High-purity phosphorus reduction collection device and collection method thereof

By designing a high-purity phosphorus reduction and collection device, and utilizing sealed connections and inert gas replacement, efficient and safe high-purity phosphorus collection was achieved, solving the problems of low collection efficiency and poor safety in existing technologies, and simplifying the collection process.

CN118491434BActive Publication Date: 2025-12-19FIRST RARE MATERIALS CO LTD
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Patent Information

Application Number
CN202410469263.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-04-18
Publication Date
2025-12-19
Estimated Expiration
2044-04-18

AI Technical Summary

Technical Problem

Existing technologies have low efficiency and difficulty in collecting high-purity phosphorus. Furthermore, the high requirements for equipment sealing when collecting phosphorus under cooling in an inert gas atmosphere result in unsafe production processes and poor treatment of organic impurities.

Method used

Design a high-purity phosphorus reduction and collection device, including a reaction component, a collection tower, a spray component, a circulation component, and a tail gas treatment component. A sealed space is formed by a sealed connection. Inert gas is used to replace the air. The spray component cools the generated gaseous phosphorus and separates it into liquid phosphorus under gravity. The tail gas treatment component treats the uncollected hydrochloric acid gas.

Benefits of technology

It achieves efficient and safe collection of high-purity phosphorus, reduces human intervention, improves collection efficiency and production safety, reduces the introduction of organic impurities, and simplifies the collection process.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to the technical field of chemical equipment, and discloses a high-purity phosphorus reduction collecting device and a collecting method thereof, which comprises a reaction component, a collecting tower, a spraying component, a circulating component for recycling the spraying liquid and a tail gas treatment component for absorbing the tail gas in the main body of the absorption tower; the collecting tower comprises a tower main body, a tower end plate and a separation tank, the tower main body is provided with a collecting cavity and a reaction gas inlet, the reaction component is connected to the reaction gas inlet and communicates with the collecting cavity, the separation tank is provided with a separation cavity, a circulating liquid outlet, a finished product outlet and a finished product valve, the tower main body is inserted into the separation cavity and is in sealing connection with the separation tank, the circulating liquid outlet is located at the upper portion of the separation tank, the finished product outlet is located at the lower portion of the separation tank, the circulating liquid outlet and the finished product outlet respectively communicate with the separation cavity, and the finished product valve is connected to the finished product outlet; the spraying component comprises a nozzle and a connecting water pipe, and the connecting water pipe communicates with the nozzle through the tower end plate. The high-purity phosphorus reduction collecting device and the collecting method thereof are simple in collecting method.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical equipment, in particular to a high-purity phosphorus reduction collection device and a collection method thereof. BACKGROUND

[0002] High-purity phosphorus generally refers to elemental phosphorus containing 99.9999% (6N) of phosphorus in the product. Elemental phosphorus above 6N is an important raw material for the production of electronic-grade red phosphorus and phosphorus compounds, such as phosphorus oxychloride, electronic-grade phosphoric acid, etc. The acid oxidation method for purifying commercial-grade yellow phosphorus is a traditional yellow phosphorus purification process that has been widely studied. It mainly utilizes the principle that liquid yellow phosphorus is insoluble in aqueous solution. However, the loss rate of yellow phosphorus in this process is 30%-40%, and many organic impurities such as CS2, benzene, etc. are introduced in the production process, and the oxidative system has poor treatment effect on organic impurities.

[0003] The device is a coexistence body of red phosphorus and yellow phosphorus generated by the reduction reaction of phosphorus trichloride and hydrogen gas through heating, mainly yellow phosphorus. In the prior art, the finished product phosphorus is cooled and collected in an inert gas atmosphere, which has low collection efficiency and high difficulty in collection, and high requirement for the sealing performance of the equipment. SUMMARY

[0004] The present application aims to at least solve one of the technical problems existing in the prior art. The present application provides a high-purity phosphorus reduction collection device and a collection method thereof, which has simple collection method and high collection efficiency.

[0005] In order to achieve the above-mentioned purpose, the present application provides a high-purity phosphorus reduction collection device, which comprises a reaction assembly, a collection tower, a spraying assembly, a circulating assembly and a tail gas treatment assembly.

[0006] The collection tower comprises a tower main body, a tower end plate and a separation tank, the upper end of the tower main body is sealingly connected with the tower end plate, the tower main body is provided with a collection cavity and a reaction gas inlet, the reaction assembly is connected to the reaction gas inlet and communicates with the collection cavity, the separation tank is provided with a separation cavity, a circulating liquid outlet, a finished product outlet and a finished product valve, the lower end of the tower main body is inserted into the separation cavity and sealingly connected with the separation tank, the circulating liquid outlet is located at the upper part of the separation tank, the finished product outlet is located at the lower part of the separation tank, the circulating liquid outlet and the finished product outlet respectively communicate with the separation cavity, and the finished product valve is connected to the finished product outlet.

[0007] The spraying assembly comprises a nozzle and a connecting water pipe, the nozzle is connected in the collection cavity, the reaction gas inlet is located between the nozzle and the lower end of the tower main body in the height direction, and the connecting water pipe communicates with the nozzle through the tower end plate.

[0008] The circulating assembly comprises a water tank and a water return pipe, the water return pipe is communicated with the circulating liquid outlet and the water tank respectively, and the water tank is communicated with the connecting water pipe.

[0009] The tail gas treatment assembly comprises a tail gas pipeline and a tail gas treatment tank for containing water, one end of the tail gas pipeline is connected to the tower end plate and communicated with the collecting cavity, and the other end of the tail gas pipeline is communicated with the tail gas treatment tank.

[0010] As a preferred solution, the reaction assembly comprises a main pipe body, a baffle and a heating element for heating the main pipe body, the main pipe body is provided with a collecting port, a raw material filling port and a reaction cavity, the baffle is located in the reaction cavity, the peripheral side of the baffle is connected to the inner wall of the main pipe body, the upper part of the baffle is provided with a reaction through hole, the baffle divides the reaction cavity into a reaction zone and a collecting zone, the raw material filling port is communicated with the reaction zone, the reaction zone is communicated with the collecting zone through the reaction through hole, the collecting zone is communicated with the collecting port, and the collecting port is communicated with the reaction gas inlet.

[0011] As a preferred solution, the main pipe body comprises a reaction pipe section and a filling pipe section, the reaction cavity and the baffle are located in the reaction pipe section, the collecting port is located at one end of the reaction pipe section, one end of the filling pipe section is communicated with the other end of the reaction pipe section, the other end of the filling pipe section away from the reaction pipe section is provided with the raw material filling port, and the reaction assembly further comprises a first inner pipe body and a second inner pipe body located in the reaction pipe section, one end of the first inner pipe body is connected to the baffle, the other end of the first inner pipe body has a first flow gap with the end of the reaction pipe section away from the collecting port, the second inner pipe body is connected to the end of the reaction pipe section away from the collecting port, one end of the second inner pipe body extends into the first inner pipe body and has a second flow gap with the baffle, and the other end of the second inner pipe body is communicated with the raw material filling port through the filling pipe section.

[0012] As a preferred solution, the reaction through hole is arranged between the outer wall of the first inner pipe body and the inner wall of the reaction pipe section.

[0013] As a preferred solution, the raw material filling port comprises a gas filling port and a liquid filling port, the liquid filling port and the gas filling port are respectively communicated with the end of the second inner pipe body away from the first inner pipe body through the filling pipe section, the axial distance between the liquid filling port and the baffle is a, the axial distance between the gas filling port and the baffle is b, and b>a.

[0014] As a preferred solution, the spraying assembly further comprises a spraying dispersion plate connected in the tower main body, the spraying dispersion plate is provided with a plurality of dispersion through holes, and the spraying dispersion plate is located between the nozzle and the reaction gas inlet in the height direction.

[0015] As a preferred solution, the lower end of the tail gas treatment tank is provided with a wastewater discharge port and a wastewater discharge valve connected to the wastewater discharge port, one end of the tail gas pipeline is inserted into the tower body through the tower end plate and communicates with the collection cavity, the other end of the tail gas pipeline communicates with the tail gas treatment tank, and the upper end of the tail gas treatment tank is provided with a tail gas discharge port for discharging tail gas.

[0016] As a preferred solution, the circulating assembly further comprises a first partition plate and at least two second partition plates, the water tank comprises a main tank body, a top plate and a bottom plate, opposite sides of the main tank body are respectively provided with a liquid inlet and a liquid outlet, the liquid inlet communicates with the circulating liquid outlet through the backwater pipe, the liquid outlet communicates with the collection cavity through the connecting water pipe, the main tank body, the top plate and the bottom plate enclose a circulating cavity, the liquid inlet and the liquid outlet respectively communicate with the circulating cavity, the first partition plate and the second partition plates are respectively connected in the circulating cavity and located between the liquid inlet and the liquid outlet, the bottom surface of the second partition plate is connected with the bottom plate, the side surface of the second partition plate is respectively connected with the side surface of the main tank body, the top surface of the second partition plate forms an upper circulating channel with the top plate, adjacent second partition plates are arranged in a first direction, the first partition plate is located between two adjacent second partition plates, the top surface of the first partition plate is connected with the top plate, the side surface of the first partition plate is connected with the side surface of the main tank body, and the lower circulating channel is formed between the bottom surface of the first partition plate and the bottom plate.

[0017] As a preferred solution, the liquid outlet is connected with a first liquid supply pipe, the first liquid supply pipe communicates with the circulating cavity, a water pump is connected to the first liquid supply pipe, the water outlet end of the water pump communicates with the connecting water pipe, the top plate is connected with a third liquid supply pipe, the third liquid supply pipe is connected with a valve, one end of the third liquid supply pipe communicates with the connecting water pipe, and the other end thereof communicates with the circulating cavity.

[0018] A high-purity phosphorus reduction collection method, in which phosphorus trichloride and hydrogen are reacted and collected in a high-purity phosphorus reduction collection device, includes the following steps:

[0019] A reaction step, in which phosphorus trichloride and hydrogen are heated in the reaction assembly to generate gaseous phosphorus and gaseous hydrochloric acid, and the gaseous phosphorus and gaseous hydrochloric acid enter the collection cavity through the reaction gas inlet;

[0020] A cooling collection step, in which water in the water tank communicates with the nozzle through the connecting water pipe, and the nozzle sprays water to cool the gaseous phosphorus and gaseous hydrochloric acid to form liquid phosphorus and liquid hydrochloric acid;

[0021] Separation step, the liquid phosphorus, the liquid hydrochloric acid and the sprayed water flow downward into the separation cavity under the action of gravity, the liquid phosphorus is precipitated at the bottom of the separation cavity, the finished product valve is opened, the liquid phosphorus is discharged from the finished product outlet to storage, the liquid hydrochloric acid is dissolved in water and is above the liquid phosphorus, and is recycled to the water tank through the circulating liquid outlet for the nozzle to be used for cooling circulation;

[0022] Tail gas collection step, the tail gas treatment tank contains water, part of the gaseous hydrochloric acid enters the tail gas treatment tank through the tail gas pipeline and is dissolved in the water in the tail gas treatment tank.

[0023] Compared with the prior art, the high-purity phosphorus reduction collection device and the collection method thereof have the beneficial effects that the phosphorus trichloride and the hydrogen gas are heated in the reaction assembly to produce the gaseous phosphorus and the gaseous hydrochloric acid through a reduction reaction. The device comprises a reaction assembly, a collection tower, a spraying assembly, a circulating assembly and a tail gas treatment assembly. These regions are connected through sealing to ensure that a closed space is formed inside the whole device. Before production, inert gas is used to replace air inside the device to maintain a low-oxygen-content environment, thereby effectively preventing the yellow phosphorus from reacting with oxygen to cause combustion and improving production safety. The raw material phosphorus trichloride and hydrogen gas are injected into the reaction assembly, the reaction assembly heats the raw material, and when the set temperature is reached, the raw material will undergo a hydrogenation reduction reaction to generate phosphorus vapor and hydrochloric acid gas. The phosphorus vapor and the hydrochloric acid gas then enter the collection cavity through the reaction gas inlet. The collection tower comprises a tower main body, a tower end plate and a separation tank, the nozzle in the spraying assembly is connected in the collection cavity, the water pipe is connected with the water tank and the nozzle in communication, the liquid in the water tank is sprayed out through the nozzle in the collection cavity to cool the gaseous phosphorus, the phosphorus vapor is cooled and converted into liquid phosphorus, at the same time, the hydrochloric acid gas is dissolved in water to form an aqueous hydrochloric acid solution, the liquid phosphorus and the aqueous hydrochloric acid solution flow to the separation tank under the action of gravity and are collected, the liquid phosphorus then flows into the separation tank with the water flow, the liquid phosphorus and the aqueous hydrochloric acid solution are not miscible, and the liquid phosphorus naturally deposits at the bottom of the separation tank because its specific gravity is greater than that of the aqueous hydrochloric acid solution, the finished product valve is opened, the liquid phosphorus flows out from the finished product outlet to realize collection, thereby realizing an efficient and pure collection process, and the liquid phosphorus is convenient to store and transport. The aqueous hydrochloric acid solution located in the upper part of the separation tank is recycled after entering the water tank through the circulating liquid outlet through the backwater pipe. The tail gas treatment assembly collects the uncollected hydrochloric acid gas again to ensure the environmental protection and safety of the production process, the collection method of the liquid phosphorus is simple, human auxiliary operation is reduced, and the collection efficiency is improved. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 is the overall structure schematic diagram of the embodiment of the present application.

[0025] Figure 2 is the overall structure schematic diagram of the reaction assembly of the embodiment of the present application.

[0026] Figure 3 is a cross-sectional view of the overall structure of the embodiment of the present application.

[0027] Figure 4 is a cross-sectional view of the overall structure of the embodiment of the present application Figure 2 .

[0028] Figure 5 is an enlarged structural schematic view of D in the embodiment of the present application Figure 3 .

[0029] Figure 6 is a schematic view of the flow path of the reactants in the main body, the first inner tube and the second inner tube in the embodiment of the present application.

[0030] Figure 7 is a schematic view of the assembly structure of the separation tank and the tower main body in the embodiment of the present application.

[0031] Figure 8 is a schematic view of the spray assembly in the tower main body in the embodiment of the present application.

[0032] Figure 9 is a schematic view of the use state of the nozzle in the embodiment of the present application.

[0033] Figure 10 is a schematic view of the spray assembly in the tower main body in the embodiment of the present application.

[0034] Figure 11 is a schematic view of the structure of the tail gas treatment assembly in the embodiment of the present application.

[0035] Figure 12 is a schematic view of the structure of the water tank in the embodiment of the present application.

[0036] Figure 13 is a schematic view of the component disassembly structure of the water tank in the embodiment of the present application.

[0037] Figure 14 is a schematic view of the internal structure of the water tank in the embodiment of the present application.

[0038] Figure 15 is a side view of the water tank in the embodiment of the present application.

[0039] Figure 16 is a cross-sectional view of A-A in the embodiment of the present application Figure 15 .

[0040] in the figure:

[0041] 01, reaction assembly; 10, main pipe body; 11, collection port; 12, raw material filling port; 13, gas filling port; 14, liquid filling port; 15, reaction cavity; 16, reaction zone; 17, collection zone; 18, reaction pipe section; 19, filling pipe section; 20, baffle; 21, reaction through hole; 30, heating piece; 40, first inner pipe body; 41, first flow-through gap; 42, second connecting part; 50, second inner pipe body; 51, second flow-through gap; 52, first connecting part;

[0042] 02, collection tower; 59, separation cavity; 60, separation tank; 61, finished product outlet; 62, finished product valve; 63, circulating liquid outlet; 64, tower main body; 65, reaction gas inlet; 66, tower end plate; 67, dispersion connecting rod; 68, collection temperature sensor; 69, liquid phosphorus; 70, collection cavity;

[0043] 03, spraying assembly; 71, nozzle; 72, connecting water pipe; 74, spraying dispersion plate; 76, dispersion through hole; 77, spraying pipe;

[0044] 04, tail gas treatment assembly; 81, tail gas pipe; 82, tail gas treatment tank; 83, tail gas inlet; 84, waste water discharge port; 85, waste water discharge valve; 86, tail gas discharge port; 87, anti-suck-back tank; 88, tail gas insertion pipe; 89, upper interface; 90, lower interface;

[0045] 05, circulating assembly; 100, water tank; 101, main tank body; 102, circulating cavity; 103, upper circulating channel; 104, lower circulating channel; 105, top plate; 106, bottom plate; 107, first end; 108, second end; 109, liquid inlet; 110, liquid supply port; 111, first liquid supply pipe; 112, water pump; 114, third liquid supply pipe; 115, valve; 116, first partition plate; 117, second partition plate; 118, clamping through slot; 119, limiting slot; 120, limiting plate; 121, heat exchanger; 122, circulating temperature sensor; 123, backwater pipe; DETAILED DESCRIPTION

[0046] The specific embodiments of the present application will be further described in detail below with reference to the accompanying drawings and examples. The following examples are used to illustrate the present application, but are not used to limit the scope of the present application.

[0047] In the description of the present application, it should be understood that the terms "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like indicating the orientation or positional relationship in the present application are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application.

[0048] In the description of the present application, it should be understood that the terms "connected", "connected", "fixed" and the like in the present application should be understood in a broad sense, for example, it can be fixedly connected, or it can be detachably connected, or it can be integrated; it can be mechanically connected, or it can be weldedly connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the internal communication of two elements or the interaction relationship of two elements, unless otherwise explicitly limited. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0049] As shown in Figures 1 to 16 The high-purity phosphorus reduction and collection device of the preferred embodiment of the present application comprises a reaction assembly 01, a collection tower 02, a spraying assembly, a circulating assembly 05 and a tail gas treatment assembly 04.

[0050] The collection tower 02 comprises a tower main body 64, a tower end plate 66 and a separation tank 60, the upper end of the tower main body 64 is sealingly connected with the tower end plate 66, the tower main body 64 is provided with a collection cavity 70 and a reaction gas inlet 65, the reaction assembly 01 is connected to the reaction gas inlet 65 and communicates with the collection cavity 70, the separation tank 60 is provided with a separation cavity 59, a circulating liquid outlet 63, a finished product outlet 61 and a finished product valve 62, the lower end of the tower main body 64 is inserted into the separation cavity 59 and sealingly connected with the separation tank 60, the circulating liquid outlet 63 is located at the upper part of the separation tank 60, the finished product outlet 61 is located at the lower part of the separation tank 60, the circulating liquid outlet 63 and the finished product outlet 61 respectively communicate with the separation cavity 59, and the finished product valve 62 is connected to the finished product outlet;

[0051] The spraying assembly 03 comprises a nozzle 71 and a connecting water pipe 72, the nozzle 71 is connected in the tower main body 64, the reaction gas inlet 65 is located between the nozzle 71 and the lower end of the tower main body 64 in the height direction, and the connecting water pipe 72 communicates with the nozzle 71 through the tower end plate 66;

[0052] The circulating assembly 05 comprises a water tank 100 and a backwater pipe 123, the backwater pipe 123 respectively communicates with the circulating liquid outlet 63 and the water tank 100, and the water tank 100 communicates with the connecting water pipe 72;

[0053] The tail gas treatment assembly 04 includes a tail gas pipe 81 and a tail gas treatment tank 82 for containing water, one end of the tail gas pipe 81 is connected to the tower end plate 66 and communicates with the collection cavity 70, and the other end of the tail gas pipe 81 communicates with the tail gas treatment tank 82.

[0054] A high-purity phosphorus reduction collection method, in which phosphorus trichloride and hydrogen gas are reacted and collected in a high-purity phosphorus reduction collection device, includes the following steps:

[0055] A reaction step, in which phosphorus trichloride and hydrogen gas are heated in the reaction assembly 01 to generate gaseous phosphorus and gaseous hydrochloric acid, and the gaseous phosphorus and gaseous hydrochloric acid enter the collection cavity 70 through the reaction inlet 65;

[0056] A cooling collection step, in which the water in the water tank 100 communicates with the nozzle 71 through the connecting water pipe 72, and the nozzle 71 sprays water to cool the gaseous phosphorus and gaseous hydrochloric acid to form liquid phosphorus 69 and liquid hydrochloric acid;

[0057] A separation step, in which the liquid phosphorus 69, liquid hydrochloric acid, and sprayed water flow downward into the separation cavity 59 under the action of gravity, and the liquid phosphorus 69, which has a large specific gravity, precipitates at the bottom of the separation cavity 59, the finished product valve 62 is opened, and the liquid phosphorus 69 is discharged from the finished product outlet 61 for storage, the liquid hydrochloric acid dissolves in water and is located above the liquid phosphorus 69, and is recycled to the water tank 100 through the circulating outlet 63 for use by the nozzle 71 for cooling and recycling;

[0058] A tail gas collection step, in which the tail gas treatment tank 82 contains water, and part of the gaseous hydrochloric acid enters the tail gas treatment tank 82 through the tail gas pipe 81 and dissolves in the water in the tail gas treatment tank 82.

[0059] The high-purity phosphorus reduction collection device and the collection method thereof, the phosphorus trichloride and the hydrogen gas are heated to produce gaseous phosphorus and gaseous hydrochloric acid in the reaction assembly 01. The device includes the reaction assembly 01, the collection tower 02, the spraying assembly, the circulation assembly 05 and the tail gas treatment assembly 04. These areas are connected by sealing to ensure that the entire device forms a closed space. Before production, the device will use inert gas to replace air to maintain a low oxygen content environment, thereby effectively preventing the reaction of yellow phosphorus and oxygen to cause combustion and improving production safety. The raw material phosphorus trichloride and hydrogen gas are injected into the reaction assembly 01, and the reaction assembly 01 heats the raw material. When the set temperature is reached, the raw material will undergo a hydrogenation reduction reaction to generate phosphorus vapor and hydrochloric acid gas. The phosphorus vapor and the hydrochloric acid gas then enter the collection cavity 70 through the reaction gas inlet. The collection tower 02 includes the tower body 64, the tower end plate 66 and the separation tank 60. The nozzle 71 in the spraying assembly 03 is connected to the collection cavity 70, and the water pipe 72 is connected to the water tank 100 and the nozzle 71. The liquid in the water tank 100 is sprayed into the collection cavity 70 through the nozzle 71 to cool the gaseous phosphorus. The phosphorus vapor is cooled and converted into liquid phosphorus 69. At the same time, the hydrochloric acid gas is dissolved in water to form hydrochloric acid aqueous solution. The liquid phosphorus 69 and the hydrochloric acid aqueous solution flow to the separation tank 60 under the action of gravity and are collected. The liquid phosphorus 69 then flows into the separation tank 60 with the water flow. The liquid phosphorus 69 and the hydrochloric acid aqueous solution are immiscible, and the liquid phosphorus 69 naturally deposits at the bottom of the separation tank 60 because its specific gravity is greater than that of the hydrochloric acid aqueous solution. The finished product valve 62 is opened, and the liquid phosphorus 69 flows out of the finished product outlet to realize collection, thereby realizing an efficient and pure collection process. The liquid phosphorus 69 is easy to store and transport. The hydrochloric acid aqueous solution at the upper part of the separation tank 60 enters the water tank 100 from the circulation liquid outlet 63 and is recycled. The tail gas treatment assembly 04 collects the uncollected hydrochloric acid gas again to ensure the environmental protection and safety of the production process. The collection method of the liquid phosphorus 69 is simple, reduces manual operation and improves collection efficiency.

[0060] Further, as Figures 2 to 6As shown, the reaction assembly 01 includes a main pipe body 10, a baffle 20, and a heating element 30 for heating the main pipe body 10, the main pipe body 10 is provided with a collection port 11, a raw material filling port 12, and a reaction cavity 15, the baffle 20 is located in the reaction cavity 15, the peripheral side of the baffle 20 is connected to the inner wall of the main pipe body 10, the upper part of the baffle 20 is provided with a reaction through hole 21, the baffle 20 divides the reaction cavity 15 to form a reaction zone 16 and a collection zone 17, the raw material filling port 12 is communicated with the reaction zone 16, the reaction zone 16 is communicated with the collection zone 17 through the reaction through hole 21, the collection zone 17 is communicated with the collection port 11, and the collection port 11 is communicated with a reaction gas inlet 65. The heating element 30 heats the main pipe body 10 to make the raw material reach the reaction temperature. The reaction cavity 15 is divided into the reaction zone 16 and the collection zone 17 along the axial direction by the baffle 20, the reaction zone 16 is communicated with the raw material filling port 12, the raw material phosphorus trichloride and hydrogen gas enter the reaction zone 16 through the raw material filling port 12 and react in the reaction zone 16, under the action of the baffle 20, the reactants are blocked when flowing out to the collection zone 17, the residence time of the reactants in the pipe is increased, the gas is more dispersed, the reaction is more sufficient, the yield of phosphorus vapor is improved, the production efficiency is improved, the residual raw material is reduced, and the production safety is improved. After the phosphorus trichloride is gasified, it enters the collection zone 17 through the reaction through hole 21 and is discharged from the collection port 11 to a collection cavity 70, so that the product phosphorus vapor is collected. Since the reaction assembly 01 mainly reduces phosphorus trichloride to obtain phosphorus vapor, the specific gravity of the gasified phosphorus trichloride is heavier than that of hydrogen, and most of it will deposit at the lower part of the main pipe body 10. The reaction through hole 21 is arranged at the upper part of the baffle 20, so that the flow of phosphorus trichloride gas is blocked, the reaction is more sufficient, and the utilization rate of raw materials is improved.

[0061] As one of the embodiments, the chemical reaction formula in the main pipe body 10 is: 2PCl3+3H2→2P+6HCl, and the gaseous phosphorus and gaseous hydrochloric acid are discharged from the collection port 11 to the collection cavity 70.

[0062] As one of the embodiments, as shown in Figures 3 to 5 The reaction through hole 21 is arranged at the upper part of the baffle 20, so that the flow of phosphorus trichloride gas is blocked, the reaction is more sufficient, and the utilization rate of raw materials is improved.

[0063] As one of the embodiments, as shown in Figures 2 to 3 The reaction through hole 21 is arranged at the upper part of the baffle 20, so that the flow of phosphorus trichloride gas is blocked, the reaction is more sufficient, and the utilization rate of raw materials is improved.

[0064] Further, as shown in Figures 2 to 6As shown, the main body comprises a reaction tube section 18 and a filling tube section 19, the reaction cavity 15 and the baffle 20 are located in the reaction tube section 18, the collection port 11 is located at one end of the reaction tube section 18, one end of the filling tube section 19 communicates with the other end of the reaction tube section 18, and the other end of the filling tube section 19 away from the reaction tube section 18 is provided with the raw material filling port 12. The reaction assembly 01 further comprises a first inner tube body 40 and a second inner tube body 50 located in the reaction tube section 18. One end of the first inner tube body 40 is connected to the baffle 20, and the other end has a first flow gap 41 with the end of the reaction tube section 18 away from the collection port 11. The second inner tube body 50 is connected to the end of the reaction tube section 18 away from the collection port 11. One end of the second inner tube body 50 extends into the first inner tube body 40 and has a second flow gap 51 with the baffle 20, and the other end communicates with the raw material filling port 12 through the filling tube section 19. The first inner tube body 40 and the second inner tube body 50 extend axially in the reaction tube section 18. The raw material enters the second inner tube body 50 from the raw material filling port 12, passes through the first flow gap 41 between the inner circumferential wall of the first inner tube body 40 and the outer circumferential wall of the second inner tube body 50, and then passes through the second flow gap 51 between the outer circumferential wall of the first inner tube body 40 and the inner circumferential wall of the reaction tube section 18, and then enters the collection area 17 through the reaction through hole 21, and then enters the collection cavity 70 of the tower main body 64 from the collection port 11. By arranging the first inner tube body 40 and the second inner tube body 50 in the reaction area 16, and inserting the second inner tube body 50 into the first inner tube body 40, the travel path of the reactants in the reaction tube section 18 is lengthened, and the reaction is more complete.

[0065] Further, as shown in Figures 4 to 5 The reaction through hole 21 is arranged between the outer wall of the first inner tube body 40 and the inner wall of the reaction tube section 18, so that all the reaction raw materials injected into the first inner tube body 40 through the second inner tube body 50 must pass through the second flow gap 51 before being discharged from the collection area 17, avoiding the reactants directly entering the collection area 17 from the reaction through hole 21 and being discharged, and ensuring that the reactants flow along the set travel path, ensuring the completeness of the reaction and improving the utilization rate of the raw materials.

[0066] Further, as shown in Figure 2As shown, the raw material filling port 12 includes a gas filling port 13 and a liquid filling port 14, and the liquid filling port 14 and the gas filling port 13 are communicated with the second inner tube body 50 away from the first inner tube body 40 through the filling pipe section 19 respectively. The raw material gas is filled through the gas filling port 13, and the raw material liquid is filled through the liquid filling port 14. The gas and the liquid are filled through separate filling ports at the same time, which improves the raw material operation efficiency and the production efficiency. The axial distance between the liquid filling port 14 and the baffle 20 is a, and the axial distance between the gas filling port 13 and the baffle 20 is b, b>a. The gas filling port 13 is located at the rear side of the liquid filling port 14. During the raw material filling, the liquid raw material is blown into the reaction cavity 15 by the gas, which improves the efficiency of the liquid raw material flowing to the reaction cavity 15.

[0067] As one of the embodiments, the liquid phosphorus trichloride in the raw material is added from the liquid filling port 14, and the hydrogen gas in the raw material is added from the gas filling port 13.

[0068] As one of the embodiments, as shown in Figure 5 The reaction assembly 01 further includes a first connecting part 52 and a second connecting part 42. One end of the first connecting part 52 is connected with the outer wall of the second inner tube body 50, and the other end is connected with the inner wall of the first inner tube body 40, which improves the connection strength of the first inner tube body 40 and the second inner tube body 50 and the relative position stability of the first inner tube body 40 and the second inner tube body 50. One end of the second connecting part 42 is connected with the outer wall of the first inner tube body 40, and the other end is connected with the inner wall of the reaction tube section 18. This improves the connection strength of the first inner tube body 40 and the reaction tube section 18 and the relative position stability of the first inner tube body 40 and the reaction tube section 18.

[0069] As one of the embodiments, as shown in Figure 3 and Figure 6 The collection port 11 is located below the filling port, and the collection port 11 is located outside the heating element 30. The main tube body 10 is inclined as a whole. Since the collection port 11 is located at a lower position, the product is condensed into a liquid state at the collection port 11, and the liquid product can smoothly flow out of the collection port 11 to the collection cavity of the tower main body for collection, thereby avoiding the blockage caused by the solidification of the collection port 11.

[0070] As one of the embodiments, as shown in Figure 3 and Figure 6 The heating element 30 surrounds the outer periphery of the main tube body 10, and the collection port 11 and the filling port of the main tube body 10 respectively protrude out of the heating element 30, which improves the heating uniformity of the main tube body 10. Preferably, the heating element 30 is a heating furnace.

[0071] Further, as shown in Figures 7 to 10As shown, the spraying assembly 03 further comprises a spraying dispersion plate 74 connected in the tower body 64, the spraying dispersion plate 74 is provided with a plurality of dispersion holes 76, and the spraying dispersion plate 74 is located between the nozzle 71 and the reaction gas inlet 65 in the height direction. The phosphorus vapor and gaseous hydrochloric acid enter the tower body 64 from the reaction gas inlet 65, and the spraying dispersion plate 74 is used to disperse the phosphorus vapor and slow down the gaseous flow rate, so that the spray sprayed by the nozzle 71 is in contact with the phosphorus vapor and gaseous hydrochloric acid through the dispersion hole 76, so that the cooling is more sufficient.

[0072] As one of the embodiments, as shown in the figure, Figures 8 to 9 As shown, the dispersion holes 76 are uniformly distributed on the spraying dispersion plate 74, which improves the dispersion effect of the phosphorus vapor and gaseous hydrochloric acid, and makes the cooling effect better.

[0073] As one of the embodiments, as shown in the figure, Figures 8 to 9 As shown, the upper end of the tower body 64 is connected with the tower end plate 66, and the spraying assembly 03 further comprises a spraying pipe 77 located in the tower body 64. One end of the spraying pipe 77 is connected to the tower end plate 66 and communicates with the connecting water pipe 72. A plurality of nozzles 71 are connected to the spraying pipe 77 in the height direction, and the plurality of nozzles 71 respectively communicate with the spraying pipe. The tower end plate 66 is connected to the upper end of the tower body 64 to realize the sealing of the upper end of the tower body 64. One end of the spraying pipe 77 is connected to the tower end plate 66 to realize the fixation of the spraying pipe 77. The spraying pipe 77 is connected with a plurality of nozzles 71 arranged at intervals in the height direction. One end of the spraying pipe communicates with the water tank 100 through the connecting water pipe 72, and the plurality of nozzles 71 respectively communicate with the spraying pipe, which improves the number of sprays sprayed by the nozzles 71 and improves the cooling efficiency. Further, the tower body is provided with a plurality of reaction gas inlets arranged at intervals in the height direction, and the tower body 64 extends in the height direction as a whole, so that the collection tower 02 and the reaction assembly 01 connected thereto are arranged in the height direction as a whole, thereby reducing the equipment floor area.

[0074] As one of the embodiments, as shown in the figure, Figures 8 to 9 As shown, the tower end plate 66 is connected with a dispersion connecting rod 67 extending in the height direction, one end of the dispersion connecting rod 67 is connected to the tower end plate 66, and the tower end plate 66 is connected with a plurality of spraying dispersion plates 74 at intervals in the height direction, and one spraying dispersion plate 74 is arranged below each nozzle 71. One end of the dispersion connecting rod 67 is connected to the tower end plate 66, and a plurality of spraying dispersion plates 74 are connected to the dispersion connecting rod 67 to realize the fixation of the plurality of spraying dispersion plates 74. The arrangement of the plurality of spraying dispersion plates 74 helps to reduce the flow rate of the phosphorus vapor and gaseous hydrochloric acid and improve the dispersion degree, so that the cooling is more sufficient.

[0075] As one of the embodiments, as shown in the figure, Figures 7 to 9As shown, the tower body 64 further comprises a collection temperature sensor 68 for measuring the temperature inside the tower body 64, the collection temperature sensor 68 is connected to the tower end plate 66 and at least a part of the collection temperature sensor 68 extends into the tower body 64. The temperature data inside the tower body 64 is obtained by the collection temperature sensor 68 so as to control the flow rate of the spray nozzles 71 properly to obtain better cooling effect.

[0076] As one of the embodiments, as shown in Figure 7 As shown, the lower end surface of the tower body 64 is located at the upper portion of the separation tank 60 and is lower than the circulating liquid outlet 63, and a product precipitation zone is formed between the lower end surface of the tower body 64 and the product outlet 61. The tower body 64 extends into the separation tank 60 through the upper end surface of the separation tank 60, and the outer peripheral surface of the tower body 64 is sealingly connected to the upper end surface of the separation tank 60 to ensure that the cooled liquid phosphorus 69 in the tower body 64 precipitates in the separation tank 60 under the action of gravity and prevents overflow. The sprayed liquid in the tower body 64 is not miscible with the liquid phosphorus 69, and the liquid phosphorus 69 has a relatively large specific gravity and precipitates in the product precipitation zone at the bottom of the separation tank 60. The liquid phosphorus 69 is discharged and collected from the product outlet 61 under the action of gravity. The sprayed liquid flows out of the water tank 100 through the circulating liquid outlet 63, so that the sprayed liquid can be recycled.

[0077] As one of the embodiments, the initial liquid in the water tank 100 is water, which is sprayed into the tower body 64 through the spray nozzles 71. The gaseous hydrochloric acid dissolves in the water and then drops and collects at the upper end of the separation tank 60, and then enters the water tank 100 through the circulating liquid outlet 63 and is recycled through the spray nozzles 71.

[0078] As one of the embodiments, as shown in Figure 9 As shown, the spray nozzles 71 are atomizing spray nozzles 71, which can spray a conical spray that can cover the radial cross section of the tower body 64. The radial cross section is perpendicular to the axis of the tower body 64.

[0079] Further, as shown in Figure 11As shown, the lower end of the tail gas treatment tank 82 is provided with a waste water discharge port 84 and a waste water discharge valve 85, the waste water discharge valve 85 is connected to the waste water discharge port 84, one end of the tail gas pipeline 81 is inserted into the tower main body 64 through the tower end plate 66 and communicates with the collection cavity 70, the other end of the tail gas pipeline 81 communicates with the tail gas treatment tank 82, and the upper end of the tail gas treatment tank 82 is provided with a tail gas discharge port 86 for discharging tail gas. The tail gas treatment tank 82 contains water, the gaseous hydrochloric acid in the tower main body 64 flows upward and enters the tail gas treatment tank 82 to form tail gas, the hydrochloric acid in the tail gas dissolves in the water in the tail gas treatment tank 82 to form waste water, the waste water in the tail gas treatment tank 82 opens the waste water discharge valve 85 and is discharged through the waste water discharge port 84. The upper end of the tail gas treatment tank 82 is provided with a tail gas discharge port 86 for discharging tail gas. If the water in the tail gas treatment tank 82 is saturated by absorbing tail gas, the tail gas is discharged from the tail gas discharge port 86. Or a small amount of phosphorus trichloride gas that is not completely reacted is discharged from the tail gas discharge port.

[0080] As one of the embodiments, as shown in Figure 11 The tail gas treatment assembly 04 further includes an anti-suck-back tank 87 and a tail gas insertion pipe 88 for inserting into the liquid in the tail gas treatment tank 82, the anti-suck-back tank 87 is provided with an upper interface 89 and a lower interface 90, the upper interface 89 is located at the upper part of the anti-suck-back tank 87 and communicates with the tail gas pipeline 81, the lower interface 90 is located at the lower part of the anti-suck-back tank 87 and communicates with the tail gas insertion pipe 88, and the upper end of the tail gas treatment tank 82 is provided with a tail gas inlet 83, the lower end of the tail gas insertion pipe 88 is inserted into the liquid in the tail gas treatment tank 82 through the tail gas inlet 83. The anti-suck-back tank 87 is located between the tail gas pipeline 81 and the tail gas treatment tank 82, the two ends of the anti-suck-back tank 87 respectively communicate with the tail gas pipeline 81 and the tail gas treatment tank 82, the gaseous phosphorus and gaseous hydrochloric acid in the tower main body 64 enter the tail gas treatment tank 82 through the anti-suck-back tank 87, the lower interface 90 of the anti-suck-back tank 87 is connected with the tail gas insertion pipe 88, the lower end of the tail gas insertion pipe 88 is inserted into the liquid in the tail gas treatment tank 82, which prevents negative pressure from being generated when the collection tower 02 fails, provides storage space for backflow waste water, and prevents the waste water in the tail gas treatment tank 82 from flowing back into the collection cavity 70.

[0081] Further, as shown in Figures 12 to 16As shown, the circulating assembly 05 further comprises a first partition 116 and at least two second partitions 117, the water tank 100 comprises a main tank body 101, a top plate 105 and a bottom plate 106, opposite sides of the main tank body 101 are respectively provided with a liquid inlet 109 and a liquid outlet 110, the liquid inlet 109 is communicated with the circulating liquid outlet 63, the liquid outlet 110 is communicated with the collecting cavity 70 through the connecting water pipe 72, the main tank body 101, the top plate 105 and the bottom plate 106 enclose to form a circulating cavity 102, the liquid inlet 109 and the liquid outlet 110 are respectively communicated with the circulating cavity 102, the first partition 116 and the second partition 117 are respectively connected in the circulating cavity 102 and located between the liquid inlet 109 and the liquid outlet 110, the bottom surface of the second partition 117 is connected with the bottom plate 106, the side surface of the second partition 117 is respectively connected with the side surface of the main tank body 101, the top surface of the second partition 117 forms an upper circulating channel 103 with the top plate 105, the adjacent second partitions 117 are arranged in a spaced manner along a first direction, the first partition 116 is located between two adjacent second partitions 117, the top surface of the first partition 116 is connected with the top plate 105, the side surface of the first partition 116 is connected with the side surface of the main tank body 101, and the bottom surface of the first partition 116 and the bottom plate 106 form a lower circulating channel 104. The backflow liquid for circulation enters the circulating cavity 102 through the liquid inlet 109. Among them, the liquid inlet 109, the upper circulating channel 103 close to the liquid inlet 109 side, the lower circulating channel 104, and the upper circulating channel 103 close to the liquid outlet 110 side and the liquid outlet 110 are communicated to form a liquid circulating flow channel. The circulating liquid flows in the circulating cavity 102 along the liquid circulating flow channel. The first partition 116 is connected to the top plate 105 and located between two second partitions 117, when the circulating liquid flows from the liquid inlet 109 into the upper circulating channel 103 and flows towards the liquid outlet 110, the circulating liquid flows downward from the upper circulating channel 103 into the lower circulating channel 104 under the blockage of the first partition 116, the solid particles in the circulating liquid precipitate between two adjacent second partitions 117 along the first partition 116, the circulating liquid continues to flow towards the liquid outlet 110, the circulating liquid flows upward from the lower circulating channel 104 into the upper circulating channel 103 close to the liquid outlet 110 side, the solid particles in the circulating liquid precipitate between two second partitions 117 under the self-weight, that is, the precipitation of solid particles is realized in the circulating cavity 102, and finally the circulating liquid flows out of the liquid outlet 110 to enter the next cooling circulation, thereby reducing the solid particles in the circulating liquid and avoiding the blockage of the nozzles of the spraying assembly.

[0082] As one of the embodiments, the upper part of the separation tank 60 collects the gaseous hydrochloric acid solution formed by dissolving the salt in water, and the hydrochloric acid solution flows out of the circulating liquid outlet 63 with a small part of liquid phosphorus 69, which is further cooled to form solid particles during entering the water tank 100.

[0083] As one of the embodiments, as shown in Figures 12 to 16 the top plate 105 is movably closed on the main box 101, the second partition plate 117 is movably inserted into the main box 101, and the liquid inlet 109 is located at the lower end of the main box 101. When cleaning the solid particles, the top plate 105 is opened and the second partition plate 117 is removed, so that the entire circulating cavity 102 is communicated with the liquid inlet 109, which facilitates the solid particles in the circulating cavity 102 to be cleaned and discharged from the liquid inlet 109, thereby improving the cleaning efficiency.

[0084] As one of the embodiments, as shown in Figures 12 to 16 the liquid supply port 110 is located at the upper middle part of the main box 101.

[0085] As one of the embodiments, as shown in Figures 13 to 14 the bottom plate 106 is arranged in a V shape, and the bottom surface of the second partition plate 117 is arranged in a shape corresponding to the shape of the bottom plate 106, so that the bottom surface of the second partition plate 117 is attached to the bottom plate 106, so as to ensure that the liquid inlet 109 is arranged at the bottom end of the bottom plate 106. The bottom plate 106 is arranged in a V shape, which promotes the solid particles to be deposited at the bottom end of the bottom plate 106, improves the deposition concentration of the solid particles, and improves the cleaning efficiency of the solid particles.

[0086] As one of the embodiments, as shown in Figure 13 , Figure 14 and Figure 16 the main box 101 is connected with a clamping through slot 118 extending in the height direction, the second partition plate 117 is movably inserted into the clamping through slot 118, and the bottom surface of the second partition plate 117 is movably abutted to the bottom plate 106. The clamping through slot 118 is located in the circulating cavity 102, and the installation position of the second partition plate 117 is limited by the clamping through slot 118 and the bottom plate 106. At the same time, since the second partition plate 117 is movably inserted into the clamping through slot 118 and movably abutted to the bottom surface, the assembly and disassembly of the second partition plate 117 are facilitated, and the cleaning efficiency of the solid particles is improved.

[0087] As one of the embodiments, as shown in Figure 13 , Figure 14 and Figure 16As shown, the main box body 101 is connected with a limiting groove 119 extending along the height direction, the lower end of the limiting groove 119 is provided with a limiting plate 120, the limiting plate 120 has a preset distance with the bottom plate 106, the first partition plate 116 is movably inserted into the limiting groove 119, the bottom surface of the first partition plate 116 movably abuts against the limiting plate 120, and the top surface of the first partition plate 116 movably abuts against the top plate 105. The installation position of the first partition plate 116 is limited by the limiting groove 119, and the connection in the circulating cavity 102 is realized. The limiting plate 120 limits the installation position of the bottom surface of the first partition plate 116, so that the lower circulating channel 104 is formed between the bottom surface of the first partition plate 116 and the bottom plate 106. Since the first partition plate 116 is movably inserted into the limiting groove 119 and the top surface movably abuts against the top plate 105, the assembly and disassembly of the first partition plate 116 are facilitated, and the cleaning efficiency of the solid particles is improved.

[0088] As one of the embodiments, as shown in Figure 16 The bottom plate 106 is inclined, one end of the bottom plate 106 towards the liquid supply port 110 is the first end 107, and the other end of the bottom plate 106 towards the liquid inlet port 109 is the second end 108. The first end 107 is higher than the second end 108. When cleaning the solid particles, the lower end of the bottom plate 106 is inclined towards the liquid inlet port 109, which promotes the cleaning and discharge of the solid particles.

[0089] Further, as shown in Figure 1 The liquid supply port 110 is connected with the first liquid supply pipe 111, the first liquid supply pipe 111 is communicated with the circulating cavity 102, the water pump 112 is connected on the first liquid supply pipe 111, the water outlet end of the water pump 112 is communicated with the connecting water pipe 72, the third liquid supply pipe 114 is connected with the top plate 105, the valve 115 is connected with the third liquid supply pipe 114, one end of the third liquid supply pipe 114 is communicated with the connecting water pipe 72, and the other end is communicated with the circulating cavity 102. The circulating liquid in the main box body 101 is supplied by the water pump 112. The delivery flow of the connecting water pipe 72 is controlled by the third liquid supply pipe 114 and the valve 115.

[0090] Further, as shown in Figure 1As shown, the circulating assembly 05 further comprises a heat exchanger 121, a controller and a circulating temperature sensor 122 for measuring the temperature of the circulating liquid in the circulating cavity 102, the measuring end of the circulating temperature sensor 122 is located in the circulating cavity 102, the inlet end of the heat exchanger 121 is used for communication with the circulating outlet, the outlet end of the heat exchanger 121 is in communication with the liquid inlet 109, and the heat exchanger 121 and the circulating temperature sensor 122 are respectively electrically connected with the controller. The temperature of the recovered liquid is reduced by the heat exchanger 121, so that the temperature of the circulating liquid discharged from the liquid supply port 110 meets the cooling demand. The circulating temperature sensor 122 obtains the temperature of the liquid in the circulating cavity 102 and feeds back to the controller, and the temperature of the heat exchanger 121 is controlled by the controller to improve the accuracy of the circulating liquid temperature control of the liquid supply port 110.

[0091] In summary, the embodiment of the present application provides a high-purity phosphorus reduction and collection device and a collection method thereof. Phosphorus trichloride and hydrogen gas are heated in the reaction assembly 01 to produce gaseous phosphorus and gaseous hydrochloric acid through a reduction reaction. The device includes a reaction assembly 01, a collection tower 02, a spraying assembly, a circulating assembly 05, and a tail gas treatment assembly 04. These areas are connected by airtight connection to ensure that the entire device forms a sealed space. Before production, inert gas is used to replace air in the device to maintain a low-oxygen environment, effectively preventing yellow phosphorus from reacting with oxygen to cause combustion and improving production safety. The raw materials, phosphorus trichloride and hydrogen gas, are injected into the reaction assembly 01, which heats the raw materials. When the set temperature is reached, the raw materials will undergo a hydrogenation reduction reaction to generate phosphorus vapor and hydrochloric acid gas. The phosphorus vapor and hydrochloric acid gas then enter the collection cavity 70 through the reaction gas inlet 65. The collection tower 02 includes a tower body 64, a tower end plate 66, and a separation tank 60. The nozzles 71 in the spraying assembly 03 are connected to the collection cavity 70, and the water pipes 72 are connected to the water tank 100 and the nozzles 71, respectively. The liquid in the water tank 100 is sprayed into the collection cavity 70 through the nozzles 71 to cool the gaseous phosphorus. The phosphorus vapor is cooled and converted into liquid phosphorus 69. At the same time, the hydrochloric acid gas dissolves in water to form an aqueous hydrochloric acid solution. The liquid phosphorus 69 and the aqueous hydrochloric acid solution flow to the separation tank 60 under the action of gravity and are collected. The liquid phosphorus 69 then flows into the separation tank 60 with the water flow. The liquid phosphorus 69 and the aqueous hydrochloric acid solution are immiscible, and the liquid phosphorus 69 naturally deposits at the bottom of the separation tank 60 because its specific gravity is greater than that of the aqueous hydrochloric acid solution. Opening the finished product valve 62, the liquid phosphorus 69 flows out of the finished product outlet to achieve collection, thereby realizing an efficient and pure collection process. The liquid phosphorus 69 is easy to store and transport. The aqueous hydrochloric acid solution at the upper part of the separation tank 60 is recycled after entering the water tank 100 through the water return pipe 123. The tail gas treatment assembly 04 collects the uncollected hydrochloric acid gas again to ensure the environmental protection and safety of the production process. The collection method of the liquid phosphorus 69 is simple, reducing manual operation and improving collection efficiency.

[0092] The above merely is the preferred embodiment of the present application, it should be pointed out that, for ordinary skilled in the art, without departing from the technical principles of the present application, can also make several improvements and replacements, these improvements and replacements also should be considered as the protection scope of the present application.

Claims

1. A high purity phosphorus reduction collection apparatus, characterized by: The reaction assembly, the collecting tower, the spraying assembly, the circulating assembly and the tail gas treatment assembly are included. The collecting tower includes a tower main body, a tower end plate and a separation tank, the upper end of the tower main body is sealingly connected with the tower end plate, the tower main body is provided with a collecting cavity and a reaction gas inlet, the reaction assembly is connected with the reaction gas inlet and communicates with the collecting cavity, the separation tank is provided with a separation cavity, a circulating liquid outlet, a product outlet and a product valve, the lower end of the tower main body is inserted into the separation cavity and sealingly connected with the separation tank, the circulating liquid outlet is located at the upper part of the separation tank, the product outlet is located at the lower part of the separation tank, the circulating liquid outlet and the product outlet respectively communicate with the separation cavity, and the product valve is connected with the product outlet. The spraying assembly includes a nozzle and a connecting water pipe, the nozzle is connected in the collecting cavity, and the reaction gas inlet is located between the nozzle and the lower end of the tower main body in the height direction. The circulating assembly includes a water tank and a backwater pipe, the backwater pipe respectively communicates with the circulating liquid outlet and the water tank, and the water tank communicates with the connecting water pipe. The tail gas treatment assembly includes a tail gas pipeline and a tail gas treatment tank for containing water, one end of the tail gas pipeline is connected with the tower end plate and communicates with the collecting cavity, and the other end of the tail gas pipeline communicates with the tail gas treatment tank. The circulating assembly further includes a first partition plate and at least two second partition plates, the water tank includes a main tank body, a top plate and a bottom plate, opposite sides of the main tank body are respectively provided with a liquid inlet and a liquid supply port, the liquid inlet communicates with the circulating liquid outlet through the backwater pipe, the liquid supply port communicates with the collecting cavity through the connecting water pipe, the main tank body, the top plate and the bottom plate enclose a circulating cavity, the liquid inlet and the liquid supply port respectively communicate with the circulating cavity, the first partition plate and the second partition plate are respectively connected in the circulating cavity and located between the liquid inlet and the liquid supply port, the bottom surface of the second partition plate is connected with the bottom plate, the side surface of the second partition plate is respectively connected with the side surface of the main tank body, the top surface of the second partition plate forms an upper circulating channel with the top plate, adjacent second partition plates are arranged in a first direction, the first partition plate is located between two adjacent second partition plates, the top surface of the first partition plate is connected with the top plate, the side surface of the first partition plate is connected with the side surface of the main tank body, and the lower circulating channel is formed between the bottom surface of the first partition plate and the bottom plate.

2. The high purity phosphorus reduction collection apparatus of claim 1, wherein: The reaction assembly includes a main pipe body, a baffle and a heating member for heating the main pipe body, the main pipe body is provided with a collecting port, a raw material filling port and a reaction cavity, the baffle is located in the reaction cavity, the peripheral side surface of the baffle is connected with the inner wall of the main pipe body, the upper part of the baffle is provided with a reaction through hole, the baffle divides the reaction cavity to form a reaction zone and a collecting zone, the raw material filling port communicates with the reaction zone, the reaction zone communicates with the collecting zone through the reaction through hole, the collecting zone communicates with the collecting port, and the collecting port communicates with the reaction gas inlet.

3. The high purity phosphorus reduction collection apparatus of claim 2, wherein: The main body comprises a reaction tube section and a filling tube section, the reaction cavity and the baffle are located in the reaction tube section, the collecting port is located at one end of the reaction tube section, one end of the filling tube section is communicated with the other end of the reaction tube section, and the other end of the filling tube section away from the reaction tube section is provided with a raw material filling port, the reaction assembly further comprises a first inner tube body and a second inner tube body located in the reaction tube section, one end of the first inner tube body is connected to the baffle, the other end of the first inner tube body has a first flow gap with the end of the reaction tube section away from the collecting port, the second inner tube body is connected to the end of the reaction tube section away from the collecting port, one end of the second inner tube body extends into the first inner tube body and has a second flow gap with the baffle, and the other end of the second inner tube body is communicated with the raw material filling port through the filling tube section.

4. The high purity phosphorus reduction collection apparatus of claim 3, wherein: The reaction through holes are all arranged between the outer wall of the first inner tube body and the inner wall of the reaction tube section.

5. The high purity phosphorus reduction collection apparatus of claim 3, wherein: The raw material filling port comprises a gas filling port and a liquid filling port, the liquid filling port and the gas filling port are respectively communicated with the end of the second inner tube body away from the first inner tube body through the filling tube section, the axial distance between the liquid filling port and the baffle is a, the axial distance between the gas filling port and the baffle is b, and b>a.

6. The high purity phosphorus reduction trap of claim 1, wherein: The spraying assembly further comprises a spraying dispersion plate connected in the tower main body, the spraying dispersion plate is provided with a plurality of dispersion through holes, and the spraying dispersion plate is located between the nozzle and the reaction gas inlet in the height direction.

7. The high purity phosphorus reduction collection apparatus of claim 6, wherein: The lower end of the tail gas treatment tank is provided with a wastewater discharge port and a wastewater discharge valve, the wastewater discharge valve is connected to the wastewater discharge port, one end of the tail gas pipeline is inserted into the tower main body through the tower end plate and communicated with the collecting cavity, the other end of the tail gas pipeline is communicated with the tail gas treatment tank, and the upper end of the tail gas treatment tank is provided with a tail gas discharge port for discharging tail gas.

8. The high purity phosphorus reduction trap of claim 1, wherein: The liquid supply port is connected with a first liquid supply pipe, the first liquid supply pipe is communicated with the circulating cavity, a water pump is connected to the first liquid supply pipe, the water outlet end of the water pump is communicated with the connecting water pipe, the top plate is connected with a third liquid supply pipe, the third liquid supply pipe is connected with a valve, one end of the third liquid supply pipe is communicated with the connecting water pipe, and the other end of the third liquid supply pipe is communicated with the circulating cavity.

9. A high purity phosphorus reduction collection method, characterized by: Phosphorus trichloride and hydrogen are reacted and collected in the high-purity phosphorus reduction collection device according to any one of claims 1-8, comprising the following steps: In the reaction step, phosphorus trichloride and hydrogen are heated in the reaction assembly to generate gaseous phosphorus and gaseous hydrochloric acid, and the gaseous phosphorus and gaseous hydrochloric acid enter the collecting cavity through the reaction gas inlet; In the cooling and collecting step, the water in the water tank is communicated with the nozzle through the connecting water pipe, and the nozzle sprays water to cool the gaseous phosphorus and gaseous hydrochloric acid to form liquid phosphorus and liquid hydrochloric acid; The separation step, the liquid phosphorus, the liquid hydrochloric acid and the sprayed water flow downward into the separation cavity under the action of gravity, the liquid phosphorus is precipitated at the bottom of the separation cavity, the finished product valve is opened, the liquid phosphorus is discharged from the finished product outlet to storage, the liquid hydrochloric acid is dissolved in water and is located above the liquid phosphorus, and is recycled to the water tank through the circulating liquid outlet for use by the nozzle for cooling and recycling; The tail gas collection step, the tail gas treatment tank contains water, part of the gaseous hydrochloric acid enters the tail gas treatment tank through the tail gas pipeline, and is dissolved in the water in the tail gas treatment tank.

Citation Information

Patent Citations

  • Collecting tower for high-purity phosphorus

    CN222400836U