters the gap. When the system cools, the material in the gap also crystallizes, resulting in material waste. Furthermore, some incompletely dissolved materials, especially those with a density greater than the recrystallization solvent, enter the cavity during melting, agglomerate upon cooling, and cause equipment blockage. Utility Model Content

[0004] The technical problem to be solved by this utility model is to overcome the defects of existing washing, filtering and drying three-in-one equipment that easily causes material waste and equipment blockage due to material agglomeration during cooling, and to provide a device for material recrystallization.

[0005] The present invention solves the above-mentioned technical problems through the following technical solution:

[0006] This utility model provides a device for material recrystallization, including a reactor body. The reactor body has a filter element located at the bottom of the reactor body. The filter element divides the interior of the reactor body into an upper chamber and a lower chamber. The lower chamber has a movable component. The movable component is configured to move in a direction that is close to or away from the filter element, and the movable component can prevent liquid in the upper chamber from flowing into the lower chamber below the movable component.

[0007] The movable component has a first through hole in its center, and a closing mechanism for closing the first through hole is provided inside the first through hole. A push rod is provided below the movable component, and the push rod is used to press against the closing mechanism to open the first through hole when the movable component moves away from the filter element. The filter element can be a filter plate or a filter screen.

[0008] In this design, using the aforementioned structure, when recrystallization of materials is required, the movable component is first moved to a position close to the filter element, keeping the first through-hole closed. Then, the material to be recrystallized and the solvent are added for crystallization. After crystallization, the movable component is moved downwards, and the push rod presses against the closing mechanism, opening the first through-hole. The liquid material flows through the first through-hole into the lower chamber, separating the crystallized solid from the liquid material and retaining it above the filter element. This design prevents dissolved material from flowing below the filter element before crystallization, thus avoiding material waste and preventing incompletely dissolved material from entering the cavity below the filter element during melting, which could cause clumping and blockage after cooling.

[0009] Preferably, the movable component includes a mounting plate and a seal, the mounting plate having a first through hole in the middle, the seal being disposed on the mounting plate, and the seal being used to seal the gap between the mounting plate and the mating component.

[0010] In this solution, by setting a sealing element, a good sealing effect is formed on the outer periphery of the mounting plate and the inner side of the first through hole, thereby preventing the dissolved material from flowing into the lower chamber through the gap between the mounting plate and other mating parts.

[0011] Preferably, the closing mechanism includes a movable plate adapted to the first through hole, the movable plate being connected to the mounting plate via an automatic closing device, the automatic closing device being used to close the first through hole with the movable plate.

[0012] In this solution, the above structure is adopted so that the closing mechanism can be easily opened by the push rod when the moving component moves away from the filter element; and the first through hole can be automatically closed by the automatic closing device when the moving component moves towards the filter element.

[0013] Preferably, the movable plate includes a first movable plate and a second movable plate, the first movable plate and the second movable plate are respectively connected to two opposite sides of the first through hole by the automatic closing device, and the opposite side of the first movable plate and the second movable plate is provided with a matching stepped structure.

[0014] In this design, by setting two cooperating movable plates, the sealing effect of the closing mechanism is improved when it is closed.

[0015] Preferably, the bottom of the reactor body is provided with a liquid material outlet, the push rod is a hollow structure, the lower end of the push rod is installed in the liquid material outlet, and the portion of the push rod located in the lower chamber is provided with a second through hole.

[0016] In this solution, the above structure is adopted, which facilitates the installation of the top rod and the extraction of liquid materials from the lower chamber.

[0017] Preferably, the upper end of the push rod has a tapered structure;

[0018] And / or, a filter screen is provided outside the second through hole;

[0019] And / or, there are multiple second through holes.

[0020] Preferably, the upper chamber is provided with a stirring mechanism;

[0021] And / or, the upper end of the reactor body is provided with a feed inlet communicating with the upper chamber, and the feed inlet is used to introduce the material to be recrystallized;

[0022] And / or, the upper end of the reactor body is provided with a gas phase outlet and a reflux port communicating with the upper chamber. The gas phase outlet and the reflux port are respectively connected to an external cooling mechanism through pipes. The gas phase outlet is used to allow the material volatilized in the reactor body to enter the cooling mechanism for recooling and liquefaction. The reflux port is used to allow the liquefied material to flow back into the reactor body.

[0023] And / or, the reactor body is further provided with a solid material outlet, which is located in the upper chamber near the filter element;

[0024] And / or, the reactor body is provided with a jacket on the outer periphery of the upper chamber, and the jacket is used to introduce a heating medium or a cooling medium.

[0025] Preferably, the reactor vessel body includes a separable upper vessel body and a lower vessel body, with the upper chamber located within the upper vessel body and the lower chamber located within the lower vessel body.

[0026] Preferably, the lower vessel body has an opening with a mounting portion, and the filter element is fixed on the mounting portion;

[0027] And / or, the device further includes a hydraulic mechanism, one end of the telescopic rod of which is connected to the upper vessel body, and the hydraulic mechanism is used to lift the upper vessel body.

[0028] Preferably, the device further includes a drive mechanism for driving the moving component to move.

[0029] The positive and progressive effects of this utility model are as follows: the equipment for material recrystallization of this utility model prevents the dissolved material to be crystallized from flowing into the bottom of the filter element before crystallization. This not only avoids material waste, but also prevents some incompletely dissolved material from entering the cavity below the filter element during the melting process, which could cause the material to clump together and block the equipment after cooling. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the structure of the device for material recrystallization in an embodiment of this utility model.

[0031] Figure 2 for Figure 1 A magnified view of a portion of point A in the middle.

[0032] Figure 3 for Figure 1 A magnified view of a portion of point B in the middle.

[0033] Explanation of reference numerals in the attached figures:

[0034] The reactor body is 100, the upper chamber is 110, the lower chamber is 120, the feed inlet is 101, the gas phase outlet is 102, the reflux port is 103, the solid material outlet is 104, and the mounting part is 105.

[0035] Filter element 200;

[0036] Movable component 300, mounting plate 310, movable plate 320, first movable plate 321, second movable plate 322, automatic closure device 330, seal 340;

[0037] Top rod 400, second through hole 401;

[0038] Jacket 500, inlet and outlet 501;

[0039] 600 stirring mechanism;

[0040] Hydraulic mechanism 700;

[0041] Drive mechanism 800;

[0042] Cooling mechanism 900. Detailed Implementation

[0043] The present invention will be described more clearly and completely below with reference to the accompanying drawings, using a preferred embodiment.

[0044] like Figure 1-3As shown, this embodiment discloses an apparatus for material recrystallization, including a reactor body 100. A filter element 200 is located at the bottom of the reactor body 100, dividing the interior of the reactor body 100 into an upper chamber 110 and a lower chamber 120. A movable component 300 is located in the lower chamber 120, configured to move towards or away from the filter element 200, and preventing liquid in the upper chamber 110 from flowing into the lower chamber 120 below the movable component 300. A first through-hole (not shown) is located in the middle of the movable component 300, and a closing mechanism is provided within the first through-hole. A push rod 400 is located below the movable component 300, used to press against the closing mechanism to open the first through-hole when the movable component 300 moves away from the filter element 200.

[0045] In this material recrystallization device, when recrystallization is required, the movable component 300 is first moved to a position close to the filter element 200, keeping the first through-hole closed. Then, the material to be recrystallized and solvent are added for crystallization. After crystallization, the movable component 300 is moved downwards, and the push rod 400 presses against the closing mechanism, opening the first through-hole. The liquid material flows into the lower chamber 120 through the first through-hole, separating the crystallized solid from the liquid material and retaining it above the filter element 200. This device prevents dissolved material from flowing into the space below the filter element 200 before crystallization. This not only avoids material waste but also prevents incompletely dissolved material from entering the cavity below the filter element 200 during melting, which could cause clumping and blockage after cooling.

[0046] In this embodiment, the filter element 200 is a filter screen. The filter element 200 is configured to leave the crystallized material in the upper chamber 110, while the uncrystallized solvent can flow down through the mesh of the filter element 200, thereby separating it from the crystallized material.

[0047] In this embodiment, the movable component 300 includes a mounting plate 310 and a sealing member 340. A first through hole is formed in the center of the mounting plate 310, and the sealing member 340 is disposed on the mounting plate 310. The sealing member 340 is used to seal the gap between the mounting plate 310 and other mating components. By providing the sealing member 340, a good sealing effect is formed on the outer periphery of the mounting plate 310 and the inner side of the first through hole, thereby preventing dissolved material from flowing into the lower chamber 120 through the gap between the mounting plate 310 and other components. Preferably, the sealing member 340 has good elasticity. Providing the sealing member 340 also allows the space between the mounting plate 310 and the filter element 200 to be filled as much as possible by the sealing member 340, avoiding gaps between the filter element 200 and the movable component 300.

[0048] In this embodiment, a sealing element 340 is also provided on the closing mechanism. When the closing mechanism closes the first through hole, the gap between the closing mechanism and the first through hole can be further closed, thereby further preventing the dissolved but uncrystallized material from flowing from the upper chamber 110 to the lower chamber 120 or into the gap between the closing mechanism and the first through hole.

[0049] Preferably, the closing mechanism includes a movable plate 320, which is adapted to the first through hole. The movable plate 320 is connected to the mounting plate 310 via an automatic closing device 330, which is used to close the first through hole with the movable plate. The automatic closing device 330 is a conventional hinge structure component, which adds an elastic element to a regular hinge, allowing the hinge to automatically reset after the external force is removed after it has been opened.

[0050] In this solution, the above structure is adopted so that the closing mechanism can be easily opened by the push rod 400 when the movable component 300 moves away from the filter element 200; and the first through hole can be automatically closed by the automatic closing device 330 when the movable component 300 moves towards the filter element 200.

[0051] like Figure 2 As shown, in this embodiment, the movable plate 320 includes a first movable plate 321 and a second movable plate 322. The first movable plate 321 and the second movable plate 322 are respectively connected to two opposite sides of the first through hole via an automatic closing device 330. A mating stepped structure is provided on the opposite side of the first movable plate 321 and the second movable plate 322. By providing two mating movable plates, the sealing effect of the closing mechanism is improved when closed. In some other embodiments, only one movable plate 320 may be provided.

[0052] like Figure 3 As shown, in this embodiment, the bottom of the reactor body 100 is provided with a liquid material outlet, and the push rod 400 has a hollow structure. The lower end of the push rod 400 is installed inside the liquid material outlet, and the portion of the push rod 400 located in the lower chamber 120 has a second through hole 401. This structure facilitates both the installation of the push rod 400 and the extraction of liquid material from the lower chamber 120.

[0053] In some other embodiments, the liquid material outlet and the push rod 400 may be located at different positions, but the push rod 400 must be located in a position that allows the closing mechanism to be opened.

[0054] In this embodiment, the upper end of the top rod 400 has a tapered structure, and the tapered structure is provided with a plurality of second through holes 401. A filter screen (not shown in the figure) can be installed outside the second through holes 401.

[0055] like Figure 1 As shown, a stirring mechanism 600 is provided in the upper chamber 110. The stirring mechanism 600 includes a stirring paddle and is driven by a motor outside the reactor body 100. The stirring mechanism 600 can be configured to move up and down. After the recrystallized material and solvent are put into the reactor, the stirring paddle is raised to a certain height and stirring is started to accelerate the dissolution of the recrystallized material.

[0056] In this embodiment, the upper end of the reactor body 100 is provided with a feed inlet 101 communicating with the upper chamber 110. The feed inlet 101 is used to introduce the material to be recrystallized. The upper end of the reactor body 100 is also provided with a gas phase outlet 102 and a reflux outlet 103 communicating with the upper chamber 110. The gas phase outlet 102 and the reflux outlet 103 are respectively connected to an external cooling mechanism 900 through pipes. The gas phase outlet 102 is used to allow the material volatilized in the reactor body 100 to enter the cooling mechanism 900 for recooling and liquefaction. The reflux outlet 103 is used to allow the liquefied material to flow back into the reactor body 100. The external cooling mechanism 900 can be a liquid cooling mechanism, which uses external coolant to liquefy the material volatilized in the reactor body 100 through heat exchange.

[0057] The reactor body 100 is also provided with a solid material outlet 104, which is located in the upper chamber 110 near the filter element 200, so as to facilitate the discharge of the crystallized material.

[0058] The reactor body 100 is equipped with a jacket 500 on the outer periphery of the upper chamber 110. The jacket 500 is used to introduce heating or cooling media. Heating media is introduced into the jacket 500 through the inlet / outlet 501 to dissolve the recrystallized material. After the temperature inside the reactor body 100 reaches a certain level and the material is refluxed for a period of time (so that the material volatilized due to heating is liquefied through the cooling mechanism 900 and flows back into the reactor), the medium in the jacket 500 is switched to cooling media to cool the material inside the reactor body 100. After the material crystallizes and precipitates, it is then filtered.

[0059] In this embodiment, the reactor body 100 includes a separable upper body and a lower body, with an upper chamber 110 located inside the upper body and a lower chamber 120 located inside the lower body. A mounting portion 105 is provided at the opening of the lower body, and a filter element 200 is fixed to the mounting portion 105.

[0060] In this embodiment, the device further includes a hydraulic mechanism 700. One end of the telescopic rod of the hydraulic mechanism 700 is connected to the upper vessel body, and the hydraulic mechanism 700 is used to lift the upper vessel body. The hydraulic mechanism 700 facilitates the separation of the upper vessel body from the lower vessel body, making it easier to replace internal parts.

[0061] In this embodiment, the device further includes a drive mechanism 800, which is used to drive the movable component 300 to move. For example... Figure 1 As shown, the drive mechanism 800 in this embodiment is a pneumatic telescopic mechanism. The telescopic rod of this mechanism extends from the bottom of the lower vessel body into the lower chamber 120 and is connected to the mounting plate 310 of the movable component 300. The telescopic rod is extended and retracted by the pneumatic telescopic mechanism, which drives the movable component 300 to move in a direction that is close to or away from the filter element 200. The connection between the telescopic rod and the wall of the lower vessel body is sealed by a sealing mechanism to prevent the solution flowing into the lower chamber 120 from leaking out from there.

[0062] In this embodiment, the movable component 300 moves up and down via a pneumatic telescopic mechanism. Before feeding, the movable component 300 is moved upward, ensuring close contact between the lower end of the movable component 300 and the filter element 200, with no gaps between them. Then, the material to be recrystallized is introduced into the reactor body 100 through the feed inlet 101. The material to be crystallized is dissolved and crystallized by introducing a heating or cooling medium into the jacket 500. After crystallization, the movable component 300 moves downward, and the movable plate 320 of the closing mechanism is opened via the push rod 400. A nitrogen pressurization mechanism can be connected to the upper end of the reactor body, using nitrogen pressure to force the liquid out and flow into the lower chamber through the first through hole. After the liquid is forced out, the movable component 300 is moved upward again, and the automatic closure device 330 automatically closes the first through hole, allowing for secondary crystallization. After crystallization is complete, the drying mode is activated to dry and discharge the material.

[0063] While specific embodiments of this utility model have been described above, those skilled in the art should understand that these are merely illustrative examples, and the scope of protection of this utility model is defined by the appended claims. Those skilled in the art can make various changes or modifications to these embodiments without departing from the principles and essence of this utility model, but all such changes and modifications fall within the scope of protection of this utility model.

Claims

1. An apparatus for recrystallizing materials, comprising a reactor body, characterized in that, The interior of the reactor body is equipped with a filter element at the bottom of the reactor body. The filter element divides the interior of the reactor body into an upper chamber and a lower chamber. The lower chamber is equipped with a movable component. The movable component is configured to move in a direction that is close to or away from the filter element, and the movable component can prevent liquid in the upper chamber from flowing into the lower chamber below the movable component. The movable component has a first through hole in the middle, and a closing mechanism for closing the first through hole is provided in the first through hole. A top rod is provided below the movable component, and the top rod is used to press against the closing mechanism to open the first through hole when the movable component moves away from the filter element.

2. The apparatus for material recrystallization as described in claim 1, characterized in that, The movable component includes a mounting plate and a seal. The mounting plate has a first through hole in the middle. The seal is disposed on the mounting plate and is used to seal the gap between the mounting plate and the mating component.

3. The apparatus for material recrystallization as described in claim 2, characterized in that, The closing mechanism includes a movable plate that is adapted to the first through hole. The movable plate is connected to the mounting plate via an automatic closing device, which is used to close the first through hole with the movable plate.

4. The apparatus for material recrystallization as described in claim 3, characterized in that, The movable plate includes a first movable plate and a second movable plate. The first movable plate and the second movable plate are respectively connected to two opposite sides of the first through hole through the automatic closing device. The opposite sides of the first movable plate and the second movable plate are provided with a matching stepped structure.

5. The apparatus for material recrystallization as described in claim 1, characterized in that, The bottom of the reactor body is provided with a liquid material outlet. The push rod has a hollow structure, and the lower end of the push rod is installed in the liquid material outlet. The part of the push rod located in the lower chamber is provided with a second through hole.

6. The apparatus for material recrystallization as described in claim 5, characterized in that, The upper end of the top rod has a tapered structure; And / or, a filter screen is provided outside the second through hole; And / or, there are multiple second through holes.

7. The apparatus for material recrystallization as described in claim 1, characterized in that, The upper chamber is equipped with a stirring mechanism; And / or, the upper end of the reactor body is provided with a feed inlet communicating with the upper chamber, and the feed inlet is used to introduce the material to be recrystallized; And / or, the upper end of the reactor body is provided with a gas phase outlet and a reflux port communicating with the upper chamber. The gas phase outlet and the reflux port are respectively connected to an external cooling mechanism through pipes. The gas phase outlet is used to allow the material volatilized in the reactor body to enter the cooling mechanism for recooling and liquefaction. The reflux port is used to allow the liquefied material to flow back into the reactor body. And / or, the reactor body is further provided with a solid material outlet, which is located in the upper chamber near the filter element; And / or, the reactor body is provided with a jacket on the outer periphery of the upper chamber, and the jacket is used to introduce a heating medium or a cooling medium.

8. The apparatus for material recrystallization as described in claim 1, characterized in that, The reactor vessel body includes a separable upper vessel body and a lower vessel body, with the upper chamber located within the upper vessel body and the lower chamber located within the lower vessel body.

9. The apparatus for material recrystallization as described in claim 8, characterized in that, The lower vessel body has an opening with a mounting part, and the filter element is fixed on the mounting part; And / or, the device further includes a hydraulic mechanism, one end of the telescopic rod of which is connected to the upper vessel body, and the hydraulic mechanism is used to lift the upper vessel body.

10. The apparatus for recrystallization of materials as described in claim 1, characterized in that, The device also includes a drive mechanism for driving the moving component to move.

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