A crystallization dish for m-bromo benzoic acid crystallization

Abstract

The utility model belongs to crystallization equipment technical field especially relates to a crystallizing dish for m-bromobenzoic acid crystallization. The utility model discloses a crystallizing dish for m-bromobenzoic acid crystallization to solve the problem of the cooling speed not being easy to control in the prior art, and provide a crystallizing dish for m-bromobenzoic acid crystallization, which comprises a crystallizing dish main body having a crystallization space inside, a cover body for closing the crystallization space is arranged above the crystallizing dish main body, a heat exchange cavity for circulating heat exchange medium is further arranged in the side wall of the crystallizing dish main body, the upper end of the heat exchange cavity is communicated with the medium outlet, the lower end is communicated with the medium inlet, and the medium outlet and the medium inlet are protruded from the surface of the side wall of the crystallizing dish main body. The utility model discloses that the heat exchange cavity is arranged in the side wall of the crystallizing dish main body, the heat exchange medium can enter the heat exchange cavity and exchange heat with the solution in the crystallization space, so that the cooling speed in the crystallization process is better controlled, and the crystallization effect of m-bromobenzoic acid is ensured.

Description

Technical Field

[0001] This utility model belongs to the technical field of crystallization equipment, and in particular relates to a crystallizing dish for the crystallization of m-bromobenzoic acid. Background Technology

[0002] Crystallizing dishes are specialized vessels used in laboratories for the crystallization and purification of substances. During the cooling crystallization process of m-bromobenzoic acid, an oily substance is prone to form. This is mainly because rapid cooling causes the solution to quickly become supersaturated, preventing the solute from uniformly nucleating and forming crystals, resulting in liquid precipitation. However, most crystallizing dishes in existing technologies use natural cooling crystallization, making it difficult to control the cooling rate.

[0003] For example, a Chinese utility model patent discloses a freeze-drying glass crystallizer [application number: 201721087510.2]. This utility model patent includes a cylindrical glass body with an opening; a glass sealing cap is provided at the opening, the sealing cap having a circular cap body corresponding to the opening, and an annular cap rim extending downward from the cap body; the circular cap body is provided with multiple vent holes. The height of the cap rim is 10 mm.

[0004] This utility model patent has the advantage of effectively avoiding the introduction of solid impurities through punctures when sealing with plastic wrap or other sealing films. However, it still uses a natural cooling crystallization method, which still has the problem of difficulty in controlling the cooling rate. Summary of the Invention

[0005] The purpose of this invention is to address the above-mentioned problems by providing a crystallizing dish for the crystallization of m-bromobenzoic acid.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: A crystallizing dish for crystallizing m-bromobenzoic acid includes a crystallizing dish body with an internal crystallization space, a cover for sealing the crystallization space on the top of the crystallizing dish body, and a heat exchange cavity for circulating heat exchange medium in the side wall of the crystallizing dish body. The upper end of the heat exchange cavity is connected to the medium outlet and the lower end is connected to the medium inlet. Both the medium outlet and the medium inlet protrude from the side wall surface of the crystallizing dish body.

[0007] In the crystallizing dish for m-bromobenzoic acid crystallization described above, a guide plate is also provided in the heat exchange cavity to guide the flow direction of the heat exchange medium. The guide plate has a spiral structure and extends along the axis of the crystallizing dish body.

[0008] In the crystallizing dish for m-bromobenzoic acid crystallization described above, the guide plate is made of metal material, and the side of the guide plate is sealed to the side wall of the heat exchange cavity.

[0009] In the crystallizing dish described above for the crystallization of m-bromobenzoic acid, a heat-insulating pad is also fixedly connected to the bottom surface of the crystallizing dish body.

[0010] In the crystallizing dish for m-bromobenzoic acid crystallization described above, the inner bottom surface of the crystallizing dish body also has a frosted area, which is located at the edge of the inner bottom surface and is connected end to end in a ring shape.

[0011] In the crystallizing dish for m-bromobenzoic acid crystallization described above, the cover includes a cover body and a boss fixedly connected to the bottom of the cover body. A handle is fixedly connected to the upper surface of the cover body, and a sealing ring is provided on the side of the boss. When the cover body is closed on the main body of the crystallizing dish, the boss extends into the crystallization space and the sealing ring abuts against the inner wall of the boss.

[0012] In the crystallizing dish for m-bromobenzoic acid crystallization described above, the boss is provided with a pressurized cavity, a pressurized airbag is disposed in the pressurized cavity, the pressurized airbag is connected to a gas inlet, the end of the gas inlet away from the pressurized airbag extends to the outside of the cover body, the inner surface of the sealing ring is in contact with the pressurized cavity, after the gas is blown into the pressurized airbag through the gas inlet, the outer wall of the pressurized airbag abuts against the inner surface of the sealing ring.

[0013] In the crystallizing dish described above for the crystallization of m-bromobenzoic acid, the pressurized airbags are connected end to end in a ring shape, and the length of the pressurized airbags in the direction of the boss axis is less than the length of the sealing ring in the direction of the boss axis.

[0014] In the crystallizing dish for m-bromobenzoic acid crystallization described above, an operating port is also provided on the cover. The operating port penetrates the cover and is connected to the crystallization space. A sealing element for closing the operating port is detachably connected to the operating port.

[0015] In the crystallizing dish for m-bromobenzoic acid crystallization described above, the sealing element includes an outer shell detachably connected to the operating port. A first sealing ring and a second sealing ring are fixedly disposed inside the outer shell. The first sealing ring is located on the outer side and has a cross-shaped slit. The second sealing ring is located on the inner side and has a through-hole. When the operating rod is inserted into the crystallization space through the operating port, the side of the operating rod is sealed to the through-hole.

[0016] Compared with existing technologies, the advantages of this utility model are: 1. This utility model has a heat exchange cavity in the side wall of the crystallizing dish body. The heat exchange medium can enter the heat exchange cavity and exchange heat with the solution in the crystallization space, thereby better controlling the cooling rate during the crystallization process and ensuring the crystallization effect of m-bromobenzoic acid.

[0017] 2. This utility model features a continuous spiral guide plate with a certain angle inside the heat exchange cavity. This forces the heat exchange medium to flow along the spiral path, spiraling upwards from the bottom to the top, avoiding dead zones caused by natural convection. This ensures that the medium at every vertical height in the heat exchange cavity is freshly flowing in with the most accurate temperature. At the same time, the spiral flow generates significant turbulence, which greatly enhances the heat exchange efficiency between the medium and the vessel wall, even at low flow velocities. It also breaks down the boundary stagnant layer, resulting in better control of the solution temperature within the crystallization space.

[0018] 3. The sealing element of this utility model adopts a two-layer sealing structure of a first sealing ring and a second sealing ring. The first sealing ring is a self-sealing silicone valve with a cross slit, and the second sealing ring is a sealing valve with a sealing port. When the operating rod is not inserted, the first sealing ring plays a sealing role. After the operating rod is inserted, the operating rod and the second sealing ring cooperate to play a sealing role, so that the external operating rod can enter the crystallizing dish body through this channel to rub and promote crystallization, while preventing dust from entering. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the structure of this utility model; Figure 2 This is a cross-sectional view of the present invention; Figure 3 This is an exploded view of this utility model; Figure 4 This is a top view of the main body of the crystallizing dish; Figure 5 This is a structural schematic diagram of the sealing element; In the diagram: 1. Crystallization space; 2. Crystallization dish body; 3. Cover; 4. Heat exchange cavity; 5. Medium outlet; 6. Medium inlet; 7. Guide plate; 8. Insulation pad; 9. Operating port; 10. Seal; 11. Outer shell; 12. First sealing ring; 13. Second sealing ring; 14. Cross-shaped slit; 15. Sealing port; 16. Frosted area; 31. Cover body; 32. Boss; 33. Handle; 34. Sealing ring; 35. Pressurized cavity; 36. Pressurized airbag; 37. Gas outlet. Detailed Implementation

[0020] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0021] Combination Figure 1 and Figure 2As shown, a crystallizing dish for crystallizing m-bromobenzoic acid includes a crystallizing dish body 2 with an internal crystallization space 1. A cover 3 for sealing the crystallization space 1 is provided on the upper part of the crystallizing dish body 2. A heat exchange cavity 4 for circulating heat exchange medium is also provided in the side wall of the crystallizing dish body 2. The upper end of the heat exchange cavity 4 is connected to the medium outlet 5 and the lower end is connected to the medium inlet 6. Both the medium outlet 5 and the medium inlet 6 protrude from the side wall surface of the crystallizing dish body 2.

[0022] In this invention, during use, the heat exchange medium flows into the heat exchange cavity 4 through the medium inlet 6 and then flows out from the medium outlet 5. Therefore, this invention provides a heat exchange cavity 4 in the side wall of the crystallizing dish body 2. The heat exchange medium can enter the heat exchange cavity 4 and exchange heat with the solution in the crystallization space 1, thereby better controlling the cooling rate during the crystallization process and ensuring the crystallization effect of m-bromobenzoic acid.

[0023] Preferably, the heat exchange cavity 4 is further provided with a guide plate 7 to guide the flow direction of the heat exchange medium. The guide plate 7 has a spiral structure and extends along the axis of the crystallizer body 2. The guide plate 7 is made of metal material, and the side of the guide plate 7 is sealed to the side wall of the heat exchange cavity 4.

[0024] The guide plate 7 is a continuous spiral structure with a certain inclination angle located inside the heat exchange cavity 4. In this way, the heat exchange medium is forced to flow along the spiral path, spiraling up from the bottom to the top, avoiding dead zones caused by natural convection. This ensures that the medium at each vertical height in the heat exchange cavity 4 is the freshly flowing medium with the most accurate temperature. At the same time, the spiral flow generates significant turbulence, which greatly enhances the heat exchange efficiency between the medium and the container wall, even if the flow velocity is not high. It also breaks the boundary stagnant layer and achieves better control of the solution temperature in the crystallization space.

[0025] like Figure 2 As shown, a heat insulation layer 8 is also fixedly connected to the bottom surface of the crystallizing dish body 2. The heat insulation layer 8 can prevent excessive heat from escaping from the bottom of the crystallizing dish body 2, which would cause uneven temperature distribution of the solution in the crystallization space 1.

[0026] like Figure 4 As shown, the inner bottom surface of the crystallizing dish body 2 also has a frosted region 16, which is located at the edge of the inner bottom surface and is connected end to end in a ring shape. The frosted region 16 is a slightly rough frosted surface, which can provide preferential nucleation sites for crystals, guiding the nucleation process from the random interior of the solution to a controllable specific region, so as to facilitate subsequent crystal growth without interference.

[0027] Combination Figure 2 and Figure 3As shown, the cover 3 includes a cover body 31 and a protrusion 32 fixedly connected to the lower part of the cover body 31. A handle 33 is fixedly connected to the upper surface of the cover body 31. A sealing ring 34 is provided on the side of the protrusion 32. When the cover body 31 is closed on top of the crystallizing dish body 2, the protrusion 32 extends into the crystallization space 1 and the sealing ring 34 abuts against the inner wall of the protrusion 32. The sealing ring 34 is used to achieve a seal between the protrusion 32 and the crystallizing dish body 2.

[0028] like Figure 2 As shown, the boss 32 is provided with a pressurized cavity 35, and a pressurized airbag 36 is disposed in the pressurized cavity 35. The pressurized airbag 36 is connected to an air inlet 37. The end of the air inlet 37 away from the pressurized airbag 36 extends to the outside of the cover body 31. The inner surface of the sealing ring 34 is in contact with the pressurized cavity 35. After the gas is blown into the pressurized airbag 36 through the air inlet 37, the outer wall of the pressurized airbag 36 abuts against the inner surface of the sealing ring 34.

[0029] Preferably, the pressurized airbag 36 is connected end to end in a ring shape, and the length of the pressurized airbag 36 in the direction of the axis of the boss 32 is less than the length of the sealing ring 34 in the direction of the axis of the boss 32.

[0030] During use, gas can be pumped into the pressurized airbag 36 through the gas inlet 37, causing the pressurized airbag 36 to expand and compress the sealing ring 34, thereby improving the sealing effect. When it is necessary to separate the cover 3 from the crystallizer body 2, the gas in the pressurized airbag 36 can be discharged through the gas inlet 37 to reduce the pressure between the sealing ring 34 and the inner wall of the crystallizer body 2, facilitating separation.

[0031] Combination Figure 3 and Figure 5 As shown, the cover 3 also has an operation port 9, which penetrates the cover 3 and communicates with the crystallization space 1. A sealing element 10 for closing the operation port 9 is detachably connected to the operation port 9. An operation rod, such as a glass rod, can be inserted into the crystallization space 1 through the operation port 9 and promote crystallization by rubbing the bottom surface or side wall of the crystallization dish body 2.

[0032] Specifically, the sealing element 10 includes a housing 11 detachably connected to the operating port 9. A first sealing ring 12 and a second sealing ring 13 are fixedly disposed within the housing 11. The first sealing ring 12 is located on the outer side and has a cross-shaped slit 14. The second sealing ring 13 is located on the inner side and has a through-hole 15. When the operating rod is inserted into the crystallization space 1 through the operating port 9, the side of the operating rod is sealed to the through-hole 15. The sealing element 10 of this invention employs a two-layer sealing structure with a first sealing ring 12 and a second sealing ring 13. The first sealing ring 12 is a self-sealing silicone valve with a cross-shaped slit, and the second sealing ring 13 is a sealing valve with a through-hole 15. When the operating rod is not inserted, the first sealing ring 12 provides a sealing effect. After the operating rod is inserted, the operating rod and the second sealing ring 13 cooperate to provide a sealing effect, facilitating the entry of an external operating rod into the crystallizing dish body 2 through this channel to promote crystallization through friction, while simultaneously preventing dust from entering.

[0033] The specific embodiments described herein are merely illustrative examples illustrating the spirit of this utility model. Those skilled in the art to which this utility model pertains may make various modifications or additions to the described specific embodiments or use similar methods to substitute them, without departing from the spirit of this utility model or exceeding the scope defined by the appended claims.

[0034] Although this document frequently uses terms such as crystallization space 1, crystallizing dish body 2, cover 3, heat exchange cavity 4, medium outlet 5, medium inlet 6, guide plate 7, heat insulation pad 8, operating port 9, sealing element 10, outer shell 11, first sealing ring 12, second sealing ring 13, cross-shaped slit 14, sealing port 15, frosted area 16, cover body 31, boss 32, handle 33, sealing ring 34, pressurizing cavity 35, pressurizing airbag 36, and air outlet 37, the possibility of using other terms is not excluded. The use of these terms is merely for the convenience of describing and explaining the essence of this utility model; interpreting them as any additional limitation would contradict the spirit of this utility model.

Claims

1. A crystallizing dish for crystallizing m-bromobenzoic acid, comprising a crystallizing dish body (2) having an internal crystallization space (1), wherein a cover (3) for sealing the crystallization space (1) is provided above the crystallizing dish body (2), characterized in that: The crystallizer body (2) is also provided with a heat exchange cavity (4) for the flow of heat exchange medium in the side wall. The upper end of the heat exchange cavity (4) is connected to the medium outlet (5) and the lower end is connected to the medium inlet (6). The medium outlet (5) and the medium inlet (6) both protrude from the side wall surface of the crystallizer body (2).

2. The crystallizing dish for m-bromobenzoic acid crystallization as described in claim 1, characterized in that: The heat exchange cavity (4) is also provided with a guide plate (7) to guide the flow direction of the heat exchange medium. The guide plate (7) has a spiral structure and extends along the axis of the crystallizer body (2).

3. The crystallizing dish for m-bromobenzoic acid crystallization as described in claim 2, characterized in that: The guide plate (7) is made of metal material, and the side of the guide plate (7) is sealed to the side wall of the heat exchange cavity (4).

4. The crystallizing dish for m-bromobenzoic acid crystallization as described in claim 1, characterized in that: A heat insulation pad (8) is also fixedly connected to the bottom surface of the crystallizing dish body (2).

5. A crystallizing dish for the crystallization of m-bromobenzoic acid as described in claim 1, characterized in that: The inner bottom surface of the crystallizing dish body (2) also has a frosted area (16), which is located at the edge of the inner bottom surface and is connected end to end in a ring shape.

6. A crystallizing dish for the crystallization of m-bromobenzoic acid as described in claim 1, characterized in that: The cover (3) includes a cover body (31) and a boss (32) fixedly connected to the bottom of the cover body (31). A handle (33) is fixedly connected to the upper surface of the cover body (31). A sealing ring (34) is provided on the side of the boss (32). When the cover body (31) is closed on the crystallizing dish body (2), the boss (32) extends into the crystallization space (1) and the sealing ring (34) abuts against the inner wall of the boss (32).

7. A crystallizing dish for the crystallization of m-bromobenzoic acid as described in claim 6, characterized in that: The boss (32) is provided with a pressurized cavity (35), and a pressurized airbag (36) is disposed in the pressurized cavity (35). The pressurized airbag (36) is connected to an air inlet (37). The end of the air inlet (37) away from the pressurized airbag (36) extends to the outside of the cover body (31). The inner surface of the sealing ring (34) is in contact with the pressurized cavity (35). After the gas is blown into the pressurized airbag (36) through the air inlet (37), the outer wall of the pressurized airbag (36) abuts against the inner surface of the sealing ring (34).

8. A crystallizing dish for the crystallization of m-bromobenzoic acid as described in claim 7, characterized in that: The pressurized airbag (36) is connected end to end in a ring shape, and the length of the pressurized airbag (36) in the direction of the axis of the boss (32) is less than the length of the sealing ring (34) in the direction of the axis of the boss (32).

9. A crystallizing dish for the crystallization of m-bromobenzoic acid as described in claim 1, characterized in that: An operation port (9) is also provided on the cover (3). The operation port (9) penetrates the cover (3) and is connected to the crystallization space (1). A sealing element (10) for closing the operation port (9) is detachably connected to the operation port (9).

10. A crystallizing dish for the crystallization of m-bromobenzoic acid as described in claim 9, characterized in that: The sealing element (10) includes an outer shell (11) detachably connected to the operating port (9). A first sealing ring (12) and a second sealing ring (13) are fixedly disposed inside the outer shell (11). The first sealing ring (12) is located on the outside and has a cross-shaped slit (14). The second sealing ring (13) is located on the inside and has a through sealing port (15). When the operating rod is inserted into the crystallization space (1) through the operating port (9), the side of the operating rod is sealed to the sealing port (15).

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