Crystallizer

Abstract

The crystallizer comprises a vertical container, the vertical container is installed on a fixing support through an elastic mechanism, and a vibration unit is further installed on the vertical container; a jacket matched with the vertical container in shape is arranged outside the vertical container, a refrigerant cavity is formed between the jacket and the vertical container, and the jacket is further provided with a refrigerant inlet and a refrigerant outlet which are communicated with the refrigerant cavity; the vertical container is provided with a mother liquor feed port, a nitrogen inlet, a mother liquor outlet and a discharge port; the discharge port is positioned at the bottom of the vertical container and is used for discharging crystallized materials, and meanwhile, a discharge valve for controlling the discharge port to be opened and closed is also arranged at the discharge port; the nitrogen inlet and the mother liquor outlet are positioned at the top of the vertical container, and a mother liquor insertion pipe downwards extending into the vertical container is also arranged at the mother liquor outlet. The device is simple in structure, easy to operate and capable of prohibiting external air from making contact with materials, controlling the amount of insoluble substances of lithium hexafluorophosphate and ensuring the stability of the quality of lithium hexafluorophosphate.

Description

Technical Field

[0001] This invention relates to the field of fluorochemical production technology, specifically to a crystallizer. Background Technology

[0002] Lithium hexafluorophosphate (LiPF6) is a core material for new energy batteries, and producing high-quality LiPF6 is particularly important. In the current mainstream production process, the core equipment for producing LiPF6 is the crystallizer. The saturated mother liquor from synthesis enters the crystallizer to complete the crystal precipitation.

[0003] Throughout the entire process of lithium hexafluorophosphate (LiPF6) crystallization, air must not come into contact with the material. If the material comes into contact with air, it will rapidly decompose, increasing the amount of insoluble lithium hexafluorophosphate. This indicator is a crucial standard for determining the quality of lithium hexafluorophosphate products. However, existing crystallizers struggle to meet this requirement. Therefore, this application proposes a new crystallizer that ensures the material does not come into contact with air throughout the entire crystallization process, and that the insoluble content of the material is controlled within national standards, thus ensuring the stability of lithium hexafluorophosphate quality. Summary of the Invention

[0004] The purpose of this invention is to provide a crystallizer that at least partially solves one of the technical problems in the related art.

[0005] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: A crystallizer includes a vertical container, which is mounted on a fixed support via an elastic mechanism; a vibration unit is also installed on the vertical container, which drives the vertical container to vibrate. The vertical container is equipped with a jacket that fits its shape. A refrigerant cavity is formed between the jacket and the vertical container. The jacket is also equipped with a refrigerant inlet and a refrigerant outlet that communicate with the refrigerant cavity. The vertical container is equipped with a mother liquor inlet, a nitrogen inlet, a mother liquor outlet, and a discharge outlet. The discharge outlet is located at the bottom of the vertical container and is used to discharge the crystallized material. A discharge valve is also provided at the discharge outlet to control the opening and closing of the discharge outlet. The nitrogen inlet and the mother liquor outlet are located at the top of the vertical container. A mother liquor insertion pipe extending downward into the vertical container is also provided at the mother liquor outlet.

[0006] Preferably, control valves are provided at the refrigerant inlet, refrigerant outlet, mother liquor inlet, nitrogen inlet, and mother liquor outlet, respectively.

[0007] Preferably, the vertical container is mainly composed of an upper end cap, a cylindrical body, and a lower end cap. A cylindrical body jacket and a lower end cap jacket are respectively provided outside the cylindrical body and the lower end cap. A cylindrical body refrigerant cavity is formed between the cylindrical body jacket and the cylindrical body, and a lower end cap refrigerant cavity is formed between the lower end cap jacket and the lower end cap. The cylindrical body refrigerant cavity and the lower end cap refrigerant cavity are connected.

[0008] Preferably, the mother liquor inlet, nitrogen inlet, and mother liquor outlet are located at the upper end cap.

[0009] Preferably, the cylinder is also provided with a temperature measuring port, and the upper end cap is provided with a pressure measuring port.

[0010] Preferably, the discharge port is located at the lower end cap and is connected to the interior of the lower end cap.

[0011] Preferably, the discharge valve is a downward discharge valve.

[0012] Preferably, the outer periphery of the cylindrical jacket is provided with multiple fixed lugs, and each fixed lug is connected to the fixed bracket by an elastic mechanism.

[0013] Preferably, the elastic mechanism is a spring.

[0014] Preferably, the vibration unit is a vibration motor installed at the bottom of the lower end cap sleeve.

[0015] The beneficial effects of this invention are: This invention has a simple structure and is easy to operate. It can prevent the contact between the outside air and the material, laying a solid foundation for the production of high-purity lithium hexafluorophosphate.

[0016] The crystallization process of this invention involves the synthesis of a saturated mother liquor, which is then introduced into a vertical container. Upon cooling, crystals precipitate out, with the clear liquid at the top and the crystalline material settling at the bottom, creating a clear boundary for easy separation. The liquid-solid separation process involves filling the container with nitrogen to force the clear liquid out. The material inside the vertical container is predominantly crystalline. A vibration unit is then activated to break down large crystals into smaller particles, which are discharged through the discharge port. Throughout this process, the material does not come into contact with air, thus controlling the amount of insoluble matter in lithium hexafluorophosphate and ensuring stable quality. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the structure of the present invention.

[0018] The accompanying drawings are for illustrative purposes only and should not be construed as limiting the scope of this patent. To better illustrate this embodiment, some components in the drawings may be omitted, enlarged, or reduced, and do not represent the actual dimensions of the product. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings. Detailed Implementation

[0019] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.

[0020] like Figure 1As shown, this embodiment provides a crystallizer, including a vertical container. The vertical container mainly consists of an upper end cap 1, a cylindrical body 2, and a lower end cap 3. The cylindrical body 2 is provided with a cylindrical body jacket 21 adapted to its shape, and a cylindrical body refrigerant cavity 20 is formed between the cylindrical body jacket 21 and the cylindrical body. The lower end cap 3 is provided with a lower end cap jacket 31 adapted to its shape, and a lower end cap refrigerant cavity 30 is formed between the lower end cap jacket 31 and the lower end cap 3. The cylindrical body refrigerant cavity 20 and the lower end cap refrigerant cavity 30 are connected.

[0021] The cylindrical jacket 21 is equipped with a refrigerant inlet 15 and a refrigerant outlet 17, which communicate with the refrigerant chamber 20 of the cylindrical body. Valves are installed at the refrigerant inlet 15 and the refrigerant outlet 17, respectively. The refrigerant enters the refrigerant chamber 20 of the cylindrical body and the refrigerant chamber 30 of the lower end cap through the refrigerant inlet 15 and is discharged from the refrigerant outlet 17. In this process, the refrigerant plays a role in cooling the material inside the container.

[0022] The cylinder 2 has a temperature measuring port 18 to monitor the temperature of the material inside the container in real time.

[0023] Four fixed lugs 22 are arranged around the outer periphery of the cylindrical sleeve 21, and the four fixed lugs 22 are connected to the corresponding fixed supports 24 by springs 23. A vibration motor 32 is installed on the bottom of the lower end sleeve 31, and the vibration of the vibration motor 32 causes the entire vertical container to vibrate through the four springs 23.

[0024] The upper end cap 1 is provided with a mother liquor inlet 11, a nitrogen inlet 12, a pressure measuring port 13, and a mother liquor outlet 14. Valves are provided at the mother liquor inlet 11, the nitrogen inlet 12, and the mother liquor outlet 14. The mother liquor outlet 14 is also provided with a mother liquor insertion tube 141 that extends downward into the vertical container, reaching a certain depth into the liquid part of the container.

[0025] A manhole 19 is also provided at the top end cap for easy maintenance.

[0026] The lower end cap 3 is connected to a lower expansion valve 33, which has a discharge port 16 located at the bottom of the vertical container for discharging crystalline materials.

[0027] Except for the manhole, all other openings on the vertical container need to be connected to the pipeline with flexible connectors. The crystallizer of the present invention is composed of the above components to complete the entire crystallization process. It has a simple structure and is easy to operate.

[0028] The specific working principle is as follows: The saturated lithium hexafluorophosphate mother liquor synthesized in the previous section is fed into a vertical container through the mother liquor inlet 11. Once the liquid in the vertical container reaches 80% of the container volume, the valve of the mother liquor inlet 11 is closed to stop feeding mother liquor into the container.

[0029] Then, refrigerant is introduced from refrigerant inlet 15 into refrigerant chamber 20 of cylinder and refrigerant chamber 30 of lower head. The refrigerant cools down the saturated solution in the container. After cooling down to the specified temperature, the solution in the container is transformed into an unsaturated solution through cooling, and many crystals will precipitate. The clear liquid is in the upper part of the container, and the precipitated crystals are in the lower part of the container.

[0030] Then, nitrogen gas is introduced into the container through nitrogen inlet 12, and positive pressure is generated inside the container to force the clear liquid out of the container through mother liquid insertion pipe 141 and mother liquid outlet 14. Most of the contents of the container are crystalline materials. The valve of refrigerant inlet 15 is closed to stop the refrigerant supply.

[0031] When the vibrating motor 32 is turned on, the container begins to vibrate. After a period of vibration, the large clumps of crystallized material inside the container are broken down into smaller crystals through vibration and collision. The lower discharge valve 33 is then opened, and the material is discharged from the outlet 16 to the next stage. Once the material inside the container has been completely discharged, the vibrating motor 32 stops vibrating, and the lower discharge valve 33 is closed, completing a full crystallization operation.

[0032] Then, the above operations are repeated. The saturated mother liquor synthesized again enters the container for crystallization, drainage, vibration, crushing, and discharge. Throughout the entire crystallization process, the container and all connecting pipes are not opened, and the outside air has no chance to come into contact with the material, thereby controlling the amount of insoluble matter in lithium hexafluorophosphate and ensuring the stability of lithium hexafluorophosphate quality.

[0033] The above embodiments are only used to illustrate and not limit the technical solutions of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the present invention without departing from the spirit and scope of the present invention. Any modifications or partial substitutions should be covered within the scope of the claims of the present invention.

[0034] If the terms "first" or "second" are used in this document to define components, those skilled in the art should know that the use of "first" or "second" is merely for the convenience of describing the invention and simplifying the description, and unless otherwise stated, the above terms have no special meaning.

[0035] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0036] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; 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; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

Claims

1. A crystallizer, characterized in that: It includes a vertical container, which is mounted on a fixed support via an elastic mechanism; the vertical container is also equipped with a vibration unit, which drives the vertical container to vibrate. The vertical container is equipped with a jacket that fits its shape. A refrigerant cavity is formed between the jacket and the vertical container. The jacket is also equipped with a refrigerant inlet and a refrigerant outlet that communicate with the refrigerant cavity. The vertical container is equipped with a mother liquor inlet, a nitrogen inlet, a mother liquor outlet, and a discharge outlet. The discharge outlet is located at the bottom of the vertical container and is used to discharge the crystallized material. A discharge valve is also provided at the discharge outlet to control the opening and closing of the discharge outlet. The nitrogen inlet and the mother liquor outlet are located at the top of the vertical container. A mother liquor insertion pipe extending downward into the vertical container is also provided at the mother liquor outlet.

2. The crystallizer according to claim 1, characterized in that: Control valves are respectively installed at the refrigerant inlet, refrigerant outlet, mother liquor inlet, nitrogen inlet, and mother liquor outlet.

3. The crystallizer according to claim 1 or 2, characterized in that: The vertical container is mainly composed of an upper end cap, a cylindrical body, and a lower end cap. The cylindrical body and the lower end cap are respectively provided with a cylindrical body jacket and a lower end cap jacket. A cylindrical body refrigerant cavity is formed between the cylindrical body jacket and the cylindrical body, and a lower end cap refrigerant cavity is formed between the lower end cap jacket and the lower end cap. The cylindrical body refrigerant cavity and the lower end cap refrigerant cavity are connected.

4. The crystallizer according to claim 3, characterized in that: The mother liquor inlet, nitrogen inlet, and mother liquor outlet are located at the upper end cap.

5. The crystallizer according to claim 3, characterized in that: The cylinder is also equipped with a temperature measuring port, and the upper end cap is equipped with a pressure measuring port.

6. The crystallizer according to claim 3, characterized in that: The discharge port is located at the lower end cap and is connected to the interior of the lower end cap.

7. The crystallizer according to claim 3, characterized in that: The discharge valve is a bottom-discharge valve.

8. The crystallizer according to claim 3, characterized in that: The outer periphery of the cylindrical jacket is provided with multiple fixed lugs, and each fixed lug is connected to the fixed bracket by an elastic mechanism.

9. The crystallizer according to claim 8, characterized in that: The elastic mechanism is a spring.

10. The crystallizer according to claim 8, characterized in that: The vibration unit is a vibration motor installed at the bottom of the lower end cap sleeve.

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