Preparation method of phosphorus oxyfluoride based on reaction separation equipment

Abstract

The invention discloses a preparation method of phosphorus oxyfluoride based on reaction separation equipment, which comprises the following specific steps: S1, a heat exchange medium enters a driving pipe fitting through a heat exchange medium inlet pipe of the reaction separation equipment, is pressurized at a discharge end of the driving pipe fitting and then is sprayed out in a horizontally outward inclined manner, a heat exchange mechanism and a second filler layer of the reaction separation equipment are driven to integrally rotate, so that a circulating heat source circularly passes through the whole reaction area; s2, respectively feeding liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride when the reaction temperature of the reaction zone reaches a set value; s3, liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride are in contact on the surface of the rotating second filler layer and react to generate phosphorus oxyfluoride gas; and S4, extracting phosphorus oxyfluoride gas generated by the reaction along the top of the reaction separation tower body. The controllability of the reaction process can be effectively ensured, and the reaction effect is obviously improved.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation and processing of phosphorus oxyfluoride, and specifically refers to a preparation method of phosphorus oxyfluoride based on a reaction separation device. Background Art

[0002] At present, phosphorus oxyfluoride (POF3) is a colorless gas with a pungent odor under normal conditions, and it emits weak fumes in the air. The preparation of phosphorus oxyfluoride (POF3) mainly involves the reaction of CaF2 with anhydrous sulfurous acid to first form CaF(SO3F), and then reacting with H3PO4 to form the intermediate product POF3. However, since CaF2 is a solid, continuous production is difficult, the process is complex, the production cost is high, and the generated CaSO4 will pollute the environment and must be treated necessarily. For this reason, a preparation method for obtaining high-purity phosphorus oxyfluoride by continuous reactive distillation using industrial phosphoric acid and anhydrous hydrogen fluoride as raw materials has begun to be studied and applied.

[0003] In the method for preparing high-purity phosphorus oxyfluoride by continuous reactive distillation, it has been found in actual application that due to the use of the method of reacting first and then separating, the equipment for preparing phosphorus oxyfluoride is numerous and complex. Moreover, in the reactive distillation column, since industrial phosphoric acid is a liquid and anhydrous hydrogen fluoride is a gas, during the process of the two-phase contact of industrial phosphoric acid and anhydrous hydrogen fluoride passing through the trays, the contact time between them is short, resulting in insufficient reaction between industrial phosphoric acid and anhydrous hydrogen fluoride. Therefore, it is necessary to achieve cyclic reaction by controlling the reflux, which leads to an increase in the energy consumption of the production reaction. Therefore, during the actual production process, the applicant has designed a phosphorus oxyfluoride reaction and separation integrated preparation column (patent application number CN202510154810.0), which effectively solves the problem of insufficient contact during the reaction between industrial phosphoric acid and anhydrous hydrogen fluoride, and can also effectively separate high-purity phosphorus oxyfluoride, thereby reducing the energy consumption of phosphorus oxyfluoride production and lowering the production cost.

[0004] However, during the actual use of this phosphorus oxyfluoride reaction and separation integrated preparation column, since the heat exchange tubes of the shell-and-tube heat exchanger located in the reaction zone are evenly arranged and fixed in position, in order to ensure the convenience of filling the packing layer in the reaction zone, the interval between the heat exchange tubes is required to be relatively large. As a result, it is only possible to maintain the temperature of the entire reaction zone by increasing the temperature of the heat exchange medium. In this way, the reaction temperature near the heat exchange tubes will be too high, resulting in insufficient uniformity of the reaction temperature in the entire reaction zone, thereby having an adverse impact on the reaction process. And the setting of the swirl distributors at the lower part of each reaction zone, although to a certain extent improves the uniform distribution effect of the reaction materials, however, in order to ensure that the materials can achieve a better distribution effect when passing through the swirl distributors, it is required that the pressure of the materials passing through the swirl distributors is relatively high. Obviously, this is unreasonable for the synthesis process of phosphorus oxyfluoride.

[0005] Therefore, the research objective of the present invention is to design a preparation method of phosphorus oxytetrafluoride based on a reaction separation device, which 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 technical problems existing in the above-mentioned prior art, the present invention provides a preparation method of phosphorus oxytetrafluoride 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 as follows: A preparation method of phosphorus oxytetrafluoride based on a reaction separation device, The reaction separation device includes: A reaction separation tower body, in which a feed zone, a plurality of reaction zones, and a separation zone are sequentially arranged from the lower end upwards. In the feed 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 at equal angles outward 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, and corresponding driving pipe fittings are rotatably installed upwards at the feed ends. The driving pipe fittings movably penetrate through the movable support plate and are rotatably installed at the center of the corresponding heat exchange medium inlet container. The discharge ends of the driving pipe fittings are horizontally inclined and folded outwards and are arranged in a constricted shape, and inclined teeth facing the discharge ends of the driving pipe fittings are arranged on the inner side walls of the heat exchange medium inlet containers; A plurality of heat exchange medium discharge pipes, and the feed ends are respectively rotatably installed at the centers of the corresponding heat exchange medium outlet containers; The preparation method of phosphorus oxytetrafluoride includes the following specific steps: S1. The heat exchange medium enters the driving pipe fitting through the heat exchange medium inlet pipe, is pressurized at the discharge end of the driving pipe fitting, and then 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 overall rotation of the heat exchange mechanism and the second packing layer to circulate the flowing heat source around the entire reaction zone; S2. When the reaction temperature in the reaction zone reaches the set value, liquid industrial phosphoric acid is fed downward along the upper side of the reaction zone, and gaseous anhydrous hydrogen fluoride is fed upward along the bottom side of the feeding zone; S3. Liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride come into contact on the surface of the rotating second packing layer and react to generate phosphorus oxyfluoride gas; S4. The generated phosphorus oxyfluoride gas is fractionated by the first packing layer on the separation zone and then withdrawn from the top of the reaction separation tower body.

[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; auxiliary support ridges are fixedly connected to the reaction separation tower body below the main support ridges and are arranged at intervals with the main support ridges. The auxiliary support ridges are respectively fixedly connected upward with corresponding support frames through second plain bearings. The driving pipe fitting penetrates and is fixedly connected to the middle of the support frame. A plurality of support balls with their tops abutted against the bottom side of the movable support plate are rollingly installed at the upper end of the support frame; a plurality of corresponding dispersion guide plates are respectively obliquely fixedly connected to the support frame.

[0009] In the step S1, the reaction force generated by the pressurized spray of the heat exchange medium along the discharge end of the driving pipe fitting 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 plate.

[0010] An anhydrous hydrogen fluoride inlet is arranged on the reaction separation tower body and is located at the bottom side of the feeding zone. An industrial phosphoric acid inlet is also arranged on the reaction separation tower body and is located at the upper side of the reaction zone. A liquid material redistributor for evenly distributing the industrial phosphoric acid material is arranged below the discharge end of the industrial phosphoric acid inlet.

[0011] In the step S2, liquid industrial phosphoric acid enters the upper side of the reaction zone along the industrial phosphoric acid inlet and is evenly fed downward through the liquid material redistributor. Gaseous anhydrous hydrogen fluoride enters the bottom side of the feeding zone along the anhydrous hydrogen fluoride inlet and is evenly fed upward after passing through the rotating dispersion guide plate.

[0012] A product discharge port for discharging phosphorus oxyfluoride gas is provided at the top of the reaction separation tower body. In step S4, after the phosphorus oxyfluoride gas generated by the reaction is fractionated through the first packing layer on the separation zone, it is withdrawn along the product discharge port.

[0013] Two reaction zones are provided. 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.

[0014] After step S4, step S5 is further included. 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 and collected for centralized treatment.

[0015] 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 respectively rotationally connected through corresponding waterproof and sealed bearings.

[0016] A structured redistributor is provided at the upper part of the separation zone of the reaction separation tower body, and a wire mesh demister is provided at the upper part of the structured redistributor. In step S4, during the extraction 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 structured redistributor to achieve gas - liquid separation.

[0017] Advantages of the present invention: 1) During the reaction process of the present invention, first, 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 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, which can effectively circulate the flowing heat source around the entire reaction zone, greatly improving the uniformity of the reaction temperature in the reaction zone, and further effectively improving the controllability of the subsequent reaction process and enhancing the reaction effect.

[0018] Moreover, this low - speed rotation will not only not cause excessive wall - hanging phenomena of the liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride during the reaction process, but on the contrary, it can significantly increase the uniform distribution effect of the materials in the second packing layer, assisting in enhancing the reaction effect of the materials, and further effectively improving the overall reaction efficiency and reaction effect of the present invention.

[0019] 2) In the present invention, the main support convex edge provided on the reaction separation tower body cooperates with the first plain bearing to rotationally mount 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 to the reaction separation tower body on the lower side of the main support convex edge. The auxiliary support convex edges are respectively fixedly connected upward with corresponding support frames through second plain bearings, and a plurality of support balls with their tops abutted against the bottom side of the movable support plate are rotatably mounted 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 that the overall reaction efficiency and reaction effect of the present invention can be effectively maintained.

[0020] 3) The driving 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 driving pipe fitting can simultaneously drive the driving 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 liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride still have sufficient 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.

[0021] 4) The driving for the rotation of the heat exchange mechanism and the second packing layer of the present invention, as well as the reverse rotation driving of the support frame provided with the dispersion guide plates, all adopt the liquid thrust generated by the flow of the heat exchange medium, without the need to additionally increase other power mechanisms, thereby being able to effectively reduce the preparation cost of phosphorus oxyfluoride. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 is the process flow chart of the preparation process of the present invention.

[0023] Figure 2 Schematic structural diagram of the reaction separation equipment of the present invention.

[0024] Figure 3 is the schematic structural diagram of the heat exchange mechanism.

[0025] Figure 4 is the schematic structural diagram of the movable support plate installed on the upper side of the main support convex edge.

[0026] Figure 5 is Figure 4 the partial enlarged view of part A in

[0027] Figure 6 is the schematic structural diagram of the heat exchange medium discharge pipe installed into the heat exchange medium discharge container in the second embodiment.

[0028] Figure 7 Schematic 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 circulation 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 balls 16, dispersion guide plate 17, waterproof seal bearing 18, anhydrous hydrogen fluoride feed port 19, industrial phosphoric acid feed port 20, product discharge port 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 implementation manners

[0030] For the convenience of those skilled in the art to understand, the structure of the present invention will be further described in detail below in conjunction with the accompanying drawings: Embodiment 1: Refer to Figures 1-5 , a preparation method of phosphorus oxyfluoride based on a reaction separation device, The reaction separation device includes: 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 upward from the lower end 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 upward through corresponding fixed support plates 2, and in the reaction zones 102, corresponding second packing layers 5 are filled upward through corresponding movable support plates 4; A heat exchange mechanism 6, including 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 of the second packing layer 5. A plurality of corresponding heat exchange conduits 603 are evenly distributed outward at equal angles around the heat exchange medium inlet container 601 and the heat exchange medium outlet container 602. Heat exchange medium circulation pipes 604 embedded in the second packing layer 5 are longitudinally connected between the heat exchange conduits 603, and the heat exchange medium circulation pipes 604 connected to different heat exchange conduits 603 are arranged in a staggered manner; A plurality of heat exchange media enter the pipe 7, and corresponding driving pipe fittings 8 are respectively rotatably installed upward at the feed end. The driving pipe fittings 8 movably penetrate through the movable support plate 4 and are rotatably installed at the center of the corresponding heat exchange medium inlet container 601. Moreover, the discharge end thereof is horizontally and outwardly inclined and folded and is arranged in a necked shape. The inner side walls of the heat exchange medium inlet container 601 are respectively provided with inclined teeth 9 facing the discharge end of the driving pipe fitting 8; A plurality of heat exchange medium discharge pipes 10, and the feed ends are respectively rotatably installed at the centers of the corresponding heat exchange medium discharge containers 602; The preparation method of phosphorus oxychloride includes the following specific steps: S1, 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 is horizontally and outwardly inclined and ejected to form an impact force on the inclined teeth 9 on the inner side wall of the heat exchange medium inlet container 601, so as to drive the overall rotation of the heat exchange mechanism 6 and the second packing layer 5, so as to circulate the flowing heat source around the entire reaction zone; S2, When the reaction temperature in the reaction zone reaches the set value, liquid industrial phosphoric acid is fed downward along the upper side of the reaction zone 102, and gaseous anhydrous hydrogen fluoride is fed upward along the bottom side of the feed zone 101; S3, Liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride come into contact on the surface of the rotating second packing layer 5 and react to generate phosphorus oxychloride gas; S4, The generated phosphorus oxychloride gas is fractionated by the first packing layer 3 on the separation zone 103 and then taken out from the top of the reaction separation tower body 1.

[0031] In the reaction process of the present invention, first, 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 is horizontally and outwardly inclined and ejected to form an impact force on the inclined teeth 9 on the inner side wall of the heat exchange medium inlet container 601, so as to drive the overall rotation of the heat exchange mechanism 6 and the second packing layer 5, and this rotation is a low-speed rotation, so that the flowing heat source can be effectively circulated around the entire reaction zone, so as to greatly improve the uniformity of the reaction temperature in the reaction zone, and further effectively improve the controllability of the subsequent reaction process and improve the reaction effect. And this low-speed rotation will not only not cause excessive wall hanging of liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride during the reaction process, but on the contrary, it can significantly increase the uniform distribution effect of the materials in the second packing layer 5, so as to assist in improving the reaction effect of the materials, and further effectively improve the overall reaction efficiency and reaction effect of the present invention.

[0032] A plurality 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; auxiliary support ridges 13 spaced 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 respectively fixedly connected with corresponding support frames 15 upward 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 abutting against the bottom side of the movable support plate 4 are rotatably installed at the upper end of the support frame 15; a plurality of corresponding dispersion guide plates 17 are respectively obliquely fixedly connected to the support frame 15.

[0033] In the step S1, the reaction force generated by the pressurized ejection of the heat exchange medium 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.

[0034] In the present invention, the main support ridges 11 and the first plain bearings 12 provided on the reaction separation tower body 1 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 ridges 13 to the reaction separation tower body 1 below the main support ridges 11. The auxiliary support ridges 13 are respectively fixedly connected with corresponding support frames 15 upward through second plain bearings 14. A plurality of support balls 16 with their tops abutting against the bottom side of the movable support plate 4 are rotatably installed at the upper end of the support frame 15. As the movable support plate 4 rotates, the support frame 15 forms a support with a fixed trajectory at its bottom, thereby effectively maintaining the support stability of the movable support plate 4 to ensure that the overall reaction efficiency and reaction effect of the present invention can be effectively maintained.

[0035] 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 obliquely fixedly connected to the support frame 15. During the reaction, the reaction force generated during the process of the heat exchange medium being pressurized and ejected along the discharge end of the driving pipe fitting 8 can simultaneously drive 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 liquid industrial phosphoric acid and the gaseous anhydrous hydrogen fluoride still have sufficient 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.

[0036] The driving force for the rotation of the heat exchange mechanism 6 and the second packing layer 5 of the present invention, as well as the reverse rotation driving force of the support frame 15 provided with the dispersion guide plate 17, is the liquid thrust generated by the circulation of the heat exchange medium, without the need to additionally increase other power mechanisms, thereby effectively reducing the preparation cost of phosphorus oxyfluoride.

[0037] 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 further provided on the reaction separation tower body 1 at the upper side of the reaction zone 102. 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.

[0038] In the step S2, the liquid industrial phosphoric acid enters the upper side of the reaction zone 102 along the industrial phosphoric acid feed port 20 and is evenly 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 evenly fed upward after passing through the rotating dispersion guide plate 17.

[0039] A product discharge port 21 for discharging the synthesized phosphorus oxyfluoride gas is provided at the top of the reaction separation tower body 1. In the step S4, the generated phosphorus oxyfluoride gas is fractionated by the first packing layer 3 on the separation zone 103 and then withdrawn along the product discharge port 21.

[0040] The reaction zone 102 is provided with two. In the 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.

[0041] The industrial phosphoric acid is branched into the upper part of the reaction zone 102 and enters the surface of the packing in the reaction zone 102, and reacts with the rising anhydrous hydrogen fluoride gas in the reaction zone 102. Inside the upper reaction zone 102, the concentration of the industrial phosphoric acid is high and the concentration of the anhydrous hydrogen fluoride is low, enabling the industrial phosphoric acid to completely react with the anhydrous hydrogen fluoride gas to form phosphorus oxyfluoride gas, avoiding the excess anhydrous hydrogen fluoride from being lifted to the separation zone together with the generated phosphorus oxyfluoride gas through the upper reaction zone. Therefore, through the above settings, the purity of the phosphorus oxyfluoride gas can be greatly improved; while in the lower reaction zone, the concentration of the industrial phosphoric acid is low, but the concentration of the anhydrous hydrogen fluoride is high. The anhydrous hydrogen fluoride in the reaction zone completely reacts with the industrial phosphoric acid, making the reaction between the industrial phosphoric acid and the anhydrous hydrogen fluoride more gentle, stable, and complete, and avoiding the excess process phosphoric acid from remaining at the bottom of the reaction separation tower body 1 through the reaction zone and the feed zone.

[0042] After the step S4, there is further a step S5, in which the redundant industrial phosphoric acid liquid and the residual side reaction liquid generated in small amounts are regularly discharged through the waste outlet 25 at the bottom of the reaction separation tower body 1 and collected for centralized treatment.

[0043] Between the heat exchange medium inlet pipe 7 and the driving pipe fitting 8, between the driving pipe fitting 8 and the heat exchange medium inlet container 601, and between the heat exchange medium discharge pipe 10 and the heat exchange medium discharge container 602, rotational connections are respectively made through corresponding waterproof and sealed bearings 18.

[0044] In the reaction separation tower body 1, a structured redistributor 23 is provided at the upper part of the separation zone 103, and a wire mesh demister 24 is provided at the upper part of the structured redistributor 23; in the step S4, during the extraction of the phosphorus oxytetrafluoride gas generated by the reaction, the industrial phosphoric acid entrained in the phosphorus oxytetrafluoride 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 structured redistributor 23 to achieve gas-liquid separation.

[0045] Embodiment 2: Reference Figures 6-7 , the difference between this embodiment and Embodiment 1 is that in the reaction separation equipment of this embodiment, the discharge ends of the heat exchange conduits 603 connected to the heat exchange medium discharge container 602 are respectively inclined, the inclination directions of the discharge ends of the heat exchange conduits 603 are opposite to the inclination direction of the driving pipe fitting 8, and corresponding limiting ring plates 26 are respectively fixedly connected to the discharge ends of the heat exchange conduits 603. Corresponding fixed 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 fixed 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. In the reaction separation tower body 1, a photoelectric sensor (not marked) for detecting the rotation speed of the second packing layer 5 is provided, and the heat exchange medium inlet pipe 7 is connected to an external material source through a flow-adjustable pumping pump (not marked).

[0046] 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 velocity 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 a jet is formed 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.

[0047] It should be noted that the implementation principle and technical effects of this embodiment are the same as those of Embodiment 1. For the sake of brief description, for the parts not mentioned in this embodiment, reference may be made to the corresponding content in Embodiment 1.

[0048] 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 modifications can be made, and these improvements and modifications should also be regarded as the protection scope 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 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), each having a corresponding driving pipe fitting (8) installed at the inlet end thereof so as to be rotated upwards, the driving pipe fitting (8) movably passing through the movable support plate (4) and being rotatably installed at the center of the corresponding heat exchange medium inlet container (601), and the outlet end thereof is tilted and folded outwardly horizontally and is arranged in a constricted shape, and the inner side wall of the heat exchange medium inlet container (601) is respectively provided with oblique teeth (9) facing the outlet end of the driving pipe fitting (8); A plurality of heat exchange medium discharge pipes (10), the feed ends of which are rotatably mounted at the center of the corresponding heat exchange medium discharge containers (602); The preparation method of phosphorus oxyfluoride 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 outlet 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, 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 from the upper side of the reaction zone (102), and gaseous anhydrous hydrogen fluoride is fed upwardly from 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 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 installed between the bottom of the movable support plate (4) and the main support ridges (11); the reaction separation tower body (1) at the lower side of the main support ridges (11) is respectively fixedly connected with auxiliary support ridges (13) spaced apart from the main support ridges (11), and the auxiliary support ridges (13) are respectively fixedly connected upward with corresponding support frames (15) through second plane bearings (14); the driving pipe (8) passes through and is fixedly connected to the middle part of the support frame (15), and 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); and a plurality of corresponding dispersion guide plates (17) are respectively fixedly connected to the support frame (15) in an inclined manner.

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 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).

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 top side of the reaction zone (102). 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).

5. The method for preparing phosphorus oxyfluoride based on a reaction separation device according to claim 4, characterized in that: In the step S2, the 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), and 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 reaction zones (102) are provided in two. In the step S1, the reaction temperature of the reaction zone (102) located at the lower part is controlled at 80-100°C, and the temperature of the reaction zone (102) located at the upper part 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 by-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 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).

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 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); in the step S4, during the extraction 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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