A reaction separation device for preparing phosphorus oxyfluoride

Abstract

The present invention discloses a reaction separation device for preparing phosphorus oxytrifluoride, comprising: a reaction separation tower body, wherein a feed zone, a plurality of reaction zones, and a separation zone are sequentially arranged from the lower end of the reaction separation tower body upward, wherein the feed zone and the separation zone are fixedly filled with a first packing layer, and the reaction zone is filled with a second packing layer; a heat exchange mechanism, comprising a heat exchange medium inlet container and a heat exchange medium outlet container, wherein the heat exchange medium inlet container and the heat exchange medium outlet container are respectively uniformly provided with a plurality of heat exchange pipes on the periphery thereof, wherein the heat exchange pipes are respectively longitudinally connected with a heat exchange medium circulation pipe pre-buried in the second packing layer; a plurality of heat exchange medium inlet pipes, wherein corresponding drive pipes are respectively installed at the discharge end thereof for rotating upward; and a plurality of heat exchange medium outlet pipes. The present invention can effectively improve the uniformity of the reaction temperature in each reaction zone and ensure that the material has a sufficiently uniform distribution effect when slowly flowing through the reaction zone.

Description

Technical Field

[0001] The present invention relates to the field of industrial equipment for preparing phosphorus oxyfluoride, in particular to reaction and separation equipment for preparing phosphorus oxyfluoride. Background Art

[0002] Currently, phosphorus oxyfluoride (POF3) is a colorless gas with a pungent odor under normal conditions, emitting faint smoke in the air. The primary method for preparing POF3 is to react CaF2 with anhydrous sulfurous acid to produce CaF(SO3F), which then reacts with H3PO4 to form the intermediate product POF3. However, since CaF2 is a solid, continuous production is difficult, the process is complex, and the production cost is high. Furthermore, the generated CaSO4 can pollute the environment and must be treated. Therefore, a method for preparing POF3 of higher purity using industrial phosphoric acid and anhydrous hydrogen fluoride as raw materials through continuous reactive distillation has begun to be studied and applied.

[0003] In the actual application of the method for preparing high-purity phosphorus oxyfluoride by continuous reactive distillation, it was found that due to the use of the method of reaction before separation, the equipment for preparing phosphorus oxyfluoride is numerous and complicated. Moreover, in the reactive distillation tower, since industrial phosphoric acid is a liquid and anhydrous hydrogen fluoride is a gas, the industrial phosphoric acid and anhydrous hydrogen fluoride have little contact time with each other during the two-phase contact process through the tower plates, resulting in insufficient reaction between the industrial phosphoric acid and anhydrous hydrogen fluoride. Therefore, a cyclic reaction must be achieved by controlling reflux, which increases the energy consumption of the production reaction. Therefore, in the actual production process, the applicant has designed a phosphorus oxyfluoride reaction and separation integrated preparation tower (patent application number CN202510154810.0), which effectively solves the problem of insufficient contact between industrial phosphoric acid and anhydrous hydrogen fluoride during the reaction process, and can also effectively separate high-purity phosphorus oxyfluoride, thereby reducing the energy consumption of phosphorus oxyfluoride production and lowering production costs.

[0004] However, in actual use, the integrated phosphorus oxyfluoride reaction and separation tower has a problem: because the heat exchange tubes of the shell-and-tube heat exchanger located in the reaction zone are evenly distributed and fixed in position, the spacing between the heat exchange tubes is required to be relatively large to ensure the convenient loading of the packing layer in the reaction zone. As a result, the temperature of the entire reaction zone can only be maintained by increasing the temperature of the heat exchange medium. This will cause the reaction temperature near the heat exchange tubes to be higher, resulting in insufficient uniformity of the reaction temperature throughout the reaction zone, which will adversely affect the reaction process. The provision of a swirl distributor at the bottom of each reaction zone improves the uniform distribution of the reaction materials to a certain extent. However, in order to ensure that the materials can achieve a good distribution effect when passing through the swirl distributor, the pressure of the materials passing through the swirl distributor must be relatively high. Obviously, this is unreasonable for the phosphorus oxyfluoride synthesis process.

[0005] Therefore, the research purpose of the present invention is to design a reaction separation equipment for preparing phosphorus oxyfluoride that can effectively and significantly improve the uniformity of reaction temperature in each reaction zone and ensure that the material can still have a sufficiently uniform distribution effect when slowly flowing through each reaction zone, thereby effectively ensuring the controllability of the reaction process and improving the reaction effect. Summary of the Invention

[0006] In view of the technical problems existing in the above-mentioned prior art, the present invention provides a reaction and separation device for preparing phosphorus oxyfluoride, which can effectively solve the technical problems existing in the above-mentioned prior art.

[0007] The technical solution of the present invention is:

[0008] A reaction and separation device for preparing phosphorus oxyfluoride, comprising:

[0009] A reaction and separation tower body, wherein a feed zone, a plurality of reaction zones, and a separation zone are sequentially arranged upward from the lower end of the reaction and separation tower body, wherein the feed zone and the separation zone are respectively fixedly filled with corresponding first packing layers upward through corresponding fixed support plates, and the reaction zones are respectively filled with corresponding second packing layers upward through corresponding movable support plates;

[0010] The heat exchange mechanism includes a heat exchange medium inlet container fixedly mounted at the center of the movable support plate, and a heat exchange medium outlet container fixedly disposed on the upper middle side of the second packing layer. A plurality of corresponding heat exchange pipes are uniformly distributed outward at equal angles around the peripheries of the heat exchange medium inlet container and the heat exchange medium outlet container. Heat exchange medium flow pipes pre-buried in the second packing layer are longitudinally connected between the heat exchange pipes. Heat exchange medium flow pipes connected to different heat exchange pipes are staggered.

[0011] A plurality of heat exchange medium inlet pipes are respectively extended into the interior of the reaction and separation tower body, and corresponding drive pipes are respectively installed at the discharge ends of the heat exchange medium inlet pipes for upward rotation. The end of the drive pipe not connected to the heat exchange medium inlet pipe movably passes through the movable support plate and is rotatably installed at the center of the corresponding heat exchange medium inlet container, and the discharge end thereof is horizontally tilted outward and folded in a constricted shape. The inner side wall of the heat exchange medium inlet container is respectively provided with bevel teeth facing the discharge end of the drive pipe at a position not connected to the heat exchange pipe;

[0012] A plurality of heat exchange medium discharge pipes respectively extend through the interior of the reaction separation tower body, and the feed ends of the heat exchange medium discharge pipes are respectively rotatably mounted to the center of the corresponding heat exchange medium discharge container.

[0013] The reaction and separation tower body is fixedly connected with a plurality of main supporting protrusions respectively located at the lower side of the movable supporting plate, and corresponding first plane bearings are respectively installed between the bottom of the movable supporting plate and the main supporting protrusions.

[0014] Auxiliary support ridges spaced apart from the main support ridges are fixedly connected to the reaction separation tower body at the lower side of the main support ridges, and the auxiliary support ridges are fixedly connected upward to corresponding support frames through second plane bearings. The driving pipe passes through and is fixed to the middle part of the support frame, and a plurality of support balls are rollingly installed on the upper end of the support frame, with the top ends abutting against the bottom side of the movable support plate.

[0015] A plurality of corresponding dispersion guide plates are fixedly and obliquely connected to the support frame respectively; during reaction, the heat exchange medium enters the driving pipe through the heat exchange medium inlet pipe, and is pressurized at the discharge end of the driving pipe and then sprayed out horizontally and obliquely outward, so as to form an impact force on the helical teeth on the inner wall of the heat exchange medium entering the container, thereby driving the heat exchange mechanism and the second packing layer to rotate as a whole; the reaction force generated in the process of pressurizing and spraying the heat exchange medium along the discharge end of the driving pipe simultaneously drives the driving pipe to rotate in the opposite direction to the heat exchange mechanism and the second packing layer, thereby actively dispersing the material flowing through the dispersion guide plate.

[0016] The heat exchange medium inlet pipe and the driving pipe, the driving pipe and the heat exchange medium inlet container, and the heat exchange medium discharge pipe and the heat exchange medium discharge container are rotatably connected through corresponding waterproof sealing bearings.

[0017] The reaction and separation tower body is provided with an anhydrous hydrogen fluoride feed port located at the bottom side of the feed zone, the reaction and separation tower body is also provided with an industrial phosphoric acid feed port located at the upper side of the reaction zone, and the top of the reaction and separation tower body is provided with a product discharge port for discharging synthetic phosphorus oxytrifluoride gas.

[0018] A liquid material redistributor for evenly distributing the industrial phosphoric acid material is provided at the lower side of the discharge end of the industrial phosphoric acid feed port.

[0019] There are two reaction zones, wherein the reaction temperature of the lower reaction zone is controlled at 80-100°C, and the temperature of the upper reaction zone is controlled at 100-120°C.

[0020] The reaction separation tower body is provided with a structural redistributor at the upper part of the separation zone, and the reaction separation tower body is provided with a wire mesh demister at the upper part of the structural redistributor.

[0021] The discharge ends of the heat exchange pipes connected to the heat exchange medium discharge container are respectively tilted, and the tilting direction of the discharge ends of the heat exchange pipes is opposite to the tilting direction of the driving pipes, and the discharge ends of the heat exchange pipes are respectively fixed with corresponding limiting ring plates, and corresponding fixed protrusions are respectively fixed on the heat exchange pipes on the inner sides of the limiting ring plates, and corresponding water-permeable ring plates are movably installed on the outer sides of the fixed protrusions through connecting springs, and a plurality of corresponding water-permeable holes are evenly distributed on the water-permeable ring plates, and corresponding jet pipes are respectively arranged outward in a bucket shape at the centers of the water-permeable ring plates, and a photoelectric sensor for detecting the rotational speed of the second packing layer is provided in the reaction separation tower body, and the heat exchange medium inlet pipe is connected to an external material source through a flow-adjustable pump.

[0022] Advantages of the present invention:

[0023] 1) The present invention first improves the design of the heat exchange mechanism, which includes a heat exchange medium inlet container fixedly installed at the center of the movable support plate, and a heat exchange medium discharge container fixedly set on the upper side of the middle part of the second packing layer, and then the heat exchange pipe and the heat exchange medium circulation pipe staggered on different heat exchange pipes are intervened to achieve uniform circulation of the heat exchange medium; then the drive pipe is installed at the feed end of the heat exchange medium inlet pipe, and the end of the drive pipe that is not connected to the heat exchange medium inlet pipe is rotated and installed at the center of the corresponding heat exchange medium inlet container; the most important thing is that the discharge end of the drive pipe is tilted and folded horizontally outward and arranged in a constricted shape, and at the same time, the inner side wall of the heat exchange medium inlet container is respectively provided with bevel teeth facing the discharge end of the drive pipe.

[0024] During the reaction, the heat exchange medium enters the drive pipe through the heat exchange medium inlet pipe and is pressurized at the discharge end of the drive pipe before being ejected horizontally and outwardly, creating an impact force on the helical teeth on the inner wall of the heat exchange medium entry container, thereby driving the heat exchange mechanism and the second packing layer to rotate as a whole, and this rotation is low-speed. This can effectively circulate the circulating heat source around the entire reaction zone, greatly improving the uniformity of the reaction temperature within the reaction zone, thereby effectively improving the controllability of the reaction process and enhancing the reaction effect. Moreover, this low-speed rotation not only does not cause excessive wall hanging of the material, but can significantly increase the uniform distribution of the material within the second packing layer, thereby helping to improve the reaction effect of the material.

[0025] 2) The present invention utilizes a main support lip provided on the reaction and separation tower body in conjunction with a first planar bearing to provide a rotatable mounting for the movable support plate. To compensate for the lack of support stability associated with the rotatable mounting of the movable support plate, the present invention further secures auxiliary support lip portions to the reaction and separation tower body below the main support lip portions. These auxiliary support lip portions are securely connected upward to corresponding support frames via second planar bearings. The upper ends of the support frames are rollingly mounted with multiple support balls, whose top ends abut against the bottom side of the movable support plate. As the movable support plate rotates, the support frame provides fixed support at its bottom, effectively maintaining the support stability of the movable support plate and ensuring the practical effects of the present invention.

[0026] 3) The drive tube of the present invention extends through and is affixed to the middle of the support frame, to which a plurality of corresponding dispersion guide plates are affixed at an angle. During the reaction, the reaction force generated by the pressurized discharge of the heat exchange medium along the discharge end of the drive tube simultaneously drives the drive tube to rotate in the opposite direction of the heat exchange mechanism and the second packing layer, thereby actively dispersing the material flowing through the dispersion guide plates. This ensures that the material is sufficiently evenly distributed as it slowly flows through the various reaction zones, effectively further ensuring the controllability of the reaction process and improving the reaction effect.

[0027] 4) The heat exchange mechanism of the present invention, the rotation drive of the second packing layer, and the reverse rotation drive of the support frame provided with the dispersion guide plate are mostly powered by the liquid thrust generated by the circulation of the heat exchange medium. No additional power mechanism is required, thereby effectively reducing the manufacturing cost and operation and maintenance cost of the equipment.

[0028] 5) The discharge ends of the heat exchange conduits connected to the heat exchange medium discharge container of the present invention are respectively inclined, and their inclination direction is opposite to the inclination direction of the drive pipe, and the discharge ends of the devices are respectively fixedly connected to corresponding limiting ring plates, and the heat exchange conduits on the inner sides of the limiting ring plates are respectively fixedly connected to corresponding fixed protrusions, and the outer sides of the fixed protrusions are movably mounted with corresponding water-permeable ring plates through connecting springs, and a plurality of corresponding water-permeable holes are evenly distributed on the water-permeable ring plates, and corresponding spray pipes are respectively provided outward in a bucket shape at the center of the water-permeable ring plates. Under normal circumstances, the heat exchange medium is output through the water permeable holes of the water permeable ring plate and the jet holes of the jet pipe. When the photoelectric sensor detects that the rotation speed of the second packing layer in the reaction separation tower body is lower than the set value, the power of the flow-adjustable pump is increased to increase the circulation volume of the heat exchange medium, thereby increasing the circulation speed and pressure of the heat exchange medium, so as to drive the water permeable ring plate and the jet pipe to be pushed outward and abut against the limiting ring plate, so that the water permeable holes on the water permeable ring plate are closed, thereby forming a jet through the jet pipe to assist in increasing the rotation speed of the second packing layer in the reaction separation tower body, thereby effectively improving the practical effect of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a structural schematic diagram of the present invention.

[0030] Figure 2 It is a structural diagram of the heat exchange mechanism.

[0031] Figure 3 This is a structural diagram of the movable support plate installed on the upper side of the main support convex edge.

[0032] Figure 4 for Figure 3 A partial enlarged view of part A in .

[0033] Figure 5 This is a structural diagram of the heat exchange medium discharge pipe in Example 2 being installed in the heat exchange medium discharge container.

[0034] Figure 6 This is a schematic structural diagram of the discharge end of the heat exchange pipe in Example 2.

[0035] In the figure: reaction separation tower body 1, feed zone 101, reaction zone 102, separation zone 103, fixed support plate 2, first packing layer 3, movable support plate 4, second packing layer 5, heat exchange mechanism 6, heat exchange medium inlet container 601, heat exchange medium outlet container 602, heat exchange conduit 603, heat exchange medium circulation pipe 604, heat exchange medium inlet pipe 7, drive pipe 8, bevel gear 9, heat exchange medium outlet pipe 10, main support flange 11, first flat Surface bearing 12, auxiliary supporting ridge 13, second plane bearing 14, supporting frame 15, supporting ball 16, dispersion guide plate 17, waterproof sealed bearing 18, anhydrous hydrogen fluoride feed port 19, industrial phosphoric acid feed port 20, product discharge port 21, liquid material redistributor 22, structural redistributor 23, wire mesh demister 24, waste material outlet 25, limiting ring plate 26, fixed ridge 27, connecting spring 28, permeable ring plate 29, and jet pipe 30. DETAILED DESCRIPTION

[0036] To facilitate understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings.

[0037] Example 1:

[0038] refer to Figure 1-4 , a reaction and separation device for preparing phosphorus oxyfluoride, comprising:

[0039] A reaction and separation tower body 1, wherein a feed zone 101, a plurality of reaction zones 102, and a separation zone 103 are sequentially arranged upward from the lower end of the reaction and separation tower body 1. The feed zone 101 and the separation zone 103 are respectively filled with corresponding first packing layers 3 fixed upward through corresponding fixed support plates 2, and the reaction zone 102 is respectively filled with corresponding second packing layers 5 upward through corresponding movable support plates 4;

[0040] The heat exchange mechanism 6 includes a heat exchange medium inlet container 601 fixedly mounted at the center of the movable support plate 4, and a heat exchange medium outlet container 602 fixedly disposed on the upper middle side of the second packing layer 5. A plurality of corresponding heat exchange pipes 603 are uniformly distributed outward at equal angles around the periphery of the heat exchange medium inlet container 601 and the heat exchange medium outlet container 602. Heat exchange medium circulation pipes 604 pre-buried in the second packing layer 5 are longitudinally connected between the heat exchange pipes 603. The heat exchange medium circulation pipes 604 connected to different heat exchange pipes 603 are staggered.

[0041] Several heat exchange medium inlet pipes 7 extend through the interior of the reaction and separation tower body 1, and corresponding drive pipes 8 are respectively installed at the discharge ends of the heat exchange medium inlet pipes 7 so as to rotate upward. The end of the drive pipe 8 not connected to the heat exchange medium inlet pipe 7 movably passes through the movable support plate 4 and is rotatably installed at the center of the corresponding heat exchange medium inlet container 601, and its discharge end is horizontally tilted and folded outward and is arranged in a constricted shape. Bevel teeth 9 facing the discharge end of the drive pipe 8 are respectively provided on the inner side wall of the heat exchange medium inlet container 601 where the heat exchange conduit 603 is not connected;

[0042] A plurality of heat exchange medium discharge pipes 10 extend through the interior of the reaction separation tower body 1 , and the feed ends of the heat exchange medium discharge pipes 10 are rotatably mounted to the center of the corresponding heat exchange medium discharge container 602 .

[0043] The present invention first improves the design of the heat exchange mechanism 6, which includes a heat exchange medium inlet container 601 fixedly installed at the center of the movable support plate 4, and a heat exchange medium discharge container 602 fixedly set on the upper side of the middle part of the second packing layer 5, and then the heat exchange pipe 603 and the heat exchange medium circulation pipe 604 staggered on different heat exchange pipes 603 are intervened to realize the uniform circulation of the heat exchange medium; then the driving pipe 8 is installed at the feed end of the heat exchange medium inlet pipe 7, and the end of the driving pipe 8 that is not connected to the heat exchange medium inlet pipe 7 is rotated and installed at the center of the corresponding heat exchange medium inlet container 601; the most important thing is that the discharge end of the driving pipe 8 is horizontally tilted outward and arranged in a constricted shape. At the same time, the inner side wall of the heat exchange medium inlet container 601 is respectively provided with bevel teeth 9 facing the discharge end of the driving pipe. During the reaction, the heat exchange medium enters the drive pipe 8 through the heat exchange medium inlet pipe 7, and is pressurized at the discharge end of the drive pipe 8 and then ejected horizontally and outwardly, so as to form an impact force on the helical teeth 9 on the inner wall of the heat exchange medium inlet container 601, thereby driving the heat exchange mechanism 6 and the second packing layer 5 to rotate as a whole, and the rotation is a low-speed rotation. In this way, the circulating heat source can be effectively circulated around the entire reaction zone 102 to greatly improve the uniformity of the reaction temperature in the reaction zone 102, thereby effectively improving the controllability of the reaction process and improving the reaction effect. Moreover, this low-speed rotation not only does not cause the material to form excessive wall hanging phenomenon, but can significantly increase the uniform distribution effect of the material in the second packing layer 5, thereby helping to improve the reaction effect of the material.

[0044] The reaction and separation tower body 1 is fixed with a plurality of main support protrusions 11 located at the lower side of the movable support plate 4 , and corresponding first plane bearings 12 are respectively installed between the bottom of the movable support plate 4 and the main support protrusions 11 .

[0045] Auxiliary support ridges 13 spaced apart from the main support ridges 11 are fixedly connected to the reaction separation tower body 1 at the lower side of the main support ridges 11. The auxiliary support ridges 13 are fixedly connected upward to corresponding support frames 15 through second plane bearings 14. The driving pipe 8 passes through and is fixed to the middle of the support frame 15. The upper end of the support frame 15 is rollingly mounted with a plurality of support balls 16 whose top ends abut against the bottom side of the movable support plate 4.

[0046] The present invention forms a rotatable mounting for the movable support plate 4 by cooperating the main support ridge 11 and the first plane bearing 12 provided on the reaction and separation tower body 1. To compensate for the insufficient support stability of the rotatable mounting of the movable support plate 4, the present invention further fixes auxiliary support ridges 13 on the reaction and separation tower body 1 below the main support ridge 11. The auxiliary support ridges 13 are respectively fixed upwardly to corresponding support frames 15 through second plane bearings 14. The upper end of the support frame 15 is rollingly mounted with a plurality of support balls 16, the top ends of which abut against the bottom side of the movable support plate 4. As the movable support plate 4 rotates, the support frame 15 forms a fixed track support for it at its bottom, thereby effectively maintaining the support stability of the movable support plate 4 and ensuring the practical effect of the present invention.

[0047] A plurality of corresponding dispersion guide plates 17 are fixedly and obliquely connected to the support frame 15; during reaction, the heat exchange medium enters the driving pipe 8 through the heat exchange medium inlet pipe 7, and is pressurized at the discharge end of the driving pipe 8 and then sprayed out horizontally and obliquely outward, so as to form an impact force on the helical teeth 9 on the inner wall of the heat exchange medium entry container 601, thereby driving the heat exchange mechanism 6 and the second packing layer 5 to rotate as a whole; the reaction force generated in the process of pressurizing and spraying the heat exchange medium along the discharge end of the driving pipe 8 simultaneously drives the driving pipe 8 to rotate in the opposite direction to the heat exchange mechanism 6 and the second packing layer 5, thereby actively dispersing the material flowing through the dispersion guide plate 17.

[0048] The drive pipe 8 of the present invention passes through and is fixed to the middle portion of the support frame 15, to which a plurality of corresponding dispersion guide plates 17 are fixedly and obliquely attached. During the reaction, the reaction force generated by the pressurized discharge of the heat exchange medium along the discharge end of the drive pipe 8 simultaneously drives the drive pipe 8 to rotate in the opposite direction to the heat exchange mechanism 6 and the second packing layer 5, thereby actively dispersing the material flowing through the dispersion guide plates 17. This ensures that the material is sufficiently evenly distributed as it slowly flows through each reaction zone 102, thereby effectively further ensuring the controllability of the reaction process and improving the reaction effect.

[0049] The heat exchange medium inlet pipe 7 and the driving pipe 8, the driving pipe 8 and the heat exchange medium inlet container 601, and the heat exchange medium discharge pipe 10 and the heat exchange medium discharge container 602 are rotationally connected through corresponding waterproof sealing bearings 18.

[0050] The heat exchange mechanism 6, the rotation drive of the second packing layer 5, and the reverse rotation drive of the support frame 15 provided with the dispersion guide plate 17 of the present invention mostly use the liquid thrust generated by the circulation of the heat exchange medium. There is no need to add other power mechanisms, which can effectively reduce the production cost and operation and maintenance cost of the equipment.

[0051] The reaction and separation tower body 1 is provided with an anhydrous hydrogen fluoride feed port 19 located at the bottom of the feed zone 101. It is also provided with an industrial phosphoric acid feed port 20 located above the reaction zone 102. A product outlet 21 for synthesized phosphorus oxytrifluoride gas is located at the top of the reaction and separation tower body 1. A liquid material distributor 22 is located below the discharge end of the industrial phosphoric acid feed port 20 to evenly distribute the industrial phosphoric acid material. Two reaction zones 102 are provided, with the reaction temperature of the lower reaction zone 102 controlled at 80-100°C, and the temperature of the upper reaction zone 102 controlled at 100-120°C.

[0052] During the reaction, industrial phosphoric acid is fed through the industrial phosphoric acid feed port 20 and is evenly dispersed into the upper reaction zone 102 by the liquid-material redistributor 22. Anhydrous hydrogen fluoride gas enters through the anhydrous hydrogen fluoride feed port 19 and is actively dispersed into the lower reaction zone 102 by the rotatable support frame 15 and dispersion guide plate 17. The evenly distributed industrial phosphoric acid and anhydrous hydrogen fluoride fully contact and react within the second packing layer 5 of the reaction zone 102. The phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer 3 in the separation zone 103 and then enters the next process through the product outlet 21. Excess industrial phosphoric acid liquid and a small amount of residual side reaction liquid can be regularly discharged through the waste outlet 25 at the bottom of the reaction and separation tower body 1 for centralized collection and treatment.

[0053] The reaction separation tower body 1 is provided with a structural redistributor 23 at the upper portion of the separation zone 103 , and the reaction separation tower body 1 is provided with a wire mesh demister 24 at the upper portion of the structural redistributor 23 .

[0054] The first packing layer 3 of the upper separation zone 103 increases the resistance and path of the rising phosphorus oxytrifluoride gas. Therefore, the mist of industrial phosphoric acid entrained in the rising phosphorus oxytrifluoride gas is accumulated and absorbed through contact with the surface of the first packing layer 3 and then refluxes into the reaction zone 102 after sedimentation. Therefore, the separation zone 103 can effectively separate the mist of phosphorus oxytrifluoride and the entrained industrial phosphoric acid, thereby improving the purity of the phosphorus oxytrifluoride product. In addition, a structural redistributor 23 and a wire mesh demister 24 are provided at the upper part of the reaction and separation tower body 1. The industrial phosphoric acid entrained in the phosphorus oxytrifluoride can be further removed by the wire mesh demister, and the captured mist and generated liquid enter the separation zone 103 through the structural redistributor 22 to achieve gas-liquid separation.

[0055] Example 2:

[0056] refer to Figure 5-6, the difference between this embodiment and the first embodiment is that: the discharge ends of the heat exchange pipes 603 connected to the heat exchange medium discharge container 602 are respectively inclined, and the inclination direction of the discharge ends of the heat exchange pipes 603 is opposite to the inclination direction of the drive pipe 8, and the discharge ends of the heat exchange pipes 603 are respectively fixedly connected to corresponding limiting ring plates 26, and corresponding fixed protrusions 27 are respectively fixedly connected to the heat exchange pipes 603 on the inner sides of the limiting ring plates 26. The outer sides of the fixed protrusions 27 are movably mounted with corresponding water-permeable ring plates 29 through connecting springs 28. A plurality of corresponding water-permeable holes are evenly distributed on the water-permeable ring plates 29, and corresponding spray pipes 30 are respectively provided outwardly in a bucket shape at the centers of the water-permeable ring plates 29. A photoelectric sensor (not marked) for detecting the rotation speed of the second packing layer 5 is provided in the reaction and separation tower body 1, and the heat exchange medium inlet pipe 7 is connected to an external material source through a flow-adjustable pump (not marked).

[0057] Under normal circumstances, the heat exchange medium is output through the water permeable holes of the water permeable ring plate 29 and the jet holes of the jet pipe 30. When the photoelectric sensor detects that the rotation speed of the second packing layer 5 in the reaction separation tower body 1 is lower than the set value, the power of the flow-adjustable pump is increased to increase the circulation volume of the heat exchange medium, thereby increasing the circulation speed and pressure of the heat exchange medium, so as to drive the water permeable ring plate 29 and the jet pipe 30 to be pushed outward and abut against the limit ring plate 26, so that the water permeable holes on the water permeable ring plate 29 are closed, thereby forming a jet through the jet pipe 30 to assist in increasing the rotation speed of the second packing layer 5 in the reaction separation tower body 1, thereby effectively improving the practical effect of the present invention.

[0058] It should be noted that the implementation principle and technical effects of this embodiment are the same as those of the first embodiment. For the sake of brief description, for matters not mentioned in this embodiment, reference may be made to the corresponding content in the first embodiment.

[0059] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A reaction and separation device for preparing phosphorus oxyfluoride, characterized in that: Includes: A reaction separation tower body (1), wherein a feed zone (101), a plurality of reaction zones (102), and a separation zone (103) are sequentially arranged upward from the lower end of the reaction separation tower body (1); the feed zone (101) and the separation zone (103) are respectively filled with corresponding first packing layers (3) fixed upward through corresponding fixed support plates (2); and the reaction zone (102) is respectively filled with corresponding second packing layers (5) upward through corresponding movable support plates (4); The heat exchange mechanism (6) comprises a heat exchange medium inlet container (601) fixedly mounted at the center of the movable support plate (4), and a heat exchange medium outlet container (602) fixedly arranged on the upper side of the middle portion of the second packing layer (5), wherein a plurality of corresponding heat exchange pipes (603) are uniformly arranged outward at equal angles on the periphery of the heat exchange medium inlet container (601) and the heat exchange medium outlet container (602), and the heat exchange medium circulation pipes (604) pre-buried in the second packing layer (5) are longitudinally connected between the heat exchange pipes (603), and the heat exchange medium circulation pipes (604) connected to different heat exchange pipes (603) are staggered. A plurality of heat exchange medium inlet pipes (7) are respectively extended through the interior of the reaction separation tower body (1); corresponding drive pipes (8) are respectively installed at the discharge ends of the heat exchange medium inlet pipes (7) so as to be rotated upward; one end of the drive pipe (8) not connected to the heat exchange medium inlet pipe (7) movably passes through the movable support plate (4) and is rotatably installed at the center of the corresponding heat exchange medium inlet container (601); and its discharge end is horizontally tilted outward and folded and arranged in a constricted shape; and oblique teeth (9) facing the discharge end of the drive pipe (8) are respectively provided at positions on the inner side wall of the heat exchange medium inlet container (601) not connected to the heat exchange conduit (603); A plurality of heat exchange medium discharge pipes (10) are respectively extended through the interior of the reaction separation tower body (1), and the feed ends of the heat exchange medium discharge pipes (10) are respectively rotatably mounted to the center of the corresponding heat exchange medium discharge container (602).

2. A reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The reaction separation tower body (1) is fixedly connected to a plurality of main support ridges (11) located respectively on the lower side of the movable support plate (4), and corresponding first plane bearings (12) are respectively installed between the bottom of the movable support plate (4) and the main support ridges (11).

3. A reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 2, characterized in that: Auxiliary support ridges (13) spaced apart from the main support ridges (11) are fixedly connected to the reaction separation tower body (1) below the main support ridges (11). The auxiliary support ridges (13) are fixedly connected upward to corresponding support frames (15) through second plane bearings (14). The driving pipe (8) passes through and is fixedly connected to the middle of the support frame (15). The upper end of the support frame (15) is rollingly mounted with a plurality of support balls (16) whose top ends abut against the bottom side of the movable support plate (4).

4. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 3, characterized in that: A plurality of corresponding dispersion guide plates (17) are fixedly connected to the support frame (15) at an angle. During the reaction, the heat exchange medium enters the drive pipe (8) through the heat exchange medium inlet pipe (7), and is pressurized at the discharge end of the drive pipe (8) and then sprayed out horizontally and outwardly, so as to form an impact force on the helical teeth (9) on the inner wall of the heat exchange medium inlet container (601), thereby driving the heat exchange mechanism (6) and the second packing layer (5) to rotate as a whole. The reaction force generated during the process of pressurizing and spraying the heat exchange medium along the discharge end of the drive pipe (8) simultaneously drives the drive pipe (8) to rotate in the opposite direction to the heat exchange mechanism (6) and the second packing layer (5), thereby actively dispersing the material flowing through the dispersion guide plate (17).

5. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The heat exchange medium inlet pipe (7) and the driving pipe (8), the driving pipe (8) and the heat exchange medium inlet container (601), and the heat exchange medium discharge pipe (10) and the heat exchange medium discharge container (602) are rotatably connected via corresponding waterproof sealing bearings (18).

6. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The reaction separation tower body (1) is provided with an anhydrous hydrogen fluoride feed port (19) located at the bottom side of the feed zone (101), the reaction separation tower body (1) is also provided with an industrial phosphoric acid feed port (20) located at the upper side of the reaction zone (102), and the top of the reaction separation tower body (1) is provided with a product discharge port (21) for discharging the synthetic phosphorus oxytrifluoride gas.

7. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 6, characterized in that: A liquid material redistributor (22) for evenly distributing the industrial phosphoric acid material is provided at the lower side of the discharge end of the industrial phosphoric acid feed port (20).

8. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The reaction zones (102) are provided in two configurations, wherein the reaction temperature of the lower reaction zone (102) is controlled at 80-100°C, and the temperature of the upper reaction zone (102) is controlled at 100-120°C.

9. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The reaction separation tower body (1) is provided with a structural redistributor (23) at the upper part of the separation zone (103), and the reaction separation tower body (1) is provided with a wire mesh demister (24) at the upper part of the structural redistributor (23).

10. The reaction and separation equipment for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The discharge ends of the heat exchange pipes (603) connected to the heat exchange medium discharge container (602) are respectively tilted, and the tilting direction of the discharge ends of the heat exchange pipes (603) is opposite to the tilting direction of the driving pipe (8), and the discharge ends of the heat exchange pipes (603) are respectively fixed with corresponding limiting ring plates (26), and the heat exchange pipes (603) on the inner side of the limiting ring plates (26) are respectively fixed with corresponding fixed protrusions (27), and the outer side of the fixed protrusions (27) is movably mounted with corresponding water-permeable ring plates (29) through connecting springs (28), and a plurality of corresponding water-permeable holes are evenly distributed on the water-permeable ring plates (29), and the centers of the water-permeable ring plates (29) are respectively provided with corresponding spray pipes (30) in a bucket shape facing outwards. A photoelectric sensor for detecting the rotation speed of the second packing layer (5) is provided in the reaction separation tower body (1), and the heat exchange medium inlet pipe (7) is connected to an external material source through a flow-adjustable pump.

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