A yellow phosphorus rinsing and refining system and its process

By designing a yellow phosphorus rinsing and refining system, using the multi-stage dynamic separation technology in the rinsing and refining tower, the existing yellow phosphorus purifying process is solved, with a large area of ​​equipment and high cost, and an efficient and continuous yellow phosphorus purifying process is achieved.

CN117285020BActive Publication Date: 2025-06-13CHENGDU EMEI CHEM ENG DESIGN INST
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Patent Information

Application Number
CN202211017722.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-08-24
Publication Date
2025-06-13
Estimated Expiration
2042-08-24

AI Technical Summary

Technical Problem

The existing yellow phosphorus purification process is complex and cumbersome, the equipment covers a large area, is costly and has low efficiency, making it difficult for the purity and output of yellow phosphorus to meet the needs.

Method used

A yellow phosphorus rinsing and refining system is designed, including a crude phosphorus storage tank, a rinsing and refining tower, a clean water storage tank and related pipelines. By achieving multi-stage dynamic separation of crude phosphorus and cleaning water in the rinsing and refining, dust is separated by convection flushing technology to achieve continuous feed refining.

Benefits of technology

Multi-stage dynamic separation of dust in crude phosphorus is achieved, the refining process is simplified, the refining cycle is shortened, the equipment and water needs are reduced, and the purity and yield of yellow phosphorus is improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a yellow phosphorus rinsing and refining system and its process, which includes a crude phosphorus storage tank, a rinsing and refining tower, a clean water storage tank, a crude phosphorus supply pipeline, a clean water supply pipeline and a cleaning water outlet pipeline. A cleaning water outlet is provided at the top of the rinsing and refining tower. A crude liquid phosphorus nozzle is provided in the upper part of the rinsing and refining tower. A clean water inlet pipe is provided in the lower part of the rinsing and refining tower. A refined phosphorus liquid outlet is provided at the bottom of the rinsing and refining tower. An exhaust port is provided at the top of the rinsing and refining tower. Compared with the prior art, the yellow phosphorus rinsing and refining system of the present invention realizes multi-stage dynamic separation and rinsing of dust in crude phosphorus through the yellow phosphorus rinsing and refining tower, thereby obtaining refined yellow phosphorus. It can achieve continuous feeding and refining without interruption, and the refining process is completed in one step, reducing the intermediate links of the refining process and shortening the refining cycle of yellow phosphorus. The recycling and reuse of cleaning water are realized, greatly reducing the water consumption of the system. The equipment required for this system is extremely small and the floor area is small.
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Description

Technical Field

[0001] The present invention relates to the field of yellow phosphorus preparation, and particularly to a yellow phosphorus rinsing and refining system and its process. Background Art

[0002] At present, the production of yellow phosphorus uses a water spray tower to spray and condense yellow phosphorus furnace gas for recovery. After spraying, crude phosphorus containing a large amount of dust will be generated, and the crude phosphorus needs to be refined and purified to obtain high-purity yellow phosphorus. Among them, the refining of crude phosphorus is a very cumbersome and lengthy process. The refining equipment is a set of refining equipment with complex structure and large floor area. The crude phosphorus needs to be cooked into liquid yellow phosphorus in a refining pot, and the dust is removed by rinsing. In this way, the yellow phosphorus settles level by level, is cooked and rinsed level by level, and the dust drifts out in stages. The efficiency is low, and the yellow phosphorus is often lost with the dust drift. During this process, since it is necessary to repeatedly refine many times to obtain refined yellow phosphorus with qualified purity, the process flow is long, there are many devices, and the investment and maintenance costs are high. Summary of the Invention

[0003] The purpose of the present invention is to provide a yellow phosphorus rinsing and refining system and its process that solve the above problems.

[0004] To achieve the above purpose, the technical solution adopted by the present invention is: a yellow phosphorus rinsing and refining system, including a crude phosphorus storage tank, a rinsing and refining tower, a clean water storage tank, a crude phosphorus supply pipeline, a clean water supply pipeline, and a cleaning water outlet pipeline. A cleaning water outlet is provided at the top of the rinsing and refining tower, and the cleaning water outlet pipeline is communicated with the cleaning water outlet. A crude liquid phosphorus spray pipe is provided in the upper part of the rinsing and refining tower, and the crude phosphorus storage tank is communicated with the crude liquid phosphorus spray pipe through the crude phosphorus supply pipeline. A clean water inlet pipe is provided in the lower part of the rinsing and refining tower, and the clean water storage tank is communicated with the clean water inlet pipe through the clean water supply pipeline. A refined phosphorus liquid outlet is provided at the bottom of the rinsing and refining tower, and an exhaust port is provided at the top of the rinsing and refining tower. A clean water make-up pipeline is also provided on the clean water storage tank.

[0005] Preferably, it further includes a wash water filter, and the cleaning water outlet pipeline is communicated with the clean water storage tank through the wash water filter.

[0006] Preferably, the wash water filter is of a kettle structure, with a straight cylinder section at the upper end and a conical section at the lower end. A dust filter screen is horizontally provided in the middle of the straight cylinder section of the wash water filter. The dust filter screen divides the wash water filter into an upper clean water tank and a lower sewage tank. A sewage inlet pipe is provided on the lower sewage tank, a clean water outlet pipe is provided on the clean water tank, the cleaning water outlet pipeline is communicated with the sewage inlet pipe, the clean water outlet pipe is communicated with the inside of the clean water storage tank, and a mud-containing wastewater drain port is provided at the bottom of the wash water filter.

[0007] Preferably, an annular diversion groove is provided in the sewage bin of the water-washing filter, the opening of the diversion groove faces upward, and the water outlet of the sewage inlet pipe is located in the diversion groove.

[0008] Preferably, the nozzle of the crude liquid phosphorus spray pipe faces downward, and the water outlet of the clean water inlet pipe faces upward.

[0009] Preferably, a crude phosphorus pump is provided on the crude phosphorus supply pipeline, and a steam heat exchanger and a clean water pump are provided on the clean water supply pipeline.

[0010] Preferably, a heating jacket is installed outside the rinsing and refining tower and the crude phosphorus storage tank, and both the steam heat exchanger and the heating jacket are provided with a hot steam inlet and a condensate outlet.

[0011] Preferably, a steam heating pipeline is further included, and the steam heating pipeline is respectively communicated with the hot steam inlets of the clean water heater, the rinsing and refining tower, and the crude phosphorus storage tank.

[0012] Preferably, the rinsing and refining tower is successively divided into a slow descent section, a coarse powder floating separation section, a medium powder floating separation section, a fine powder floating separation section, a micro powder floating separation section, and a refined liquid phosphorus sedimentation section from top to bottom. The crude liquid phosphorus spray pipe is located in the upper part of the coarse powder floating separation section, and the clean water inlet pipe is located in the lower part of the micro powder floating separation section.

[0013] A process for a yellow phosphorus rinsing and refining system, the method steps are as follows:

[0014] a. First, the crude phosphorus is stored in the crude phosphorus storage tank and heated into a crude phosphorus liquid;

[0015] b. Then, the crude phosphorus liquid is continuously pumped into the crude liquid phosphorus spray pipe at the upper part of the rinsing and refining tower through the crude phosphorus pump, and at the same time, the heated cleaning water is continuously pumped into the clean water inlet pipe at the lower part of the rinsing and refining tower;

[0016] c. After the crude phosphorus enters the rinsing and refining tower, it moves from top to bottom, while the cleaning water moves from bottom to top. The two form a countercurrent flushing. During the sinking process of the crude phosphorus, the dust in the crude phosphorus is separated by multi-stage flushing and discharged from the cleaning water outlet at the top with the cleaning water. The refined phosphorus after being separated and purified by multi-stage flushing sinks to the bottom of the rinsing and refining tower for recovery;

[0017] d. The cleaning water discharged from the cleaning water outlet pipeline is filtered and then enters the clean water supply pipeline again for recycling as cleaning water.

[0018] Compared with the prior art, the advantages of the present invention are as follows:

[0019] (1) The yellow phosphorus rinsing and refining system of the present invention realizes the multi-stage dynamic separation and rinsing of dust in crude phosphorus through the yellow phosphorus rinsing and refining tower. The crude phosphorus liquid flows down the tower from the top, and the cleaning water moves upward. The crude phosphorus liquid and the cleaning water impact and scour each other, separating the dust from the crude phosphorus. Since the dust is lighter in mass, it will be discharged from the top of the tower along with the water flow after separation, while the specific gravity of yellow phosphorus is greater than that of water and it will fall to the bottom of the tower for sedimentation and waiting for recovery, thereby obtaining refined yellow phosphorus.

[0020] (2) In the yellow phosphorus rinsing and refining system of the present invention, continuous feeding and refining of crude phosphorus can be achieved without interruption. During the descent process of the dust in the crude phosphorus in the rinsing and refining tower, it will be automatically classified and filtered according to the particle size of the dust, so as to achieve the effect of multi-stage refining, continuously refine high-quality yellow phosphorus, complete the refining process in one step, reduce the intermediate links of the refining process, and shorten the refining cycle of yellow phosphorus.

[0021] (3) In order to realize the recycling of the cleaning water after refining, the present invention also designs a wash water filter. When the cleaning water with dust enters the sewage storage tank from the sewage inlet pipe, the dust is filtered through the dust filter screen. The filtered clean water enters the clean water storage tank and flows into the clean water storage tank through the clean water outlet pipe, realizing the recycling and reuse of the cleaning water, and greatly reducing the water consumption of the system.

[0022] (4) In order to prevent the dust filter screen from blocking the filter holes during the filtering process, an annular diversion groove is provided in the sewage storage tank of the wash water filter, which can scour the dust on the dust filter screen, so that the dust on the dust filter screen falls off and sinks to the bottom of the wash water filter.

[0023] (5) The equipment required for this system is extremely small. The area occupied by the yellow phosphorus rinsing and refining tower in the refining process is also small, about 100 square meters, which is 1 / (10 - 20) of the existing process system. Moreover, the equipment investment is low, and the equipment cost is less than one-fourth of the existing process system. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 is the schematic diagram of the system structure of the present invention;

[0025] Figure 2 is the schematic diagram of the structure of the rinsing and refining tower of the present invention;

[0026] Figure 3 is the schematic diagram of the structure of the wash water filter of the present invention.

[0027] In the figure: 1. crude phosphorus storage tank; 2. rinsing and refining tower; 20. connecting section; 21. slow-down section; 22. separation section for floating coarse powder; 23. separation section for floating medium powder; 24. separation section for floating fine powder; 25. separation section for floating micro powder; 26. sedimentation section for refined liquid phosphorus; 27. coarse-hole separation plate; 28. medium-hole separation plate; 29. fine-hole separation plate; 3. clean water storage tank; 4. crude phosphorus supply pipeline; 5. clean water supply pipeline; 6. cleaning water outlet pipeline; 7. cleaning water outlet; 8. crude liquid phosphorus spray pipe; 9. clean water inlet pipe; 10. refined phosphorus liquid outlet; 11. exhaust port; 12. clean water make-up pipeline; 13. washing water filter; 131. dust filter screen; 132. clean water tank; 133. sewage tank; 134. sewage inlet pipe; 135. clean water outlet pipe; 136. muddy wastewater drain port; 137. diversion trough; 14. crude phosphorus pump; 15. clean water pump; 16. steam heat exchanger; 17. steam heating pipeline; 18. hot steam inlet; 19. condensate outlet. Detailed implementation mode

[0028] Due to the complexity of the existing refining process, multiple pools are required to wash dust during refining. The required equipment is numerous, large in volume, high in energy consumption, and usually occupies an area of more than 300 square meters. Moreover, the refining process is discontinuous, and refined yellow phosphorus can only be obtained through multiple repeated rinses each time. Therefore, there is an urgent need to design a brand-new yellow phosphorus rinsing and refining system. The present invention reforms the existing yellow phosphorus refining process and proposes a brand-new yellow phosphorus refining system and process.

[0029] The following will further illustrate the present invention. A yellow phosphorus rinsing and refining system, see Figure 1, including a crude phosphorus storage tank 1, a rinsing and refining tower 2, a clean water storage tank 3, a crude phosphorus supply pipeline 4, a clean water supply pipeline 5 and a cleaning water outlet pipeline 6. A cleaning water outlet 7 is provided at the top of the rinsing and refining tower 2, and the cleaning water outlet pipeline 6 is communicated with the cleaning water outlet 7. A crude liquid phosphorus spray pipe 8 is provided in the upper part of the rinsing and refining tower 2. The crude liquid phosphorus spray pipe 8 serves as the feed inlet of the crude phosphorus. The crude phosphorus storage tank 1 is communicated with the crude liquid phosphorus spray pipe 8 through the crude phosphorus supply pipeline 4. A clean water inlet pipe 9 is provided in the lower part of the rinsing and refining tower 2. The clean water inlet pipe 9 serves as the inlet pipe of the cleaning water. The clean water storage tank 3 is communicated with the clean water inlet pipe 9 through the clean water supply pipeline 5. A refined phosphorus liquid outlet 10 is provided at the bottom of the rinsing and refining tower 2. The refined phosphorus liquid outlet 10 is used to recover the refined and purified high-quality yellow phosphorus. An exhaust port 11 is provided at the top of the rinsing and refining tower 2. The exhaust port 11 is used to recover the waste gas in the crude phosphorus. A clean water make-up pipeline 12 is also provided on the clean water storage tank 3. The present invention completely abandons the existing process technology. Through the rinsing and refining tower 2, multi-stage dynamic separation and rinsing of the dust in the crude phosphorus are realized. The crude phosphorus liquid flows down the tower from the top, and the cleaning water moves upward. The crude phosphorus liquid and the cleaning water impact and wash each other, so that the dust is separated from the crude phosphorus. Since the dust is lighter in mass, it will be discharged from the top of the tower along with the water flow after separation, while the specific gravity of yellow phosphorus is greater than that of water and will fall to the bottom of the tower for sedimentation and wait for recovery, so as to obtain refined yellow phosphorus. The system equipment of this process only requires one crude phosphorus storage tank 1, one rinsing and refining tower 2, one clean water storage tank 3, one crude phosphorus supply pipeline 4, one clean water supply pipeline 5 and one cleaning water outlet pipeline 6. The equipment requirement is extremely small, and the floor area is also small.

[0030] Moreover, in the yellow phosphorus rinsing and refining system of the present invention, the crude phosphorus can be continuously fed and refined without interruption. During the descending process of the crude phosphorus in the rinsing and refining tower 2, the dust in the crude phosphorus will be automatically classified and filtered according to the particle size of the dust, so as to achieve the effect of multi-stage refining, and continuously refine high-quality yellow phosphorus. The refining process is completed in one step, reducing the intermediate links of the refining process and shortening the refining cycle of yellow phosphorus.

[0031] The nozzle of the crude liquid phosphorus spray pipe 8 faces downward, so that the liquid crude yellow phosphorus moves downward, and the water outlet of the clean water inlet pipe 9 faces upward, so that the cleaning water moves upward. A crude phosphorus pump 14 is provided on the crude phosphorus supply pipeline 4, and the crude phosphorus is pumped into the rinsing and refining tower 2 through the crude phosphorus pump 14. A steam heat exchanger 16 and a clean water pump 15 are provided on the clean water supply pipeline 5. The clean water is pumped into the rinsing and refining tower 2 through the clean water pump 15, and the clean water entering the rinsing and refining tower 2 is heated by the steam heat exchanger 16 to 60 - 80 °C to avoid the condensation of yellow phosphorus into solid caused by low-temperature clean water.

[0032] The rinsing and refining tower 2 and the crude phosphorus storage tank 1 are externally provided with heating jackets to ensure that yellow phosphorus is in a liquid state during the process. The steam heat exchanger 16 and the heating jackets are both provided with a hot steam inlet 18 and a condensate outlet 19. It also includes a steam heating pipeline 17 which is respectively connected to the hot steam inlets 18 of the fresh water heater, the rinsing and refining tower 2, and the crude phosphorus storage tank 1, and heat supply to the fresh water heater, the rinsing and refining tower 2, and the crude phosphorus storage tank 1 is realized through the steam heating pipeline 17.

[0033] In addition to the design of the crude phosphorus supply pipeline 4 and the fresh water supply pipeline 5 for crude phosphorus in the present invention, a large amount of cleaning water will be generated after rinsing and discharged from the yellow phosphorus rinsing and refining tower 2 through the cleaning water outlet pipeline 6. To realize the recycling of wastewater, the present invention also includes a wash water filter 13. The cleaning water outlet pipeline 6 is connected to the fresh water storage tank 3 through the wash water filter 13. The fresh water filtered by the wash water filter 13 can be discharged into the fresh water storage tank 3 for recycling, solving the problem of large water consumption during the yellow phosphorus refining process. When the water volume in the fresh water storage tank 3 is insufficient, water can be replenished through the fresh water make-up pipeline 12.

[0034] To realize the recycling of the cleaning water after refining, the present invention also designs the wash water filter 13. Refer to Figure 3 , the wash water filter 13 is of a kettle structure, with a straight cylinder section at the upper end and a conical section at the lower end. A dust filter screen 131 is horizontally arranged in the middle of the straight cylinder section of the wash water filter 13. The dust filter screen 131 divides the wash water filter 13 into an upper fresh water chamber 132 and a lower sewage chamber 133. A sewage inlet pipe 134 is provided on the lower sewage chamber 133, and a fresh water outlet pipe 135 is provided on the fresh water chamber 132. The cleaning water outlet pipeline 6 is connected to the sewage inlet pipe 134, and the fresh water outlet pipe 135 is internally connected to the fresh water storage tank 3. A sludge-containing wastewater drain port 136 is provided at the bottom of the wash water filter 13. When the cleaning water with dust enters the sewage chamber 133 from the sewage inlet pipe 134, the dust is filtered through the dust filter screen 131. The filtered fresh water enters the fresh water chamber 132 and flows into the fresh water storage tank 3 through the fresh water outlet pipe 135. The filtered dust remains in the sewage chamber 133 and deposits at the bottom of the conical section, and then is discharged through the sludge-containing wastewater drain port 136.

[0035] During the filtration process of the dust filter screen 131, a large amount of dust will be adsorbed on the dust filter screen 131. To prevent the dust from clogging the filter holes during long-term filtration, an annular diversion groove 137 is provided in the sewage bin 133 of the wash water filter 13. The opening of the diversion groove 137 faces upward, and the water outlet of the sewage inlet pipe 134 is located within the diversion groove 137. After the refined wash water enters the diversion groove 137 from the sewage inlet pipe 134, it will flow out from the upper opening of the diversion groove 137. The opening of the diversion groove 137 is near the dust filter screen 131, and during the flowing process, it can wash the dust on the dust filter screen 131, causing the dust on the dust filter screen 131 to fall off and sink to the bottom of the wash water filter 13.

[0036] The technological process of the present invention is as follows:

[0037] A process for refining yellow phosphorus by rinsing, see Figure 1 , and the method steps are as follows:

[0038] a. First, the crude phosphorus is stored in the crude phosphorus storage tank 1 and heated into a crude phosphorus liquid; the crude phosphorus in the crude phosphorus storage tank 1 is sourced from the yellow phosphorus spray recovery tower. To ensure that the yellow phosphorus is in a liquid state and prevent it from condensing into a solid, the crude phosphorus storage tank 1 can heat the crude phosphorus to above 44.1° through a heating jacket. To ensure the stability of the system, the heating temperature is set to 60 - 80°.

[0039] b. Then, the crude phosphorus liquid is continuously pumped into the liquid phosphorus crude product spray pipe 8 at the upper part of the rinsing and refining tower 2 through the crude phosphorus pump 14, and at the same time, the heated wash water is continuously pumped into the clean water inlet pipe 9 at the lower part of the rinsing and refining tower 2; during the process of refining crude phosphorus, it is necessary to ensure that the yellow phosphorus is in a liquid state, so the temperature inside the rinsing and refining tower 2 needs to reach above 44.1° for multi-stage dynamic separation and rinsing. The rinsing and refining tower 2 can be heated through a heating jacket wrapped around its outer wall, and the specific heating temperature depends on the on-site situation. To ensure the stability of the system, the heating temperature is set to 60 - 80°, and it must not be higher than the vaporization temperature of yellow phosphorus, which is 280°.

[0040] c. After the crude phosphorus enters the rinsing and refining tower 2, it moves from top to bottom, while the wash water moves from bottom to top, forming a countercurrent wash. During the sinking process of the crude phosphorus, the dust in the crude phosphorus is separated through multi-stage washing and discharged from the wash water outlet 7 at the top along with the wash water. The refined phosphorus after multi-stage washing, separation, and purification sinks to the bottom of the rinsing and refining tower 2 for recovery.

[0041] d. The wash water discharged from the wash water outlet pipeline 6 is filtered and then enters the clean water supply pipeline 5 again for use as recycled wash water.

[0042] This process flow is simpler and more convenient compared with the existing process. It involves fewer devices and can achieve continuous refining of yellow phosphorus, greatly shortening the refining time, reducing operation steps, and the extracted yellow phosphorus fully meets the refining standards.

[0043] In order to improve the rinsing and refining effect of the yellow phosphorus rinsing tower, the present invention designs the rinsing tower. Refer to Figure 2 , a yellow phosphorus rinsing and refining tower 2, which is successively divided into a slow descent section 21, a coarse powder floating separation section 22, a medium powder floating separation section 23, a fine powder floating separation section 24, a micro powder floating separation section 25, and a refined liquid phosphorus sedimentation section 26 from top to bottom. An exhaust port 11 is provided at the top of the slow descent section 21, and a cleaning water outlet 7 is provided on the side of the slow descent section 21. A liquid phosphorus crude product spray pipe 8 is provided at the upper part of the coarse powder floating separation section 22, a clean water inlet pipe 9 is provided at the lower part of the micro powder floating separation section 25, a refined phosphorus liquid outlet 10 is provided at the bottom of the refined liquid phosphorus sedimentation section 26. A coarse hole separation plate 27 is provided between the coarse powder floating separation section 22 and the medium powder floating separation section 23, a medium hole separation plate 28 is provided between the medium powder floating separation section 23 and the fine powder floating separation section 24, and a fine hole separation plate 29 is provided between the fine powder floating separation section 24 and the micro powder floating separation section 25. The present invention divides the yellow phosphorus rinsing and refining tower 2 into six sections from top to bottom, and the crude phosphorus is refined step by step from top to bottom, while the cleaning water flushes the crude phosphorus at each level from bottom to top in the reverse direction. First, the crude phosphorus liquid is sprayed into the coarse powder floating separation section 22 in the tower. When encountering the reverse cleaning water flushing in the coarse powder floating separation section 22, the dust-grade crude phosphorus is subjected to the first-stage flushing and separation. During the flushing and separation process, the crude phosphorus falls, and the separated dust flows out from the cleaning and blowing outlet with the cleaning water. The crude phosphorus that meets the first-stage refining standard passes through the coarse hole separation plate 27 and enters the medium floating separation section for further flushing and refining. The crude phosphorus that does not meet the standard is isolated in the coarse powder floating separation section 22 by the coarse hole separation plate 27 and continues to be separated. A part of the crude phosphorus will be flushed into the slow descent section 21 with the water and then naturally settle and fall back to continue the separation in the coarse powder floating separation section 22, and so on. The crude phosphorus will successively pass through the coarse powder floating separation section 22, the medium powder floating separation section 23, the fine powder floating separation section 24, and the micro powder floating separation section 25 for four times of flushing and refining from top to bottom. The finer the dust separated at each stage, the higher the purity of the yellow phosphorus. After the refining is completed, the refined liquid phosphorus enters the refined liquid phosphorus sedimentation section 26 and then passes through the refined phosphorus liquid outlet 10. Through the above structural design, multi-stage flushing and refining are carried out during the sinking process of the crude phosphorus. During the refining period, there is no need to stop the machine, no need to cache through an intermediate water tank, and no need to transfer between devices. The refining of yellow phosphorus can be completed in one step, greatly reducing the yellow phosphorus refining cycle. Moreover, the occupied area of the refining tower is small, the required auxiliary equipment is also few, the equipment cost is low, the stability is strong, and it can operate continuously without stopping for refining, with good economy.

[0044] The injection port of the crude liquid phosphorus nozzle 8 is located on the central axis of the rinsing and refining tower 2, and the injection direction is downward. The water outlet of the clean water inlet pipe 9 is located on the central axis of the rinsing and refining tower 2, and the water outlet is upward. The water outlet and the crude phosphorus feeding direction on the central axis can be straight up and down, and the tower wall can be avoided from being scoured.

[0045] The coarse powder upward floating separation section 22, the medium powder upward floating separation section 23, the fine powder upward floating separation section 24, and the micro powder upward floating separation section 25 are of variable diameter structures. When the water inflow of the clean water inlet pipe 9 is constant, as the diameters of the separation sections gradually increase from top to bottom, the flow velocities of the separation sections from bottom to top will gradually increase, so as to meet the requirements of dust flushing and separation in each stage.

[0046] The coarse powder upward floating separation section 22 and the micro powder upward floating separation section 25 are straight pipes. The medium powder upward floating separation section 23 and the fine powder upward floating separation section 24 are gradually expanding pipes with a narrower upper part and a wider lower part. The diameter of the upper end of the medium powder upward floating separation section 23 is the same as the diameter of the lower end of the coarse powder upward floating separation section 22. The diameter of the lower end of the medium powder upward floating separation section 23 is the same as the diameter of the upper end of the fine powder upward floating separation section 24. The diameter of the lower end of the fine powder upward floating separation section 24 is the same as the diameter of the upper end of the micro powder upward floating separation section 25. The straight pipe design of the coarse powder upward floating separation section 22 and the micro powder upward floating separation section 25 makes the flow velocity of the crude phosphorus in this separation section more uniform. The gradually expanding pipe design of the medium powder upward floating separation section 23 and the fine powder upward floating separation section 24 forms different flow velocity cleaning water between each separation section to meet the dust separation needs. The diameters and heights of each separation section are designed according to the on-site conditions.

[0047] Both the slow descent section 21 and the refined liquid phosphorus sedimentation section 26 are conical kettle body structures with a wider upper part and a narrower lower part. The diameter of the lower end of the slow descent section 21 is the same as the diameter of the upper end of the coarse powder upward floating separation section 22, and it is fixedly connected to the coarse powder upward floating separation section 22 through a connecting flange. The conical kettle body structure of the slow descent section 21 can reduce the cleaning water flow velocity, so that the crude phosphorus carried into the slow descent section 21 by the cleaning water can be effectively sedimented, and the sedimentation returns to the coarse powder upward floating separation section 22 for flushing and separation. The diameter of the upper end of the refined liquid phosphorus sedimentation section 26 is the same as the diameter of the lower end of the micro powder upward floating separation section 25, and it is fixedly connected to the micro powder upward floating separation section 25 through a connecting flange. The conical kettle body structure of the refined liquid phosphorus sedimentation section 26 can make the refined high-quality yellow phosphorus converge to the refined phosphorus liquid outlet 10 for recovery. The flange connection is convenient for the disassembly and assembly of each separation section, and it is also very convenient when the corresponding separation section needs to be replaced.

[0048] The diameter of the clean water inlet pipe 9 is smaller than that of the cleaning water outlet 7, which can achieve that the water outlet speed at the top of the rinsing and refining tower 2 is less than the water inlet flow rate at the bottom, so as to achieve the purpose of slow water outlet in the slow descent section 21, and ensure that the crude phosphorus can be effectively deposited in the slow descent section 21 and will not flow out with the cleaning water. Since the crude liquid phosphorus spray pipe 8 and the clean water inlet pipe 9 are located inside the rinsing and refining tower 2 and are not easy to disassemble, in order to facilitate the connection of the crude phosphorus supply pipeline 4 and the clean water supply pipeline 5, connection flanges are provided at the water outlet of the cleaning water outlet 7, the feed port of the crude liquid phosphorus spray pipe 8, and the water inlet of the clean water inlet pipe 9, and the pipeline connection is realized through the connection flanges.

[0049] If the yellow phosphorus rinsing and refining tower 2 is integrally formed, it is inconvenient to install and maintain the internal coarse pore separation plate 27, medium pore separation plate 28, and fine pore separation plate 29. Therefore, connection sections 20 are provided between the coarse powder floating separation section 22 and the medium powder floating separation section 23, between the medium powder floating separation section 23 and the fine powder floating separation section 24, and between the fine powder floating separation section 24 and the fine powder floating separation section 25. The pore diameters of the coarse pore separation plate 27, medium pore separation plate 28, and fine pore separation plate 29 are different and are used to isolate dust with different particle sizes. They are purchased and selected according to actual conditions and are respectively arranged in the corresponding connection sections 20. The connection sections 20 are connected between the separation sections through connection flanges. The connection sections 20 can realize the transition connection between the separation sections. Since the connection sections 20 are detachable and the coarse pore separation plate 27, medium pore separation plate 28, and fine pore separation plate 29 are installed in the connection sections 20, it is also convenient for the installation and disassembly of the separation plates and subsequent maintenance.

[0050] The outer jacket of the yellow phosphorus rinsing and refining tower 2 is equipped with a heating jacket. The heating jacket is provided with a heating steam inlet 18 at the upper end and a condensate outlet 19 at the lower end. The rinsing and refining tower 2 can be heated through the heating jacket to ensure that the crude phosphorus is in a liquid state during the refining process.

[0051] The above has introduced in detail a yellow phosphorus rinsing and refining system and its process provided by the present invention. Specific examples are used in this article to elaborate on the principle and implementation manner of the present invention. The description of the above embodiments is only used to help understand the method and its core idea of the present invention; at the same time, for those of ordinary skill in the art, according to the idea of the present invention, there will be changes in the specific implementation manner and application scope. It is possible to make changes and improvements to the present invention without exceeding the concept and scope defined by the appended claims. In summary, the content of this specification should not be construed as a limitation to the present invention.

Claims

1. A yellow phosphorus rinsing and refining system, characterized in that: It includes a crude phosphorus storage tank, a rinsing and refining tower, a clean water storage tank, a crude phosphorus supply pipeline, a clean water supply pipeline and a cleaning water outlet pipeline. A cleaning water outlet is provided at the top of the rinsing and refining tower, and the cleaning water outlet pipeline is communicated with the cleaning water outlet. A crude liquid phosphorus spray pipe is provided in the upper part of the rinsing and refining tower. The crude phosphorus storage tank is communicated with the crude liquid phosphorus spray pipe through the crude phosphorus supply pipeline. A clean water inlet pipe is provided in the lower part of the rinsing and refining tower. The clean water storage tank is communicated with the clean water inlet pipe through the clean water supply pipeline. The nozzle of the crude liquid phosphorus spray pipe faces downward, and the water outlet of the clean water inlet pipe faces upward. The rinsing and refining tower is successively divided into a slow descent section, a coarse powder floating separation section, a medium powder floating separation section, a fine powder floating separation section, a micro powder floating separation section and a refined liquid phosphorus sedimentation section from top to bottom. The crude liquid phosphorus spray pipe is located in the upper part of the coarse powder floating separation section, and the clean water inlet pipe is located in the lower part of the micro powder floating separation section. A refined phosphorus liquid outlet is provided at the bottom of the rinsing and refining tower, and an exhaust port is provided at the top of the rinsing and refining tower. A clean water make-up pipeline is also provided on the clean water storage tank.

2. A yellow phosphorus rinsing and refining system according to claim 1, characterized in that: It further includes a washing water filter, and the cleaning water outlet pipeline is communicated with the clean water storage tank through the washing water filter.

3. A yellow phosphorus rinsing and refining system according to claim 2, characterized in that: The washing water filter is of a kettle body structure, with a straight cylinder section at the upper end and a conical section at the lower end. A dust filter screen is horizontally provided in the middle of the straight cylinder section of the washing water filter. The dust filter screen divides the washing water filter into an upper clean water bin and a lower sewage bin. A sewage inlet pipe is provided on the lower sewage bin, and a clean water outlet pipe is provided on the clean water bin. The cleaning water outlet pipeline is communicated with the sewage inlet pipe, and the clean water outlet pipe is communicated with the inside of the clean water storage tank. A mud-containing wastewater drain port is provided at the bottom of the washing water filter.

4. A yellow phosphorus rinsing and refining system according to claim 3, characterized in that: An annular diversion groove is provided in the sewage bin of the washing water filter, the opening of the diversion groove faces upward, and the water outlet of the sewage inlet pipe is located in the diversion groove.

5. A yellow phosphorus rinsing and refining system according to claim 1, characterized in that: A crude phosphorus pump is provided on the crude phosphorus supply pipeline, and a steam heat exchanger and a clean water pump are provided on the clean water supply pipeline.

6. A yellow phosphorus rinsing and refining system according to claim 5, characterized in that: The rinsing and refining tower and the crude phosphorus storage tank are externally sleeved with heating jackets, and both the steam heat exchanger and the heating jacket are provided with a hot steam inlet and a condensate outlet.

7. A yellow phosphorus rinsing and refining system according to claim 6, characterized in that: It further includes a steam heating pipeline, and the steam heating pipeline is respectively communicated with the hot steam inlets of the clean water heater, the rinsing and refining tower and the crude phosphorus storage tank.

8. The refining process of a yellow phosphorus rinsing and refining system according to claim 1, characterized in that, The method steps are as follows: a. First, the crude phosphorus is stored in the crude phosphorus storage tank and heated into crude phosphorus liquid; b. Then, continuously pump the crude phosphorus liquid into the crude liquid phosphorus spray pipe at the upper part of the rinsing and refining tower through the crude phosphorus pump, and at the same time, continuously pump the heated cleaning water into the clean water inlet pipe at the lower part of the rinsing and refining tower; c. After the crude phosphorus enters the rinsing and refining tower, it moves from top to bottom, while the cleaning water moves from bottom to top. The two form a countercurrent rinse. During the sinking process of the crude phosphorus, the dust in the crude phosphorus is separated through multiple rinses and discharged from the cleaning water outlet at the top along with the cleaning water. The refined phosphorus after being purified through multiple rinses and separations sinks to the bottom of the rinsing and refining tower for recovery; d. The cleaning water discharged from the cleaning water outlet pipe is filtered and then enters the clean water supply pipeline again for recycling as cleaning water.

Citation Information

Patent Citations

  • Yellow phosphorus rinsing and refining system

    CN218115024U