Reaction separation equipment for preparing phosphorus oxyfluoride

Abstract

The invention discloses reaction separation equipment for preparing phosphorus oxyfluoride, which comprises a reaction separation tower body, the lower end of the reaction separation tower body is sequentially provided with a feeding zone, a plurality of reaction zones and a separation zone from top to bottom, the feeding zone and the separation zone are fixedly filled with first filler layers, and the reaction zones are filled with second filler layers; the heat exchange mechanism comprises a heat exchange medium inlet container and a heat exchange medium outlet container, a plurality of heat exchange guide pipes are evenly distributed on the periphery of the heat exchange medium inlet container and the periphery of the heat exchange medium outlet container respectively, and heat exchange medium circulation pipes pre-buried in the second packing layer are longitudinally connected between the heat exchange guide pipes respectively; corresponding driving pipe fittings are upwards and rotationally mounted at the feeding ends of the heat exchange medium inlet pipes respectively; and a plurality of heat exchange medium discharge pipes. According to the invention, the reaction temperature uniformity in each reaction zone can be effectively improved, and the sufficient uniform distribution effect is ensured when materials slowly flow through the reaction zones.

Description

Technical Field

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

[0002] At present, phosphorus oxyfluoride (POF3) is a colorless gas with a pungent odor under normal conditions, and emits faint smoke in the air. The preparation of phosphorus oxyfluoride (POF3) mainly uses CaF2 to react with anhydrous sulfurous acid to first generate CaF (SO3F), and then react with H3PO4 to generate the intermediate product POF3. However, since CaF2 is a solid, continuous production is difficult, the process is complicated, the production cost is high, and the generated CaSO4 will pollute the environment, so necessary treatment must be carried out. For this reason, a preparation method of phosphorus oxyfluoride with 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] The method for preparing high-purity phosphorus oxyfluoride by continuous reaction distillation is found in actual application that due to the use of the method of first reaction and then separation, the equipment for preparing phosphorus oxyfluoride is numerous and complicated. Moreover, in the reaction distillation tower, since industrial phosphoric acid is liquid and anhydrous hydrogen fluoride is gas, the industrial phosphoric acid and anhydrous hydrogen fluoride are in contact with each other for a short time during the two-phase contact through the tower plate, which makes the reaction between industrial phosphoric acid and anhydrous hydrogen fluoride insufficient. Therefore, the cyclic reaction must be achieved by controlling the reflux, resulting in increased energy consumption of the production reaction. Therefore, in the actual production process, the applicant has studied and 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 concentration phosphorus oxyfluoride, thereby reducing the energy consumption of phosphorus oxyfluoride production and reducing production costs.

[0004] However, in the actual use of the phosphorus oxyfluoride reaction and separation integrated preparation tower, since the heat exchange tubes of the tube-in-tube heat exchanger located in the reaction zone are evenly arranged and fixed in position, in order to ensure the convenience of loading the packing layer in the reaction zone, the intervals between the heat exchange tubes are also required to be relatively large, resulting in the temperature of the entire reaction zone can only be maintained by increasing the temperature of the heat exchange medium. In this way, the reaction temperature near the heat exchange tube position is high, resulting in insufficient uniformity of the reaction temperature in the entire reaction zone, which has an adverse effect on the reaction process. Although the setting of the cyclone distributor arranged at the bottom of each reaction zone improves the uniform distribution effect of the reaction materials to a certain extent, in order to ensure that the materials can achieve a better distribution effect when passing through the cyclone distributor, the pressure of the materials passing through the cyclone distributor is required to be high, which is obviously unreasonable for the phosphorus oxyfluoride synthesis process.

[0005] Therefore, the research objective of the present invention is to design a reaction separation device for preparing phosphorus oxyfluoride that can effectively and significantly improve the reaction temperature uniformity in each reaction zone and ensure that the material still has sufficient 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 above technical problems existing in the prior art, the present invention provides a reaction separation device for preparing phosphorus oxyfluoride, which can effectively solve the above technical problems existing in the prior art.

[0007] The technical solution of the present invention is as follows: A reaction separation device for preparing phosphorus oxyfluoride, comprising: A reaction separation tower body, in which a feeding zone, a plurality of reaction zones, and a separation zone are sequentially arranged from the lower end upwards. In the feeding zone and the separation zone, corresponding first packing layers are fixedly filled upwards through corresponding fixed support plates, and in each reaction zone, a corresponding second packing layer is loaded upwards through a corresponding movable support plate; A heat exchange mechanism, including a heat exchange medium inlet container fixedly installed at the center of the movable support plate and a heat exchange medium outlet container fixedly arranged on the upper side of the middle part of the second packing layer. A plurality of corresponding heat exchange conduits are evenly arranged outward at equal angles around the heat exchange medium inlet container and the heat exchange medium outlet container. Heat exchange medium flow pipes buried in the second packing layer are longitudinally connected between the heat exchange conduits, and the heat exchange medium flow pipes connected to different heat exchange conduits are arranged in a staggered manner; A plurality of heat exchange medium inlet pipes respectively penetrate and extend into the interior of the reaction separation tower body. At the feeding ends of the heat exchange medium inlet pipes, corresponding driving pipe fittings are rotatably installed upwards. One end of the driving pipe fitting not connected to the heat exchange medium inlet pipe movably penetrates the movable support plate and is rotatably installed at the center of the corresponding heat exchange medium inlet container, and its discharging end is horizontally tilted and folded outwards and is arranged in a constricted shape. Oblique teeth facing the discharging end of the driving pipe fitting are respectively arranged at positions on the inner side wall of the heat exchange medium inlet container not connected to the heat exchange conduits; A plurality of heat exchange medium outlet pipes respectively penetrate and extend into the interior of the reaction separation tower body, and the feeding ends of the heat exchange medium outlet pipes are respectively rotatably installed at the centers of the corresponding heat exchange medium outlet containers.

[0008] A plurality of main support ridges are fixedly connected to the reaction separation tower body and are respectively located below the movable support plate. Corresponding first plain bearings are respectively assembled between the bottom of the movable support plate and the main support ridges.

[0009] On the reaction separation tower body below the main support convex edge, auxiliary support convex edges are fixedly connected respectively at intervals with the main support convex edge. The auxiliary support convex edges are fixedly connected upward with corresponding support frames through second plane bearings respectively. The driving pipe fitting penetrates through and is fixedly connected to the middle of the support frame. At the upper end of the support frame, a plurality of support balls with their tops abutted against the bottom side of the movable support plate are installed in a rolling manner.

[0010] On the support frames, a plurality of corresponding dispersion guide plates are fixedly connected obliquely respectively; during the reaction, the heat exchange medium enters the driving pipe fitting through the heat exchange medium inlet pipe, and after being pressurized at the discharge end of the driving pipe fitting, it sprays out horizontally and obliquely outward to form 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 integrally; during the process of the heat exchange medium spraying out with pressure at the discharge end of the driving pipe fitting, the reaction force generated simultaneously drives the driving pipe fitting to rotate in a direction opposite to the rotation direction of the heat exchange mechanism and the second packing layer, thereby actively dispersing the material flowing through the dispersion guide plates.

[0011] Between the heat exchange medium inlet pipe and the driving pipe fitting, between the driving pipe fitting and the heat exchange medium inlet container, and between the heat exchange medium discharge pipe and the heat exchange medium discharge container, they are rotationally connected through corresponding waterproof sealing bearings respectively.

[0012] On the reaction separation tower body, there is an anhydrous hydrogen fluoride inlet located at the bottom side of the feeding area, and there is also an industrial phosphoric acid inlet located at the upper side of the reaction area. At the top of the reaction separation tower body, there is a product discharge port for discharging phosphorus oxytetrafluoride gas.

[0013] Below the discharge end of the industrial phosphoric acid inlet, there is a liquid material redistributor for evenly distributing the industrial phosphoric acid material.

[0014] The reaction area is set to be two. Among them, the reaction temperature of the lower reaction area is controlled at 80 - 100 °C, and the temperature of the upper reaction area is controlled at 100 - 120 °C.

[0015] On the reaction separation tower body, a structured redistributor is provided at the upper part of the separation area, and a wire mesh demister is provided at the upper part of the structured redistributor.

[0016] The discharge ends of the heat exchange conduits connected to the heat exchange medium discharge container are respectively inclined, and the inclination directions of the discharge ends of the heat exchange conduits are opposite to the inclination direction of the driving pipe fitting. Moreover, corresponding limiting ring plates are respectively fixedly connected to the discharge ends of the heat exchange conduits. Corresponding fixed convex edges are respectively fixedly connected to the heat exchange conduits on the inner sides of the limiting ring plates. Corresponding water-permeable ring plates are respectively movably installed outside the fixed convex edges through corresponding connecting springs. A plurality of corresponding water-permeable holes are uniformly arranged on the water-permeable ring plates. Moreover, corresponding jet pipes are respectively arranged in a funnel shape outward at the centers of the water-permeable ring plates. An optoelectronic sensor for detecting the rotation speed of the second packing layer is arranged inside the reaction separation tower body. The heat exchange medium inlet pipe is connected to an external material source through a flow-adjustable pumping pump.

[0017] Advantages of the present invention: 1) Firstly, the heat exchange mechanism of the present invention is improved and designed. It 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 arranged on the upper side of the middle part of the second packing layer. Then, through the intervention of heat exchange conduits and heat exchange medium flow pipes arranged in a staggered manner on different heat exchange conduits, the uniform circulation of the heat exchange medium is realized. Then, a driving pipe fitting is installed at the feed end of the heat exchange medium inlet pipe, and the end of the driving pipe fitting not connected to the heat exchange medium inlet pipe is rotatably installed at the center of the corresponding heat exchange medium inlet container. Most importantly, the discharge end of the driving pipe fitting is horizontally folded outward obliquely and is arranged in a reduced diameter shape. At the same time, inclined teeth facing the discharge end of the driving pipe fitting are respectively arranged on the inner side walls of the heat exchange medium inlet container.

[0018] During the reaction, the heat exchange medium enters the driving pipe fitting through the heat exchange medium inlet pipe, and after being pressurized at the discharge end of the driving pipe fitting, it is sprayed out horizontally and obliquely outward to form an impact force on the inclined teeth on the inner side wall of the heat exchange medium inlet container, thereby driving the overall rotation of the heat exchange mechanism and the second packing layer, and this rotation is a low-speed rotation. Thus, the circulating heat source can be effectively circulated around the entire reaction zone, greatly improving the temperature uniformity in the reaction zone, thereby effectively improving the controllability of the reaction process and the reaction effect. Moreover, this low-speed rotation will not cause excessive wall hanging of the material, but can significantly increase the uniform distribution effect of the material in the second packing layer to assist in improving the reaction effect of the material.

[0019] 2) The main support convex edge provided on the reaction separation tower body of the present invention cooperates with the first plain bearing to form a rotational installation for the movable support plate. To make up for the problem of insufficient support stability existing in the rotational setting of the movable support plate, the present invention further fixedly connects auxiliary support convex edges on the reaction separation tower body below the main support convex edge. The auxiliary support convex edges are respectively fixedly connected upward with corresponding support frames through second plain bearings. A plurality of support balls with their tops abutted against the bottom side of the movable support plate are rotatably installed at the upper ends of the support frames. As the movable support plate rotates, the support frames form a support with a fixed trajectory at its bottom, thereby effectively maintaining the support stability of the movable support plate to ensure the practical effect of the present invention.

[0020] 3) The drive pipe fitting of the present invention penetrates through and is fixedly connected to the middle of the support frame, and a plurality of corresponding dispersion guide plates are respectively obliquely fixedly connected to the support frame. During the reaction, the reaction force generated during the pressurized ejection of the heat exchange medium along the discharge end of the drive pipe fitting simultaneously drives the drive pipe fitting to rotate in a direction opposite to the rotation directions of the heat exchange mechanism and the second packing layer, thereby actively dispersing the material flowing through the dispersion guide plates to ensure that the material still has sufficient uniform distribution effect when slowly flowing through each reaction zone, thereby effectively further ensuring the controllability of the reaction process and improving the reaction effect.

[0021] 4) The rotational drives of the heat exchange mechanism and the second packing layer of the present invention, as well as the reverse rotational drive of the support frame provided with the dispersion guide plates, all adopt the liquid thrust generated by the flow of the heat exchange medium as the power, without the need to additionally increase other power mechanisms, thereby effectively reducing the manufacturing cost and operation and maintenance cost of the equipment.

[0022] 5) The discharge ends of the heat exchange conduits connected to the heat exchange medium discharge container of the present invention are respectively obliquely arranged, and their inclination directions are opposite to the inclination direction of the drive pipe fitting. And the discharge ends are respectively fixedly connected with corresponding limit ring plates, and corresponding fixed convex edges are respectively fixedly connected to the heat exchange conduits inside the limit ring plates. Corresponding water-permeable ring plates are respectively movably installed outside the fixed convex edges through corresponding connecting springs. A plurality of corresponding water-permeable holes are uniformly arranged on the water-permeable ring plates, and corresponding jet pipes are respectively arranged in a funnel shape outward at the centers 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 plates and the jet holes of the jet pipes. 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 rate adjustable pumping and feeding pump is increased to increase the flow rate of the heat exchange medium, thereby increasing the flow speed and pressure of the heat exchange medium to drive the water-permeable ring plates and the jet pipes to be pushed outwards and abutted against the limit ring plates, so that the water-permeable holes on the water-permeable ring plates are closed, and thus a jet flow is formed through the jet pipes 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. Description of the Drawings

[0023] Figure 1 This is a schematic structural diagram of the present invention.

[0024] Figure 2 This is a schematic structural diagram of the heat exchange mechanism.

[0025] Figure 3 This is a schematic structural diagram of the movable support plate installed on the upper side of the main support flange.

[0026] Figure 4 is Figure 3 a partial enlarged view of part A in

[0027] Figure 5 This is a schematic structural diagram of the heat exchange medium discharge pipe in Embodiment 2 installed into the heat exchange medium discharge container.

[0028] Figure 6 This is a schematic structural diagram of the discharge end of the heat exchange conduit in Embodiment 2.

[0029] In the attached drawings: 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 flow pipe 604, heat exchange medium inlet pipe 7, driving pipe fitting 8, helical teeth 9, heat exchange medium discharge pipe 10, main support flange 11, first plain bearing 12, auxiliary support flange 13, second plain bearing 14, support frame 15, support ball 16, dispersion guide plate 17, waterproof seal bearing 18, anhydrous hydrogen fluoride inlet 19, industrial phosphoric acid inlet 20, product outlet 21, liquid material redistributor 22, structured redistributor 23, wire mesh demister 24, waste outlet 25, limit ring plate 26, fixed flange 27, connecting spring 28, permeable ring plate 29, jet pipe 30. Detailed Embodiments

[0030] For the convenience of those skilled in the art to understand, the embodiments will now be described in further detail in conjunction with the attached drawings for the structure of the present invention: Embodiment 1: Refer to Figures 1-4 , a reaction separation device for preparing phosphorus oxyfluoride, comprising: A reaction separation tower body 1, in which a feed zone 101, a plurality of reaction zones 102, and a separation zone 103 are sequentially arranged from the lower end upwards of the reaction separation tower body 1. In the feed zone 101 and the separation zone 103, corresponding first packing layers 3 are fixedly filled upwards through corresponding fixed support plates 2, and in the reaction zones 102, corresponding second packing layers 5 are filled upwards through corresponding movable support plates 4; The heat exchange mechanism 6 includes a heat exchange medium inlet container 601 fixedly installed 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 part of the second packing layer 5. A number of corresponding heat exchange conduits 603 are evenly distributed outward at equal angles respectively around the heat exchange medium inlet container 601 and the heat exchange medium outlet container 602. Heat exchange medium flow pipes 604 embedded in the second packing layer 5 are longitudinally connected between the heat exchange conduits 603 respectively, and the heat exchange medium flow pipes 604 connected to different heat exchange conduits 603 are arranged in a staggered manner; A number of heat exchange medium inlet pipes 7 respectively penetrate and extend into the interior of the reaction separation tower body 1. Corresponding driving pipe fittings 8 are rotatably installed upward at the feed ends of the heat exchange medium inlet pipes 7. One end of the driving pipe fitting 8 not connected to the heat exchange medium inlet pipe 7 movably penetrates 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. Oblique teeth 9 facing the discharge end of the driving pipe fitting 8 are respectively arranged at positions on the inner side wall of the heat exchange medium inlet container 601 not connected to the heat exchange conduit 603; A number of heat exchange medium outlet pipes 10 respectively penetrate and extend into the interior of the reaction separation tower body 1. The feed ends of the heat exchange medium outlet pipes 10 are respectively rotatably installed at the centers of the corresponding heat exchange medium outlet containers 602.

[0031] The present invention first makes an improved design on 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 arranged on the upper side of the middle part of the second packing layer 5. Then, through the intervention of the heat exchange conduit 603 and the heat exchange medium flow pipes 604 arranged in a staggered manner on different heat exchange conduits 603, the uniform circulation of the heat exchange medium is realized. Then, a driving pipe fitting 8 is installed at the feeding end of the heat exchange medium inlet pipe 7, and one end of the driving pipe fitting 8 that is not connected to the heat exchange medium inlet pipe 7 is rotatably installed at the center of the corresponding heat exchange medium inlet container 601. Most importantly, the discharging end of the driving pipe fitting 8 is horizontally tilted and folded outwards and is arranged in a constricted shape. At the same time, inclined teeth 9 facing the discharging end of the driving pipe fitting are respectively arranged on the inner side wall of the heat exchange medium inlet container 601. During the reaction, the heat exchange medium enters the driving pipe fitting 8 through the heat exchange medium inlet pipe 7, and after being pressurized at the discharging end of the driving pipe fitting 8, it is horizontally sprayed outwards obliquely to form an impact force on the inclined teeth 9 on the inner side wall of the heat exchange medium inlet container 601, thereby driving the overall rotation of the heat exchange mechanism 6 and the second packing layer 5, and this rotation is a low-speed rotation. Thereby, the circulating heat source can be effectively circulated around the entire reaction zone 102, so as to greatly improve the uniformity of the reaction temperature in the reaction zone 102, thereby effectively improving the controllability of the reaction process and the reaction effect. And this low-speed rotation will not only cause excessive wall sticking of the material, but on the contrary, it can significantly increase the uniform distribution effect of the material in the second packing layer 5 to assist in improving the reaction effect of the material.

[0032] A number of main support ridges 11 are fixedly connected to the reaction separation tower body 1 and are respectively located below the movable support plate 4. Corresponding first plain bearings 12 are respectively assembled between the bottom of the movable support plate 4 and the main support ridges 11.

[0033] Auxiliary support ridges 13 spaced from the main support ridges 11 are respectively fixedly connected to the reaction separation tower body 1 below the main support ridges 11. The auxiliary support ridges 13 are respectively fixedly connected upwards with corresponding support frames 15 through second plain bearings 14. The driving pipe fitting 8 penetrates through and is fixedly connected to the middle of the support frame 15. A plurality of support balls 16 with their tops abutted against the bottom side of the movable support plate 4 are rotatably installed at the upper end of the support frame 15.

[0034] In the present invention, the main support convex edge 11 provided on the reaction separation tower body 1 and the first plain bearing 12 cooperate to rotatably mount the movable support plate 4. To make up for the problem of insufficient support stability existing in the rotational setting of the movable support plate 4, the present invention further fixedly connects auxiliary support convex edges 13 to the reaction separation tower body 1 on the lower side of the main support convex edge 11. The auxiliary support convex edges 13 are respectively and upwardly fixedly connected with corresponding support frames 15 through second plain bearings 14. A plurality of support balls 16 with their tops abutted against the bottom side of the movable support plate 4 are rotatably mounted at the upper ends of the support frames 15. As the movable support plate 4 rotates, the support frames 15 form a support with a fixed trajectory at their bottoms for it, thereby effectively maintaining the support stability of the movable support plate 4 to ensure the practical effect of the present invention.

[0035] A plurality of corresponding dispersion guide plates 17 are respectively and obliquely fixedly connected to the support frames 15; during the reaction, the heat exchange medium enters the driving pipe fitting 8 through the heat exchange medium inlet pipe 7, and after being pressurized at the discharge end of the driving pipe fitting 8, it sprays out horizontally and obliquely to form an impact force on the helical teeth 9 on the inner side wall of the heat exchange medium inlet container 601, thereby driving the overall rotation of the heat exchange mechanism 6 and the second packing layer 5; during the process of the heat exchange medium being pressurized and sprayed out along the discharge end of the driving pipe fitting 8, the reaction force generated simultaneously drives the driving pipe fitting 8 to rotate in a direction opposite to the rotation directions of the heat exchange mechanism 6 and the second packing layer 5, thereby actively dispersing the material flowing through the dispersion guide plates 17.

[0036] The driving pipe fitting 8 of the present invention penetrates through and is fixedly connected to the middle of the support frame 15, and a plurality of corresponding dispersion guide plates 17 are respectively and obliquely fixedly connected to the support frames 15. During the reaction, the reaction force generated during the process of the heat exchange medium being pressurized and sprayed out along the discharge end of the driving pipe fitting 8 simultaneously drives the driving pipe fitting 8 to rotate in a direction opposite to the rotation directions of the heat exchange mechanism 6 and the second packing layer 5, thereby actively dispersing the material flowing through the dispersion guide plates 17 to ensure that the material still has sufficient uniform distribution effect when slowly flowing through each reaction zone 102, thereby effectively further ensuring the controllability of the reaction process and improving the reaction effect.

[0037] The heat exchange medium inlet pipe 7 and the driving pipe fitting 8, the driving pipe fitting 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 respectively rotationally connected through corresponding waterproof seal bearings 18.

[0038] The driving for the rotation of the heat exchange mechanism 6 and the second packing layer 5 of the present invention, and the reverse driving for the rotation of the support frame 15 provided with the dispersion guide plates 17 all adopt the liquid thrust generated by the flow of the heat exchange medium as the power, without the need to additionally increase other power mechanisms, thereby effectively reducing the manufacturing cost and operation and maintenance cost of the equipment.

[0039] An anhydrous hydrogen fluoride feed port 19 is provided on the reaction separation tower body 1 at the bottom side of the feed zone 101. An industrial phosphoric acid feed port 20 is also provided on the reaction separation tower body 1 at the upper side of the reaction zone 102. A product discharge port 21 for discharging the synthesized phosphorus oxyfluoride gas is provided at the top of the reaction separation tower body 1. 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. The reaction zone 102 is provided with two. Among them, 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.

[0040] During the reaction process, after the industrial phosphoric acid is fed through the industrial phosphoric acid feed port 20, under the action of the liquid material redistributor 22, it is evenly dispersed and enters the upper reaction zone 102. The anhydrous hydrogen fluoride gas enters through the anhydrous hydrogen fluoride feed port 19 and actively disperses into the lower reaction zone 102 through the rotatably arranged support frame 15 and the dispersion guide plate 17. The evenly distributed industrial phosphoric acid and anhydrous hydrogen fluoride fully contact and react in the second packing layer 5 of the reaction zone 102. The generated phosphorus oxyfluoride gas is fractionated by the first packing layer 3 in the separation zone 103 and then enters the next process through the product discharge port 21. The excess industrial phosphoric acid liquid and a small amount of by - reaction liquid residues generated can be regularly discharged through the waste discharge port 25 at the bottom of the reaction separation tower body 1 for centralized collection and treatment.

[0041] A structured redistributor 23 is provided on the reaction separation tower body 1 at the upper part of the separation zone 103. A wire mesh demister 24 is provided on the reaction separation tower body 1 at the upper part of the structured redistributor 23.

[0042] The resistance and path of the rising phosphorus oxyfluoride gas are increased by the first packing layer 3 in the upper separation zone 103. Therefore, the mist of industrial phosphoric acid entrained in the rising phosphorus oxyfluoride gas accumulates and is absorbed through contact with the surface of the first packing layer 3 and then settles and flows back into the reaction zone 102. Therefore, the separation of phosphorus oxyfluoride and the entrained industrial phosphoric acid mist can be well achieved through the separation zone 103, improving the purity of the phosphorus oxyfluoride product. Moreover, a structured redistributor 23 and a wire mesh demister 24 are provided at the upper part of the reaction separation tower body 1. The industrial phosphoric acid entrained in the phosphorus oxyfluoride can be further removed by the wire mesh demister, and the captured mist and the generated liquid enter the separation zone 103 through the structured redistributor 22 to achieve gas - liquid separation.

[0043] Example Two: Reference Figures 5-6, the difference between this embodiment and the first embodiment is that the discharging ends of the heat exchange conduits 603 connected to the heat exchange medium discharging container 602 are respectively inclined, the inclination directions of the discharging ends of the heat exchange conduits 603 are opposite to the inclination direction of the driving pipe fitting 8, and the discharging ends of the heat exchange conduits 603 are respectively fixedly connected with corresponding limiting ring plates 26. Corresponding fixing convex edges 27 are respectively fixedly connected to the heat exchange conduits 603 inside the limiting ring plates 26. Corresponding water-permeable ring plates 29 are respectively movably installed outside the fixing convex edges 27 through corresponding connecting springs 28. A plurality of corresponding water-permeable holes are uniformly arranged on the water-permeable ring plates 29, and corresponding jet pipes 30 are respectively arranged in a funnel shape outward at the centers of the water-permeable ring plates 29. A photoelectric sensor (not labeled) for detecting the rotation speed of the second packing layer 5 is arranged in the reaction separation tower body 1. The heat exchange medium inlet pipe 7 is connected to an external material source through a flow-adjustable pumping pump (not labeled).

[0044] 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 pumping pump is increased to increase the flow rate of the heat exchange medium, thereby increasing the flow speed and pressure of the heat exchange medium to drive the water-permeable ring plate 29 and the jet pipe 30 to push outwards and abut against the limiting ring plate 26, so that the water-permeable holes on the water-permeable ring plate 29 are closed, and thus 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.

[0045] It should be noted that the implementation principles and the technical effects produced by this embodiment and the first embodiment are the same. For the sake of brief description, for the parts not mentioned in this embodiment, reference can be made to the corresponding content in the first embodiment.

[0046] The above are only the preferred embodiments of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A reaction separation device for preparing phosphorus oxyfluoride, characterized in that: include: 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 from the lower end of the reaction separation tower body (1) upwards, wherein the feed zone (101) and the separation zone (103) are respectively filled with corresponding first filler layers (3) upwards through corresponding fixed support plates (2), and the reaction zone (102) is respectively filled with corresponding second filler layers (5) upwards 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 at the middle upper side of the second packing layer (5), a plurality of corresponding heat exchange pipes (603) being evenly arranged outward at equal angles on the peripheries of the heat exchange medium inlet container (601) and the heat exchange medium outlet container (602), the heat exchange medium flow pipes (604) pre-buried in the second packing layer (5) being longitudinally connected between the heat exchange pipes (603), and the heat exchange medium flow 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 feed 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 the discharge end thereof is horizontally tilted and folded outward and is arranged in a constricted shape; and oblique teeth (9) facing the discharge end of the drive pipe (8) are respectively arranged at positions of 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 at the center of the corresponding heat exchange medium discharge container (602).

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

3. A reaction separation device 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 upwardly to corresponding support frames (15) via second plane bearings (14); the drive pipe (8) passes through and is fixedly connected to the middle of the support frame (15); and a plurality of support balls (16) are rollingly mounted on the upper end of the support frame (15), the top ends of which abut against the bottom side of the movable support plate (4).

4. A reaction and separation device for preparing phosphorus oxyfluoride according to claim 3, characterized in that: A plurality of corresponding dispersion guide plates (17) are respectively fixedly connected to the support frame (15) at an angle. During reaction, the heat exchange medium enters the drive pipe (8) through the heat exchange medium inlet pipe (7), and is pressurized at the outlet end of the drive pipe (8) and then sprayed out horizontally and outwardly at an angle, 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 in the process of pressurizing and spraying the heat exchange medium along the outlet 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. A reaction and separation device for preparing phosphorus oxyfluoride according to claim 1, characterized in that: The heat exchange medium inlet pipe (7) and the drive pipe (8), the drive pipe (8) and the heat exchange medium inlet container (601), and the heat exchange medium outlet pipe (10) and the heat exchange medium outlet container (602) are rotatably connected via corresponding waterproof sealing bearings (18).

6. A reaction and separation device 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 top 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 synthesized phosphorus oxyfluoride gas.

7. A reaction and separation device 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 portions, 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 an upper portion of the separation zone (103), and the reaction separation tower body (1) is provided with a wire mesh demister (24) at an upper portion 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 arranged to be inclined, respectively; 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); the heat exchange pipes (603) on the inner side of the limiting ring plates (26) are respectively fixedly connected to corresponding fixed protrusions (27), which are connected to the limiting ring plates (26) by corresponding connecting springs (28). Corresponding water-permeable ring plates (29) are movably mounted on the outer sides of the fixed convex edges (27), and a plurality of corresponding water-permeable holes are evenly distributed on the water-permeable ring plates (29). Corresponding jet pipes (30) are arranged outward in a bucket shape at the center of the water-permeable ring plates (29). A photoelectric sensor for detecting the rotation speed of the second packing layer (5) is arranged in the reaction separation tower body (1), and the heat exchange medium inlet pipe (7) is connected to an external material source via a flow-adjustable pump.

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