Preparation equipment of high-purity electronic-grade molybdenum hexafluoride

Abstract

The invention relates to preparation equipment of high-purity electronic-grade molybdenum hexafluoride, which comprises a molybdenum hexafluoride reactor used for heating molybdenum powder and fluorine gas to react; the cyclone separator is connected to the discharge end of the molybdenum hexafluoride reactor and is used for carrying out gas-solid separation on the molybdenum hexafluoride original gas to obtain crude molybdenum hexafluoride gas; the variable-pressure condensation filter is connected to the gas outlet end of the cyclone separator, and the variable-pressure condensation filter is used for carrying out variable-pressure condensation on the molybdenum hexafluoride crude gas and filtering impurities solidified after condensation to obtain molybdenum hexafluoride crude liquid; the light component removal tower is connected to the liquid outlet end of the variable-pressure condensation filter, and hydrogen fluoride is removed from the molybdenum hexafluoride crude product liquid by the light component removal tower; the liquid inlet end of the bubble breaking rectifying tower is connected to the bottom of the light component removal tower, and the bubble breaking rectifying tower is used for purifying molybdenum hexafluoride in the molybdenum hexafluoride crude product liquid to obtain the electronic grade molybdenum hexafluoride.

Description

Technical Field

[0001] The present invention relates to the field of molybdenum hexafluoride preparation equipment, and in particular to a preparation equipment for high-purity electronic-grade molybdenum hexafluoride. Background Art

[0002] Molybdenum hexafluoride (MoF6) is the highest-valent fluoride of molybdenum and is an inorganic compound. In the presence of strong oxidants, MoF6 can corrode many metals. The main application of MoF6 is in the microelectronics industry, where it is used to deposit molybdenum silicide or molybdenum using chemical vapor deposition to produce low-resistance, high-melting-point interconnects. It is an important chemical for the preparation of microelectronics.

[0003] During the preparation process, molybdenum hexafluoride is prone to mixing with unreacted raw materials and producing incompletely reacted byproducts. Therefore, it needs to be purified after preparation. In the existing technology, crude molybdenum hexafluoride is generally purified through conventional gas-solid separation, condensation separation, distillation purification, etc. However, the existing technology does not yet purify the molybdenum hexafluoride according to the physical and chemical characteristics of molybdenum hexafluoride and impurities, making it difficult to prepare molybdenum hexafluoride to electronic grade.

[0004] The purpose of this invention is to design a preparation device for high-purity electronic-grade molybdenum hexafluoride in response to the above-mentioned problems in the prior art. Summary of the Invention

[0005] In response to the problems existing in the above-mentioned prior art, the present invention provides a preparation device for high-purity electronic-grade molybdenum hexafluoride, which can effectively solve at least one problem existing in the above-mentioned prior art.

[0006] The technical solution of the present invention is: A preparation device for high-purity electronic grade molybdenum hexafluoride, characterized by comprising: A molybdenum hexafluoride reactor, the feed end of which is connected to a molybdenum powder raw material tank and a fluorine gas raw material tank, for heating the molybdenum powder and fluorine gas to react and generate molybdenum hexafluoride raw gas; A cyclone separator is connected to the discharge end of the molybdenum hexafluoride reactor and is used to separate the molybdenum hexafluoride raw gas into gas and solid to obtain a crude molybdenum hexafluoride gas; A pressure-variable condensation filter is connected to the gas outlet of the cyclone separator, and the pressure-variable condensation filter performs pressure-variable condensation on the crude molybdenum hexafluoride gas and filters the impurities solidified after condensation to obtain a crude molybdenum hexafluoride liquid; The light removal tower is connected to the liquid outlet of the pressure transformer condensation filter, and the light removal tower removes hydrogen fluoride from the crude molybdenum hexafluoride liquid; The bubble-breaking distillation tower has its liquid inlet connected to the bottom of the lightness removal tower. The bubble-breaking distillation tower purifies the molybdenum hexafluoride in the crude molybdenum hexafluoride liquid to obtain electronic grade molybdenum hexafluoride.

[0007] Furthermore, the molybdenum hexafluoride reactor comprises: Reactor body; A top cover, the bottom of which is fixedly connected to the upper side of the reactor body, and an exhaust pipe is provided on the upper side of the top cover; The gas delivery pipe is located on the reactor body. A circular hole is opened on the outside of the reactor body, and the inner wall of the circular hole is fixedly connected to the outside of the gas delivery pipe; The feed pipe is located on the top cover, and an orifice is opened on the outside of the top cover. The inner wall of the orifice is fixedly connected to the outside of the feed pipe. A spiral rod is provided in the feed pipe, and the outside of the feed pipe is fixedly connected to a motor. The output end of the motor is connected to one end of the spiral rod through a coupling, and a feeding hopper is provided on the feed pipe; Electric heating tube, the electric heating tube is located in the reactor body; The waste heat recovery module is located on the reactor body and is used to recover and reuse the heat contained in the molybdenum hexafluoride gas generated by the reactor; The reaction enhancement module is located in the reactor body and is used to increase the contact area between the fluorine gas and the molybdenum powder in the reactor.

[0008] Furthermore, the waste heat recovery module includes a baffle, the outside of which is fixedly connected to the inner wall of the reactor body, a conical hole is provided on the baffle, a heat collecting tube is provided above the conical hole, two symmetrical hangers are fixedly connected to the upper side of the heat collecting tube, the outside of the hanger is fixedly connected to the inner wall of the reactor body, and a plurality of circumferentially equidistant grooves are provided at the bottom of the heat collecting tube, the inner walls of the grooves are fixedly connected to snowflake-shaped heat conducting plates, a fine hole is provided on the upper side of the heat collecting tube, a stirring paddle is movably connected in the fine hole, a motor 1 is fixedly connected to the upper side of the heat collecting tube, and the output end of the motor 1 is connected to the upper side of the stirring paddle through a coupling.

[0009] Furthermore, the pressure variable condensation filter comprises: The tank body is provided with a cold water inlet, a cold water outlet, a gas phase inlet, and a liquid phase outlet, and a low-temperature cavity is formed in the tank body; The condensation pipe is connected between the gas phase inlet and the liquid phase outlet, and the condensation pipe is immersed in the low temperature cavity; There are several controllable heat exchange layers, which are made of elastic and flexible materials. The condensation pipe is provided with several through holes in the middle and rear sections of the gas path, and the controllable heat exchange layers cover the through holes respectively. The pressed molded part is arranged in the condensing pipe and is spaced apart from the heat exchange controllable layer; The pressure member is provided in the tank body. After the pressure member applies pressure to the tank body, the heat exchange controllable layer expands into the condensation pipe and approaches the compression molding member. After the heat exchange controllable layer expands, the heat exchange efficiency is improved, and the semi-solid molybdenum pentafluoride adhered to the inner wall of the heat exchange controllable layer is filled between the compression molding member and the heat exchange controllable layer, so that the semi-solid molybdenum pentafluoride is cooled and solidified into molybdenum pentafluoride block crystals. After the pressure member releases pressure from the tank body, the heat exchange controllable layer contracts and the molybdenum pentafluoride block crystals fall off. The filter plate is arranged on one side of the condensation pipe close to the liquid phase outlet. The filter plate is used to intercept the molybdenum pentafluoride block crystals and filter the molybdenum pentafluoride fine crystals generated by condensation in the rear section of the condensation pipe through the molybdenum pentafluoride block crystals.

[0010] Furthermore, the condensation pipe is provided with a through hole in a region corresponding to an internal temperature of 60°C-67°C.

[0011] Furthermore, the pressurizing member includes a connecting cylinder, which is connected to the tank body. A piston is provided in the connecting cylinder, and the piston is driven by a corresponding piston driving cylinder. When the piston moves toward the inside of the tank body in the connecting cylinder, the inside of the tank body is pressurized.

[0012] Furthermore, the pressed molded part has an arc-shaped concave structure, and a plurality of protrusions are provided on one side of the pressed molded part close to the heat exchange controllable layer. The protrusions make the formed molybdenum pentafluoride block crystals have a plurality of fragile holes, and after the heat exchange controllable layer shrinks, the molybdenum pentafluoride block crystals break through the fragile holes.

[0013] Furthermore, movable fins are provided on the outer surface of the heat exchange controllable layer, which are used to adjust the heat exchange efficiency of the heat exchange controllable layer. When the heat exchange controllable layer is in a contracted state, the movable fins are close to the condensation pipe. When the heat exchange controllable layer is in an expanded state, the movable fins are away from the condensation pipe.

[0014] Furthermore, the bubble breaking distillation tower comprises: The distillation tower body is provided with a heavy component reflux port and a steam return port at the bottom of the distillation tower body, a light component reflux port and a steam outlet at the top of the distillation tower body, a plurality of guide plates are provided in the distillation tower body, and a first mounting bracket and a second mounting bracket are provided at the bottom of the distillation tower body, and the second mounting bracket is provided above the first mounting bracket; The distillation tower condenser is connected to the steam outlet and is used to condense the gas phase flow at the top of the distillation tower body to form reflux liquid; The reflux tank is connected between the condenser of the distillation column and the light component reflux port and is used to store and reflux the reflux liquid; The reboiler is connected between the heavy component reflux port and the steam return port and is used to heat and vaporize the heavy component liquid at the bottom of the distillation tower body; The bubble stretching and thinning mechanism is provided in a plurality of ways. The bubble stretching and thinning mechanism includes a gas guide frame, a fixed plate, and a bubble attachment plate. The first mounting bracket is provided with a plurality of bubble rising holes. The gas guide frame and the fixed plate are spaced apart and arranged on the first mounting bracket. The middle portion of the bubble attachment plate is laterally hinged to the top of the fixed plate. When the bubble attachment plate is not under stress, it blocks the opening of the gas guide frame. A gap is provided between the gas guide frame and the bubble attachment plate. There are several liquid driving devices, which are arranged on the second mounting bracket. The liquid driving devices are used to output liquid toward the top of the bubble attachment plate, thereby driving the bubble attachment plate to swing away from the fixed plate body. During the rapid swinging of the bubble attachment plate, the contact line between the foam corresponding to the fixed plate body and the bubble attachment plate is stretched and thinned. After an opening appears between the bubble attachment plate and the gas guide frame, the bubble attachment plate drives air to flow into the opening, thereby breaking the stretched and thinned part.

[0015] Furthermore, the liquid driving device includes a liquid receiving chamber, a liquid receiving port is provided at the top of the liquid receiving chamber, a nozzle is provided at the bottom of the liquid receiving chamber, the nozzle is directed toward the upper end of one of the bubble attachment plates, a movable plug is provided in the liquid receiving chamber, and the movable plug is driven by a corresponding movable plug driving cylinder; The liquid receiving port is arranged on the second mounting bracket at a position close to the inner wall of the distillation tower body, and the nozzle is arranged on the second mounting bracket at a position away from the inner wall of the distillation tower body. When the movable plug is away from the nozzle, the liquid receiving port is communicated with the liquid receiving chamber. A blocking ball is provided at the opening of the nozzle via a contraction spring. The blocking ball has a tendency to move closer to the opening of the nozzle and is provided with a liquid passage toward the upper end of one of the bubble attachment plates. When the movable plug driving cylinder drives the movable plug to move at a low speed, the blocking ball blocks the opening of the nozzle, and the liquid in the liquid receiving chamber is concentratedly sprayed to the upper end of the bubble attachment plate through the liquid channel, thereby driving the bubble attachment plate to swing; When the movable plug driving cylinder drives the movable plug to move at high speed, the liquid in the liquid receiving chamber will flush the blocking ball away from the opening of the nozzle. After the liquid flows out of the opening of the nozzle, it spreads to all sides under the action of the blocking ball.

[0016] Therefore, the present invention provides the following effects and / or advantages: This application utilizes a molybdenum hexafluoride reactor, cyclone separator, pressure-switching condensation filter, and bubble-breaking distillation column designed specifically for the specific characteristics of the molybdenum hexafluoride production process. These components implement the reaction, gas-solid separation, condensation filtration, and distillation steps of the molybdenum hexafluoride production process. Furthermore, by configuring the connections between the various devices, continuous synthesis of molybdenum hexafluoride is achieved.

[0017] The molybdenum hexafluoride reactor provided in the present application enables the device to utilize the waste heat contained in the produced molybdenum hexafluoride gas to preheat the molybdenum powder serving as the raw material, thereby reducing the heat consumption in the reactor body, ensuring that the temperature in the reactor body is always at the optimal reaction temperature, ensuring that the molybdenum powder can fully react with the fluorine gas, improving the device's conversion efficiency of the raw materials, and at the same time improving energy utilization.

[0018] The pressure-variable condensation filter provided in this application utilizes a design that utilizes a controllable heat exchange layer. This layer has expansion properties that can increase the contact area between the inner wall of the pipe and the molybdenum pentafluoride under pressurized conditions, thereby improving heat exchange efficiency. This changes the efficiency of molybdenum pentafluoride condensation and crystallization, causing the originally adhered semi-solidified molybdenum pentafluoride to quickly condense and solidify. Furthermore, through the cooperation of the controllable heat exchange layer and the pressed molding, the solidified molybdenum pentafluoride block crystals are broken up and separated from the controllable heat exchange layer, forming a gravel-like structure that is collected and intercepted by the filter plate. The molybdenum pentafluoride crystals then form a filter layer near the filter plate, further intercepting fine molybdenum pentafluoride crystals.

[0019] The bubble-breaking distillation tower provided in the present application utilizes the characteristics that molybdenum hexafluoride is in low-temperature distillation during the distillation process, and the impurities remaining in the bottom liquid are in a viscous state, which is easy to slowly generate large bubbles. The bubble attachment plate is driven to swing rapidly by the impact force of the liquid, and a shear force is generated at the contact line of the bubble, so that the contact line of the bubble is quickly stretched, thereby thinning the side wall of the bubble, and breaking the bubble through the flow of air in the bubble, so that the bubble is mechanically broken before rising, reducing the problem of internal high-pressure impurities ejected after the bubble bursts naturally.

[0020] Other features and advantages of the present invention will be described in the following description, and in part will become apparent from the description, or understood by practicing the present invention. The purpose and other advantages of the present invention are realized and obtained by the structures particularly pointed out in the description and the drawings.

[0021] It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 Schematic diagram of the structure of an embodiment of the present invention.

[0023] Figure 2 Schematic diagram of the overall structure of the molybdenum hexafluoride reactor.

[0024] Figure 3 This is a schematic diagram of the cross-sectional structure of a molybdenum hexafluoride reactor.

[0025] Figure 4 This is a schematic diagram of the waste heat recovery module structure of the molybdenum hexafluoride reactor.

[0026] Figure 5 Schematic diagram of the heat collecting tube structure of the molybdenum hexafluoride reactor.

[0027] Figure 6 This is a schematic diagram of the structure of the collecting box and heat collecting box of the molybdenum hexafluoride reactor.

[0028] Figure 7 Schematic diagram of the reaction enhancement module structure of the molybdenum hexafluoride reactor.

[0029] Figure 8 Schematic diagram of the annular tube structure of the molybdenum hexafluoride reactor.

[0030] Figure 9 Schematic diagram of the cleaning module structure of the molybdenum hexafluoride reactor.

[0031] Figure 10 This is a structural diagram of the pressure variable condensation filter.

[0032] Figure 11 2 is a cross-sectional view of a pressure swing condensation filter, wherein the heat exchange controllable layer is not expanded.

[0033] Figure 12 for Figure 11 An enlarged schematic diagram of part A.

[0034] Figure 13 A cross-sectional view of a pressure swing condensation filter with controllable layer expansion for heat exchange.

[0035] Figure 14 Schematic diagram of the exploded structure of the heat exchange controllable layer, pressed molded parts, and movable fins.

[0036] Figure 15 Schematic diagram of the structure of the raised part.

[0037] Figure 16 Schematic diagram of the state of molybdenum pentafluoride block crystals after being intercepted by the filter plate.

[0038] Figure 17 Schematic diagram of the structure of the bubble-breaking distillation tower.

[0039] Figure 18 This is a cross-sectional view of the bubble-breaking distillation tower.

[0040] Figure 19 for Figure 18 A partial enlarged schematic diagram of part B.

[0041] Figure 20 Schematic diagram of the structure of the bubble stretching and thinning mechanism and the liquid driving device.

[0042] Figure 21 Schematic diagram of the nozzle structure.

[0043] Figure 22 Schematic diagram of the working state when the blocking ball of the nozzle has not left the opening.

[0044] Figure 23 Schematic diagram of the working state of the nozzle when the blocking ball leaves the opening. DETAILED DESCRIPTION

[0045] In order to facilitate understanding by those skilled in the art, the structure of the present invention is further described in detail with reference to the embodiments and the accompanying drawings: refer to Figure 1 , a preparation device for high-purity electronic grade molybdenum hexafluoride, comprising: A molybdenum hexafluoride reactor 1, wherein the feed end of the molybdenum hexafluoride reactor 1 is connected to a molybdenum powder raw material tank and a fluorine gas raw material tank, and is used to heat the molybdenum powder and fluorine gas to react to generate molybdenum hexafluoride raw gas; A cyclone separator 2, connected to the discharge end of the molybdenum hexafluoride reactor 1, for performing gas-solid separation on the molybdenum hexafluoride raw gas to obtain a crude molybdenum hexafluoride gas; A pressure-switching condensation filter 3 connected to the gas outlet of the cyclone separator 2, the pressure-switching condensation filter 3 performs pressure-switching condensation on the crude molybdenum hexafluoride gas and filters the impurities solidified after condensation to obtain a crude molybdenum hexafluoride liquid; A light removal tower 5, connected to the liquid outlet of the pressure-switching condensation filter 3, for removing hydrogen fluoride from the crude molybdenum hexafluoride liquid; A bubble-breaking distillation tower 4, wherein the liquid inlet end of the bubble-breaking distillation tower 4 is connected to the bottom of the lightness removal tower 5, and the bubble-breaking distillation tower 4 purifies the molybdenum hexafluoride in the crude molybdenum hexafluoride liquid to obtain electronic grade molybdenum hexafluoride.

[0046] In this embodiment, molybdenum powder (Mo) and fluorine gas (F2) are added proportionally to a molybdenum hexafluoride reactor 1 for reaction. The raw MoF6 gas generated at 150-250°C undergoes gas-solid separation in a cyclone separator 2 to produce a crude MoF6 gas. The crude MoF6 gas then enters a pressure-switching condensation filter 3 for condensation. The condensed liquid is filtered through the pressure-switching condensation filter 3 to produce a crude MoF6 liquid. The filtered MoF6 crude liquid is then pumped into a lightness removal tower 5, where light components such as hydrogen fluoride are removed from the top of the tower at 20-100°C and atmospheric pressure. The bottoms of the lightness removal tower 5 are further distilled and purified in a bubble-breaking distillation tower 4. A high-purity product (99.999% MoF6) is obtained from the top of the bubble-breaking distillation tower 4 at 40-80°C and atmospheric pressure.

[0047] refer to Figure 2-3 , the molybdenum hexafluoride reactor 1 comprises: Reactor body 11; A top cover 12, the bottom of which is connected to the upper side of the reactor body 11 by bolts, and an exhaust pipe 13 is provided on the upper side of the top cover 12; The gas delivery pipe 14 is located on the reactor body 11. A circular hole is opened on the outside of the reactor body 11. The inner wall of the circular hole is connected to the outside of the gas delivery pipe 14 by bolts. The feed pipe 15 is located on the top cover 12. The top cover 12 has an opening on its exterior. The inner wall of the opening is connected to the exterior of the feed pipe 15 by bolts. A screw rod 111 is provided inside the feed pipe 15. The exterior of the feed pipe 15 is connected to a motor 112 by bolts. The output end of the motor 112 is connected to one end of the screw rod 111 by a coupling. A hopper 16 is provided on the feed pipe 15. The electric heating tube 110 is located in the reactor body 11; The waste heat recovery module 17 is located on the reactor body 11 and is used to recover and reuse the heat contained in the molybdenum hexafluoride gas generated by the reactor; The reaction efficiency enhancement module 18 is located in the reactor body 11 and is used to increase the contact area between the fluorine gas and the molybdenum powder in the reactor.

[0048] Specifically, the device utilizes the waste heat recovery module 17 to enable the device to utilize the waste heat contained in the produced molybdenum hexafluoride gas to preheat the molybdenum powder as the raw material, thereby reducing the heat consumption in the reactor body 11, ensuring that the temperature in the reactor body 11 is always at the optimal reaction temperature, ensuring that the molybdenum powder can fully react with the fluorine gas, improving the device's conversion efficiency of the raw materials, and at the same time improving energy utilization.

[0049] Reference Figure 4 、 Figure 5 and Figure 6In a preferred embodiment, the waste heat recovery module 17 includes a baffle 1701, the outside of the baffle 1701 is connected to the inner wall of the reactor body 11 by bolts, a conical hole 1702 is provided on the baffle 1701, a heat collecting tube 1703 is provided above the conical hole 1702, the upper side of the heat collecting tube 1703 is connected to two symmetrical hangers 1704 by bolts, the outside of the hanger 1704 is connected to the inner wall of the reactor body 11 by bolts, and the bottom of the heat collecting tube 1703 is provided with a plurality of circumferentially equidistant grooves, the inner walls of the grooves are all connected to snowflake-shaped heat conducting plates 1708 by bolts, and a fine hole is provided on the upper side of the heat collecting tube 1703, and a stirring paddle 17 is rotatably connected to the fine hole through a bearing. 10. The upper side of the heat collecting tube 1703 is connected to the motor 1709 by bolts, and the output end of the motor 1709 is connected to the upper side of the stirring paddle 1710 by a coupling; the outside of the heat collecting tube 1703 is provided with two symmetrical holes, and the holes are connected with the delivery pipes 1711 by bolts. The ends of the two delivery pipes 1711 away from the heat collecting tube 1703 pass through the top cover 12 and are connected to the same collection box 1713 by bolts. The collection box 1713 is located outside the reactor body 11, and the collection box 1713 is connected to the delivery pipe 1711. The bottom of the collection box 1713 is provided with multiple equally spaced rectangular openings, and the rectangular openings are connected with heat spreaders 1714 by bolts, and the outside of the multiple heat spreaders 1714 The same support frame 1712 is provided, the upper side of the support frame 1712 is connected to the bottom of the collection box 1713 by bolts, and the support frame 1712 is connected to the side opposite to the reactor body 11 by bolts; the outside of the collection box 1713 is connected to a pump 1715 by bolts, and the output end of the pump 1715 is connected to one of the delivery pipes 1711 through a conduit, and the outsides of the plurality of heat spreaders 1714 are slidably connected to the same heat collecting box 1716, and the bottom of the heat collecting box 1716 is connected to a support 1717 by bolts, and a base 1718 is provided below the support 1717, and the base 1718 is connected to the side opposite to the reactor body 11 by bolts, and the upper side of the base 1718 is connected to two There are two symmetrical hydraulic rods 1719, and the output ends of the hydraulic rods 1719 are connected to the bottom of the base 1717 by bolts. Two symmetrical narrow openings are opened on the outside of the heat collecting box 1716, and the inner walls of the narrow openings are connected to the guide pipes 1706 by bolts. The outside of the heat collecting box 1716 is connected to the second pump 1720 by bolts, and the output end of the second pump 1720 is connected to one of the guide pipes 1706 through a circular pipe; the two guide pipes 1706 are connected to the same hollow sleeve 1705 at one end away from the heat collecting box 1716 by bolts, and the guide pipes 1706 are connected to the hollow sleeve 1705. The hollow sleeve 1705 is located outside the feed pipe 15, and the outside of the hollow sleeve 1705 is provided with an insulation sleeve 1707.

[0050] Specifically, the motor 112 is started, and the motor 112 drives the screw 111 to rotate, pushing the molybdenum powder in the hopper 16 into the reactor body 11 through the feed pipe 15, and using the gas pipe 14 to transport the fluorine gas into the reactor body 11, and starting the electric heating tube 110. When the molybdenum powder and fluorine gas in the reactor body 11 react at high temperature to generate molybdenum hexafluoride gas, the gas blocked by the baffle 1701 will flow upward through the conical hole 1702 and flow out of the exhaust pipe 13, and the snowflake-shaped heat conducting plate 1708 will absorb the heat in the gas and heat the heat conducting oil in the heat collecting tube 1703, and start the motor 1709, and the motor 1709 drives the stirring The paddle 1710 rotates to stir the heat transfer oil, and the pump 1715 is started. The pump 1715 circulates the heat transfer oil in the collection box 1713 and the heat collecting tube 1703 through the delivery pipe 1711, so that the heat spreader 1714 transfers heat to the heat transfer oil in the heat collecting box 1716. The hydraulic rod 1719 is started, and the output end of the hydraulic rod 1719 is extended or shortened to control the depth of the heat spreader 1714 inserted into the heat collecting box 1716. The pump 1720 is started. The pump 1720 circulates the heat transfer oil in the heat collecting box 1716 and the hollow sleeve 1705 through the guide pipe 1706 to preheat the raw molybdenum powder in the feed pipe 15.

[0051] In a specific application scenario, the waste heat recovery module 17 is mainly suitable for the waste heat recovery link in the waste heat recovery process, that is, the waste heat recovery module 17 uses the snowflake-shaped heat conduction plate 1708 and the stirring paddle 1710 to enable the device to fully absorb the waste heat in the molybdenum hexafluoride gas flowing out of the conical hole 1702. The snowflake-shaped heat conduction plate 1708 with a large contact area is used to improve the heat absorption efficiency of the device. The two isolated heat conduction systems formed by the heat collecting tube 1703, the collecting box 1713, the heat spreader 1714 and the heat collecting box 1716 are used to effectively control the preheating temperature of the molybdenum powder. While ensuring the reaction effect of the molybdenum powder and the fluorine gas, it avoids the waste of raw materials caused by the premature reaction of the molybdenum powder with oxygen in the air due to overheating in the feed pipe 15.

[0052] Reference Figure 7 and Figure 8In a preferred embodiment, the reaction efficiency enhancement module 18 includes an annular frame 1801, the annular frame 1801 is located below the tapered hole 1702, the outside of the annular frame 1801 is connected to the inner wall of the reactor body 11 by bolts, the inner wall of the annular frame 1801 is connected to a plurality of circumferentially equidistantly distributed stabilizing springs 1802 by bolts, the ends of the plurality of stabilizing springs 1802 away from the annular frame 1801 are connected to the same fine-mesh sieve 1803 by bolts, and the upper side of the fine-mesh sieve 1803 is connected to a connecting frame 1804 by bolts; the upper side of the connecting frame 1804 is connected to an elliptical ring 1805 by bolts, and a driving motor 1807 is provided above the elliptical ring 1805, and the outer side of the driving motor 1807 is connected to the driving motor 1807. The reactor body 11 is connected to a heat shield 1808 by bolts, and the outside of the heat shield 1808 is connected to the inner wall of the reactor body 11 by bolts, and the output end of the drive motor 1807 is connected to a cam 1806 through a coupling, and the cam 1806 is located in the elliptical ring 1805, and the outside of the cam 1806 is in contact with the inner wall of the elliptical ring 1805; an annular tube 1809 is provided in the reactor body 11, and the annular tube 1809 is connected to the gas pipe 14, and a plurality of short tubes equidistantly distributed around the circumference are provided on the outside of the annular tube 1809, and the upper side of the short tubes are connected to a microporous diffuser head 1810 by bolts, and the microporous diffuser heads 1810 are all located below the fine-pore sieve 1803, and a cleaning module 19 is provided above the annular frame 1801.

[0053] Specifically, after the molybdenum powder in the feed pipe 15 falls into the fine-pore sieve 1803, the drive motor 1807 is started, and the drive motor 1807 drives the cam 1806 to rotate, so that the cam 1806 continuously contacts the short-radius inner wall of the elliptical ring 1805, so that the elliptical ring 1805 drives the fine-pore sieve 1803 to shake evenly, so that the molybdenum powder falls finely from the fine-pore sieve 1803 and contacts the fluorine gas diffused from the microporous diffusion head 1810 at high temperature, and the generated molybdenum hexafluoride gas flows upward from the orifice on the annular frame 1801.

[0054] In a specific application scenario, the reaction enhancement module 18 is mainly used in the reaction enhancement link of the reaction enhancement process, that is, the reaction enhancement module 18 uses the cam 1806 and the elliptical ring 1805 to make the fine-pore sieve 1803 evenly spread the molybdenum powder, increase the floating time of the molybdenum powder in the reactor body 11, and make the fluorine gas diffused from the microporous diffusion head 1810 fully mixed with the molybdenum powder, significantly increase the contact area between the fluorine gas and the molybdenum powder, and improve the reaction effect of the molybdenum powder and the fluorine gas, thereby reducing the generation rate of non-target gases or impurities and improving the reaction effect.

[0055] Reference Figure 9In a preferred embodiment, the cleaning module 19 includes a fixed ring 1901, the outside of the fixed ring 1901 is connected to the inner wall of the reactor body 11 by bolts, the inner wall of the fixed ring 1901 is connected to an inner gear ring 1902 by bolts, the inner wall of the fixed ring 1901 is slidably connected to a mounting frame 1903, the mounting frame 1903 is located below the fixed ring 1901, the inner wall of the mounting frame 1903 is connected to a rotating motor 1904 by bolts, the output end of the rotating motor 1904 passes through the mounting frame 1903 and is connected to a gear 1905 by a coupling, and the gear 1905 is meshed with the fixed ring 1901; the bottom of the mounting frame 1903 is connected to a scraper 1906 by bolts, and the outside of the scraper 1906 contacts the inner wall of the reactor body 11, and the bottom of the scraper 1906 is slidably connected to the upper side of the annular frame 1801.

[0056] Specifically, after the reactor body 11 has been used for a period of time, a layer of solid impurities mixed with molybdenum element and molybdenum tetrafluoride will gradually adhere to the inner wall of the reactor body 11. The rotating motor 1904 is started, and the rotating motor 1904 drives the gear 1905 engaged with the inner gear ring 1902 to rotate, so that the mounting frame 1903 moves along the inner wall of the fixed ring 1901, so that the scraper 1906 can scrape off the solid impurities attached to the inner wall of the reactor body 11.

[0057] In a specific application scenario, the cleaning module 19 is mainly suitable for the cleaning link in the cleaning process, that is, the cleaning module 19 uses the inner gear ring 1902 and the gear 1905 to enable the scraper 1906 to quickly and conveniently complete the cleaning of impurities on the inner wall of the reactor body 11, thereby reducing the impact of impurities on the reaction when the reactor body 11 reacts to generate molybdenum hexafluoride gas, and effectively ensuring the purity of the target gas generated in the reactor body 11.

[0058] Working principle: Start the motor 112, which drives the screw rod 111 to rotate, pushes the molybdenum powder in the hopper 16 into the reactor body 11 through the feed pipe 15, uses the gas pipe 14 to transport the fluorine gas into the reactor body 11, starts the electric heating tube 110, and when the molybdenum powder and fluorine gas in the reactor body 11 react at high temperature to generate molybdenum hexafluoride gas, the gas blocked by the baffle 1701 will flow upward through the conical hole 1702 and out of the exhaust pipe 13, and the snowflake-shaped heat conducting plate 1708 will absorb the heat in the gas and conduct heat to the heat collecting tube 1703 The oil is heated, and motor 1709 is started. Motor 1709 drives stirring paddle 1710 to rotate and stir the heat transfer oil. Pump 1715 is started. Pump 1715 circulates the heat transfer oil in collection box 1713 and heat collecting tube 1703 through delivery pipe 1711, so that heat plate 1714 transfers heat to the heat transfer oil in heat collecting box 1716. Hydraulic rod 1719 is started. The output end of hydraulic rod 1719 is extended or shortened to control the depth of heat transfer plate 1714 inserted into heat collecting box 1716. Pump 2 1720 is started. Pump 2 1720 circulates the heat transfer oil in collection box 1713 and heat collecting tube 1703 through delivery pipe 1711, so that heat plate 1714 transfers heat to the heat transfer oil in heat collecting box 1716. The flow pipe 1706 circulates the heat transfer oil in the heat collecting box 1716 and the hollow sleeve 1705 to preheat the raw molybdenum powder in the feed pipe 15. After the molybdenum powder in the feed pipe 15 falls into the fine-mesh sieve 1803, the drive motor 1807 is started. The drive motor 1807 drives the cam 1806 to rotate, so that the cam 1806 continuously contacts the short radius inner wall of the elliptical ring 1805, so that the elliptical ring 1805 drives the fine-mesh sieve 1803 to shake evenly, so that the molybdenum powder falls from the fine-mesh sieve 1803 finely and mixes with the molybdenum powder from the microporous diffusion head 181 at high temperature. 0 contacts the fluorine gas diffused from the reactor body 11, and the generated molybdenum hexafluoride gas flows upward from the hole on the annular frame 1801. After the reactor body 11 has been used for a period of time, a layer of solid impurities mixed with molybdenum element and molybdenum tetrafluoride will gradually adhere to the inner wall of the reactor body 11. The rotating motor 1904 is started, and the rotating motor 1904 drives the gear 1905 engaged with the inner gear ring 1902 to rotate, so that the mounting frame 1903 moves along the inner wall of the fixed ring 1901, so that the scraper 1906 can scrape off the solid impurities attached to the inner wall of the reactor body 11.

[0059] As the high-temperature crude molybdenum hexafluoride gas passes through the condensing device, the temperature of the high-temperature crude molybdenum hexafluoride gas will gradually decrease. When the crude molybdenum hexafluoride gas is cooled to between 60 and 67°C, the molybdenum pentafluoride therein will form a viscous semi-solid, thereby adhering to the side wall of the condensing device. When the crude molybdenum hexafluoride gas is cooled to between 40 and 60°C, the molybdenum pentafluoride therein will form fine crystals, making it difficult to be captured.

[0060] Therefore, reference Figure 10-16 , the pressure variable condensation filter 3 includes: The tank body 31 is provided with a cold water inlet 311, a cold water outlet 312, a gas phase inlet 313, and a liquid phase outlet 314, and a low-temperature cavity is formed in the tank body 31; In this embodiment, the cold water inlet 311 and the cold water outlet 312 are connected to the interior of the tank 31, thereby enabling cold water to circulate within the tank 31, forming a low-temperature chamber. Preferably, the cold water temperature of the cold water inlet 311 is 0-30°C, which can effectively cool and condense the molybdenum hexafluoride in the crude molybdenum hexafluoride gas into a liquid phase, while also cooling and condensing the molybdenum pentafluoride in the crude molybdenum hexafluoride gas into a solid phase.

[0061] A condensation pipe 32 is connected between the gas phase inlet 313 and the liquid phase outlet 314, and the condensation pipe 32 is immersed in the low temperature chamber; In this embodiment, the condensation pipe 32 is used to pass the crude molybdenum hexafluoride gas. Simultaneously, the crude molybdenum hexafluoride gas undergoes heat exchange with the surrounding cold water within the condensation pipe 32, thereby cooling and condensing the crude molybdenum hexafluoride gas. Furthermore, when the crude molybdenum hexafluoride gas enters the condensation pipe 32 at a high temperature, typically above 150°C, the temperature within the condensation pipe 32 gradually decreases along with the temperature of the gas path.

[0062] The heat exchange controllable layers 33 are multiple in number and are made of elastic and flexible material. The condensation pipe 32 is provided with multiple through holes in the middle and rear sections of the gas path, and the heat exchange controllable layers 33 respectively cover the through holes; In this embodiment, when the controllable heat exchange layer 33 is unstressed, it flatly covers the through-holes. At this point, the area of ​​the controllable heat exchange layer 33 is small, resulting in average heat exchange efficiency with the surrounding cold water. However, when the controllable heat exchange layer 33 is expanded by pressure, its area increases, increasing its efficiency. The controllable heat exchange layer 33 can be made of a corrosion-resistant elastomer such as perfluoroelastomer (FFKM).

[0063] A pressed molded part 34 is disposed in the condensing pipe 32 and spaced apart from the heat exchange controllable layer 33; A pressurizing member 35 is provided in the tank body 31. After the pressurizing member 35 applies pressure to the tank body 31, the heat exchange controllable layer 33 expands into the condensing pipe 32 and approaches the press-molded member 34. After the heat exchange controllable layer 33 expands, the heat exchange efficiency is improved, and the semi-solid molybdenum pentafluoride adhered to the inner wall of the heat exchange controllable layer 33 is filled between the press-molded member 34 and the heat exchange controllable layer 33, so that the semi-solid molybdenum pentafluoride is cooled and solidified into molybdenum pentafluoride block crystals. After the pressurizing member 35 releases pressure from the tank body 31, the heat exchange controllable layer 33 contracts and the molybdenum pentafluoride block crystals fall off. In this embodiment, the molybdenum pentafluoride in the middle and rear sections of the condensation pipe 32 condenses to form a cohesive semi-solid. A press-molding member 34 is positioned near the controllable heat exchange layer 33. After the controllable heat exchange layer 33 expands, it approaches or adheres to the press-molding member 34. Simultaneously, the press-molding member 34 compresses and molds the molybdenum pentafluoride semi-solid adhered to the inner wall of the controllable heat exchange layer 33. After condensing for a period of time, the molybdenum pentafluoride condenses to form an adhesive semi-solid attached to the inner surface of the unexpanded heat exchange controllable layer 33. At this time, the pressure member 35 pressurizes the inside of the tank body 31 to pressurize and expand the heat exchange controllable layer 33. On the one hand, the area of ​​the heat exchange controllable layer 33 increases after expansion, and the heat exchange efficiency with the surrounding cold water is significantly increased, so that the adhesive semi-solid molybdenum pentafluoride is quickly cooled and solidified into a solid state. On the other hand, the heat exchange controllable layer 33 drives the adhesive semi-solid molybdenum pentafluoride to approach or adhere to the pressing molding member 34, so that the adhesive semi-solid molybdenum pentafluoride is pressed and solidified to form a specific shape. Then, the pressing piece releases the pressure in the tank body 31. At this time, the heat exchange controllable layer 33 drives the solidified molybdenum pentafluoride block crystals away from the pressing molding piece 34. At the same time, the heat exchange controllable layer 33 contracts, causing the brittle molybdenum pentafluoride block crystals to separate from the molybdenum pentafluoride block crystals. At the same time, the molybdenum pentafluoride block crystals are fragile solids. During the contraction of the heat exchange controllable layer 33, the molybdenum pentafluoride block crystals are easily broken, resulting in several small block structures that flow toward the liquid phase outlet 314 together with the liquid phase inside the condensation pipe 32.

[0064] The filter plate 37 is arranged on one side of the condensation pipe 32 close to the liquid phase outlet 314. The filter plate 37 is used to intercept the molybdenum pentafluoride block crystals and filter the molybdenum pentafluoride fine crystals condensed in the rear section of the condensation pipe 32 through the molybdenum pentafluoride block crystals.

[0065] In the rear section of the condensation pipe 32, molybdenum pentafluoride condenses to form fine crystals. In this embodiment, the filter plate 37 can intercept the massive crystals of molybdenum pentafluoride. Furthermore, after the massive crystals of molybdenum pentafluoride irregularly converge on one side of the filter plate 37, the pores between the massive crystals and the cracks within the massive crystals can effectively intercept the fine crystals formed after the condensation of molybdenum pentafluoride. This can thereby separate the semi-solidified molybdenum pentafluoride adhering to the condensation pipe 32, and use the separated massive crystals of molybdenum pentafluoride as a filter material to filter out the fine crystals.

[0066] Furthermore, the through hole is provided in the region of the condensation pipe 32 corresponding to the internal temperature of 60° C.-67° C.

[0067] In this embodiment, since the semi-cured molybdenum pentafluoride deposit only forms in the condensation duct 32 within the corresponding internal temperature range of 60°C-67°C, providing a temperature in this region can better coordinate the condensation process. Temperature measurements can be taken at multiple points in the condensation duct 32 without a through hole to determine the 60°C-67°C region, and then a through hole can be provided in this region.

[0068] Furthermore, the pressed molded part 34 is an arc-shaped concave structure, and a plurality of protrusions 341 are provided on a side of the pressed molded part 34 close to the heat exchange controllable layer 33. The protrusions 341 cause the formed molybdenum pentafluoride block crystals to have a plurality of fragile holes, and after the heat exchange controllable layer 33 shrinks, the molybdenum pentafluoride block crystals are broken through the fragile holes.

[0069] In this embodiment, the raised portion 341 can control the structure of the formed molybdenum pentafluoride block crystals, forming a flat and porous structure. During the contraction of the controllable heat exchange layer 33, the molybdenum pentafluoride block crystals can be squeezed and folded, causing the molybdenum pentafluoride block crystals to fracture around the fragile pores and ultimately break, thereby forming fragmented molybdenum pentafluoride block crystals. Simultaneously, the pressed molding 34 can be supported and connected to the inner wall of the condensation duct 32 via a plurality of connecting rods, thereby allowing the pressed molding 34 to be suspended above the inner wall of the condensation duct 32. Dislodged molybdenum pentafluoride block crystals can better pass through the suspended space and flow backward with the internal liquid phase.

[0070] Furthermore, the raised portion 341 is a structure with a cross-sectional area gradually decreasing from an end close to the pressed molded part 34 to an end away from the pressed molded part 34 , and the top surface of the raised portion 341 is set as a cross-shaped raised structure.

[0071] In this embodiment, the gradually decreasing cross-sectional area of ​​the protrusions 341 allows the solidified molybdenum pentafluoride bulk crystals to form a trapezoidal structure. Furthermore, the molybdenum pentafluoride bulk crystals near the heat exchange controllable layer 33 have a thinner structure. This thinner structure allows them to collide with each other during the contraction of the heat exchange controllable layer 33, thereby breaking and squeezing the molybdenum pentafluoride bulk crystals, making it easier for the molybdenum pentafluoride bulk crystals to break away from the heat exchange controllable layer 33. Furthermore, the cross-shaped protrusions can form cross-shaped marks on the edges of the fragile pores of the molybdenum pentafluoride bulk crystals, facilitating their fracture.

[0072] Furthermore, the pressurizing member 35 includes a connecting cylinder 351, which is connected to the tank body 31. A piston 352 is provided in the connecting cylinder 351. The piston 352 is driven by a corresponding piston driving cylinder 353. When the piston 352 moves in the connecting cylinder 351 toward the interior of the tank body 31, the interior of the tank body 31 is pressurized.

[0073] In this embodiment, the pressure inside the tank body 31 is increased by pressing the piston 352 inward.

[0074] Furthermore, the cold water inlet 311 and the cold water outlet 312 are both provided with controllable valves. When the pressurizing member 35 is working, the controllable valves close the cold water inlet 311 and the cold water outlet 312 .

[0075] In this embodiment, after the controllable valve is closed, it can prevent the cold water from flowing out of the tank body 31 and thus releasing the pressure during the operation of the pressurizing member 35.

[0076] Furthermore, movable fins 36 are provided on the outer surface of the heat exchange controllable layer 33, and the movable fins 36 are used to adjust the heat exchange efficiency of the heat exchange controllable layer 33. When the heat exchange controllable layer 33 is in a contracted state, the movable fins 36 are close to the condensation pipe 32, and when the heat exchange controllable layer 33 is in an expanded state, the movable fins 36 are away from the condensation pipe 32.

[0077] Furthermore, the movable fin 36 is hinged to the outer surface of the heat exchange controllable layer 33, and a blocking plate 38 is provided on the outer surface of the condensation pipe 32 near the heat exchange controllable layer 33. The blocking plate 38 is provided with a fin passing hole. When the heat exchange controllable layer 33 is in a contracted state, the hinged end of the movable fin 36 is staggered with the fin passing hole.

[0078] In this embodiment, the movable fins 36 can help the heat exchange controllable layer 33 to further improve the heat exchange efficiency after expansion. When the heat exchange controllable layer 33 is in an expanded state, the movable fins 36 are away from the condensation pipe 32, thereby improving the contact efficiency between the movable fins 36 and the cold water, thereby improving the heat exchange efficiency, and making the heat exchange controllable layer 33 quickly cool down after expansion, thereby solidifying the semi-solidified molybdenum pentafluoride on the inner surface of the heat exchange controllable layer 33.

[0079] Through the structural design of the movable fins 36, when the heat exchange controllable layer 33 is in a contracted state, the hinged end of the movable fin 36 is close to the fin through-hole, so that it is squeezed by the staggered fin through-holes and contracts downward. When the heat exchange controllable layer 33 is in an expanded state, the hinged end of the movable fin 36 is away from the fin through-hole, and the fin through-hole swings the movable fin 36 outward to expand it.

[0080] Furthermore, a waste outlet 315 is included and is disposed on one side of the filter plate 37 .

[0081] In this embodiment, after the condensation filtration is completed, the waste outlet 315 can be opened to recover the molybdenum pentafluoride.

[0082] The control method of the pressure variable condensation filter 3 comprises the following steps: S1, filling the tank 31 with cold water, and inputting the crude molybdenum hexafluoride gas into the condensation pipe 32 to condense the crude molybdenum hexafluoride in the condensation pipe 32; S2 is executed every first time: controlling the pressurizing member 35 to pressurize the inside of the tank body 31 and maintaining the pressurization for the second time, so that the heat exchange controllable layer 33 expands into the condensing pipe 32 and approaches the pressing molding member 34, so that the semi-solid molybdenum pentafluoride is cooled and solidified into molybdenum pentafluoride block crystals, and then controlling the pressurizing member 35 to release the pressure in the tank body 31, so that the heat exchange controllable layer 33 shrinks and the molybdenum pentafluoride block crystals fall off.

[0083] The principle of the control method has been explained above.

[0084] The boiling point of molybdenum hexafluoride is about 34°C, and the boiling points of other impurities are much higher than that of molybdenum hexafluoride. In addition, during the purification process, on the one hand, the distillation tower adopts low-temperature distillation, and the bottom temperature of the distillation tower is generally controlled at about 40°C. The heating speed of the distillation tower is slow. On the other hand, during the distillation process, a large amount of molybdenum hexafluoride accumulates at the top of the distillation tower, and the impurities such as molybdenum tetrafluoride, molybdenum pentafluoride, and molybdenum oxyfluoride are left at the bottom of the tower. The impurities composed of molybdenum tetrafluoride, molybdenum pentafluoride, and molybdenum oxyfluoride are viscous. During the low-temperature heating process, the viscous bottom liquid will slowly form large bubbles. After the internal air pressure of the large bubbles slowly rises and bursts, the high-pressure gas inside the large bubbles is ejected outward. During the ejection process, impurities in the bottom liquid are easily ejected outward, thereby introducing impurities into the gas phase, resulting in poor distillation effect of the distillation tower.

[0085] Therefore, reference Figure 17-23 , the bubble breaking distillation tower 4 comprises: A distillation tower body 41 is provided with a heavy component reflux port 411 and a steam return port 412 at the bottom of the distillation tower body 41, a light component reflux port 413 and a steam outlet 414 at the top of the distillation tower body 41, a raw material inlet is provided in the middle of the distillation tower body 41, a plurality of guide plates 415 are provided in the distillation tower body 41, and a first mounting bracket 416 and a second mounting bracket 417 are provided at the bottom of the distillation tower body 41, with the second mounting bracket 417 being provided above the first mounting bracket 416; The distillation tower condenser 42 is connected to the steam outlet 414 and is used to condense the gas phase flow at the top of the distillation tower body 41 to form a reflux liquid; A reflux tank 43 is connected between the distillation tower condenser 42 and the light component reflux port 413 and is used to store and reflux the reflux liquid; The reboiler 44 is connected between the heavy component reflux port 411 and the steam return port, and is used to heat and vaporize the heavy component liquid at the bottom of the distillation tower body 41; In this embodiment, the distillation tower body 41, distillation tower condenser 42, reflux drum 43, and reboiler 44 are directly adapted from existing technologies. The principle in this embodiment is to use the reboiler 44 at the bottom to continuously heat and vaporize the liquid at the bottom of the tower, causing the liquid to vaporize and flow toward the top of the tower. The distillation tower condenser 42 condenses the gaseous phase flow at the top of the tower to form reflux liquid, which then returns to the top of the tower through the light component reflux port 413 and flows downward from the top of the tower. As the reflux liquid flows downward, it comes into contact with the gaseous phase flow produced by the reboiler 44. The gaseous phase flow and the reflux liquid exchange energy, and some of the energy in the gaseous phase flow is transferred to the reflux liquid, causing some of the reflux liquid to vaporize while absorbing heat during the downward flow, while some of the gaseous phase flow loses heat and liquefies during the upward flow. By continuously repeating this process, the lightest and lowest-boiling-point components in the liquid at the bottom of the tower are separated and brought to the top of the tower, where they are condensed and stored in the reflux drum 43, thereby achieving a purification effect.

[0086] There are several bubble stretching and thinning mechanisms 45, each comprising a gas guide frame 451, a fixed plate 452, and a bubble attachment plate 453. The first mounting bracket 416 is provided with a plurality of bubble rising holes 4161. The gas guide frame 451 and the fixed plate 452 are spaced apart on the first mounting bracket 416. The middle portion of the bubble attachment plate 453 is laterally hinged to the top of the fixed plate 452. When the bubble attachment plate 453 is not under stress, it blocks the opening of the gas guide frame 451. A gap is provided between the gas guide frame 451 and the bubble attachment plate 453. In this embodiment, the tower bottom liquid is a viscous, high-concentration impurity mixture of molybdenum tetrafluoride, molybdenum pentafluoride, and molybdenum oxyfluoride, while the tower top liquid is a liquid with a low boiling point of molybdenum hexafluoride. Bubbles generated by the tower bottom liquid slowly expand upward, and bubble riser holes 4161 provide a path for the bubbles generated by the tower bottom liquid to expand upward. After the bubbles expand upward, the gas guide frame 451 and the fixed plate 452 are spaced apart, allowing the bubbles to expand upward and extend into the space between them. There, the bubbles adhere to the space between the gas guide frame 451 and the fixed plate 452. A gap is provided between the gas guide frame 451 and the bubble attachment plate 453, allowing the bubbles to adhere to the space between the gas guide frame 451 and the bubble attachment plate 453, creating a contact line at their intersection. As the bubble attachment plate 453 oscillates, shear and tensile forces are exerted on the bubbles at the contact line.

[0087] There are several liquid driving devices 46, which are arranged on the second mounting bracket 417. The liquid driving devices 46 are used to output liquid toward the top of the bubble attachment plate 453, thereby driving the bubble attachment plate 453 to swing away from the fixed plate body 452. During the rapid swinging of the bubble attachment plate 453, the foam is stretched and thinned corresponding to the contact line between the fixed plate body 452 and the bubble attachment plate 453. After an opening appears between the bubble attachment plate 453 and the gas guide frame 451, the bubble attachment plate 453 drives air to flow into the opening, thereby breaking the stretched and thinned part.

[0088] As described above, after bubbles attach between the gas deflector frame 451 and the bubble attachment plate 453, a contact line is formed at the intersection. At this point, the liquid drive device 46 drives the bubble attachment plate 453 to swing away from the fixed plate 452. This rapidly increases the distance between the bubble attachment plate 453 and the fixed plate 452, stretching the bubble's contact line. The viscous liquid at the contact line is rapidly stretched, causing the position of the bubble's contact line to become thinner. Furthermore, since the bubble attaches between the bubble attachment plate 453 and the fixed plate 452, the bubble's volume can be considered unchanged at the moment of stretching. At this point, the bubble attachment plate 453 swings outward, increasing the distance between the bubble attachment plate 453 and the gas deflector frame 451. The air within the bubble is directed toward the increased space created by the swinging of the bubble attachment plate 453. Then, after an opening appears between the bubble attachment plate 453 and the gas guide frame 451, the air in the bubble is guided toward the opening between the bubble attachment plate 453 and the gas guide frame 451, and the internal air breaks through the contact line and is stretched to cover the part at the opening, so that the bubble can burst when the internal pressure is low. Therefore, the bubble can burst under low pressure, preventing the high pressure inside the bubble from causing the ejection effect after the burst, and preventing other impurities from being ejected outward to form gaseous impurities.

[0089] Furthermore, the liquid driving device 46 includes a liquid receiving chamber 461, the top of the liquid receiving chamber 461 is provided with a liquid receiving port 462, the bottom of the liquid receiving chamber 461 is provided with a nozzle 464, and the nozzle 464 is directed toward the upper end of one of the bubble attachment plates 453. A movable plug 465 is provided in the liquid receiving chamber 461, and the movable plug 465 is driven by a corresponding movable plug driving cylinder 466.

[0090] In this embodiment, the liquid receiving chamber 461 and the movable plug 465 form a structure similar to a syringe. When the movable plug 465 moves toward the nozzle 464, the movable plug 465 outputs the liquid in the liquid receiving chamber 461 through the nozzle 464. The liquid receiving port 462 is arranged at the top of the liquid receiving chamber 461. During the distillation process, the liquid phase flows downward from the top of the distillation tower body 41 and enters the liquid receiving chamber 461 through the liquid receiving port 462, and is temporarily stored in the liquid receiving chamber 461.

[0091] Furthermore, the liquid receiving port 462 is arranged on the second mounting bracket 417 at a position close to the inner wall of the distillation tower body 41, and the nozzle 464 is arranged on the second mounting bracket 417 at a position away from the inner wall of the distillation tower body 41. After the movable plug 465 is away from the nozzle 464, the liquid receiving port 462 is connected to the liquid receiving chamber 461.

[0092] In this embodiment, the position of the liquid receiving port 462 allows the liquid received by the liquid receiving port 462 to flow into the liquid receiving chamber 461 after the movable plug 465 exits the position of the liquid receiving port 462. At the same time, the driving cylinder extends into the liquid receiving chamber 461 and connects to the movable plug 465 through a sealed connection, thereby preventing the internal liquid from flowing out.

[0093] Furthermore, a blocking ball 468 is provided at the opening of the nozzle 464 via a contraction spring 469. The blocking ball 468 has a tendency to move closer to the opening of the nozzle 464. The blocking ball 468 has a liquid channel 467 formed toward the upper end of one of the bubble attachment plates 453. When the movable plug driving cylinder 466 drives the movable plug 465 to move at a low speed, the blocking ball 468 blocks the opening of the nozzle 464, and the liquid in the liquid receiving chamber 461 is concentratedly sprayed toward the upper end of the bubble attachment plate 453 through the liquid channel 467, thereby driving the bubble attachment plate 453 to swing; When the movable plug driving cylinder 466 drives the movable plug 465 to move at high speed, the liquid in the liquid receiving chamber 461 flushes the blocking ball 468 away from the opening of the nozzle 464. After the liquid flows out of the opening of the nozzle 464, it spreads to the surroundings under the action of the blocking ball 468.

[0094] In this embodiment, the shape of the liquid flowing out of nozzle 464 can be controlled by controlling the movement speed of movable plug 465. A blocking sphere 468 is positioned at the opening of nozzle 464 via a contraction spring 469. When movable plug 465 moves at a low speed, the pressure of the liquid prevents blocking sphere 468 from leaving the opening of nozzle 464. Consequently, liquid is ejected from liquid channel 467 of blocking sphere 468, forming a thin, high-speed stream of liquid that sprays the top of bubble attachment plate 453, causing it to oscillate. When movable plug 465 moves at a high speed, the pressure of the liquid forces blocking sphere 468 away from the opening of nozzle 464. At this point, the liquid, after flowing out of nozzle 464, is dispersed by the surface of blocking sphere 468 into an umbrella-like structure, which is then sprayed outward at a high flow rate. In this state, nozzle 464 can flush the bubble stretching and thinning mechanism 45 with the dispersed liquid, preventing viscous tower bottom liquid from continuously adhering to the surface of the bubble stretching and thinning mechanism 45 and affecting its performance.

[0095] Furthermore, the upper portion of the bubble attachment plate 453 is coated with an oleophobic layer.

[0096] In this embodiment, the oleophobic layer can prevent bubbles from adhering to and quickly climbing to the upper part of the bubble attachment plate 453, thereby generating larger bubbles. In this way, the oil phase inside the oily bubbles is not easy to spread on the surface of the bubble attachment plate 453, which is conducive to maintaining the stability of the spherical shape of the bubbles between the bubble attachment plate 453 and the gas guide frame 451.

[0097] Furthermore, the gas guide frame 451 and the bubble attachment plate 453 are respectively provided with serrated edges.

[0098] Furthermore, the serrated edge is an acute-angled serration, and the serrated edge of the gas guide frame 451 and the serrated edge of the bubble attachment plate 453 are complementary serrations.

[0099] In this embodiment, the serrated edge can increase the local curvature of the bubble at the contact line, limiting the spreading of the bubble at the structural edge of the gas guide frame 451 and the bubble attachment plate 453, thereby facilitating the rupture of the corresponding edge of the bubble when the bubble attachment plate 453 swings rapidly.

[0100] Furthermore, the width of the gas guide frame 451 is greater than the thickness of the bubble attachment plate 453 .

[0101] In this embodiment, the width of the gas guide frame 451 is relatively large. In the initial stage of the swinging of the bubble attachment plate 453, the movement of the bubble attachment plate 453 can drive the air in the bubble to flow into between the gas guide frame 451 and the bubble attachment plate 453, forming a vortex. In the second half of the swinging of the bubble attachment plate 453, a part of the bubble attachment plate 453 leaves the guide frame, and an opening is generated at this time. The gas flows into the opening to form a transient vortex and breaks through the bubble side wall corresponding to the opening, which can be more conducive to the bubble rupture.

[0102] Furthermore, an oleophilic layer is provided on the lower surface of the first mounting bracket 416 .

[0103] In this embodiment, the oleophilic layer provided on the first mounting bracket 416 can attract bubbles generated by the bottom liquid to the bottom of the tower to the bottom of the first mounting bracket 416 , and then through the gradual expansion of the bubbles, more bubbles can be concentrated on the bubble stretching and thinning mechanism 45 .

[0104] A control method for a distillation device for preparing high-purity electronic-grade molybdenum hexafluoride is further provided. The control method is based on the distillation device for preparing high-purity electronic-grade molybdenum hexafluoride, comprising the following steps: Every first distillation time, executing: controlling the liquid driving device 46 to centrally spray liquid toward the top of the bubble attachment plate 453, thereby driving the bubble attachment plate 453 to swing and burst the bubbles; Every second distillation time, the following is performed: controlling the liquid driving device 46 to output liquid in a scattered manner to flush the surface of the bubble stretching and thinning mechanism 45 , and the second distillation time is greater than the first distillation time.

[0105] In this embodiment, by lifting and switching the liquid output mode of the liquid driving device 46, it is possible to regularly switch between driving the bubble attachment plate 453 to swing and flushing the surface of the bubble stretching and thinning mechanism 45, thereby achieving a cleaning effect on the bubble attachment plate 453.

[0106] It should be noted that in the claims, any reference signs placed between parentheses shall not be construed as limiting the claims. The word "comprising" does not exclude the presence of components or steps not listed in the claim. The word "a" or "an" preceding a component does not exclude the presence of a plurality of such components. The invention can be implemented by means of hardware comprising several different components and by means of a suitably programmed computer. In a unit claim enumerating several means, several of these means may be embodied by one and the same item of hardware. The use of the words first, second, third etc. does not indicate any order. These words may be interpreted as names.

[0107] Although the preferred embodiments of the present invention have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention.

[0108] In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "connect," "fixed," etc. should be understood broadly. For example, they may refer to fixed connection, detachable connection, or integration; mechanical connection or electrical connection; direct connection or indirect connection through an intermediate medium; internal communication between two components or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0109] In the description of this specification, the reference terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" mean that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic expressions of the above terms should not be understood as necessarily referring to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification and features of different embodiments or examples without contradiction.

Claims

1. A preparation device for high-purity electronic grade molybdenum hexafluoride, characterized by: include: A molybdenum hexafluoride reactor (1), wherein a feed end of the molybdenum hexafluoride reactor (1) is connected to a molybdenum powder raw material tank and a fluorine gas raw material tank, and is used to heat the molybdenum powder and the fluorine gas to react and generate molybdenum hexafluoride raw gas; A cyclone separator (2), the cyclone separator (2) being connected to the discharge end of the molybdenum hexafluoride reactor (1) and used for performing gas-solid separation in the molybdenum hexafluoride raw gas to obtain a crude molybdenum hexafluoride gas; A pressure-variable condensation filter (3), the pressure-variable condensation filter (3) being connected to the gas outlet end of the cyclone separator (2), the pressure-variable condensation filter (3) performing pressure-variable condensation on the molybdenum hexafluoride crude gas and filtering impurities solidified after condensation to obtain a molybdenum hexafluoride crude liquid; A light removal tower (5), the light removal tower (5) is connected to the liquid outlet end of the pressure-variable condensation filter (3), and the light removal tower (5) removes hydrogen fluoride from the molybdenum hexafluoride crude liquid; A bubble-breaking distillation tower (4), wherein the liquid inlet end of the bubble-breaking distillation tower (4) is connected to the bottom of the lightness removal tower (5), and the bubble-breaking distillation tower (4) purifies the molybdenum hexafluoride in the molybdenum hexafluoride crude liquid to obtain electronic grade molybdenum hexafluoride.

2. The preparation equipment for high-purity electronic grade molybdenum hexafluoride according to claim 1, characterized in that: The molybdenum hexafluoride reactor (1) comprises: Reactor body (11); A top cover (12), wherein the bottom of the top cover (12) is fixedly connected to the upper side of the reactor body (11), and an exhaust pipe (13) is provided on the upper side of the top cover (12); An air delivery pipe (14), the air delivery pipe (14) being located on the reactor body (11), the reactor body (11) being provided with a circular hole on its exterior, the inner wall of the circular hole being fixedly connected to the exterior of the air delivery pipe (14); A feed pipe (15), the feed pipe (15) being located on the top cover (12), the top cover (12) being provided with an orifice on the outside, the inner wall of the orifice being fixedly connected to the outside of the feed pipe (15), a screw rod (111) being provided in the feed pipe (15), the outside of the feed pipe (15) being fixedly connected to an electric motor (112), the output end of the electric motor (112) being connected to one end of the screw rod (111) via a coupling, and a feeding hopper (16) being provided on the feed pipe (15); An electric heating pipe (110), wherein the electric heating pipe (110) is located in the reactor body (11); A waste heat recovery module (17), the waste heat recovery module (17) being located on the reactor body (11), and the waste heat recovery module (17) being used to recover and reuse the heat contained in the molybdenum hexafluoride gas generated by the reactor; A reaction efficiency enhancement module (18) is located in the reactor body (11), and the reaction efficiency enhancement module (18) is used to increase the contact area between the fluorine gas and the molybdenum powder in the reactor.

3. The preparation equipment for high-purity electronic grade molybdenum hexafluoride according to claim 2, characterized in that: The waste heat recovery module (17) comprises a baffle (1701), the exterior of the baffle (1701) being fixedly connected to the inner wall of the reactor body (11), a conical hole (1702) being provided on the baffle (1701), a heat collecting tube (1703) being provided above the conical hole (1702), two symmetrical hangers (1704) being fixedly connected to the upper side of the heat collecting tube (1703), the exterior of the hanger (1704) being fixedly connected to the reactor body (11), and the heat collecting tube (1703) being fixedly connected to the upper side of the heat collecting tube (1703). The inner wall of the heat collecting tube (1703) is fixedly connected, and a plurality of grooves equidistantly distributed around the circumference are provided at the bottom of the heat collecting tube (1703), and the inner walls of the grooves are fixedly connected to snowflake-shaped heat conducting plates (1708). Fine holes are provided on the upper side of the heat collecting tube (1703), and a stirring paddle (1710) is movably connected in the fine holes. The upper side of the heat collecting tube (1703) is fixedly connected to motor 1 (1709), and the output end of motor 1 (1709) is connected to the upper side of the stirring paddle (1710) through a coupling.

4. The preparation equipment for high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: The pressure variable condensation filter (3) comprises: A tank body (31), wherein the tank body (31) is provided with a cold water inlet (311), a cold water outlet (312), a gas phase inlet (313), and a liquid phase outlet (314), and a low-temperature cavity is formed in the tank body (31); a condensation pipe (32) connected between the gas phase inlet (313) and the liquid phase outlet (314), wherein the condensation pipe (32) is immersed in the low-temperature chamber; The heat exchange controllable layers (33) are provided in a plurality and are made of an elastic and flexible material. The condensation pipe (32) is provided with a plurality of through holes in the middle and rear sections of the gas path, and the heat exchange controllable layers (33) respectively cover the through holes. A pressed molded part (34) is arranged in the condensation pipe (32) and spaced apart from the heat exchange controllable layer (33); A pressurizing member (35) is provided in the tank body (31). After the pressurizing member (35) applies pressure to the tank body (31), the heat exchange controllable layer (33) expands into the condensing pipe (32) and approaches the pressed molding member (34). After the heat exchange controllable layer (33) expands, the heat exchange efficiency is improved, and the semi-solid molybdenum pentafluoride adhered to the inner wall of the heat exchange controllable layer (33) is filled between the pressed molding member (34) and the heat exchange controllable layer (33), so that the semi-solid molybdenum pentafluoride is cooled and solidified into molybdenum pentafluoride block crystals; after the pressurizing member (35) releases pressure in the tank body (31), the heat exchange controllable layer (33) shrinks and causes the molybdenum pentafluoride block crystals to fall off; The filter plate (37) is arranged on a side of the condensation pipe (32) close to the liquid phase outlet (314), and the filter plate (37) is used to intercept the molybdenum pentafluoride block crystals and filter the molybdenum pentafluoride fine crystals generated by condensation in the rear section of the condensation pipe (32) through the molybdenum pentafluoride block crystals.

5. The preparation equipment for high-purity electronic grade molybdenum hexafluoride according to claim 4, characterized in that: The condensation pipe (32) is provided with the through hole in a region corresponding to an internal temperature of 60°C-67°C.

6. The preparation equipment for high-purity electronic grade molybdenum hexafluoride according to claim 4, characterized in that: The pressurizing member (35) includes a connecting cylinder (351), the connecting cylinder (351) is connected to the tank body (31), a piston (352) is provided in the connecting cylinder (351), the piston (352) is driven by a corresponding piston driving cylinder (353), and when the piston (352) moves in the connecting cylinder (351) toward the inside of the tank body (31), the inside of the tank body (31) is pressurized.

7. The preparation equipment for high-purity electronic grade molybdenum hexafluoride according to claim 4, characterized in that: The pressed molded part (34) is an arc-shaped concave structure. A plurality of protrusions (341) are provided on a side of the pressed molded part (34) close to the heat exchange controllable layer (33). The protrusions (341) cause the formed molybdenum pentafluoride block crystals to have a plurality of fragile holes. After the heat exchange controllable layer (33) contracts, the molybdenum pentafluoride block crystals are broken through the fragile holes.

8. The preparation equipment for high-purity electronic-grade molybdenum hexafluoride according to claim 4, characterized in that: The outer surface of the heat exchange controllable layer (33) is provided with movable fins (36), and the movable fins (36) are used to adjust the heat exchange efficiency of the heat exchange controllable layer (33). When the heat exchange controllable layer (33) is in a contracted state, the movable fins (36) are close to the condensation pipe (32); when the heat exchange controllable layer (33) is in an expanded state, the movable fins (36) are away from the condensation pipe (32).

9. The preparation equipment for high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: The bubble breaking distillation tower (4) comprises: A distillation tower body (41), wherein a heavy component reflux port (411) and a steam return port (412) are provided at the bottom of the distillation tower body (41), a light component reflux port (413) and a steam outlet (414) are provided at the top of the distillation tower body (41), a plurality of guide plates (415) are provided in the distillation tower body (41), and a first mounting bracket (416) and a second mounting bracket (417) are provided at the bottom of the distillation tower body (41), wherein the second mounting bracket (417) is provided above the first mounting bracket (416); a distillation tower condenser (42), connected to the steam outlet (414), for condensing the gas phase flow at the top of the distillation tower body (41) to form a reflux liquid; a reflux tank (43), connected between the distillation tower condenser (42) and the light component reflux port (413), for storing and refluxing the reflux liquid; a reboiler (44), connected between the heavy component reflux port (411) and the steam return port, for heating and vaporizing the heavy component liquid at the bottom of the distillation tower body (41); A plurality of bubble stretching and thinning mechanisms (45), the bubble stretching and thinning mechanisms (45) comprising a gas guide frame (451), a fixed plate (452), and a bubble attachment plate (453), the first mounting bracket (416) being provided with a plurality of bubble rising through holes (4161), the gas guide frame (451) and the fixed plate (452) being spaced apart and arranged on the first mounting bracket (416), the middle portion of the bubble attachment plate (453) being laterally hinged to the top end of the fixed plate (452), the bubble attachment plate (453) shielding the opening of the gas guide frame (451) in an unstressed state, and a gap being provided between the gas guide frame (451) and the bubble attachment plate (453); A plurality of liquid drive devices (46) are provided on the second mounting bracket (417), wherein the liquid drive devices (46) are used to output liquid toward the top of the bubble attachment plate (453), thereby driving the bubble attachment plate (453) to swing away from the fixed plate body (452). During the rapid swinging of the bubble attachment plate (453), the foam is stretched and thinned corresponding to the contact line between the fixed plate body (452) and the bubble attachment plate (453). After an opening appears between the bubble attachment plate (453) and the gas guide frame (451), the bubble attachment plate (453) drives air to flow into the opening, thereby breaking the stretched and thinned portion.

10. The preparation equipment for high-purity electronic-grade molybdenum hexafluoride according to claim 9, characterized in that: The liquid driving device (46) includes a liquid receiving chamber (461), a liquid receiving port (462) is provided at the top of the liquid receiving chamber (461), a nozzle (464) is provided at the bottom of the liquid receiving chamber (461), the nozzle (464) is directed toward the upper end of one of the bubble attachment plates (453), and a movable plug (465) is provided in the liquid receiving chamber (461), and the movable plug (465) is driven by a corresponding movable plug driving cylinder (466); The liquid receiving port (462) is arranged on the second mounting bracket (417) at a position close to the inner wall of the distillation tower body (41), and the nozzle (464) is arranged on the second mounting bracket (417) at a position away from the inner wall of the distillation tower body (41), and after the movable plug (465) is away from the nozzle (464), the liquid receiving port (462) is communicated with the liquid receiving chamber (461); A blocking ball (468) is provided at the opening of the nozzle (464) via a contraction spring (469), the blocking ball (468) having a movement tendency to approach the opening of the nozzle (464), and the blocking ball (468) is provided with a liquid channel (467) toward the upper end of one of the bubble attachment plates (453); When the movable plug driving cylinder (466) drives the movable plug (465) to move at a low speed, the blocking ball (468) blocks the opening of the nozzle (464), and the liquid in the liquid receiving chamber (461) is centrally sprayed onto the upper end of the bubble attachment plate (453) through the liquid channel (467), thereby driving the bubble attachment plate (453) to swing; When the movable plug driving cylinder (466) drives the movable plug (465) to move at a high speed, the liquid in the liquid receiving chamber (461) flushes the blocking ball (468) away from the opening of the nozzle (464). After the liquid flows out of the opening of the nozzle (464), it is dispersed to all sides under the action of the blocking ball (468).

Images