High-purity yellow phosphorus crystallization purification device

Abstract

This utility model relates to the technical field of high-purity material purification equipment, specifically a high-purity yellow phosphorus crystallization and purification device. It includes six crystallization tanks, each containing a seed crystallizing rod. The crystallization tanks are supplied with water via a cooling circulating water pipe, and the seed crystallizing rods are raised and lowered via a lifting and moving unit. Each crystallization tank is externally fitted with a jacket for heating. Each seed crystallizing rod is connected to a cooling circulating water pipe, the outer end of which is connected to a water tank. In this high-purity yellow phosphorus crystallization and purification device, the synergistic effect of the six crystallization tanks and seed crystallizing rods, combined with precise temperature control via the cooling circulating water pipe, significantly improves the crystallization efficiency and purity of yellow phosphorus. This device can increase the purity of yellow phosphorus to meet the production requirements of electronic-grade high-purity phosphorus. This device achieves crystallization and purification through a single piece of equipment, reducing equipment investment and operational steps, and greatly improving production efficiency.

Description

Technical Field

[0001] This utility model relates to the technical field of high-purity material purification equipment, specifically to a high-purity yellow phosphorus crystallization and purification device. Background Technology

[0002] In the field of high-purity material purification equipment technology, high-purity yellow phosphorus is a key basic material for the preparation of group III-V compound semiconductors, high-purity alloys, and germanium and silicon single crystal dopants. Its purity directly determines the performance and quality of downstream products. With the rapid development of the semiconductor industry, especially the surge in demand for materials such as gallium phosphide and indium phosphide, the purity requirement for high-purity yellow phosphorus has increased to over 99.999%, and even reaches 99.99999%, posing a severe challenge to traditional yellow phosphorus purification technology.

[0003] Chinese Patent Application No. 201310573001.0 discloses a yellow phosphorus purification device and method. This technology employs a multi-step process of distillation, crystallization, zone melting, and filtration to purify yellow phosphorus. Specifically, the process involves first adding a yellow phosphorus solution to a crystallizer, then adding industrial yellow phosphorus crystals and washing the crystals; after fully replacing the air in the oxidation tank, adding the oxidant, catalyst, and yellow phosphorus separately to the oxidation tank and reacting for 1-3 hours, allowing the mixture to settle and separate into layers, and then washing the yellow phosphorus; subsequently, the yellow phosphorus is sent to a zone melting device, where it is melted in zones and transferred to both ends of the zone melting pool, entering a high-purity yellow phosphorus tank and a low-arsenic yellow phosphorus tank respectively; finally, the yellow phosphorus from the high-purity yellow phosphorus tank passes through a phosphorus pressing tank and a filter before entering the final product storage system. While this method can improve phosphorus purity to some extent, it still has significant drawbacks. On the one hand, the multi-step process is complex, involving the combined use of various equipment and reagents, which not only significantly increases equipment investment and production operation difficulty, but also prolongs the production cycle and reduces production efficiency. On the other hand, in the oxidation, zone melting and other stages, it is difficult to accurately control the reaction conditions and impurity separation effect, which may lead to problems such as oxidant residue and yellow phosphorus oxidation loss, affecting the quality and final purity of yellow phosphorus, making it difficult to meet the stringent requirements of stability and efficiency for the production of electronic-grade high-purity phosphorus. Utility Model Content

[0004] The purpose of this invention is to provide a high-purity yellow phosphorus crystallization and purification device to solve the problems mentioned in the background art, such as complex multi-step process operation, the need for the combined use of various equipment and reagents, which not only significantly increases equipment investment and production operation difficulty, but also prolongs the production cycle and reduces production efficiency.

[0005] To achieve the above objectives, this utility model provides a high-purity yellow phosphorus crystallization purification device, comprising six crystallization tanks, each containing a seed crystallizing rod. The crystallization tanks are supplied with water through a set of cooling circulating water pipes, and the seed crystallizing rods are raised and lowered by a set of lifting and moving units. Each set of crystallization tanks is equipped with an external jacket for heating. Each set of seed crystallizing rods is connected to a cooling circulating water pipe, and the outer end of the cooling circulating water pipe is connected to a water tank.

[0006] This setup utilizes six parallel crystallization tanks, employing seed crystallizing rods to provide the crystallization nuclei. Temperature is controlled by cooling circulating water pipes, and the jacket regulates ambient heat, creating a controlled crystallization environment. A lifting and moving unit adjusts the position of the seed crystallizing rods, optimizing the crystallization process. The synchronized operation of the six crystallization tanks significantly improves processing efficiency; the synergistic effect of the cooling and heating systems enhances the purity of the yellow phosphorus crystals, meeting electronic-grade requirements.

[0007] Preferably, each set of crystallization tanks is equipped with a jacket for heating, and the jacket is heated by heat-conducting oil and explosion-proof and corrosion-resistant heating rods.

[0008] This design uses heat-conducting oil within the jacket as the heat transfer medium, in conjunction with explosion-proof and corrosion-resistant heating rods, to achieve uniform and stable heating. It offers high temperature control precision, preventing localized overheating that could lead to impurity buildup, extending equipment lifespan, and reducing maintenance costs.

[0009] Preferably, the crystallization tank is equipped with a temperature measuring point.

[0010] This setting allows for real-time monitoring of the temperature inside the crystallization tank via temperature measurement points, which then feeds back to the control system to adjust the heating power.

[0011] Preferably, each set of crystallization tanks is provided with a water inlet for water intake and replenishment.

[0012] This feature allows for the replenishment of process water at the inlet, maintaining a stable liquid level and preventing yellow phosphorus from coming into contact with air.

[0013] Preferably, the crystallization barrel is provided with an argon gas inlet for gas intake and replenishment.

[0014] This feature involves injecting inert gas through an argon inlet to replace the air inside the container, creating an oxygen-free environment.

[0015] Preferably, the lifting and moving unit includes a housing, inside which a lead screw is vertically installed, and a lead screw slider is installed on the lead screw. The top of the lead screw is driven to rotate by a drive motor. A strip-shaped opening is provided on one side of the housing, and one side of the lead screw slider slides vertically with the strip-shaped opening. The outer side of the lead screw slider is connected to the outer wall of the cooling circulating water pipe.

[0016] This setting involves a lead screw and a drive motor that drive the lead screw slider to precisely raise and lower the seed crystal crystallization rod.

[0017] Preferably, the seed crystal crystallizing rod is a hollow tubular structure, the top end of the seed crystal crystallizing rod is connected to the cooling circulating water pipe through a flange joint, and a limit baffle is installed at the lower end of the seed crystal crystallizing rod.

[0018] In this design, the hollow tubular seed crystallizing rod enables internal circulation of the coolant, the flange joint ensures a seal, and the limit baffle controls the immersion depth.

[0019] Preferably, the water tank is equipped with a circulation pump, and the cooling circulation water pipe includes an outlet pipe and a return pipe. The outlet pipe and the return pipe of the cooling circulation water pipe are connected to the outlet end and the inlet end of the circulation pump to realize water circulation.

[0020] This setup creates a closed-loop water system with the water tank and circulation pump, allowing for the recycling of coolant through outlet and return pipes.

[0021] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0022] This high-purity yellow phosphorus crystallization and purification device significantly improves the crystallization efficiency and purity of yellow phosphorus through the synergistic effect of six crystallization tanks and seed crystallization rods, combined with precise temperature control via cooling circulating water pipes. This device can enhance the purity of yellow phosphorus to meet the production requirements of electronic-grade high-purity phosphorus.

[0023] This device achieves crystallization and purification through a single unit, reducing equipment investment and operational steps, and significantly improving production efficiency. The jacket uses heat-conducting oil and explosion-proof, corrosion-resistant heating rods for heating, combined with real-time temperature monitoring to ensure the stability of the crystallization process, reduce impurity encapsulation, and improve product consistency. The unique lifting and moving unit, through the cooperation of a lead screw and drive motor, achieves precise lifting and lowering of the seed crystal crystallization rod with minimal positioning error, facilitating crystal collection and equipment maintenance. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0025] Figure 2 This is a schematic diagram of the seed crystallization rod in this utility model;

[0026] Figure 3 This is a schematic diagram of the lifting and moving unit in this utility model;

[0027] The meanings of the labels in the diagram are as follows:

[0028] 1. Crystallization tank; 2. Temperature measuring point; 3. Jacket; 4. Water inlet; 5. Air inlet; 6. Seed crystal crystallization rod; 61. Flange joint; 62. Limiting baffle; 7. Water tank; 8. Lifting and moving unit; 81. Outer shell; 82. Lead screw; 821. Strip-shaped opening; 83. Lead screw slider; 84. Drive motor; 9. Cooling circulating water pipe. Detailed Implementation

[0029] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0030] This invention provides a high-purity yellow phosphorus crystallization and purification device, such as... Figure 1 As shown, it includes six sets of crystallization tanks 1. Each crystallization tank 1 is equipped with a seed crystallization rod 6. The crystallization tank 1 is supplied with water through a set of cooling circulating water pipes 9. The seed crystallization rod 6 is raised and lowered through a set of lifting and moving units 8. Each set of crystallization tanks 1 is equipped with a jacket 3 for heating. Each set of seed crystallization rods 6 is connected to the cooling circulating water pipes 9, and the outer end of the cooling circulating water pipes 9 is connected to a water tank 7.

[0031] Six sets of crystallization tanks 1 are set up in parallel, using seed crystallization rods 6 to provide crystallization nuclei. Cooling circulating water pipes 9 deliver low-temperature media to control the temperature, and jackets 3 regulate ambient heat, forming a controllable crystallization environment. Lifting and moving units 8 adjust the position of seed crystallization rods 6 to optimize the crystallization process. The six sets of crystallization tanks 1 operate synchronously, improving processing efficiency; the cooling and heating systems work together to improve the purity of yellow phosphorus crystals, meeting electronic grade requirements.

[0032] In this embodiment, as Figure 1 As shown, each set of crystallization tanks 1 is equipped with a jacket 3 for heating, and the jacket 3 is heated by heat transfer oil and explosion-proof and corrosion-resistant heating rods.

[0033] The heat transfer oil inside jacket 3 serves as the heat transfer medium, working in conjunction with explosion-proof and corrosion-resistant heating rods to achieve uniform and stable heating. Improved temperature control precision prevents impurities from accumulating due to localized overheating, extending equipment lifespan and reducing maintenance costs.

[0034] Specifically, such as Figure 1 As shown, temperature measuring point 2 is set on crystallization tank 1.

[0035] Temperature monitoring point 2 monitors the temperature inside crystallization tank 1 in real time and feeds back to the control system to adjust the heating power. This ensures that the crystallization process takes place within the set temperature range, resulting in minimal fluctuations in product purity and improved batch consistency.

[0036] Furthermore, such as Figure 1 As shown, each set of crystallization tanks 1 is equipped with a water inlet 4 for water intake and replenishment into the crystallization tank.

[0037] Inlet 4 replenishes process water to maintain a stable liquid level and prevent yellow phosphorus from contacting air. This forms a water seal, reducing the risk of spontaneous combustion, and simultaneously removes heat through water circulation, optimizing crystallization conditions.

[0038] Furthermore, such as Figure 1 As shown, the crystallization tank 1 is equipped with an argon gas inlet 5, which is used for gas intake and replenishment in the crystallization tank.

[0039] Inert gas is injected through argon inlet 5 to replace the air inside the container, creating an oxygen-free environment. This further eliminates the risk of oxidation, and the low levels of impurities such as O2 and H2O improve product stability.

[0040] Furthermore, such as Figure 3 As shown, the lifting and moving unit 8 includes a housing 81. A lead screw 82 is vertically installed inside the housing 81. A lead screw slider 83 is installed on the lead screw 82. The top of the lead screw 82 is driven to rotate by a drive motor 84. A strip-shaped opening 821 is provided on one side of the housing 81. One side of the lead screw slider 83 is vertically slidably engaged with the strip-shaped opening 821. The outer side of the lead screw slider 83 is connected to the outer wall of the cooling circulating water pipe 9.

[0041] The lead screw 82 and drive motor 84 drive the lead screw slider 83, which in turn drives the seed crystal crystallization rod 6 to rise and fall precisely. This provides high positioning accuracy, facilitates crystal collection and equipment cleaning, reduces manual intervention, and increases automation.

[0042] Furthermore, such as Figure 2 As shown, the seed crystal crystallizing rod 6 is a hollow tubular structure. The top end of the seed crystal crystallizing rod 6 is connected to the cooling circulating water pipe 9 through a flange joint 61, and a limit baffle 62 is installed at the lower end of the seed crystal crystallizing rod 6.

[0043] The hollow tubular seed crystallizing rod 6 enables internal circulation of the coolant, the flange joint 61 ensures a seal, and the limiting baffle 62 controls the immersion depth. This improves heat exchange efficiency, reduces the risk of coolant leakage to zero, allows for controllable crystallization initiation, and results in more uniform crystal morphology.

[0044] Furthermore, such as Figure 2 As shown, a circulation pump is installed inside the water tank 7. The cooling circulation water pipe 9 includes an outlet pipe and a return pipe. The outlet pipe and return pipe of the cooling circulation water pipe 9 are connected to the outlet end and the inlet end of the circulation pump to realize water circulation.

[0045] Water tank 7 and the circulating pump form a closed-loop water system, enabling coolant recycling through outlet and return pipes. This saves water and electricity, reducing operating costs; constant temperature control makes the crystallization process more stable, reducing product quality fluctuations.

[0046] In operation, the high-purity yellow phosphorus crystallization purification device of this invention first injects process water into the crystallization tank 1 through the water inlet 4 to the set liquid level, forming a water seal to prevent yellow phosphorus oxidation. High-purity argon gas (≥99.999%) is introduced through the argon gas inlet 5 to replace the air in the tank, reducing the oxygen content to below 0.1 ppm. The circulation pump in the water tank 7 is then started, and coolant flows into the seed crystallization rod 6 through the cooling circulation water pipe 9, cooling it to 50-55℃ (yellow phosphorus melting point is approximately 44℃). The explosion-proof and corrosion-resistant heating rod in the jacket 3 is activated, and the heat transfer oil heats the crystallization tank 1 to 60-65℃, keeping the yellow phosphorus raw material in a molten state.

[0047] Molten yellow phosphorus with a purity of approximately 99.8% is injected into crystallization tank 1 through the feed inlet, with the liquid level controlled below the limit baffle 62. Drive motor 84 starts, and lead screw 82 lowers lead screw slider 83, immersing the seed crystal crystallizing rod 6 into the molten yellow phosphorus. The coolant temperature gradually decreases to 40-42℃, and the yellow phosphorus begins to crystallize on the surface of the seed crystal crystallizing rod 6, forming a high-purity crystal layer. Temperature measurement point 2 provides real-time temperature data, and the control system dynamically adjusts the heating power to maintain a temperature gradient at the crystallization interface of 0.5-1℃ / min.

[0048] As the crystallization process proceeds, impurities gradually accumulate in the remaining molten liquid. When the crystallization rate reaches 70-80%, the coolant circulation is stopped, and the temperature of jacket 3 rises to 50-55℃. The drive motor 84 lifts the seed crystallization rod 6, causing the attached yellow phosphorus crystals to detach from the molten liquid, and the remaining impurities are discharged with the liquid.

[0049] The seed crystallizing rod 6 is transferred to a cleaning tank and sprayed with high-purity hot water at 80-90℃ to clean the surface and remove residual impurities. The cleaned crystal is melted under nitrogen protection and mechanical impurities are removed through a filtration system to obtain electronic-grade yellow phosphorus with a purity ≥99.999%.

[0050] The discharged impurity enrichment solution is distilled to recover yellow phosphorus and then returned to the system for recrystallization. The cooling circulating water is treated by the filtration and temperature control system in water tank 7 and then recycled, achieving a water saving rate of over 60%.

[0051] Finally, it should be noted that the electronic components in the drive motor 84 and other components in this embodiment are all general standard parts or parts known to those skilled in the art. Their structure and principle can be learned by those skilled in the art through technical manuals or conventional experimental methods. In the idle part of this device, all the above-mentioned electrical components are connected by wires. The specific connection method should refer to the working order between each electrical component in the above working principle to complete the electrical connection. All of these are technologies known in the art.

[0052] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed utility model. The scope of protection of this utility model is defined by the appended claims and their equivalents.

Claims

1. A high-purity yellow phosphorus crystallization purification device, comprising six crystallization tanks (1), characterized in that: The crystallization barrel (1) is equipped with a seed crystallization rod (6). The crystallization barrel (1) is supplied with water through a set of cooling circulating water pipes (9). The seed crystallization rod (6) is lifted and lowered through a set of lifting and moving units (8). Each set of crystallization barrels (1) is equipped with a jacket (3) for heating. Each set of seed crystallization rods (6) is connected to the cooling circulating water pipes (9). The outer end of the cooling circulating water pipes (9) is connected to the water tank (7).

2. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: Each set of crystallization tanks (1) is equipped with a jacket (3) for heating, and the jacket (3) is heated by heat-conducting oil and explosion-proof and corrosion-resistant heating rods.

3. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: Temperature measuring points (2) are set on the crystallization tank (1).

4. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: Each set of crystallization tanks (1) is equipped with a water inlet (4) for water intake and replenishment.

5. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: The crystallization barrel (1) is equipped with an argon gas inlet (5) for gas intake and replenishment.

6. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: The lifting and moving unit (8) includes a housing (81), inside which a lead screw (82) is vertically installed. A lead screw slider (83) is installed on the lead screw (82). The top of the lead screw (82) is driven to rotate by a drive motor (84). A strip-shaped opening (821) is provided on one side of the housing (81). One side of the lead screw slider (83) is vertically slidably engaged with the strip-shaped opening (821). The outer side of the lead screw slider (83) is connected to the outer wall of the cooling circulating water pipe (9).

7. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: The seed crystal crystallization rod (6) is a hollow tubular structure. The top end of the seed crystal crystallization rod (6) is connected to the cooling circulating water pipe (9) through a flange joint (61). The lower end of the seed crystal crystallization rod (6) is equipped with a limit baffle (62).

8. The high-purity yellow phosphorus crystallization and purification apparatus according to claim 1, characterized in that: The water tank (7) is equipped with a circulation pump. The cooling circulation water pipe (9) includes an outlet pipe and a return pipe. The outlet pipe and return pipe of the cooling circulation water pipe (9) are connected to the outlet end and inlet end of the circulation pump to realize water circulation.

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