A method for preparing phosphorus oxyfluoride based on reaction separation equipment

Abstract

The present invention discloses a method for preparing phosphorus oxyfluoride based on a reaction separation device, comprising the following specific steps: S1, a heat exchange medium enters a drive pipe through a heat exchange medium inlet pipe of the reaction separation device, is pressurized at the discharge end of the drive pipe, and is ejected horizontally and outwardly at an angle, thereby driving the heat exchange mechanism and second packing layer of the reaction separation device to rotate as a whole, causing the circulating heat source to circulate around the entire reaction zone; S2, when the reaction temperature of the reaction zone reaches a set value, liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride are respectively fed; S3, the liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride come into contact with the surface of the rotating second packing layer and react to generate phosphorus oxyfluoride gas; S4, the generated phosphorus oxyfluoride gas is withdrawn from the top of the reaction separation tower body. The present invention can effectively ensure the controllability of the reaction process and significantly improve the reaction effect.

Description

Technical Field

[0001] The invention relates to the technical field of phosphorus oxyfluoride preparation and processing, and in particular to a method for preparing phosphorus oxyfluoride based on reaction separation equipment. Background Art

[0002] Currently, phosphorus oxyfluoride (POF3) is a colorless gas with a pungent odor that emits faint smoke in the air. The production of POF3 primarily involves the reaction of CaF2 with anhydrous sulfurous acid to form 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 purpose of the present invention is to design a method for preparing phosphorus oxyfluoride based on a reaction separation device that can effectively and significantly improve the uniformity of the 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 response to the technical problems existing in the above-mentioned prior art, the present invention provides a method for preparing phosphorus oxyfluoride based on a reaction separation device, 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 method for preparing phosphorus oxyfluoride based on reaction separation equipment,

[0009] The reaction separation equipment comprises:

[0010] 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;

[0011] 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.

[0012] Several heat exchange medium inlet pipes are provided with corresponding drive pipes that are rotatably installed at the discharge ends. The drive pipes movably penetrate the movable support plate and are rotatably installed at the center of the corresponding heat exchange medium inlet container. The discharge ends thereof are horizontally tilted and folded outward and are arranged in a constricted shape. The inner side walls of the heat exchange medium inlet container are respectively provided with bevel teeth facing the discharge ends of the drive pipes.

[0013] Several heat exchange medium discharge pipes, the feed ends of which are respectively rotatably mounted to the center of the corresponding heat exchange medium discharge container;

[0014] The preparation method of phosphorus oxytrifluoride comprises the following specific steps:

[0015] S1, 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 and then ejected horizontally and outwardly, thereby generating an impact force on the helical teeth on the inner side wall of the heat exchange medium inlet container, thereby driving the heat exchange mechanism and the second packing layer to rotate as a whole, so as to circulate the circulating heat source around the entire reaction zone;

[0016] S2, when the reaction temperature of the reaction zone reaches a set value, liquid industrial phosphoric acid is fed downwardly from the upper side of the reaction zone, and gaseous anhydrous hydrogen fluoride is fed upwardly from the bottom side of the feed zone;

[0017] S3, liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride come into contact with the surface of the rotating second packing layer and react to generate phosphorus oxytrifluoride gas;

[0018] S4, the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer on the separation zone and then taken out along the top of the reaction and separation tower body.

[0019] The reaction separation tower body is fixed with several main support ridges which are respectively located at the lower side of the movable support plate, and corresponding first plane bearings are respectively installed between the bottom of the movable support plate and the main support ridges; the reaction separation tower body at the lower side of the main support ridges is fixed with auxiliary support ridges which are spaced apart from the main support ridges, and the auxiliary support ridges are respectively fixed upward with corresponding support frames through second plane bearings, the driving pipe passes through and is fixed to the middle part of the support frame, and the upper end part of the support frame is rollingly installed with a plurality of support balls whose top ends abut against the bottom side of the movable support plate; a plurality of corresponding dispersion guide plates are respectively fixed obliquely on the support frame.

[0020] In step S1, the reaction force generated by the pressurized ejection of 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.

[0021] The reaction and separation tower body is provided with an anhydrous hydrogen fluoride feed port located at the bottom side of the feed zone, and 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. 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.

[0022] In step S2, liquid industrial phosphoric acid enters the upper side of the reaction zone along the industrial phosphoric acid feed inlet and is uniformly fed downward through the liquid material redistributor. The gaseous anhydrous hydrogen fluoride enters the bottom side of the feed zone along the anhydrous hydrogen fluoride feed inlet and is uniformly fed upward after passing through the rotating dispersion guide plate.

[0023] The top of the reaction separation tower body is provided with a product outlet for discharging the synthesized phosphorus oxyfluoride gas. In step S4, the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer on the separation zone and then withdrawn along the product outlet.

[0024] There are two reaction zones. In step S1, 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.

[0025] The step S4 is followed by a step S5 in which the excess industrial phosphoric acid liquid and a small amount of residual side reaction liquid are regularly discharged through the waste outlet at the bottom of the reaction separation tower body for centralized collection and treatment.

[0026] 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.

[0027] 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; in the step S4, during the production process of the phosphorus oxyfluoride gas generated by the reaction, the industrial phosphoric acid entrained in the phosphorus oxyfluoride gas is further removed by the wire mesh demister, and the captured mist and the generated liquid enter the separation zone through the structural redistributor to achieve gas-liquid separation.

[0028] Advantages of the present invention:

[0029] 1) In the reaction process of the present invention, the heat exchange medium is first introduced into the drive pipe through the heat exchange medium inlet pipe, and is pressurized at the discharge end of the drive pipe and then sprayed out horizontally and obliquely outward to form an impact force on the helical teeth on the inner wall of the heat exchange medium inlet container, thereby driving the heat exchange mechanism and the second packing layer to rotate as a whole, and the rotation is low-speed rotation, so that the circulating heat source can be effectively circulated around the entire reaction zone, thereby greatly improving the reaction temperature uniformity in the reaction zone, thereby effectively improving the controllability of the subsequent reaction process and improving the reaction effect.

[0030] Moreover, the low-speed rotation not only does not cause excessive wall adhesion of liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride during the reaction, but can significantly increase the uniform distribution of the materials within the second packing layer, thereby helping to improve the reaction effect of the materials, thereby effectively improving the overall reaction efficiency and reaction effect of the present invention.

[0031] 2) The present invention forms a rotatable mounting for the movable support plate by cooperating the main support ridge and the first plane bearing provided on the reaction and separation tower body. To compensate for the insufficient support stability of the rotatable mounting of the movable support plate, the present invention further fixes auxiliary support ridges on the reaction and separation tower body below the main support ridge. The auxiliary support ridges are respectively fixed upwardly to corresponding support frames through second plane bearings. The upper end of the support frame is rollingly mounted with multiple support balls, the top ends of which abut against the bottom side of the movable support plate. As the movable support plate rotates, the support frame forms a fixed track support for it at its bottom, thereby effectively maintaining the support stability of the movable support plate, thereby ensuring that the overall reaction efficiency and reaction effect of the present invention can be effectively maintained.

[0032] 3) The drive pipe of the present invention passes through and is fixed to the middle part of the support frame, and a plurality of corresponding dispersion guide plates are fixedly connected to the support frame at an angle. During the reaction, the reaction force generated by the pressurized ejection of the heat exchange medium along the discharge end of the drive pipe can simultaneously drive the drive 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, ensuring that the liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride can still have a sufficiently uniform distribution effect when slowly flowing through each reaction zone, thereby effectively further ensuring the controllability of the reaction process of the present invention and improving the reaction effect.

[0033] 4) The power used for the heat exchange mechanism, the rotational drive of the second packing layer, and the reverse rotational drive of the support frame provided with the dispersion guide plate of the present invention is the liquid thrust generated by the circulation of the heat exchange medium. No additional power mechanism is required, thereby effectively reducing the preparation cost of phosphorus oxytrifluoride. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is a flow chart of the preparation process of the present invention.

[0035] Figure 2 A schematic structural diagram of the reaction separation equipment of the present invention.

[0036] Figure 3 It is a structural diagram of the heat exchange mechanism.

[0037] Figure 4 This is a structural diagram of the movable support plate installed on the upper side of the main support convex edge.

[0038] Figure 5 for Figure 4 A partial enlarged view of part A in .

[0039] Figure 6 This is a structural diagram of the heat exchange medium discharge pipe in Example 2 being installed in the heat exchange medium discharge container.

[0040] Figure 7 This is a schematic structural diagram of the discharge end of the heat exchange pipe in Example 2.

[0041] 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

[0042] In order to facilitate understanding by those skilled in the art, the structure of the present invention is further described in detail with reference to the embodiments and the accompanying drawings:

[0043] Example 1:

[0044] refer to Figure 1-5 , a preparation method of phosphorus oxyfluoride based on reaction separation equipment,

[0045] The reaction separation equipment comprises:

[0046] 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;

[0047] 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.

[0048] Several heat exchange medium inlet pipes 7 are provided with corresponding drive pipes 8 that are rotatably installed at the discharge ends. The drive pipes 8 are movable through the movable support plate 4 and are rotatably installed at the center of the corresponding heat exchange medium inlet container 601. The discharge ends thereof are horizontally tilted and folded outward and are arranged in a constricted shape. The inner side walls of the heat exchange medium inlet container 601 are respectively provided with bevel teeth 9 facing the discharge ends of the drive pipes 8.

[0049] Several heat exchange medium discharge pipes 10, the feed ends of which are rotatably mounted to the center of the corresponding heat exchange medium discharge container 602;

[0050] The preparation method of phosphorus oxytrifluoride comprises the following specific steps:

[0051] S1, 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, thereby generating 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, so as to circulate the circulating heat source around the entire reaction zone;

[0052] S2, when the reaction temperature of the reaction zone reaches the set value, liquid industrial phosphoric acid is fed downward from the upper side of the reaction zone 102, and gaseous anhydrous hydrogen fluoride is fed upward from the bottom side of the feed zone 101;

[0053] S3, liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride come into contact with the surface of the rotating second packing layer 5 and react to generate phosphorus oxytrifluoride gas;

[0054] S4, the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer 3 on the separation zone 103 and then taken out along the top of the reaction and separation tower body 1.

[0055] In the reaction process of the present invention, the heat exchange medium is firstly introduced into 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 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, so as to effectively circulate the circulating heat source around the entire reaction zone, so as to greatly improve the uniformity of the reaction temperature in the reaction zone, thereby effectively improving the controllability of the subsequent reaction process and improving the reaction effect. Moreover, the low-speed rotation not only does not cause the liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride in the reaction process to form excessive wall hanging phenomenon, but can significantly increase the uniform distribution effect of the material in the second packing layer 5, so as to assist in improving the reaction effect of the material, thereby effectively improving the overall reaction efficiency and reaction effect of the present invention.

[0056] The reaction separation tower body 1 is fixed with several 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; the reaction separation tower body 1 on the lower side of the main support ridges 11 is respectively fixed with auxiliary support ridges 13 spaced apart from the main support ridges 11, and the auxiliary support ridges 13 are respectively fixed upward with corresponding support frames 15 through second plane bearings 14, the driving pipe 8 passes through and is fixed to the middle part of the support frame 15, and the upper end of the support frame 15 is rollingly installed with a plurality of support balls 16 whose top ends abut against the bottom side of the movable support plate 4; a plurality of corresponding dispersion guide plates 17 are respectively fixed obliquely on the support frame 15.

[0057] In step S1, the reaction force generated by the pressurized ejection 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 plate 17.

[0058] The present invention forms a rotatable installation 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 problem existing in the rotatable installation 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 whose top ends abut against the bottom side of the movable support plate 4. As the movable support plate 4 rotates, the support frame 15 forms a track-fixed support for it at its bottom, thereby effectively maintaining the support stability of the movable support plate 4, thereby ensuring that the overall reaction efficiency and reaction effect of the present invention can be effectively maintained.

[0059] The drive pipe 8 of the present invention passes through and is fixed to the middle part of the support frame 15, and a plurality of corresponding dispersion guide plates 17 are fixedly connected to the support frame 15 at an angle. During the reaction, the reaction force generated during the pressurized ejection of the heat exchange medium along the discharge end of the drive pipe 8 can simultaneously drive 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, so as to ensure that the liquid industrial phosphoric acid and the gaseous anhydrous hydrogen fluoride can still have a sufficiently uniform distribution effect when slowly flowing through each reaction zone 102, thereby effectively further ensuring the controllability of the reaction process of the present invention and improving the reaction effect.

[0060] The power used for the rotational drive of the heat exchange mechanism 6 and the second packing layer 5, and the reverse rotational drive of the support frame 15 provided with the dispersion guide plate 17 of the present invention is the liquid thrust generated by the circulation of the heat exchange medium. No additional power mechanism is required, thereby effectively reducing the preparation cost of phosphorus oxytrifluoride.

[0061] The reaction and separation tower body 1 is provided with an anhydrous hydrogen fluoride feed port 19 located at the bottom side of the feed zone 101, and the reaction and 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. A liquid material redistributor 22 for uniformly distributing the industrial phosphoric acid material is provided below the discharge end of the industrial phosphoric acid feed port 20.

[0062] In step S2, liquid industrial phosphoric acid enters the upper side of the reaction zone 102 through the industrial phosphoric acid feed port 20 and is uniformly fed downward through the liquid material redistributor 22. The gaseous anhydrous hydrogen fluoride enters the bottom side of the feed zone 101 through the anhydrous hydrogen fluoride feed port 19 and is uniformly fed upward after passing through the rotating dispersion guide plate 17.

[0063] The top of the reaction separation tower body 1 is provided with a product outlet 21 for discharging the synthesized phosphorus oxyfluoride gas. In step S4, the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer 3 on the separation zone 103 and then withdrawn along the product outlet 21.

[0064] There are two reaction zones 102. In step S1, 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.

[0065] Industrial phosphoric acid flows from the upper portion of reaction zone 102 onto the surface of the packing within reaction zone 102 , where it contacts and reacts with the rising anhydrous hydrogen fluoride gas from reaction zone 102 . Within the upper reaction zone 102 , the concentration of industrial phosphoric acid is high and the concentration of anhydrous hydrogen fluoride is low. This allows the industrial phosphoric acid to completely react with the anhydrous hydrogen fluoride gas to form phosphorus oxyfluoride gas, preventing excess anhydrous hydrogen fluoride from passing through the upper reaction zone and being lifted to the separation zone along with the generated phosphorus oxyfluoride gas. Therefore, the above arrangement significantly improves the purity of the phosphorus oxyfluoride gas. In the lower reaction zone, the concentration of industrial phosphoric acid is low, while the concentration of anhydrous hydrogen fluoride is high. The anhydrous hydrogen fluoride in the reaction zone completely reacts with the industrial phosphoric acid, resulting in a gentler, smoother, and more complete reaction between the industrial phosphoric acid and anhydrous hydrogen fluoride. This prevents excess process phosphoric acid from passing through the reaction zone and the feed zone and remaining at the bottom of the reaction and separation tower body 1 .

[0066] The step S4 is followed by a step S5 in which the excess industrial phosphoric acid liquid and a small amount of residual side reaction liquid are regularly discharged through the waste outlet 25 at the bottom of the reaction separation tower body 1 for centralized collection and treatment.

[0067] 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 through corresponding waterproof sealing bearings 18.

[0068] The reaction and separation tower body 1 is provided with a structural redistributor 23 at the upper part of the separation zone 103, and the reaction and separation tower body 1 is provided with a wire mesh demister 24 at the upper part of the structural redistributor 23; in the step S4, during the production of the phosphorus oxyfluoride gas generated by the reaction, the industrial phosphoric acid entrained in the phosphorus oxyfluoride gas is further removed by the wire mesh demister 24, and the captured mist and the generated liquid enter the separation zone 103 through the structural redistributor 23 to achieve gas-liquid separation.

[0069] Example 2:

[0070] refer to Figure 6-7 The difference between this embodiment and the first embodiment is that: in the reaction separation equipment of this embodiment, the discharge ends of the heat exchange pipes 603 connected to the heat exchange medium discharge container 602 are respectively arranged at an angle, 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. Corresponding water-permeable ring plates 29 are movably mounted on the outer sides of the fixed protrusions 27 through corresponding 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 arranged outward in a bucket shape at the center 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 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).

[0071] 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 ensuring the practical effect of the present invention.

[0072] 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 contents in the first embodiment.

[0073] 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 method for preparing phosphorus oxyfluoride based on a reaction separation device, characterized in that: The reaction separation equipment comprises: 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 provided with corresponding drive pipes (8) which are rotatably installed at the discharge ends thereof. The drive pipes (8) are movable through the movable support plate (4) and are rotatably installed at the center of the corresponding heat exchange medium inlet container (601). The discharge ends thereof are tilted and folded horizontally outward and are arranged in a constricted shape. The inner side walls of the heat exchange medium inlet container (601) are respectively provided with bevel teeth (9) facing the discharge ends of the drive pipes (8). A plurality of heat exchange medium discharge pipes (10), the feed ends of which are rotatably mounted to the center of corresponding heat exchange medium discharge containers (602); The preparation method of phosphorus oxytrifluoride comprises the following specific steps: S1, 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 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, so as to circulate the circulating heat source around the entire reaction zone; S2, when the reaction temperature of the reaction zone reaches a set value, liquid industrial phosphoric acid is fed downwardly along the upper side of the reaction zone (102), and gaseous anhydrous hydrogen fluoride is fed upwardly along the bottom side of the feed zone (101); S3, liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride come into contact with the surface of the rotating second packing layer (5), and react to generate phosphorus oxytrifluoride gas; S4, the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer (3) on the separation zone (103) and then taken out along the top of the reaction separation tower body (1).

2. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 1, characterized in that: The reaction separation tower body (1) is fixed with a plurality of main support protrusions (11) respectively located 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 protrusions (11); the reaction separation tower body (1) on the lower side of the main support protrusions (11) is fixed with auxiliary support protrusions (13) spaced apart from the main support protrusions (11), and the auxiliary support protrusions (13) are respectively fixed upward with corresponding support frames (15) through second plane bearings (14); the driving pipe (8) passes through and is fixed to the middle part of the support frame (15), and the upper end of the support frame (15) is rollingly installed with a plurality of support balls (16) whose top ends abut against the bottom side of the movable support plate (4); and a plurality of corresponding dispersion guide plates (17) are respectively fixed obliquely on the support frame (15).

3. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 2, characterized in that: In step S1, the reaction force generated by the pressurized ejection of the heat exchange medium along the discharge end of the drive pipe (8) simultaneously drives the drive pipe (8) to rotate in a direction opposite to that of the heat exchange mechanism (6) and the second packing layer (5), thereby actively dispersing the material flowing through the dispersion guide plate (17).

4. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 3, 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), and 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). A liquid material redistributor (22) for uniformly distributing the industrial phosphoric acid material is provided below the discharge end of the industrial phosphoric acid feed port (20).

5. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 4, characterized in that: In step S2, liquid industrial phosphoric acid enters the upper side of the reaction zone (102) along the industrial phosphoric acid feed port (20) and is uniformly fed downward through the liquid material redistributor (22). The gaseous anhydrous hydrogen fluoride enters the bottom side of the feed zone (101) along the anhydrous hydrogen fluoride feed port (19) and is uniformly fed upward after passing through the rotating dispersion guide plate (17).

6. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 1, characterized in that: The top of the reaction separation tower body (1) is provided with a product outlet (21) for discharging the synthesized phosphorus oxyfluoride gas. In the step S4, the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer (3) on the separation zone (103) and then withdrawn along the product outlet (21).

7. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 1, characterized in that: The number of reaction zones (102) is two. In step S1, 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.

8. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 1, characterized in that: The step S4 is followed by a step S5, wherein the excess industrial phosphoric acid liquid and a small amount of residual side reaction liquid are regularly discharged through the waste outlet (25) at the bottom of the reaction separation tower body (1) for centralized collection and treatment.

9. The method for preparing phosphorus oxyfluoride based on a reaction separation device 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).

10. The method for preparing phosphorus oxyfluoride based on a reaction separation device 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); in the step S4, during the extraction process of the phosphorus oxyfluoride gas generated by the reaction, industrial phosphoric acid entrained in the phosphorus oxyfluoride gas is further removed by the wire mesh demister (24), and the captured mist and generated liquid enter the separation zone (103) through the structural redistributor (23) to achieve gas-liquid separation.

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