A continuous fluorination reaction device, reaction system, and fluoride preparation method

Abstract

The invention discloses a continuous fluorination reaction device, a reaction system and a fluoride preparation method, and belongs to the field of rare earth metal compounds; the fluorination reaction device comprises a fluorination tube, a rotary drive device, a feeding device, a discharging device, a heating device and a hydrogen fluoride gas supply device; the feeding device feeds raw materials into the rotating fluorination tube from the feeding port of the fluorination tube, and the raw materials move toward the side of the discharging port in the rotating fluorination tube; the heating device heats the fluorination tube, and after the rare earth oxide is heated to a certain temperature, the hydrogen fluoride gas supply device feeds hydrogen fluoride gas from the side of the discharging port of the fluorination tube; the rare earth oxide reacts with the hydrogen fluoride gas for a period of time to obtain rare earth fluoride; in the present application, the rare earth oxide reacts with the hydrogen fluoride gas in countercurrent, and the hydrogen fluoride gas can be fully utilized.

Description

Technical Field

[0001] The present invention relates to the field of rare earth metal compounds, and in particular to a continuous fluorination reaction device, a reaction system and a fluoride preparation method. Background Art

[0002] Rare earth fluoride is the fluoride of rare earth elements. Rare earth fluoride has been used in semiconductor, electronics, display, communication, glass, new materials and other industries. It is mainly used as optical coating materials, crystal materials, optical fiber materials, phosphors, etc. At present, there are two main processes for producing rare earth fluoride on the market: one is the wet process, which uses rare earth carbonate and hydrofluoric acid to mix and then use a shuttle kiln to dry and crush them to prepare the required rare earth fluoride. The other is the dry process, which uses carbonates or oxides and uses an electric furnace to pass hydrogen fluoride gas for dry fluorination. Existing dry fluorination equipment can only achieve phased production, and cannot achieve continuous fluorination production. Summary of the invention

[0003] The object of the present invention is to provide a continuous fluorination reaction device, a reaction system and a fluoride preparation method for realizing continuous fluorination production of rare earth fluoride.

[0004] The technical solution adopted by the present invention is as follows:

[0005] In the first aspect, the present invention provides a continuous fluorination reaction device, comprising a fluorination tube, a rotary drive device, a feeding device, a discharging device, a heating device, and a hydrogen fluoride gas supply device; the fluorination tube is arranged at an angle, with the higher end of the fluorination tube serving as a feeding port and the lower end serving as a discharging port; the fluorination tube is driven to rotate by the rotary drive device; the feeding port of the fluorination tube is connected to the feeding device, and the discharging port of the fluorination tube is connected to the discharging device; the heating device surrounds and wraps the fluorination tube to heat the fluorination tube; one side of the discharging port of the fluorination tube is connected to the hydrogen fluoride gas supply device, and the hydrogen fluoride gas is fed in from the side of the discharging port of the fluorination tube and discharged from the side of the feeding port.

[0006] In a possible design, the fluorinated tube is rotatably supported on the first frame by a rotating bracket; the rotating bracket includes a bracket body and a first supporting roller; two oppositely arranged vertical plates are provided on the bracket body, and circular through holes are provided on the tops of the two vertical plates, and the fluorinated tube passes through the through holes on the two vertical plates; a rotatable first supporting roller is provided between the two vertical plates, and the first supporting roller is supported on the outer surface of the fluorinated tube.

[0007] In a possible design, a first annular rail is arranged at the place where the fluorinated tube passes through the through hole of the vertical plate; a rolling groove is formed on the first annular rail, and the first supporting roller rotates in the rolling groove.

[0008] In a possible design, a brake mechanism is arranged on the rotating bracket, and the brake mechanism includes a brake rotating frame, a friction member, and a brake telescopic drive; the brake rotating frame includes a first rotating shaft, a first connecting rod, and a second connecting rod, and the first rotating shaft is horizontally installed between the two vertical plates; the two second connecting rods are J-shaped, and the two second connecting rods are symmetrically arranged and connected in the middle by two first pins; the upper ends of the two second connecting rods are rotatably connected to the first rotating shaft, and the lower ends of the two second connecting rods are connected to the friction member; a horizontal plate is arranged on the top of the two vertical plates, and the brake telescopic drive is installed on the horizontal plate, the top end of the first connecting rod is hinged to the end of the piston rod of the brake telescopic drive, and the bottom end of the first connecting rod is connected to the first pin in the middle of the two second connecting rods.

[0009] In a possible design, the brake telescopic drive adopts a double-piston rod hydraulic cylinder, and two sets of brake rotating frames and friction parts are symmetrically arranged on both sides of the double-piston rod hydraulic cylinder.

[0010] In one possible design, the feeding device includes a second frame, a raw material storage tank, and a screw conveyor; the screw conveyor is mounted on the second frame, and the feed port of the screw conveyor is upwardly connected to the discharge port at the bottom of the raw material storage tank; the discharge port of the screw conveyor is rotatably connected to the feed port of the fluorinated tube through a rotating sealing joint.

[0011] In one possible design, the discharging device includes a transfer box and a storage box; the discharging port of the fluorination tube extends into the transfer box, the discharging port is arranged at the bottom of the transfer box, the discharging port is arranged at the bottom of the discharging port, and the discharging valve is arranged at the bottom of the discharging port, and the storage box is arranged at the bottom of the transfer box; an air inlet pipe is arranged in the transfer box, one end of the air inlet pipe extends into the discharging port of the fluorination tube, and the other end passes through the transfer box and is connected to the hydrogen fluoride gas supply device through the air pipe.

[0012] In a possible design, the heating device is composed of two movable semi-cylindrical heating shells, and heat exchange tubes or heating resistors are arranged in the heating shells.

[0013] In the second aspect, the present invention provides a continuous fluorination reaction system, comprising any of the above-mentioned continuous fluorination reaction devices, and also comprising a loading device, wherein the loading device is installed on a working platform, and comprises a material receiving box and a barrel dumping device, wherein the material receiving box is mounted above the top opening of a raw material storage tank through a bracket, and the bottom discharge port of the material receiving box is connected to the top opening of the raw material storage tank; a dumping port is arranged on the side of the material receiving box, and a barrel dumping device is mounted on one side of the dumping port through a third frame, and the barrel dumping device is used for flipping and dumping a cylindrical raw material barrel.

[0014] In a third aspect, the present invention provides a method for preparing fluoride, using the above-mentioned continuous fluorination reaction device, the method is as follows: a feeding device continuously feeds rare earth oxide into a rotating fluorination tube from the feeding port of the fluorination tube, and the raw material moves toward the side of the discharge port in the rotating fluorination tube; the fluorination tube is heated by a heating device, and after the rare earth oxide is heated to a set temperature, a hydrogen fluoride gas supply device feeds hydrogen fluoride gas from one side of the discharge port of the fluorination tube; the rare earth oxide reacts with the hydrogen fluoride gas for a set time to obtain rare earth fluoride, and the rare earth fluoride is discharged from the discharge port.

[0015] The beneficial effects of the present invention are as follows: the present invention provides a continuous fluorination reaction device, a reaction system, and a fluoride preparation method, wherein the fluorination reaction device comprises a fluorination tube, a rotary drive device, a feeding device, a discharging device, a heating device, and a hydrogen fluoride gas supply device; the feeding device feeds the raw material into the rotating fluorination tube from the feeding port of the fluorination tube, and the raw material moves toward the side of the discharging port in the rotating fluorination tube; the heating device heats the fluorination tube, and after the rare earth oxide is heated to a certain temperature, the hydrogen fluoride gas supply device feeds hydrogen fluoride gas from the side of the discharging port of the fluorination tube; the rare earth oxide reacts with the hydrogen fluoride gas for a period of time to obtain rare earth fluoride. In the present application, the rare earth oxide reacts with the hydrogen fluoride gas in countercurrent, and the hydrogen fluoride gas can be fully utilized. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 The structure of a continuous fluorination reaction device of the present application is shown as follows Figure 1 .

[0017] Figure 2 The structure of a continuous fluorination reaction device of the present application is shown as follows Figure 2 .

[0018] Figure 3 Shown is Figure 2 Diagram showing the connection structure of the rotating bracket on the right side of the middle.

[0019] Figure 4 Shown is a structural display diagram of the first annular track of the present application.

[0020] Figure 5 Shown is a structural display diagram of the brake mechanism of the present application.

[0021] Figure 6 Shown is an improved first connecting rod of the present application.

[0022] Figure 7 Shown is a structural display diagram of one side of the feeding device of the present application.

[0023] Figure 8 Shown is a schematic diagram of the internal structure of the sealed box of the present application.

[0024] Fig. 9 Shown is a structural display diagram of one side of the discharging device of the present application.

[0025] Fig.10 Shown is a diagram showing the internal structure of the transfer box in this application.

[0026] Fig.11 Shown is a structural display diagram of the heating shell of the present application from the first perspective.

[0027] Fig.12 Shown is a structural display diagram of the heating shell of the present application from a second viewing angle.

[0028] Fig.13 The figure shows a schematic diagram of the fluorination tube of the present application being divided into a plurality of reaction chambers along the length direction.

[0029] Fig.14 Shown is a schematic structural diagram of an improved fluorinated tube of the present application.

[0030] Fig.15 Shown is a diagram showing the overall structure of the reaction system of the present application.

[0031] Fig.16 Shown is a structural display diagram of the feeding device of the present application.

[0032] Fig.17 Shown is a diagram showing the position of the filter cover of the present application.

[0033] Fig.18 Shown is a structural display diagram of the barrel dumping device from the first perspective.

[0034] Fig.19 Shown is a structural display diagram of the barrel dumping device from a second perspective.

[0035] Fig. 20 Shown is a structural diagram of the second flip drive provided by the present application.

[0036] Fig.21 Shown is a schematic diagram of the raw material barrel of the present application in a state of being turned over and unloading.

[0037] Fig. 22 Shown is a structural display diagram of the striking mechanism of the present application.

[0038] Description of reference numerals: fluorinated tube 1, first annular rail 101, rolling groove 101.1, flap valve 102;

[0039] Rotating bracket 2, bracket body 201, first supporting roller 202; first frame 3, rotating driving device 4, first driving motor 401, reducer 402, driving sprocket 403, driven sprocket 404, transmission chain 405, protective cover 406; feeding device 5, raw material storage tank 501, screw conveyor 502, sealing box 503, exhaust pipe 504, second frame 505; discharging device 6, transfer box 601, storage box 602, air inlet pipe 603; heating device 7, heating shell 701, first guide rail 702, mobile frame 703, heat collection chamber 704, heat exchange tube 705; hydrogen fluoride gas supply device 8, brake mechanism 9, rotating frame 901, first rotating shaft 901.1, first connecting rod 901.2, The second connecting rod 901.3, the first pin shaft 901.4; the friction member 902, the brake telescopic drive 903, the shock absorber 904; the dust collector 10, the spray tower 11, the fan 12, the working platform 13, the material receiving box 14, the material pouring port 14.1, the filter cover 14.2; the turning frame 15, the placement plate 15.1, the front side baffle plate 15.2, the turning shaft 15.3, the turning drive 15.4, the roller moving surface 15.5, the arc guide plate 15.6, the arc surface 15.7; the stop mechanism 17, the support column 17.1, the stop part 17.2, the stop telescopic drive rod 17.3; the raw material barrel 18, the third frame 19, the horizontal support column 19.1, the knocking hammer 20, the housing 21, the camshaft 22, the cam 23, the reset spring 24. DETAILED DESCRIPTION

[0040] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0041] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0042] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "plurality" means two or more.

[0043] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0044] The present application embodiment first provides a continuous fluorination reaction device, see Figure 1 The structure of a continuous fluorination reaction device of the present application is shown as follows Figure 1 , Figure 2 The structure of a continuous fluorination reaction device of the present application is shown as follows Figure 2 The device mainly comprises a fluorination tube 1, a rotary drive device 4, a feeding device 5, a discharging device 6, a heating device 7, and a hydrogen fluoride gas supply device 8.

[0045] In a specific embodiment of the present application, the fluorinated tube 1 is a cylindrical tube made of a heat-conducting metal or alloy, and the fluorinated tube 1 is resistant to high temperature and corrosion. Preferably, a high temperature and corrosion-resistant coating is attached to the inner wall of the fluorinated tube 1. The fluorinated tube 1 is tilted, and the angle between it and the horizontal plane is α, α is greater than 0° and less than 90°. Preferably, 10°≤α≤20°. The higher end of the fluorinated tube 1 serves as a feed port, and the lower end serves as a discharge port. Figure 1 As shown in the figure, the right side of the fluorination tube 1 is the feed port, and the left side of the fluorination tube 1 is the discharge port. The fluorination tube 1 is rotatably supported on the first frame 3 by a rotating bracket 2. The left side of the first frame 3 is low, and the right side is high, forming an inclined mounting surface. The fluorination tube 1 is driven to rotate by a rotary drive device 4. The feed port of the fluorination tube 1 is connected to the feed device 5, and the discharge port of the fluorination tube 1 is connected to the discharge device 6. The heating device 7 surrounds and wraps the fluorination tube 1, and is used to heat the fluorination tube 1. One side of the discharge port of the fluorination tube 1 is connected to the hydrogen fluoride gas supply device 8, and the hydrogen fluoride gas is fed in from one side of the discharge port of the fluorination tube 1 and discharged from one side of the feed port.

[0046] Reference Figure 1It is understood that the working principle of the continuous fluorination reaction device of the present application is as follows: the feeding device 5 feeds the raw material (rare earth oxide) into the rotating fluorination tube 1 from the feeding port of the fluorination tube 1, and the raw material moves to the side of the discharge port in the rotating fluorination tube 1. The heating device 7 heats the fluorination tube 1, and after the rare earth oxide is heated to a certain temperature, the hydrogen fluoride gas supply device 8 feeds hydrogen fluoride gas from the side of the discharge port of the fluorination tube 1; the rare earth oxide reacts with the hydrogen fluoride gas for a period of time to obtain rare earth fluoride. In the present application, the rare earth oxide reacts with the hydrogen fluoride gas in countercurrent, which can make full use of the hydrogen fluoride gas.

[0047] Furthermore, in a specific embodiment of the present application, the fluorinated tube 1 is supported by two rotating brackets 2, and the two rotating brackets 2 are arranged on both sides of the heating device 7. The structure of the rotating bracket 2 can be in the following form. Figure 3 Shown is Figure 2 The connection structure of the rotating bracket 2 on the right side of the middle is shown in the figure. The rotating bracket 2 includes a bracket body 201 and a first support roller 202. The bracket body 201 is provided with two oppositely arranged vertical plates, and the tops of the two vertical plates are provided with circular through holes, and the fluorinated tube 1 passes through the through holes on the two vertical plates. A rotatable first support roller 202 is provided between the two vertical plates, and the first support roller 202 is supported on the outer surface of the fluorinated tube 1. Figure 3 In the illustrated embodiment, two rotatable first supporting rollers 202 are provided between the two vertical plates, and the two first supporting rollers 202 are symmetrically supported on both sides of the lower portion of the fluorinated tube 1 .

[0048] In a specific embodiment of the present application, a first annular track 101 is arranged where the fluorinated tube 1 passes through the through hole of the vertical plate; Figure 4 The figure shows the structure of the first annular rail 101 of the present application. A rolling groove 101.1 is formed on the first annular rail 101, and the first supporting roller 202 rotates in the rolling groove 101.1. Preferably, an annular rubber ring is sleeved in the rolling groove 101.1.

[0049] In a preferred embodiment of the present application, a brake mechanism 9 may be further provided on the rotating bracket 2, and the brake mechanism 9 is used to decelerate or perform emergency braking on the fluorinated tube 1. Figure 5The structure display diagram of the brake mechanism 9 of the present application is shown. The brake mechanism 9 includes a brake rotating frame 901, a friction member 902, and a brake telescopic drive 903. The brake rotating frame 901 includes a first rotating shaft 901.1, a first connecting rod 901.2, and a second connecting rod 901.3. The first rotating shaft 901.1 is horizontally installed between two vertical plates. The two second connecting rods 901.3 are J-shaped, and the two second connecting rods 901.3 are symmetrically arranged and connected in the middle by two first pins 901.4. The upper ends of the two second connecting rods 901.3 are rotatably connected to the first rotating shaft 901.1, and the lower ends of the two second connecting rods 901.3 are connected to the friction member 902. The friction member 902 is preferably made of hard rubber, and the friction member 902 faces the rolling groove 101.1 and can enter the rolling groove 101.1 to contact the inner wall of the rolling groove 101.1. Preferably, the surface of the friction member 902 facing the rolling groove 101.1 is an arc-shaped concave surface, which can fit the inner wall of the rolling groove 101.1.

[0050] A horizontal plate is set on the top of the two vertical plates, and the brake telescopic drive 903 is installed on the horizontal plate. The top end of the first connecting rod 901.2 is hinged to the piston rod end of the brake telescopic drive 903, and the bottom end of the first connecting rod 901.2 is connected to the first pin shaft 901.4 between the two second connecting rods 901.3. Figure 5 In the illustrated embodiment, the brake telescopic drive 903 adopts a double piston rod hydraulic cylinder, and two sets of brake rotating frames 901 and friction members 902 are symmetrically arranged on both sides of the double piston rod hydraulic cylinder. The double piston rod hydraulic cylinder can simultaneously control the rotation of the two brake rotating frames 901, so that the two friction members 902 enter the rolling groove 101.1 at the same time for friction deceleration.

[0051] like Figure 6 The figure shows an improved first connecting rod 901.2 of the present application. A shock absorber 904 is arranged in the middle of the first connecting rod 901.2 to avoid rigid impact on the brake telescopic drive 903.

[0052] like Figure 7 Shown is a structural display diagram of one side of the feeding device 5 of the present application. In a specific embodiment of the present application, the feeding device 5 includes a second frame 505, a raw material storage tank 501, and a screw conveyor 502. The screw conveyor 502 is mounted on the second frame 505, and the feed port of the screw conveyor 502 is arranged upward. The raw material storage tank 501 is arranged above the screw conveyor 502, and the discharge port at the bottom of the raw material storage tank 501 is connected to the feed port of the screw conveyor 502. The discharge port of the screw conveyor 502 is rotatably connected to the feed port of the fluorinated tube 1 through a rotating sealing joint. In a preferred embodiment, the discharge port of the screw conveyor 502 and the feed port of the fluorinated tube 1 are connected to the sealing box 503. As Figure 8The figure shows the internal structure of the sealed box 503 of the present application. In the sealed box 503, the outlet of the screw conveyor 502 is rotatably connected to the feed port of the fluorinated tube 1 through a rotary sealing joint. Figure 8 As shown in , the rotary sealing joint is installed in the sealing box 503, the left side of the rotary sealing joint is rotatably connected to the feed port of the fluorinated tube 1, and the right side of the rotary sealing joint is fixedly connected to the discharge port of the screw conveyor 502, and the rotary sealing joint connects the fluorinated tube 1 and the inside of the screw conveyor 502. The sealing box 503 is filled with sealing oil to prevent gas leakage. In addition, in a specific embodiment of the present application, an exhaust pipe 504 is provided on the rotary sealing joint, and the exhaust pipe 504 passes through the sealing box 503 upward, and the air outlet of the exhaust pipe 504 is connected to the dust collector 10, the spray tower 11, and the fan 12 in sequence through a pipeline. The solid particles of the tail gas after fluorination are removed by the dust collector 10, and then sent to the spray tower 11 for adsorption.

[0053] like Fig. 9 The figure shows the structure of one side of the discharging device 6 of the present application. In a specific embodiment of the present application, the discharging device 6 includes a transfer box 601 and a storage box 602. Fig.10 The figure shows the internal structure of the transfer box 601 of the present application. The discharge port of the fluorination tube 1 extends into the transfer box 601, the discharge port is arranged at the bottom of the transfer box 601, the discharge valve is arranged at the bottom of the discharge port, and the storage box 602 is arranged at the bottom of the transfer box 601. An air inlet pipe 603 is arranged in the transfer box 601, one end of the air inlet pipe 603 extends into the discharge port of the fluorination tube 1, and the other end passes through the transfer box 601, and is connected to the hydrogen fluoride gas supply device 8 through the air pipe. The hydrogen fluoride gas supply device 8 includes a gas storage tank and a flow control device. The amount of hydrogen fluoride gas is regulated by the flow control device.

[0054] like Fig. 9 As shown in , in a specific embodiment of the present application, the rotary drive device 4 adopts a chain transmission mechanism, and the rotary drive device 4 is arranged on one side of the discharge port of the fluorinated tube 1, between the transfer box 601 and the left rotating bracket 2. The rotary drive device 4 includes a first driving motor 401, a reducer 402, a driving sprocket 403, a driven sprocket 404, a transmission chain 405, and a protective cover 406; the first driving motor 401 is installed at the bottom of the first frame 3, the first driving motor 401 is connected to the reducer 402, the driving sprocket 403 is arranged on the output shaft of the reducer 402, and the annular driven sprocket 404 is sleeved on the fluorinated tube 1; the driving sprocket 403 and the driven sprocket 404 are installed with a transmission chain 405. The arched protective cover 406 covers the driven sprocket 404 and the transmission chain 405.

[0055] like Figure 1As shown in FIG. 1 , in a specific embodiment of the present application, the heating device 7 is disposed between the two rotating brackets 2. The heating device 7 is composed of two movable semi-cylindrical heating shells 701. Fig.11 The figure shows the structure of the heating shell 701 of the present application from the first perspective. Fig.12 The figure shows the structure of the heating shell 701 of the present application from a second viewing angle. Fig.12 As shown in the figure, two first guide rails 702 are arranged on the first frame 3, and the two first guide rails 702 are perpendicular to the fluorinated tube 1. Two movable heating shells 701 are symmetrically arranged on the two first guide rails 702, and the two heating shells 701 are close to each other and surround the fluorinated tube 1. Specifically, the outer side of the heating shell 701 is connected to the movable frame 703, and the bottom of the movable frame 703 is equipped with a track wheel, and the track wheel rolls on the first guide rail 702. Fig.11 As shown in , heat collecting chambers 704 are arranged on both sides of the heating shell 701, and the two heat collecting chambers 704 are connected by a plurality of heat exchange tubes 705 extending along the length direction. The hot fluid flows from one heat collecting chamber 704 to another heat collecting chamber 704 through the heat exchange tubes 705, so that a heating space is formed inside the heating shell 701. In a specific implementation of the present application, the hot fluid uses high-temperature steam, and the high-temperature steam enters from the right side of the feed port and is discharged from the left side of the discharge port. The right heat collecting chamber 704 is connected to the steam generating equipment through a pipeline, and the left heat collecting chamber 704 is connected to the water circulation system through a pipeline, and the water after the high-temperature steam heat exchange enters the water circulation system for reuse. Of course, electric heating can also be used in the present application, and a heating resistor is arranged in the heating shell 701. The present application does not limit this.

[0056] In a preferred embodiment of the present application, the fluorinated tube 1 is divided into a plurality of reaction chambers along the length direction, and adjacent reaction chambers are separated by flaps that can be opened and closed. Fig.13 The figure shows a schematic diagram of the fluorination tube 1 of the present application being divided into a plurality of reaction chambers along the length direction. Fig.13 In the illustrated embodiment, four flap valves 102 are installed along the length of the fluorination tube 1, and three sections of closable reaction chambers are separated in the middle of the fluorination tube 1. The partition of the flap valve 102 is provided with air holes that allow gas to pass through, and hydrogen fluoride gas is still allowed to enter the reaction chamber for fluorination reaction in a closed state. In this way, the residence time of the rare earth oxide in the fluorination tube 1 can be controlled, thereby controlling the fluorination degree of the product. The device of the present application can be used to produce fully fluorinated products and semi-fluorinated products. Fig.14 The structure diagram of an improved fluorinated tube 1 of the present application is shown. In an optional embodiment, the fluorinated tube 1 is assembled from multiple tube sections with different inner diameters, and the inner diameter of the tube section on the feed port side of the assembled fluorinated tube 1 is small, and the inner diameter of the tube section extending toward the discharge port gradually increases. The flap diameter of the flap valve 102 at the connection gradually increases from the feed port side to the discharge port side, so that the flap can be prevented from getting stuck.

[0057] The present application further provides a continuous fluorination reaction system, which includes the above-mentioned continuous fluorination reaction device and a feeding device, which is used to add raw materials to the raw material storage tank 501. Fig.15 The figure shows the overall structure of the reaction system of the present application. The raw material storage tank 501 is installed on the working platform 13, and the working platform 13 is erected above the feeding device 5 through a column; the feeding device is installed on the working platform 13. Fig.16 The figure shows the structure of the feeding device of the present application. The feeding device includes a material receiving box 14 and a barrel dumping device. The material receiving box 14 is mounted above the top opening of the raw material storage tank 501 through a bracket, and the bottom discharge port of the material receiving box 14 is connected to the top opening of the raw material storage tank 501. A rounded rectangular dumping port 14.1 is set on the side of the material receiving box 14, and an exhaust fan 12 is set on the top of the material receiving box 14. A partition is set below the exhaust fan 12, and a filter cover 14.2 is installed on the lower surface of the partition. Fig.17 The figure shows the position of the filter cover 14.2 of the present application. During the pouring process, the exhaust fan 12 is started to suck the dust generated by the pouring upward and filter the dust through the filter cover 14.2. This can reduce the spread of dust. Fig.16 As shown in FIG. 1 , a barrel dumping device is arranged on one side of the dumping port 14 . 1 through the third frame 19 , and the barrel dumping device is used for flipping and dumping the cylindrical raw material barrel 18 .

[0058] The barrel tipping device comprises a tilting frame 15, a tilting drive 15.4, and a stop mechanism 17. Fig.18 The figure shows the structure of the barrel dumping device from the first perspective. Fig.19 The structure of the barrel dumping device from the second perspective is shown in FIG. Fig.18 As shown, the turning frame 15 is composed of a placing plate 15.1 and a front baffle 15.2, and the front baffle 15.2 is perpendicular to the placing plate 15.1. The front side edge of the bottom of the turning frame 15 is connected to the turning shaft 15.3 on the third frame 19. The turning drive 15.4 is used to drive the turning frame 15 to turn; Fig.18 In the embodiment shown, the turning drive 15.4 uses a reduction motor, and the turning shaft 15.3 is connected to the reduction motor. Fig. 20 The figure shows the structure of the second flip drive 15.4 provided by the present application. In this embodiment, the flip drive 15.4 uses two symmetrically arranged telescopic rods, one end of which is hinged on the working platform 13, and the other end is hinged on the flip frame 15. Of course, the present application can also use other structural forms of the flip drive 15.4, and the present application does not limit this.

[0059] like Fig.19As shown in the figure, a roller moving surface 15.5 formed by a plurality of rollers arranged in parallel is arranged in the center of the placement plate 15.1. An arc guide plate 15.6 is installed on the front side baffle plate 15.2 facing the roller moving surface 15.5. An arc surface 15.7 is formed on the arc guide plate 15.6. The cylindrical raw material barrel 18 will roll to the center line position of the arc surface 15.7 in the tilted state. In this position, the raw material barrel 18 can be turned over and the raw materials inside can be accurately poured into the pouring port 14.1. Fig.21 The schematic diagram of the raw material barrel 18 of the present application in the state of overturning and unloading is shown. The raw material barrel 18 is overturned and enters the unloading port 14.1, and the raw material barrel 18 is tilted so that the raw material can slide into the receiving box 14 by gravity.

[0060] like Fig.21 As shown in FIG. 1 , in order to prevent the raw material barrel 18 from being separated from the overturning frame 15 when the raw material barrel 18 is tilted and unloaded, in a specific embodiment of the present application, a stopper mechanism 17 is provided on the overturning frame 15. Fig.19 As shown in , the stop mechanism 17 is arranged in the middle of the rear edge of the upper surface of the turning frame 15. The stop mechanism 17 includes a support column 17.1, a stop portion 17.2, and a stop telescopic driving rod 17.3. The support column 17.1 is rotatably mounted on the turning frame 15. The top of the support column 17.1 is rotatably connected to the stop portion 17.2 through a pin shaft. The stop portion 17.2 is L-shaped. After the stop portion 17.2 rotates, it can press on the upper surface of the raw material barrel 18. The stop telescopic driving rod 17.3 is installed on the support column 17.1. The bottom end of the stop telescopic driving rod 17.3 is hinged on the support column 17.1. The piston rod of the stop telescopic driving rod 17.3 extends upward and is hingedly connected to the stop portion 17.2. The piston rod of the stop telescopic driving rod 17.3 is extended, driving the stop portion 17.2 to rotate, so that the stop portion 17.2 can press on the upper surface of the raw material barrel 18.

[0061] Further, such as Fig.19 As shown in FIG. 1 , a horizontal support column 19.1 for supporting the rear side of the placement plate 15.1 is provided on the third frame 19. When the placement plate 15.1 is placed horizontally, its lower surface is pressed on the horizontal support column 19.1.

[0062] In a specific embodiment of the present application, a knocking mechanism may be provided on the lower surface of the placement plate 15.1, and the knocking mechanism is used to hammer the bottom surface of the raw material barrel 18 when the raw material barrel 18 is tilted to pour the raw materials, so that the raw materials in the raw material barrel 18 can be completely poured into the receiving box 14. Fig. 22 The structure of the knocking mechanism of the present application is shown in FIG. The knocking mechanism includes a knocking hammer 20 and a cam mechanism. The knocking hammer 20 is driven by the cam mechanism to make a reciprocating motion, thereby hammering the bottom surface of the raw material tube 18 on the placement plate 15.1. Fig. 22 In the embodiment shown, two striking mechanisms are provided, which are driven by a motor. The cam mechanism is arranged in a housing 21. Fig. 22 The structure inside the casing 21 is shown on the right side in the middle. The camshaft 22 passes through the casing 21, and one end of the camshaft 22 is connected to the motor. A cam 23 is installed inside the casing 21 and on the camshaft 22, and a percussion hammer 20 is installed above the cam 23. A roller is arranged at the bottom of the percussion hammer 20, and the roller is in rolling contact with the cam 23. The percussion hammer 20 passes upward through the roller moving surface 15.5, and a hammer head is arranged on the top. A reset spring 24 is sleeved on the percussion hammer 20 in the casing 21. The two percussion hammers 20 alternately hammer, and the powder in the vibrating raw material barrel 18 quickly enters the receiving box 14.

[0063] By using the above-mentioned continuous fluorination reaction device, the embodiment of the present application further provides a fluoride preparation method, wherein the feeding device 5 continuously feeds rare earth oxide into the rotating fluorination tube 1 from the feeding port of the fluorination tube 1, and the raw material moves toward the side of the discharge port in the rotating fluorination tube 1; the fluorination tube 1 is heated by the heating device 7, and after the rare earth oxide is heated to a set temperature, the hydrogen fluoride gas supply device 8 feeds hydrogen fluoride gas from the side of the discharge port of the fluorination tube 1; the rare earth oxide reacts with the hydrogen fluoride gas for a set time to obtain rare earth fluoride, and the rare earth fluoride is discharged from the discharge port.

[0064] It is to be understood that the present invention is described by some embodiments, and it is known to those skilled in the art that various changes or equivalent substitutions may be made to these features and embodiments without departing from the spirit and scope of the present invention. In addition, under the teachings of the present invention, these features and embodiments may be modified to adapt to specific circumstances and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are within the scope of protection of the present invention.

Claims

1. A continuous fluorination reaction device, characterized in that: The invention comprises a fluorination tube (1), a rotary drive device (4), a feeding device (5), a discharging device (6), a heating device (7), and a hydrogen fluoride gas supply device (8); the fluorination tube (1) is arranged obliquely, with the higher end of the fluorination tube (1) serving as a feeding port and the lower end serving as a discharging port; the fluorination tube (1) is driven to rotate by the rotary drive device (4); the feeding port of the fluorination tube (1) is connected to the feeding device (5), and the discharging port of the fluorination tube (1) is connected to the discharging device (6); the heating device (7) surrounds and wraps the fluorination tube (1) and is used to heat the fluorination tube (1); the discharging port of the fluorination tube (1) is connected to the discharging device (6); One side is connected to a hydrogen fluoride gas supply device (8), and hydrogen fluoride gas is fed into the fluorination tube (1) from the discharge port side and discharged from the feed port side; the fluorination tube (1) is divided into a plurality of reaction chambers along the length direction, and adjacent reaction chambers are separated by flap valves (102) that can be opened and closed; a gas hole is provided on the partition of the flap valve (102) to allow gas to pass; the feed device (5) comprises a second frame (505), a raw material storage tank (501), and a screw conveyor (502); the screw conveyor (502) is mounted on the second frame (505), and the feed port of the screw conveyor (502) is connected upwardly The material outlet at the bottom of the raw material storage tank (501); the material outlet of the screw conveyor (502) and the material feed port of the fluorinated tube (1) are connected to the sealing box (503); in the sealing box (503), the material outlet of the screw conveyor (502) and the material feed port of the fluorinated tube (1) are rotatably connected via a rotary sealing joint; the rotary sealing joint connects the inside of the fluorinated tube (1) and the screw conveyor (502); the sealing box (503) is filled with sealing oil; an exhaust pipe (504) is arranged on the rotary sealing joint, the exhaust pipe (504) passes through the sealing box (503) upward, and the exhaust pipe (504) is connected to the air outlet of the exhaust pipe (504) through the sealing box (503); The pipeline is connected to the dust collector (10), the spray tower (11), and the fan (12) in sequence; the discharge device (6) comprises a transfer box (601) and a storage box (602); the discharge port of the fluorination tube (1) extends into the transfer box (601), the discharge port is arranged at the bottom of the transfer box (601), a discharge valve is arranged at the bottom of the discharge port, and the storage box (602) is arranged at the bottom of the transfer box (601); an air inlet pipe (603) is arranged in the transfer box (601), one end of the air inlet pipe (603) extends into the discharge port of the fluorination tube (1), and the other end passes through the transfer box (601) and is connected to the hydrogen fluoride gas supply device (8) through an air pipe.

2. The continuous fluorination reaction device according to claim 1, characterized in that: The fluorinated tube (1) is rotatably supported on a first frame (3) via a rotating bracket (2); the rotating bracket (2) comprises a bracket body (201) and a first supporting roller (202); two vertical plates arranged opposite to each other are provided on the bracket body (201); circular through holes are provided on the tops of the two vertical plates, and the fluorinated tube (1) passes through the through holes on the two vertical plates; a rotatable first supporting roller (202) is provided between the two vertical plates, and the first supporting roller (202) is supported on the outer surface of the fluorinated tube (1).

3. The continuous fluorination reaction device according to claim 2, characterized in that: A first annular rail (101) is arranged at the place where the fluorinated tube (1) passes through the through hole of the vertical plate; a rolling groove (101.1) is formed on the first annular rail (101), and the first supporting roller (202) rotates in the rolling groove (101.1).

4. The continuous fluorination reaction device according to claim 3, characterized in that: The rotating bracket (2) is provided with a brake mechanism (9), the brake mechanism (9) comprising a brake rotating frame (901), a friction member (902), and a brake telescopic drive (903); the brake rotating frame (901) comprises a first rotating shaft (901.1), a first connecting rod (901.2), and a second connecting rod (901.3); the first rotating shaft (901.1) is horizontally installed between two vertical plates; the two second connecting rods (901.3) are J-shaped, the two second connecting rods (901.3) are symmetrically arranged, and are connected in the middle by two first pins ( 901.4); the upper ends of the two second connecting rods (901.3) are rotatably connected to the first rotating shaft (901.1), and the lower ends of the two second connecting rods (901.3) are connected to the friction member (902); a horizontal plate is arranged on the top of the two vertical plates, and a brake telescopic drive (903) is installed on the horizontal plate; the top end of the first connecting rod (901.2) is hinged to the piston rod end of the brake telescopic drive (903), and the bottom end of the first connecting rod (901.2) is connected to the first pin shaft (901.4) between the two second connecting rods (901.3).

5. The continuous fluorination reaction device according to claim 4, characterized in that: The brake telescopic drive (903) adopts a double piston rod hydraulic cylinder, and two sets of brake rotating frames (901) and friction members (902) are symmetrically arranged on both sides of the double piston rod hydraulic cylinder.

6. The continuous fluorination reaction device according to claim 1, characterized in that: The heating device (7) is composed of two movable semi-cylindrical heating shells (701), and heat exchange tubes or heating resistors are arranged inside the heating shells (701).

7. A continuous fluorination reaction system, characterized in that: The continuous fluorination reaction device comprises any one of claims 1 to 6, and also comprises a feeding device, wherein the feeding device is installed on a working platform (13), and comprises a material receiving box (14) and a barrel dumping device, wherein the material receiving box (14) is mounted above the top opening of a raw material storage tank (501) through a bracket, and the bottom discharge port of the material receiving box (14) is connected to the top opening of the raw material storage tank (501); a dumping port (14.1) is arranged on the side of the material receiving box (14), and a barrel dumping device is mounted on one side of the dumping port (14.1) through a third frame (19), and the barrel dumping device is used for flipping and dumping a cylindrical raw material barrel (18).

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