Device and method for producing phosphorus oxychloride using phosphorus trichloride

By using a stirring and mixing assembly and a rapid cooling assembly device in the production process of oxychloride, the problem of temperature fluctuations of reactors is solved, the yield and purity of oxychloride are improved, and the equipment cost is reduced.

CN115608296BActive Publication Date: 2025-08-29HUNAN HENGGUANG CHEM
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Patent Information

Application Number
CN202211243322.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-10-11
Publication Date
2025-08-29
Estimated Expiration
2042-10-11

AI Technical Summary

Technical Problem

In the prior art, the temperature of the reactor is difficult to maintain within an appropriate range during the production process of oxychloride, resulting in a decrease in output. The existing devices lack automatic temperature control devices, which poses safety hazards.

Method used

Using a device including a stirring and mixing assembly and a fast cooling assembly, the mixing rod is driven by a dual-axis motor, and the reactor temperature is automatically controlled through the rapid cooling assembly, and the distillation tower and the condensation tower are combined for purification and condensation treatment.

Benefits of technology

The production of oxychloride and the purity of purity have been improved, avoiding the safety hazards of excessive temperature and reducing equipment costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a device and method for producing phosphorus oxychloride using phosphorus trichloride. The device comprises a refining kettle, wherein a stirring and mixing assembly is provided in the refining kettle. The stirring and mixing assembly comprises a dual-shaft motor, a driving component, and two stirring rods. The driving component is transmission-connected to an output shaft at the bottom of the dual-shaft motor, and the two stirring rods are both transmission-connected to the driving component. A spiral cooling channel is provided in the inner wall of the refining kettle. In the invention, the stirring rods can both rotate along corresponding rotation axes and revolve around the transmission shafts, thereby fully mixing a mixture in the refining kettle and improving the yield and utilization rate of phosphorus trichloride. The rapid cooling assembly can automatically control the temperature in the refining kettle, thereby maintaining a stable reaction temperature and maintaining the production temperature of the crude phosphorus trichloride product within an appropriate range. This not only prevents the temperature in the refining kettle from being too high and causing danger, but also improves the yield of phosphorus oxychloride.
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Description

Technical Field

[0001] The invention relates to the field of wood product processing equipment, in particular to a device and method for producing phosphorus oxychloride by utilizing phosphorus trichloride. Background Art

[0002] Phosphorus oxychloride, as an important chemical product, is the main raw material for the production of halogen-free plastic flame retardants, plasticizers, pesticides, insecticides, and herbicides. Electronic-grade phosphorus oxychloride with extremely low iron and arsenic content is also an essential raw material in the solar industry, integrated circuits, separation devices, and optical fiber preform production, and has broad market prospects. Currently, the main processes used for phosphorus oxychloride production at home and abroad include PC13 chlorination hydrolysis, PC15 synthesis, and the more advanced phosphorus trichloride direct oxidation method. The most widely used direct oxidation method requires adding yellow phosphorus, phosphorus trichloride mother liquor, and chlorine gas to a reactor to react and form phosphorus trichloride.

[0003] The temperature of the reactor will also rise rapidly. In order to prevent the risk of the reactor exploding, the reactor is cooled in the existing technology. For example, patent publication number CN110898455A discloses a phosphorus trichloride refining device and process, which includes a reactor, a chiller, and a distillation tower. The reactor, chiller, and distillation tower are arranged from left to right, and further include: a cooling mechanism, which is detachably mounted on the outer wall of the reactor; and two cooling water pipes, one end of each of which is connected to the water inlet and outlet of the chiller, respectively, and the other end of each of the cooling water pipes is connected to the cooling mechanism. This invention allows the heat dissipation tube to fully absorb heat from the reactor, thereby preventing the reactor from exploding due to excessive temperature during use.

[0004] However, although this patent can cool the reactor, in the actual production process, the temperature inside the reactor will fluctuate and it is difficult to maintain it within an appropriate range. Regardless of whether the temperature inside the reactor is too high or too low, the output of phosphorus oxychloride will be reduced.

[0005] Therefore, we propose a device and method for producing phosphorus oxychloride using phosphorus trichloride to solve the above problems. Summary of the Invention

[0006] The object of the present invention is to provide an apparatus and method for producing phosphorus oxychloride using phosphorus trichloride, so as to solve the problem mentioned in the above background art that there is currently no designated apparatus for drop resistance testing of wood products, it is difficult to have a uniform standard for the drop height, and the drop test requires manual pushing to a platform at a certain height, which is very labor-intensive.

[0007] To achieve the above object, the present invention provides the following technical solutions:

[0008] A device for producing phosphorus oxychloride by utilizing phosphorus trichloride comprises:

[0009] A refining kettle, a distillation tower is provided beside the refining kettle, and the discharge port at the top of the refining kettle is connected to the feed port of the distillation tower;

[0010] A stirring and mixing assembly is provided in the refining kettle, the stirring and mixing assembly comprising a dual-shaft motor, a driving component and two stirring rods, the dual-shaft motor is vertically arranged on the top of the refining kettle, the driving component is transmission-connected to the output shaft at the bottom of the dual-shaft motor, the two stirring rods are spaced apart at the bottom of the driving component, and the two stirring rods are transmission-connected to the driving component, and a spiral cooling channel is opened in the inner wall of the refining kettle;

[0011] A rapid cooling component is arranged beside the refining kettle. The rapid cooling component includes a coolant storage tank, a conveying component, a heat dissipation component and a plurality of heat conduction plates. The coolant storage tank is arranged beside the refining kettle through a fixed platform. A closing plate is provided on the top of the coolant storage tank. Multiple heat conduction plates are arranged at intervals in the coolant storage tank, and each of the heat conduction plates passes through the closing plate. The coolant storage tank is filled with coolant, and the conveying component is used to convey the coolant to the spiral cooling channel.

[0012] In a further embodiment, the driving component includes a fixed plate, a fixed gear, a rotating plate, a transmission shaft and two driven gears. The transmission shaft is connected to the output shaft at the bottom of the dual-shaft motor through a coupling. The fixed plate is fixedly connected to the inner wall of the refining kettle, the top of the fixed gear is fixedly connected to the bottom of the fixed plate, the rotating plate is fixedly connected to the bottom of the transmission shaft, and both ends of the rotating plate are rotatably connected to a rotating shaft, each rotating shaft corresponds to a driven gear, each driven gear is fixedly connected to the corresponding rotating shaft, and the two driven gears are engaged with the fixed gear.

[0013] In a further embodiment, the driving component further includes a plurality of stirring rods, each of the stirring rods corresponds to a rotating shaft, each of the stirring rods is arranged at the bottom of the corresponding rotating shaft, and the plurality of stirring rods are spaced apart and distributed on the outer walls of two of the stirring rods.

[0014] In a further embodiment, the conveying component includes a conveying pipe, a pressure pipe, a driving member and a sealing piston. The conveying pipe is arranged on the top of the closing plate. Both side openings of the conveying pipe are provided with a one-way valve. The pressure pipe is fixedly connected to the conveying pipe, and the pressure pipe is communicated with the conveying pipe. The sealing piston slides and cooperates with the inner wall of the pressure pipe.

[0015] In a further embodiment, the input end of the delivery pipe is connected to the interior of the coolant storage tank through a liquid extraction pipe, the output end of the delivery pipe is connected to the top opening of the spiral cooling channel through a liquid outlet pipe, and the bottom opening of the spiral cooling channel is connected to the interior of the coolant storage tank through a return pipe.

[0016] In a further embodiment, the driving member includes a controller, an L-shaped bracket, a linkage shaft, an eccentric block and a push rod. The L-shaped bracket is fixedly connected to the top of the conveying pipe, the linkage shaft rotates on the L-shaped bracket, and a one-way bearing is provided on the output shaft at the top of the dual-axis motor. The one-way bearing and the linkage shaft are connected through the one-way bearing. The eccentric block is fixedly connected to the bottom of the linkage shaft, one end of the push rod is hinged to the end of the eccentric block away from the linkage shaft, and the other end of the push rod is hinged to the sealing piston.

[0017] In a further embodiment, the heat dissipation component includes a support frame, a connecting shaft and a cooling fan, the support frame is fixedly connected to the top of the L-shaped bracket, the connecting shaft is rotatably connected to the support frame, the connecting shaft is transmission-connected to the linkage shaft, and the cooling fan is arranged at one end of the connecting shaft away from the linkage shaft.

[0018] In a further embodiment, a temperature sensor is provided in the refining kettle, and the temperature sensor and the dual-axis motor are both electrically connected to the controller.

[0019] In a further embodiment, a condensation tower is provided next to the distillation tower, a spiral cooling tube is provided in the condensation tower, the top opening of the spiral cooling tube is connected to the discharge port of the distillation tower, an oxidation kettle is provided next to the condensation tower, and the bottom opening of the spiral cooling tube is connected to the feed port of the oxidation kettle.

[0020] The present invention also discloses a method for producing phosphorus oxychloride by utilizing phosphorus trichloride, comprising the following steps:

[0021] S1: introducing a mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine into a refining kettle, stirring and mixing them thoroughly with two stirring rods, and reacting to form a crude phosphorus trichloride product;

[0022] S2: The rapid cooling component automatically controls the temperature in the refining kettle to keep the reaction temperature stable:

[0023] S3: The distillation tower performs distillation and purification on the crude phosphorus trichloride to remove impurities in the crude phosphorus trichloride:

[0024] S4: A condensation tower condenses and collects the rectified phosphorus trichloride, and introduces the purified phosphorus trichloride into an oxidation kettle;

[0025] S5: Adding oxygen into the oxidation kettle to oxidize phosphorus trichloride, and finally obtaining pure phosphorus oxychloride.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] First, in the present invention, the rapid cooling component can automatically control the temperature in the refining kettle, so that the reaction temperature remains stable, and thus the production temperature of the crude phosphorus trichloride product can be maintained within an appropriate range. This not only prevents the temperature in the refining kettle from being too high and causing danger, but also further increases the output of phosphorus oxychloride.

[0028] Secondly, in the present invention, the two stirring rods in the stirring and mixing assembly can, under the action of the dual-axis motor, not only rotate along the corresponding rotating axes, but also revolve around the transmission shaft as the center, which can fully mix the mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine in the refining kettle, thereby improving the yield and utilization rate of phosphorus trichloride.

[0029] Third, in the present invention, the distillation tower can be used to purify the crude phosphorus trichloride by distillation, and impurities such as iron and arsenic in the crude phosphorus trichloride can be removed. The condensation tower can condense and collect the rectified phosphorus trichloride, and introduce the purified phosphorus trichloride into the oxidation kettle, and oxygen is added to the oxidation kettle to oxidize the phosphorus trichloride. Compared with the existing technology, the purity of the phosphorus oxychloride finally obtained by this device will be greatly improved.

[0030] Fourthly, in the present invention, when the dual-axis motor rotates clockwise, since a one-way bearing is provided on the output shaft at the top of the dual-axis motor, the linkage shaft does not rotate at this time, and the refining kettle will not be cooled, thereby avoiding unnecessary energy waste. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0032] Figure 2 Schematic diagram of the internal structure of the refining kettle in the present invention;

[0033] Figure 3 for Figure 2 A magnified view of point A in the figure;

[0034] Figure 4 Schematic diagram of the structure of the stirring rod in the present invention;

[0035] Figure 5 for Figure 4 Enlarged view of point B in FIG.

[0036] Figure 6 Schematic diagram of the structure of the heat conducting plate in the present invention;

[0037] Figure 7 Schematic diagram of the structure of the sealing piston in the present invention;

[0038] Figure 8 It is a structural schematic diagram of the V-shaped groove in the present invention.

[0039] In the figure: 1. refining kettle; 2. fixed table; 3. coolant storage tank; 4. distillation tower; 6. condensing tower; 7. oxidation kettle; 8. closing plate; 10. dual-axis motor; 11. reflux pipe; 12. liquid outlet pipe; 13. synchronous belt; 15. heat conduction plate; 16. conveying pipe; 17. liquid extraction pipe; 18. linkage shaft; 19. support frame; 20. L-shaped bracket; 21. connecting shaft; 22. cooling fan; 23. spiral cooling channel; 24. stirring rod; 25. stirring rod; 26. transmission shaft; 27. fixed plate; 28. fixed gear; 29. ​​rotating plate; 30. rotating shaft; 31. driven gear; 32. pressurizing pipe; 33. one-way valve; 34. push rod; 35. sealing piston; 36. eccentric block; 37. spiral cooling pipe; 40. one-way bearing. DETAILED DESCRIPTION

[0040] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0041] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integral connections; mechanical connections or electrical connections; direct connections or indirect connections through an intermediate medium; and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0042] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0043] Example 1

[0044] See also Figures 1-8 In an embodiment of the present invention, a device for producing phosphorus oxychloride using phosphorus trichloride includes a refining kettle 1, a distillation tower 4 is provided on the side of the refining kettle 1, a discharge port at the top of the refining kettle 1 is connected to a feed port of the distillation tower 4, a stirring and mixing assembly is provided in the refining kettle 1, and the stirring and mixing assembly includes a dual-axis motor 10, a driving component and two stirring rods 24, the dual-axis motor 10 is vertically arranged at the top of the refining kettle 1, the driving component is transmission-connected to the output shaft at the bottom of the dual-axis motor 10, the two stirring rods 24 are spaced apart at the bottom of the driving component, and the two stirring rods 24 are transmission-connected to the driving component, and a spiral cooling channel 23 is opened in the inner wall of the refining kettle 1;

[0045] In the present invention, the two stirring rods 24 in the stirring and mixing assembly can, under the action of the dual-axis motor 10, not only rotate along the corresponding rotating shaft 30, but also revolve around the transmission shaft 26 as the center, so as to fully mix the mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine gas in the refining kettle 1, thereby improving the yield and utilization rate of phosphorus trichloride.

[0046] In a further embodiment, the driving component includes a fixed plate 27, a fixed gear 28, a rotating plate 29, a transmission shaft 26 and two driven gears 31, the transmission shaft 26 is transmission-connected to the output shaft at the bottom of the dual-shaft motor 10 through a coupling, the fixed plate 27 is fixedly connected to the inner wall of the refining kettle 1, the top of the fixed gear 28 is fixedly connected to the bottom of the fixed plate 27, the rotating plate 29 is fixedly connected to the bottom of the transmission shaft 26, both ends of the rotating plate 29 are rotatably connected to a rotating shaft 30, each rotating shaft 30 corresponds to a driven gear 31, each driven gear 31 is fixedly connected to the corresponding rotating shaft 30, and the two driven gears 31 are meshed with the fixed gear 28, the driving component also includes a plurality of stirring rods 25, each stirring rod 24 corresponds to a rotating shaft 30, each stirring rod 24 is arranged at the bottom of the corresponding rotating shaft 30, and a plurality of stirring rods 25 are distributed at intervals on the outer walls of the two stirring rods 24;

[0047] When the dual-axis motor 10 rotates clockwise or counterclockwise, the driving shaft can drive the rotating plate 29 to rotate, thereby causing the two rotating shafts 30 located on the rotating plate 29 to rotate. At this time, the two stirring rods 24 at the bottom of the two rotating shafts 30 will revolve around the driving shaft. Since the top of the fixed gear 28 is fixedly connected to the bottom of the fixed plate 27, when the two stirring rods 24 revolve around the driving shaft, the two stirring rods 24 will also rotate around the rotating shaft 30 under the action of the two driven gears 31. By arranging multiple stirring rods 25 on the outer wall of each stirring rod 24, the stirring range of the stirring rod 24 can be improved.

[0048] A rapid cooling component is provided beside the refining kettle 1. The rapid cooling component includes a coolant storage tank 3, a conveying component, a heat dissipation component, and a plurality of heat conducting plates 15. The coolant storage tank 3 is provided beside the refining kettle 1 through a fixed platform 2. A closing plate 8 is provided on the top of the coolant storage tank 3. The plurality of heat conducting plates 15 are arranged in the coolant storage tank 3 at intervals, and each of the heat conducting plates 15 passes through the closing plate 8. The coolant storage tank 3 is filled with coolant, and the conveying component is used to convey the coolant to the spiral cooling channel 23.

[0049] In the present invention, the rapid cooling component can automatically control the temperature in the refining kettle 1, so that the reaction temperature remains stable, and thus the production temperature of the crude phosphorus trichloride product can be maintained within an appropriate range. This not only prevents the temperature in the refining kettle 1 from being too high and causing danger, but also further increases the yield of phosphorus oxychloride.

[0050] In a further embodiment, the conveying component includes a conveying pipe 16, a pressurizing pipe 32, a driving member and a sealing piston 35. The conveying pipe 16 is arranged at the top of the closing plate 8. Both side openings of the conveying pipe 16 are provided with a one-way valve 33. The pressurizing pipe 32 is fixedly connected to the conveying pipe 16, and the pressurizing pipe 32 is communicated with the conveying pipe 16. The sealing piston 35 slides and cooperates with the inner wall of the pressurizing pipe 32. The input end of the conveying pipe 16 is communicated with the interior of the coolant storage tank 3 through a liquid extraction pipe 17. The output end of the conveying pipe 16 is communicated with the top opening of the spiral cooling channel 23 through a liquid outlet pipe 12. The bottom opening of the spiral cooling channel 23 is connected to the coolant storage tank 3 through a reflux pipe 11. The driving member includes a controller, an L-shaped bracket 20, a linkage shaft 18, an eccentric block 36 and a push rod 34. The L-shaped bracket 20 is fixedly connected to the top of the conveying pipe 16, and the linkage shaft 18 rotates on the L-shaped bracket 20. A one-way bearing 40 is provided on the output shaft at the top of the dual-axis motor 10. The one-way bearing 40 and the linkage shaft 18 are connected by the one-way bearing 40. The eccentric block 36 is fixedly connected to the bottom of the linkage shaft 18. One end of the push rod 34 is hinged to the end of the eccentric block 36 away from the linkage shaft 18, and the other end of the push rod 34 is hinged to the sealing piston 35. A temperature sensor is provided in the refining kettle 1, and the temperature sensor and the dual-axis motor 10 are electrically connected to the controller.

[0051] When the dual-axis motor 10 rotates clockwise, since a one-way bearing 40 is provided on the output shaft at the top of the dual-axis motor 10, the linkage shaft 18 does not rotate at this time, thereby avoiding unnecessary energy waste. When the temperature sensor detects that the temperature in the refining kettle 1 is too high, the controller controls the dual-axis motor 10 to rotate counterclockwise. At this time, the synchronous belt 13 drives the linkage shaft 18 to rotate, and then drives the sealing piston 35 to reciprocate in the pressurized pipe 32 through the eccentric block 36. Since both side openings of the delivery pipe 16 are provided with a one-way valve 33, the coolant in the coolant storage tank 3 will continuously flow through the refining kettle 1. The spiral cooling channel 23 opened in the inner wall of the kettle 1 can realize rapid cooling of the refining kettle 1. When the temperature inside the refining kettle 1 is cooled to an appropriate temperature, the controller will make the dual-axis motor 10 rotate clockwise again, and the cooling of the refining kettle 1 can be stopped at this time. In this way, the automatic control of the temperature inside the refining kettle 1 can be completed, and no additional power source is required. The above control process can be completed only by the dual-axis motor 10, which can effectively reduce the manufacturing cost of the equipment. The model of the controller is C8051F020 single-chip microcomputer, and the model of the temperature sensor is THM-D20E.

[0052] In a further embodiment, the heat dissipation component includes a support frame 19, a connecting shaft 21, and a heat dissipation fan 22. The support frame 19 is fixedly connected to the top of the L-shaped bracket 20. The connecting shaft 21 is rotatably connected to the support frame 19. The connecting shaft 21 is transmission-connected to the linkage shaft 18. The heat dissipation fan 22 is arranged at an end of the connecting shaft 21 away from the linkage shaft 18.

[0053] When the dual-axis motor 10 rotates counterclockwise, it can not only circulate the coolant, but also drive the cooling fan 22 to rotate through the connecting shaft 21. The high temperature in the coolant storage tank 3 will be discharged through the multiple heat conduction plates 15, and the cooling fan 22 can accelerate the air flow between the multiple heat conduction plates 15, thereby achieving the cooling of the coolant in the coolant storage tank 3, so that the coolant can always be kept at a low temperature.

[0054] In a further embodiment, a condensation tower 6 is provided beside the distillation tower 4, and a spiral cooling pipe 37 is provided in the condensation tower 6, and the top opening of the spiral cooling pipe 37 is connected to the discharge port of the distillation tower 4. An oxidation kettle 7 is provided beside the condensation tower 6, and the bottom opening of the spiral cooling pipe 37 is connected to the feed port of the oxidation kettle 7;

[0055] The distillation tower 4 can distill and purify the crude phosphorus trichloride to remove impurities such as iron and arsenic in the crude phosphorus trichloride, while the condensation tower 6 can condense and collect the rectified phosphorus trichloride and introduce the purified phosphorus trichloride into the oxidation kettle 7. Oxygen is added to the oxidation kettle 7 to oxidize the phosphorus trichloride. Compared with the existing technology, the purity of the phosphorus oxychloride finally obtained by this device will be greatly improved.

[0056] Example 2

[0057] See also Figures 1-8 , which is different from Example 1 in that: the present invention also discloses a method for producing phosphorus oxychloride using phosphorus trichloride, comprising the following steps:

[0058] S1: introducing a mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine into a refining kettle 1, and after being fully stirred and mixed by two stirring rods 24, a crude phosphorus trichloride product is formed after reaction;

[0059] S2: The rapid cooling component automatically controls the temperature in the refining kettle 1 to keep the reaction temperature stable:

[0060] S3: The distillation tower 4 performs distillation and purification on the crude phosphorus trichloride to remove impurities in the crude phosphorus trichloride:

[0061] S4: The condensation tower 6 condenses and collects the rectified phosphorus trichloride, and introduces the purified phosphorus trichloride into the oxidation kettle 7;

[0062] S5: adding oxygen to the oxidation kettle 7 to oxidize phosphorus trichloride, and finally obtaining pure phosphorus oxychloride.

[0063] The working principle of the present invention is as follows: a mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine is introduced into a refining kettle 1, and after being fully stirred and mixed by two stirring rods 24, a crude phosphorus trichloride product is formed after reaction;

[0064] When the dual-axis motor 10 rotates clockwise or counterclockwise, the driving shaft can drive the rotating plate 29 to rotate, thereby causing the two rotating shafts 30 located on the rotating plate 29 to rotate. At this time, the two stirring rods 24 at the bottom of the two rotating shafts 30 will revolve around the driving shaft as the center. Since the top of the fixed gear 28 is fixedly connected to the bottom of the fixed plate 27, when the two stirring rods 24 revolve around the driving shaft as the center, the two stirring rods 24 will also rotate around the rotating shaft 30 as the center under the action of the two driven gears 31, thereby fully mixing the mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine gas in the refining kettle 1 to improve the yield and utilization rate of phosphorus trichloride. By arranging multiple stirring rods 25 on the outer wall of each stirring rod 24, the stirring range of the stirring rod 24 can be increased.

[0065] When the dual-axis motor 10 rotates clockwise, since a one-way bearing 40 is provided on the output shaft at the top of the dual-axis motor 10, the linkage shaft 18 does not rotate at this time, thereby avoiding unnecessary energy waste. When the temperature sensor detects that the temperature in the refining kettle 1 is too high, the controller controls the dual-axis motor 10 to rotate counterclockwise. At this time, the synchronous belt 13 drives the linkage shaft 18 to rotate, and then drives the sealing piston 35 to reciprocate in the pressurized pipe 32 through the eccentric block 36. Since both side openings of the delivery pipe 16 are provided with a one-way valve 33, the cold The coolant in the coolant storage tank 3 will continuously flow through the spiral cooling channel 23 opened in the inner wall of the refining kettle 1, thereby realizing rapid cooling of the refining kettle 1. When the temperature in the refining kettle 1 is cooled to an appropriate temperature, the controller will make the dual-axis motor 10 rotate clockwise again, and the cooling of the refining kettle 1 will be stopped at this time. In this way, the automatic control of the temperature in the refining kettle 1 can be completed, and no additional power source is required. The above control process can be completed only by the dual-axis motor 10, which can effectively reduce the manufacturing cost of the equipment.

[0066] The distillation tower 4 can distill and purify the crude phosphorus trichloride to remove impurities such as iron and arsenic in the crude phosphorus trichloride, while the condensation tower 6 can condense and collect the rectified phosphorus trichloride and introduce the purified phosphorus trichloride into the oxidation kettle 7. Oxygen is added to the oxidation kettle 7 to oxidize the phosphorus trichloride. Compared with the existing technology, the purity of the phosphorus oxychloride finally obtained by this device will be greatly improved.

[0067] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be included therein. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

[0068] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A device for producing phosphorus oxychloride using phosphorus trichloride, comprising: A refining kettle (1), a distillation tower (4) is provided on the side of the refining kettle (1), and a discharge port at the top of the refining kettle (1) is connected to a feed port of the distillation tower (4); A stirring and mixing assembly is arranged in a refining kettle (1), the stirring and mixing assembly comprising a dual-shaft motor (10), a driving component, and two stirring rods (24), the dual-shaft motor (10) being vertically arranged on the top of the refining kettle (1), the driving component being in driving connection with the output shaft at the bottom of the dual-shaft motor (10), the two stirring rods (24) being arranged at intervals at the bottom of the driving component, the two stirring rods (24) being in driving connection with the driving component, and a spiral cooling channel (23) being provided in the inner wall of the refining kettle (1); A rapid cooling component is arranged beside the refining kettle (1), and the rapid cooling component includes a coolant storage tank (3), a conveying component, a heat dissipation component, and a plurality of heat conduction plates (15). The coolant storage tank (3) is arranged beside the refining kettle (1) through a fixed platform (2). A closing plate (8) is arranged on the top of the coolant storage tank (3). The plurality of heat conduction plates (15) are arranged in the coolant storage tank (3) at intervals, and each of the heat conduction plates (15) penetrates the closing plate (8). The coolant storage tank (3) is filled with coolant, and the conveying component is used to convey the coolant to the spiral cooling channel (23); The conveying component includes a conveying pipe (16), a pressurizing pipe (32), a driving member and a sealing piston (35); the conveying pipe (16) is arranged on the top of the closing plate (8); both side openings of the conveying pipe (16) are provided with a one-way valve (33); the pressurizing pipe (32) is fixedly connected to the conveying pipe (16), and the pressurizing pipe (32) is communicated with the conveying pipe (16); the sealing piston (35) slides and cooperates with the inner wall of the pressurizing pipe (32); The input end of the delivery pipe (16) is connected to the interior of the coolant storage tank (3) through a liquid extraction pipe (17), the output end of the delivery pipe (16) is connected to the top opening of the spiral cooling channel (23) through a liquid outlet pipe (12), and the bottom opening of the spiral cooling channel (23) is connected to the interior of the coolant storage tank (3) through a return pipe (11); The driving member includes a controller, an L-shaped bracket (20), a linkage shaft (18), an eccentric block (36) and a push rod (34), wherein the L-shaped bracket (20) is fixedly connected to the top of the conveying pipe (16), the linkage shaft (18) rotates on the L-shaped bracket (20), a one-way bearing (40) is provided on the output shaft at the top of the dual-axis motor (10), the one-way bearing (40) and the linkage shaft (18) are connected to each other via a synchronous belt (13), the eccentric block (36) is fixedly connected to the bottom of the linkage shaft (18), one end of the push rod (34) is hinged to the end of the eccentric block (36) away from the linkage shaft (18), and the other end of the push rod (34) is hinged to the sealing piston (35); The heat dissipation component includes a support frame (19), a connecting shaft (21) and a heat dissipation fan (22), wherein the support frame (19) is fixedly connected to the top of the L-shaped bracket (20), the connecting shaft (21) is rotatably connected to the support frame (19), the connecting shaft (21) is transmission-connected to the linkage shaft (18), and the heat dissipation fan (22) is arranged at one end of the connecting shaft (21) away from the linkage shaft (18); A temperature sensor is provided in the refining kettle (1), and the temperature sensor and the dual-axis motor (10) are both electrically connected to the controller.

2. A device for producing phosphorus oxychloride using phosphorus trichloride according to claim 1, characterized in that: The driving component includes a fixed plate (27), a fixed gear (28), a rotating plate (29), a transmission shaft (26) and two driven gears (31), wherein the transmission shaft (26) is connected to the output shaft at the bottom of the dual-shaft motor (10) through a coupling, the fixed plate (27) is fixedly connected to the inner wall of the refining kettle (1), the top of the fixed gear (28) is fixedly connected to the bottom of the fixed plate (27), the rotating plate (29) is fixedly connected to the bottom of the transmission shaft (26), and both ends of the rotating plate (29) are rotatably connected to a rotating shaft (30), each rotating shaft (30) corresponds to a driven gear (31), each driven gear (31) is fixedly connected to the corresponding rotating shaft (30), and the two driven gears (31) are meshed with the fixed gear (28).

3. A device for producing phosphorus oxychloride using phosphorus trichloride according to claim 2, characterized in that: The driving component further includes a plurality of stirring rods (25), each stirring rod (24) corresponds to a rotating shaft (30), each stirring rod (24) is arranged at the bottom of the corresponding rotating shaft (30), and the plurality of stirring rods (25) are distributed at intervals on the outer walls of two stirring rods (24).

4. A device for producing phosphorus oxychloride using phosphorus trichloride according to claim 1, characterized in that: A condensation tower (6) is provided beside the distillation tower (4), a spiral cooling pipe (37) is provided in the condensation tower (6), and the top opening of the spiral cooling pipe (37) is connected to the discharge port of the distillation tower (4); an oxidation kettle (7) is provided beside the condensation tower (6), and the bottom opening of the spiral cooling pipe (37) is connected to the feed port of the oxidation kettle (7).

5. A method for producing phosphorus oxychloride using phosphorus trichloride, comprising the device for producing phosphorus oxychloride using phosphorus trichloride according to any one of claims 1 to 4, characterized in that: The following steps are involved: S1: introducing a mixture of yellow phosphorus, phosphorus trichloride mother liquor and chlorine into a refining kettle (1), stirring and mixing them thoroughly with two stirring rods (24), and reacting to form a crude phosphorus trichloride product; S2: The rapid cooling component automatically controls the temperature in the refining kettle (1) to keep the reaction temperature stable: S3: The distillation tower (4) performs distillation and purification on the crude phosphorus trichloride to remove impurities in the crude phosphorus trichloride: S4: The condensation tower (6) condenses and collects the rectified phosphorus trichloride, and introduces the purified phosphorus trichloride into the oxidation kettle (7); S5: Adding oxygen to the oxidation kettle (7) to oxidize phosphorus trichloride, and finally obtaining pure phosphorus oxychloride.

Citation Information

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