Preparation process of high-purity electronic-grade molybdenum hexafluoride

Abstract

The invention relates to a preparation process of high-purity electronic-grade molybdenum hexafluoride. The preparation process comprises the following steps: S1, reacting molybdenum powder with fluorine gas at 150-250 DEG C to generate original molybdenum hexafluoride gas; s2, carrying out gas-solid separation on the molybdenum hexafluoride original gas to obtain a molybdenum hexafluoride crude product gas; s3, condensing the molybdenum hexafluoride crude product gas to obtain condensate and solid impurities, and filtering the solid impurities to obtain molybdenum hexafluoride crude product liquid; s4, removing light components from the molybdenum hexafluoride crude product liquid; and S5, rectifying and purifying the molybdenum hexafluoride crude product liquid to obtain the electronic grade molybdenum hexafluoride.

Description

Technical Field

[0001] This invention relates to the field of electronic-grade molybdenum hexafluoride preparation, specifically to a preparation process for high-purity electronic-grade molybdenum hexafluoride. Background Technology

[0002] Molybdenum hexafluoride (MoF6) is the highest valence fluoride of molybdenum and belongs to inorganic compounds. In the presence of strong oxidants, molybdenum hexafluoride can corrode many metals. The main application of molybdenum hexafluoride is in the microelectronics industry to use chemical vapor deposition of molybdenum silicide or molybdenum to make interconnects with low resistance and high melting point. It is an important chemical in the preparation of microelectronics.

[0003] During the preparation of molybdenum hexafluoride (MoF6), unreacted raw materials and incompletely reacted byproducts are easily introduced, necessitating purification after preparation. Current technologies typically purify crude MoF6 using conventional gas-solid separation, condensation separation, and distillation. However, existing technologies do not yet consider the physicochemical characteristics of MoF6 and its impurities, making it difficult to achieve electronic-grade MoF6.

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

[0005] To address the problems existing in the prior art, the present invention provides a preparation process for high-purity electronic-grade molybdenum hexafluoride, which can effectively solve at least one of the problems existing in the prior art.

[0006] The technical solution of this invention is:

[0007] A process for preparing high-purity electronic-grade molybdenum hexafluoride includes the following steps:

[0008] S1, molybdenum powder and fluorine gas are reacted at 150-250℃ to generate molybdenum hexafluoride primordial gas;

[0009] S2, gas-solid separation is performed on the original molybdenum hexafluoride gas to obtain crude molybdenum hexafluoride gas;

[0010] S3, condense the crude molybdenum hexafluoride gas to obtain condensate and solid impurities, and filter the solid impurities to obtain crude molybdenum hexafluoride liquid;

[0011] S4, for removing light components from crude molybdenum hexafluoride liquid;

[0012] S5, crude molybdenum hexafluoride is purified by liquid distillation to obtain electronic-grade molybdenum hexafluoride.

[0013] Further, step S1 is achieved via a molybdenum hexafluoride reactor, which includes:

[0014] Reactor body;

[0015] The top cover is fixedly connected to the top side of the reactor body at its bottom, and an exhaust pipe is provided on the top side of the top cover.

[0016] The gas supply 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 supply pipe.

[0017] The feed pipe is located on the top cover. An opening is provided on the outside of the top cover. The inner wall of the opening is fixedly connected to the outside of the feed pipe. A screw rod is installed inside the feed pipe. A motor is fixedly connected to the outside of the feed pipe. The output end of the motor is connected to one end of the screw rod through a coupling. A feeding hopper is provided on the feed pipe.

[0018] The heating element is located inside the reactor body;

[0019] 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.

[0020] The reaction enhancement module is located inside the reactor body and is used to increase the contact area between fluorine gas and molybdenum powder inside the reactor.

[0021] Further, step S3 is achieved through a pressure swing condenser filter, which includes:

[0022] The tank body is equipped with a cold water inlet, a cold water outlet, a gas phase inlet, and a liquid phase outlet, forming a low-temperature chamber inside the tank.

[0023] The condenser pipe connects the gas phase inlet and the liquid phase outlet, and is immersed in the low-temperature chamber.

[0024] The heat exchange controllable layer, which is made of a flexible material, has several through holes in the middle and rear section of the gas path of the condensation pipe, and the heat exchange controllable layer covers the through holes respectively.

[0025] The compressed molding component is installed inside the condensation pipe and spaced apart from the heat exchange controllable layer;

[0026] A pressurizing component, installed within the tank, pressurizes the tank, causing the controllable heat exchange layer to expand into the condensation pipe and approach the compression molding component. This expansion increases heat exchange efficiency, allowing the semi-solid molybdenum pentafluoride adhering to the inner wall of the controllable heat exchange layer to fill the space between the compression molding component and the controllable heat exchange layer. The semi-solid molybdenum pentafluoride then solidifies upon cooling, forming blocky molybdenum pentafluoride crystals. Depressurization of the tank by the pressurizing component causes the controllable heat exchange layer to contract and detach the blocky molybdenum pentafluoride crystals.

[0027] The filter plate is installed on the side of the condenser pipe near the liquid phase outlet. The filter plate is used to intercept molybdenum pentafluoride block crystals and filter the fine molybdenum pentafluoride crystals generated in the condenser pipe downstream through the molybdenum pentafluoride block crystals.

[0028] Furthermore, the condensation pipe has through holes in the area corresponding to an internal temperature of 60℃-67℃.

[0029] Furthermore, the pressed molding part has an arc-shaped concave structure, and the side of the pressed molding part near the heat exchange controllable layer is provided with several protrusions. The protrusions give the formed molybdenum pentafluoride block crystals several fragile holes. After the heat exchange controllable layer shrinks, the molybdenum pentafluoride block crystals break through the fragile holes.

[0030] The pressurizing component includes a connecting cylinder that connects to the tank. A piston is installed inside the connecting cylinder and is driven by a corresponding piston drive cylinder. When the piston moves inside the connecting cylinder toward the inside of the tank, it pressurizes the inside of the tank.

[0031] Furthermore, the outer surface of the heat exchange controllable layer is provided with movable fins. The movable fins 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 condenser pipe. When the heat exchange controllable layer is in an expanded state, the movable fins are away from the condenser pipe.

[0032] Furthermore, the operation of a swing condenser filter includes the following steps:

[0033] S31, fill the tank with cold water, and introduce crude molybdenum hexafluoride gas into the condensation pipe to condense the crude molybdenum hexafluoride in the condensation pipe;

[0034] S32, executed every first time interval: control the pressurizing component to pressurize the tank and maintain it for a second time, causing the heat exchange controllable layer to expand into the condensation pipe and approach the compression molding component, so that the semi-solid molybdenum pentafluoride is cooled and solidified into molybdenum pentafluoride block crystals, and then control the pressurizing component to depressurize the tank, so that the heat exchange controllable layer contracts and the molybdenum pentafluoride block crystals fall off.

[0035] Further, step S5 is performed in a defoaming distillation column, which includes:

[0036] The distillation column body has a heavy component reflux port and a vapor return port at the bottom and a light component reflux port and a vapor outlet at the top. Several guide plates are installed inside the distillation column body. A first mounting bracket and a second mounting bracket are installed at the bottom of the distillation column body, with the second mounting bracket positioned above the first mounting bracket.

[0037] The distillation column condenser is connected to the steam outlet and is used to condense the gaseous stream at the top of the distillation column to form reflux liquid.

[0038] A reflux tank, connected between the distillation column condenser and the light component reflux port, is used to store and reflux liquid;

[0039] A reboiler is connected between the heavy component reflux port and the vapor return port and is used to heat and vaporize the heavy component liquid at the bottom of the distillation column.

[0040] A bubble stretching and thinning mechanism, comprising a gas guide frame, a fixed plate, and a bubble attachment plate, wherein a first mounting bracket is provided with a number of bubble rising through holes, the gas guide frame and the fixed plate are spaced apart on the first mounting bracket, the middle part of the bubble attachment plate is laterally hinged to the top of the fixed plate, and the bubble attachment plate blocks the opening of the gas guide frame when not under stress, and a gap is provided between the gas guide frame and the bubble attachment plate;

[0041] Several liquid driving devices are installed 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. During the rapid swing of the bubble attachment plate, the contact line between the foam and the fixed plate is stretched and thinned. After the bubble attachment plate and the gas guide frame have an opening, the bubble attachment plate drives air to flow into the opening, thereby breaking the stretched and thinned part.

[0042] 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 faces the upper end of one of the bubble attachment plates, and a movable plug is provided inside the liquid receiving chamber, which is driven by a corresponding movable plug driving cylinder.

[0043] The liquid receiving port is located on the second mounting bracket near the inner wall of the distillation column, and the nozzle is located on the second mounting bracket away from the inner wall of the distillation column. After the movable plug moves away from the nozzle, the liquid receiving port is connected to the liquid receiving chamber.

[0044] A blocking ball is provided at the opening of the nozzle by means of a compression spring. The blocking ball has a tendency to move closer to the opening of the nozzle. The blocking ball has a liquid channel toward the upper end of one of the bubble attachment plates.

[0045] When the moving piston is driven by the cylinder to move at low speed, the blocking ball blocks the opening of the nozzle, and the liquid in the liquid receiving chamber is concentratedly sprayed onto the upper end of the bubble attachment plate through the liquid channel, thereby driving the bubble attachment plate to swing.

[0046] When the moving piston is driven by the cylinder, the liquid in the liquid receiving chamber will push the blocking ball away from the nozzle opening. After the liquid flows out of the nozzle opening, it will spread outwards under the action of the blocking ball.

[0047] Furthermore, in step S4, light components are removed under conditions of 20–100°C and normal pressure;

[0048] In step S5, the sample is purified by distillation at 40–80°C and atmospheric pressure.

[0049] Therefore, the present invention provides the following effects and / or advantages:

[0050] This application, tailored to the characteristics of the molybdenum hexafluoride (MoF6) preparation process, designs a MoF6 reactor, a cyclone separator, a pressure swing condenser filter, and a defoaming distillation column to realize the various steps of the MoF6 preparation process, including reaction, gas-solid separation, condensation filtration, and distillation. Furthermore, the connection method of each device enables the continuous synthesis of MoF6.

[0051] The molybdenum hexafluoride reactor provided in this application utilizes the waste heat contained in the produced molybdenum hexafluoride gas to heat the molybdenum powder used as 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 conversion efficiency of the raw materials of the device, and improving the energy utilization rate.

[0052] The variable pressure condenser filter provided in this application utilizes a heat exchange controllable layer design. This layer has expansion characteristics, which can increase the contact area between the inner wall of the pipe and molybdenum pentafluoride under pressurization, thereby improving heat exchange efficiency. This alters the efficiency of molybdenum pentafluoride condensation and crystallization, causing the originally adhered semi-cured molybdenum pentafluoride to rapidly condense and solidify. Through the cooperation of the heat exchange controllable layer and the compression molding component, the solidified molybdenum pentafluoride block crystals break up and detach from the heat exchange controllable layer, forming a gravel-like structure. After being collected and intercepted by the filter plate, the molybdenum pentafluoride crystals form a filter layer near the filter plate, further intercepting the fine molybdenum pentafluoride crystals.

[0053] The bubble-breaking distillation column provided in this application utilizes the characteristics of low-temperature distillation during molybdenum hexafluoride distillation, where the remaining impurities in the bottom liquid are viscous and easily generate large bubbles slowly. By driving the bubble attachment plate to swing rapidly through the liquid impact force, shear force is generated at the bubble contact line, causing the bubble contact line to be stretched rapidly, thereby thinning the sidewall of the bubble. The bubble is then broken by the flow of air inside the bubble, achieving mechanical breakage of the bubble before it rises, reducing the problem of high-pressure ejection of impurities inside the bubble after natural rupture.

[0054] Other features and advantages of the invention will be set forth in the following description, and will be apparent in part from the description, or may be learned by practicing the invention. The objects and other advantages of the invention are realized and obtained through the structures particularly pointed out in the description and the drawings.

[0055] It should be understood that the above summary and the following detailed description of the invention are exemplary and explanatory, and are intended to provide further explanation of the invention as claimed. Attached Figure Description

[0056] Figure 1 This is a schematic diagram of the preparation process of the present invention.

[0057] Figure 2 This is a schematic diagram of the overall structure of a molybdenum hexafluoride reactor.

[0058] Figure 3 This is a schematic cross-sectional view of a molybdenum hexafluoride reactor.

[0059] Figure 4 This is a schematic diagram of the waste heat recovery module of the molybdenum hexafluoride reactor.

[0060] Figure 5 This is a schematic diagram of the heat collection cylinder structure of a molybdenum hexafluoride reactor.

[0061] Figure 6 This is a schematic diagram of the collecting box and heat collection box structure of the molybdenum hexafluoride reactor.

[0062] Figure 7 This is a schematic diagram of the reaction enhancement module structure for a molybdenum hexafluoride reactor.

[0063] Figure 8 This is a schematic diagram of the annular tube structure of a molybdenum hexafluoride reactor.

[0064] Figure 9 This is a schematic diagram of the cleaning module structure of the molybdenum hexafluoride reactor.

[0065] Figure 10 This is a schematic diagram of a variable pressure condenser filter.

[0066] Figure 11 This is a cross-sectional view of a variable pressure condenser filter, in which the heat exchange controllable layer is not expanded.

[0067] Figure 12 for Figure 11 Enlarged schematic diagram of part A.

[0068] Figure 13 This is a cross-sectional view of a variable pressure condenser filter, in which the heat exchange controllable layer expands.

[0069] Figure 14 This is an exploded view of the structure of the heat exchange controllable layer, the compression molding component, and the movable fins.

[0070] Figure 15 This is a schematic diagram of the protrusion.

[0071] Figure 16This is a schematic diagram showing the state of molybdenum pentafluoride block crystals after they are intercepted by a filter plate.

[0072] Figure 17 This is a schematic diagram of the structure of a defoaming distillation column.

[0073] Figure 18 This is a cross-sectional view of a defoaming distillation column.

[0074] Figure 19 for Figure 18 A magnified view of part B.

[0075] Figure 20 This is a schematic diagram of the bubble stretching and thinning mechanism and the liquid driving device.

[0076] Figure 21 This is a schematic diagram of the nozzle structure.

[0077] Figure 22 This is a schematic diagram of the working state when the nozzle is blocked and the ball has not left the opening.

[0078] Figure 23 This is a schematic diagram of the working state when the clogging ball of the nozzle leaves the opening. Detailed Implementation

[0079] To facilitate understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings:

[0080] A process for preparing high-purity electronic-grade molybdenum hexafluoride includes the following steps:

[0081] S1, molybdenum powder and fluorine gas are reacted at 150-250℃ to generate molybdenum hexafluoride primordial gas;

[0082] S2, gas-solid separation is performed on the original molybdenum hexafluoride gas to obtain crude molybdenum hexafluoride gas;

[0083] S3, condense the crude molybdenum hexafluoride gas to obtain condensate and solid impurities, and filter the solid impurities to obtain crude molybdenum hexafluoride liquid;

[0084] S4, for removing light components from crude molybdenum hexafluoride liquid;

[0085] S5, crude molybdenum hexafluoride is purified by liquid distillation to obtain electronic-grade molybdenum hexafluoride.

[0086] In this embodiment, molybdenum powder and fluorine gas are reacted at 150–250°C to generate molybdenum hexafluoride (MoF6) raw gas. This raw gas includes MoF6, unreacted molybdenum powder and fluorine gas, incompletely reacted molybdenum tetrafluoride (MoF6), molybdenum pentafluoride (MoF6), and byproduct hydrogen fluoride. In step S2, gas-solid separation of the raw MoF6 raw gas separates some of the molybdenum powder, MoF6, and MoF6. In step S3, after condensing the crude MoF6 gas, MoF6 forms a liquid, while MoF6 and MoF6 solidify, allowing for filtration and separation. In step S4, removing light components from the crude MoF6 liquid removes light components such as hydrogen fluoride. In step S5, distillation purification of the crude MoF6 liquid separates the low-boiling-point MoF6 from other high-boiling-point impurities.

[0087] refer to Figure 1 The equipment corresponding to the preparation process may include:

[0088] The molybdenum hexafluoride reactor 1 is equipped with a molybdenum powder raw material tank and a fluorine gas raw material tank at its feed end, which are used to heat and react the molybdenum powder and fluorine gas to generate molybdenum hexafluoride raw gas.

[0089] Cyclone separator 2, which is connected to the discharge end of the molybdenum hexafluoride reactor 1, is used to separate the raw molybdenum hexafluoride gas into gas and solid, and obtain crude molybdenum hexafluoride gas.

[0090] A pressure swing condenser 3 is connected to the outlet of the cyclone separator 2. The pressure swing condenser 3 performs pressure swing condensation on the crude molybdenum hexafluoride gas and filters out the impurities that solidify after condensation to obtain crude molybdenum hexafluoride liquid.

[0091] Light fluoride removal tower 5 is connected to the liquid outlet of the pressure swing condenser 3, and the light fluoride removal tower 5 removes hydrogen fluoride from the crude molybdenum hexafluoride liquid;

[0092] The defoaming distillation column 4 is connected to the bottom of the light-light product removal column 5. The defoaming distillation column 4 purifies the molybdenum hexafluoride in the crude molybdenum hexafluoride liquid to obtain electronic-grade molybdenum hexafluoride.

[0093] refer to Figure 2-3 Step S1 is achieved through molybdenum hexafluoride reactor 1, which includes:

[0094] Reactor body 11;

[0095] The top cover 12 is bolted to the top side of the reactor body 11, and an exhaust pipe 13 is provided on the top side of the top cover 12.

[0096] Gas supply pipe 14 is located on reactor body 11. A circular hole is provided on the outside of reactor body 11. The inner wall of the circular hole is connected to the outside of gas supply pipe 14 by bolts.

[0097] Feed pipe 15 is located on top cover 12. The top cover 12 has an opening on its outside. The inner wall of the opening is connected to the outside of feed pipe 15 by bolts. A screw rod 111 is installed inside feed pipe 15. A motor 112 is connected to the outside of feed pipe 15 by bolts. The output end of motor 112 is connected to one end of screw rod 111 through a coupling. Feed hopper 16 is installed on feed pipe 15.

[0098] Heating element 110 is located inside reactor body 11;

[0099] Waste heat recovery module 17 is located on reactor body 11. Waste heat recovery module 17 is used to recover and reuse the heat contained in the molybdenum hexafluoride gas generated by the reactor.

[0100] The reaction enhancement module 18 is located inside the reactor body 11 and is used to increase the contact area between fluorine gas and molybdenum powder inside the reactor.

[0101] Specifically, the waste heat recovery module 17 allows the device to use the waste heat contained in the produced molybdenum hexafluoride gas to heat the molybdenum powder used as 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 raw materials, and improving energy utilization.

[0102] Reference Figure 4 , Figure 5 and Figure 6In a preferred embodiment, the waste heat recovery module 17 includes a baffle plate 1701. The outer side of the baffle plate 1701 is bolted to the inner wall of the reactor body 11. A conical hole 1702 is formed on the baffle plate 1701. A heat collection cylinder 1703 is arranged above the conical hole 1702. Two symmetrical hangers 1704 are bolted to the upper side of the heat collection cylinder 1703. The outer side of the hangers 1704 is bolted to the inner wall of the reactor body 11. The bottom of the heat collection cylinder 1703 has multiple circumferentially distributed grooves. The inner wall of each groove is bolted with a snowflake-shaped heat-conducting plate 1708. A fine hole is formed on the upper side of the heat collection cylinder 1703. A stirring paddle 17 is rotatably connected to the fine hole through a bearing. 10. A motor 1709 is bolted to the upper side of the heat collection cylinder 1703. The output end of the motor 1709 is connected to the upper side of the agitator 1710 via a coupling. Two symmetrical slots are formed on the outside of the heat collection cylinder 1703. A conveying pipe 1711 is bolted to each slot. The ends of the two conveying pipes 1711 away from the heat collection cylinder 1703 pass through the top cover 12 and are bolted to the same collecting box 1713. The collecting box 1713 is located outside the reactor body 11 and communicates with the conveying pipes 1711. Multiple equally spaced rectangular openings are formed at the bottom of the collecting box 1713. A heat spreader plate 1714 is bolted to each rectangular opening. The outer surfaces of the multiple heat spreaders plate 1714 are... A common support frame 1712 is provided, the upper side of which is bolted to the bottom of the collecting box 1713. The side of the support frame 1712 opposite to the reactor body 11 is also bolted. A pump 1715 is bolted to the outside of the collecting box 1713. The output end of the pump 1715 is connected to one of the delivery pipes 1711 via a conduit. A common heat collection box 1716 is slidably connected to the outside of multiple heat spreaders 1714. A base 1717 is bolted to the bottom of the heat collection box 1716. A base 1718 is provided below the base 1717. The side of the base 1718 opposite to the reactor body 11 is bolted, and two bolts are bolted to the upper side of the base 1718. A symmetrical hydraulic rod 1719, the output end of which is bolted to the bottom of the support 1717. The outer side of the heat collection box 1716 has two symmetrical narrow openings, the inner walls of which are bolted to guide pipes 1706. The outer side of the heat collection box 1716 is bolted to a second pump 1720, the output end of which is connected to one of the guide pipes 1706 through a round pipe. The ends of the two guide pipes 1706 away from the heat collection box 1716 are bolted to the same hollow sleeve 1705. The guide pipes 1706 are both connected to the hollow sleeve 1705. The hollow sleeve 1705 is located outside the feed pipe 15, and the outer side of the hollow sleeve 1705 is provided with an insulation sleeve 1707.

[0103] Specifically, the motor 112 is started, which drives the screw 111 to rotate, pushing the molybdenum powder in the feeding hopper 16 into the reactor body 11 through the feed pipe 15. Fluorine gas is then transported into the reactor body 11 via the gas supply pipe 14. The heating element 110 is started. 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 plate 1701, flows upward through the conical hole 1702 and exits from the exhaust pipe 13. The snowflake-shaped heat-conducting plate 1708 absorbs the heat from the gas and heats the heat-conducting oil in the heat collection cylinder 1703. The motor 1709 is started, driving the stirring... The paddle 1710 rotates to stir the heat transfer oil. Pump 1715 is started, and pump 1715 circulates the heat transfer oil in the collection box 1713 and the heat collection cylinder 1703 through the delivery pipe 1711, so that the heat spreader 1714 transfers heat to the heat transfer oil in the heat collection box 1716. The hydraulic rod 1719 is started, and the output end of the hydraulic rod 1719 extends or shortens to control the depth of the heat spreader 1714 inserted into the heat collection box 1716. Pump 2 1720 is started, and pump 2 1720 circulates the heat transfer oil in the heat collection box 1716 and the hollow sleeve 1705 through the guide pipe 1706 to preheat the raw material molybdenum powder in the feed pipe 15.

[0104] In specific application scenarios, the waste heat recovery module 17 is mainly suitable for the waste heat recovery process in the preheating recovery process. That is, the waste heat recovery module 17 uses the snowflake-shaped heat-conducting 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-conducting plate 1708, which has a large contact area, improves the device's heat absorption efficiency. The two mutually isolated heat conduction systems formed by the heat collection cylinder 1703, the collection box 1713, the heat spreader 1714, and the heat collection box 1716 effectively control the preheating temperature of the molybdenum powder. While ensuring the reaction effect of molybdenum powder and fluorine gas, it avoids the waste of raw materials caused by premature reaction with oxygen in the air due to overheating of molybdenum powder in the feed pipe 15.

[0105] Reference Figure 7 and Figure 8In a preferred embodiment, the reaction enhancement module 18 includes an annular frame 1801, located below the conical hole 1702. The outer side of the annular frame 1801 is bolted to the inner wall of the reactor body 11. Multiple circumferentially distributed stabilizing springs 1802 are bolted to the inner wall of the annular frame 1801. The ends of the multiple stabilizing springs 1802 away from the annular frame 1801 are bolted to the same fine-mesh sieve 1803. A connecting frame 1804 is bolted to the upper side of the fine-mesh sieve 1803. An elliptical ring 1805 is bolted to the upper side of the connecting frame 1804. A drive motor 1807 is positioned above the elliptical ring 1805. The reactor body 11 is bolted to a heat insulation cover 1808. The outer side of the heat insulation cover 1808 is bolted to the inner wall of the reactor body 11. The output end of the drive motor 1807 is connected to a cam 1806 via a coupling. The cam 1806 is located inside an elliptical ring 1805, and the outer side of the cam 1806 contacts the inner wall of the elliptical ring 1805. An annular tube 1809 is provided inside the reactor body 11. The annular tube 1809 is connected to a gas supply pipe 14. Multiple circumferentially distributed short tubes are provided on the outer side of the annular tube 1809. Microporous diffuser heads 1810 are bolted to the upper side of each short tube. The microporous diffuser heads 1810 are all located below the fine sieve 1803. A cleaning module 19 is provided above the annular frame 1801.

[0106] Specifically, 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 inner wall of the short radius of the elliptical ring 1805. This causes the elliptical ring 1805 to drive the fine-mesh sieve 1803 to shake evenly, so that the molybdenum powder falls finely from the fine-mesh sieve 1803 and comes into contact with the fluorine gas diffused from the microporous diffuser head 1810 at high temperature. The resulting molybdenum hexafluoride gas flows upward from the orifice on the ring frame 1801.

[0107] In specific application scenarios, the reaction enhancement module 18 is mainly used in the reaction enhancement stage 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 sieve 1803 evenly distribute 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 diffuser head 1810 fully mix with the molybdenum powder. This significantly increases the contact area between the fluorine gas and the molybdenum powder, improves 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.

[0108] Reference Figure 9In a preferred embodiment, the cleaning module 19 includes a fixing ring 1901. The outer side of the fixing ring 1901 is bolted to the inner wall of the reactor body 11. An internal toothed ring 1902 is bolted to the inner wall of the fixing ring 1901. A mounting frame 1903 is slidably connected to the inner wall of the fixing ring 1901. The mounting frame 1903 is located below the fixing ring 1901. A rotating motor 1904 is bolted to the inner wall of the mounting frame 1903. The output end of the rotating motor 1904 passes through the mounting frame 1903 and is connected to a gear 1905 via a coupling. The gear 1905 meshes with the fixing ring 1901. A scraper 1906 is bolted to the bottom of the mounting frame 1903. The outer side 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.

[0109] Specifically, after a period of use, the inner wall of the reactor body 11 will gradually be covered with a layer of solid impurities mixed with elemental molybdenum and molybdenum tetrafluoride. The rotating motor 1904 is started, and the rotating motor 1904 drives the gear 1905 that meshes with the internal gear ring 1902 to rotate, so that the mounting frame 1903 moves along the inner wall of the fixing ring 1901, thereby allowing the scraper 1906 to scrape off the solid impurities attached to the inner wall of the reactor body 11.

[0110] In specific application scenarios, the cleaning module 19 is mainly used in the cleaning process. That is, the cleaning module 19 uses the internal gear ring 1902 and gear 1905 to enable the scraper 1906 to quickly and conveniently clean the impurities on the inner wall of the reactor body 11, thereby reducing the impact of impurities on the reaction when molybdenum hexafluoride gas is generated in the reactor body 11, and effectively ensuring the purity of the target gas generated in the reactor body 11.

[0111] Working principle: The motor 112 is started, driving the screw 111 to rotate. This pushes the molybdenum powder in the feeding hopper 16 into the reactor body 11 through the feed pipe 15. Fluorine gas is then introduced into the reactor body 11 via the gas supply pipe 14. The heating element 110 is activated. When the molybdenum powder and fluorine gas react at high temperature to generate molybdenum hexafluoride gas in the reactor body 11, the gas, blocked by the baffle plate 1701, flows upward through the conical hole 1702 and exits through the exhaust pipe 13. The snowflake-shaped heat-conducting plate 1708 absorbs the heat from the gas and conducts it into the heat collection cylinder 1703. Oil heating begins with the start of motor 1709, which drives the agitator 1710 to stir the heat transfer oil. Pump 1715 is then started, circulating the heat transfer oil through pipe 1711 between the collection tank 1713 and the heat collector 1703, allowing the heat spreader 1714 to transfer heat to the heat transfer oil in the heat collector 1716. Hydraulic rod 1719 is activated, extending or retracting its output end to control the depth of the heat spreader 1714 inserted into the heat collector 1716. Finally, pump 1720 is started, circulating the heat transfer oil through pipe 1711... The flow pipe 1706 circulates the heat transfer oil in the heat collector box 1716 and the hollow sleeve 1705 to preheat the raw material 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. This causes the elliptical ring 1805 to drive the fine-mesh sieve 1803 to produce uniform shaking, so that the molybdenum powder falls finely from the fine-mesh sieve 1803 and, at high temperature, interacts with the raw material molybdenum powder from the microporous diffuser head 181. When the fluorine gas diffused from 0 comes into contact with the generated molybdenum hexafluoride gas, it flows upward from the orifice on the annular frame 1801. After a period of use, the inner wall of the reactor body 11 will gradually be covered with a layer of solid impurities mixed with elemental molybdenum and molybdenum tetrafluoride. The rotating motor 1904 is started, and the rotating motor 1904 drives the gear 1905 meshing with the internal gear ring 1902 to rotate, so that the mounting frame 1903 moves along the inner wall of the fixing ring 1901, thereby allowing the scraper 1906 to scrape off the solid impurities attached to the inner wall of the reactor body 11.

[0112] As the crude molybdenum hexafluoride gas passes through the condenser, its temperature gradually decreases. When the gas is cooled to between 60 and 67°C, the molybdenum pentafluoride within it forms a viscous semi-solid that adheres to the side wall of the condenser. When the gas is cooled to between 40 and 60°C, the molybdenum pentafluoride forms fine crystals that are difficult to capture.

[0113] Therefore, refer to Figure 10-16Step S3 is achieved through a pressure swing condenser filter 3, which includes:

[0114] 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 inside the tank body 31.

[0115] 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 the cold water to circulate inside the tank 31 and form a low-temperature chamber. Preferably, the cold water temperature of the cold water inlet 311 is 0-30°C. This temperature can better cool and condense the molybdenum hexafluoride in the crude molybdenum hexafluoride gas into a liquid phase, and at the same time cool and condense the molybdenum pentafluoride in the crude molybdenum hexafluoride gas into a solid phase.

[0116] 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;

[0117] In this embodiment, the condenser pipe 32 is used for the passage of crude molybdenum hexafluoride gas, and simultaneously allows the crude molybdenum hexafluoride gas to exchange heat with the surrounding cold water within the condenser pipe 32, thereby cooling and condensing the crude molybdenum hexafluoride gas. Furthermore, the crude molybdenum hexafluoride gas typically enters the condenser pipe 32 at a high temperature of above 150°C, and the temperature within the condenser pipe 32 gradually decreases along with the temperature of the gas path.

[0118] The heat exchange controllable layer 33, in several quantities, is made of an elastic and flexible material. The condensation pipe 32 has several through holes in the middle and rear section of the gas path, and the heat exchange controllable layer 33 covers the through holes respectively.

[0119] In this embodiment, when the heat exchange controllable layer 33 is not under stress, it lies flat covering the through-hole. At this time, the area of ​​the heat exchange controllable layer 33 is small, resulting in generally low efficiency in heat exchange with the surrounding cold water. However, when the heat exchange controllable layer 33 is under pressure and expands, its area increases, and the efficiency of heat exchange with the surrounding cold water increases. The heat exchange controllable layer 33 can be made of corrosion-resistant elastomers such as perfluoroelastomer rubber (FFKM).

[0120] The press-formed component 34 is disposed inside the condensation pipe 32 and spaced apart from the heat exchange controllable layer 33;

[0121] A pressurizing component 35 is disposed in the tank body 31. After the pressurizing component 35 pressurizes the tank body 31, the heat exchange controllable layer 33 expands into the condensation pipe 32 and approaches the compression molding component 34. After the heat exchange controllable layer 33 expands, the heat exchange efficiency is improved, and the semi-solid molybdenum pentafluoride adhering to the inner wall of the heat exchange controllable layer 33 fills the space between the compression molding component 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 component 35 depressurizes the tank body 31, the heat exchange controllable layer 33 contracts and the molybdenum pentafluoride block crystals fall off.

[0122] In this embodiment, in the middle and rear section of the condensation pipe 32, the molybdenum pentafluoride inside the condensation pipe 32 condenses to form an adhesive semi-solid. The compression molding part 34 is disposed near the heat exchange controllable layer 33. After the heat exchange controllable layer 33 expands, the heat exchange controllable layer 33 approaches or adheres to the compression molding part 34. At the same time, the compression molding part 34 is used to compress the molybdenum pentafluoride semi-solid adhering to the inner wall of the heat exchange controllable layer 33 into a molded shape. After a period of condensation, the molybdenum pentafluoride solidifies and forms an adhesive semi-solid that adheres to the inner surface of the unexpanded heat exchange controllable layer 33. At this time, the pressurizing component 35 pressurizes the tank 31, causing the heat exchange controllable layer 33 to expand under pressure. On the one hand, the expanded heat exchange controllable layer 33 has a larger area, which significantly increases the heat exchange efficiency with the surrounding cold water, causing the adhesive semi-solid molybdenum pentafluoride to cool rapidly and solidify into a solid. 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 component 34, so that the adhesive semi-solid molybdenum pentafluoride solidifies into a specific shape after pressing. Then, the pressure component depressurizes the tank 31. At this time, the heat exchange controllable layer 33 drives the solidified molybdenum pentafluoride block crystal away from the compression molding component 34. At the same time, the heat exchange controllable layer 33 contracts, causing the brittle molybdenum pentafluoride block crystal to detach from the molybdenum pentafluoride block crystal. Meanwhile, the molybdenum pentafluoride block crystal is a fragile solid, and it is easy to break the molybdenum pentafluoride block crystal during the contraction of the heat exchange controllable layer 33, making it into several small block structures that flow towards the liquid phase outlet 314 along with the liquid phase inside the condensation pipe 32.

[0123] A filter plate 37 is disposed on the side of the condensing pipe 32 near the liquid phase outlet 314. The filter plate 37 is used to intercept molybdenum pentafluoride block crystals and filter the fine molybdenum pentafluoride crystals generated by condensation in the latter part of the condensing pipe 32 through the molybdenum pentafluoride block crystals.

[0124] In the downstream section of the condensation pipe 32, molybdenum pentafluoride condenses to form fine crystals. In this embodiment, the filter plate 37 can intercept the blocky crystals of molybdenum pentafluoride. Simultaneously, after the blocky crystals of molybdenum pentafluoride irregularly gather on one side of the filter plate 37, the pores between the blocky crystals and the cracks in the blocky crystals effectively intercept the formation of fine crystals after the condensation of molybdenum pentafluoride. This achieves the function of detaching the semi-solidified molybdenum pentafluoride adhering to the condensation pipe 32 and using the detached blocky crystals of molybdenum pentafluoride as a filter material to filter the fine crystals of molybdenum pentafluoride.

[0125] Furthermore, the condensation pipe 32 is provided with through holes in the region corresponding to an internal temperature of 60°C-67°C.

[0126] In this embodiment, since the condenser pipe 32 only forms a semi-cured molybdenum pentafluoride adhesive in the region corresponding to an internal temperature of 60°C-67°C, setting this region allows for better coordination with the condensation process. Multiple temperature measurements can be performed on the condenser pipe 32 without through-holes to obtain the 60°C-67°C region, and then through-holes can be created in this region.

[0127] Furthermore, the compression molding part 34 has an arc-shaped concave structure. The side of the compression molding part 34 near the heat exchange controllable layer 33 is provided with a number of protrusions 341. The protrusions 341 give the formed molybdenum pentafluoride block crystals a number of fragile holes. After the heat exchange controllable layer 33 shrinks, the molybdenum pentafluoride block crystals break through the fragile holes.

[0128] In this embodiment, the protrusion 341 can control the structure of the formed molybdenum pentafluoride block crystals, making them flat and porous. During the contraction of the heat exchange controllable layer 33, the molybdenum pentafluoride block crystals can be squeezed and folded, causing them to break around the fragile pores and eventually fracture, thus forming fragmented molybdenum pentafluoride block crystals. Simultaneously, the pressed molding part 34 can be supported and connected to the inner wall of the condensing pipe 32 by several connecting rods, thereby allowing the pressed molding part 34 to be suspended above the inner wall of the condensing pipe 32. The detached molybdenum pentafluoride block crystals can then pass through the suspended space and flow backward with the internal liquid phase.

[0129] Furthermore, the protrusion 341 has a structure in which the cross-sectional area gradually decreases from one end close to the compression molding part 34 to the end away from the compression molding part 34, and the top surface of the protrusion 341 is configured as a cross-shaped protrusion structure.

[0130] In this embodiment, the gradually decreasing cross-sectional area of ​​the protrusion 341 allows the solidified molybdenum pentafluoride bulk crystals to form a trapezoidal structure. Simultaneously, the molybdenum pentafluoride bulk crystals near the heat exchange controllable layer 33 have a thinner structure. This thinner structure allows them to collide and break during the contraction of the heat exchange controllable layer 33, making it easier for the molybdenum pentafluoride bulk crystals to detach from the heat exchange controllable layer 33. Furthermore, the cross-shaped protrusion structure can create cross-shaped marks on the fragile pore edges of the molybdenum pentafluoride bulk crystals, facilitating their fracture.

[0131] Furthermore, the pressurizing component 35 includes a connecting cylinder 351, which communicates with the tank 31. A piston 352 is disposed inside the connecting cylinder 351. The piston 352 is driven by a corresponding piston drive cylinder 353. When the piston 352 moves inside the connecting cylinder 351 toward the inside of the tank 31, it pressurizes the inside of the tank 31.

[0132] In this embodiment, the pressure inside the tank 31 is increased by pressing the piston 352 inward.

[0133] Furthermore, both the cold water inlet 311 and the cold water outlet 312 are equipped with controllable valves. When the pressurizing component 35 is working, the controllable valves close the cold water inlet 311 and the cold water outlet 312.

[0134] In this embodiment, the controllable valve can prevent cold water from flowing out of the tank 31 and thus depressurizing during the operation of the pressurizing component 35.

[0135] Furthermore, the outer surface of the heat exchange controllable layer 33 is provided with movable fins 36. 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.

[0136] Furthermore, the movable fin 36 is hinged to the outer surface of the heat exchange controllable layer 33, and a baffle plate 38 is provided on the outer surface of the condensation pipe 32 near the heat exchange controllable layer 33. The baffle plate 38 has fin through holes. When the heat exchange controllable layer 33 is in a contracted state, the hinged end of the movable fin 36 is offset from the fin through holes.

[0137] In this embodiment, the movable fins 36 can help the heat exchange controllable layer 33 further improve the heat exchange efficiency after expansion. When the heat exchange controllable layer 33 is in an expanded state, the movable fins 36 move away from the condensation pipe 32, thereby improving the contact efficiency between the movable fins 36 and the cold water, thus improving the heat exchange efficiency. This allows the heat exchange controllable layer 33 to cool down rapidly after expansion, thereby solidifying the semi-cured molybdenum pentafluoride on the inner surface of the heat exchange controllable layer 33.

[0138] Through the structural design of the movable fin 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, and is thus squeezed downward by the staggered fin through hole. 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.

[0139] Furthermore, a waste outlet 315 is provided on one side of the filter plate 37.

[0140] In this embodiment, after the condensation filtration is completed, the waste outlet 315 can be opened to recover molybdenum pentafluoride.

[0141] The control method for the transformer condenser filter 3 includes the following steps:

[0142] S31, cold water is filled into the tank 31, and crude molybdenum hexafluoride gas is introduced into the condensation pipe 32 to condense the crude molybdenum hexafluoride in the condensation pipe 32.

[0143] S32, executed every first time interval: control the pressurizing component 35 to pressurize the tank 31 and maintain it for a second time, causing the heat exchange controllable layer 33 to expand into the condensation pipe 32 and approach the compression molding component 34, causing the semi-solid molybdenum pentafluoride to be cooled and solidified into molybdenum pentafluoride block crystals, and then control the pressurizing component 35 to depressurize the tank 31, causing the heat exchange controllable layer 33 to contract and the molybdenum pentafluoride block crystals to fall off.

[0144] The principle of the control method has been explained above.

[0145] Molybdenum hexafluoride has a boiling point of around 34°C, while the boiling points of other impurities are much higher. Furthermore, during the purification process, on the one hand, the distillation column employs low-temperature distillation, with the bottom temperature typically controlled at around 40°C, resulting in a slow heating rate. On the other hand, during distillation, a large amount of molybdenum hexafluoride accumulates at the top of the column, leaving impurities such as molybdenum tetrafluoride, molybdenum pentafluoride, and molybdenum oxyfluoride at the bottom. These impurities are viscous, and during low-temperature heating, the viscous bottom liquid slowly forms large bubbles. As the internal pressure of these large bubbles slowly rises and they burst, the high-pressure gas inside is ejected outwards. This ejection process easily carries impurities from the bottom liquid into the gas phase, leading to poor distillation efficiency.

[0146] Therefore, refer to Figure 17-23 Step S5 is implemented in the defoaming distillation column 4, which includes:

[0147] The distillation column body 41 has a heavy component reflux port 411 and a vapor return port 412 at its bottom end, a light component reflux port 413 and a vapor outlet 414 at its top end, a raw material inlet at its middle position, and several guide plates 415 inside the distillation column body 41. A first mounting bracket 416 and a second mounting bracket 417 are provided at the bottom of the distillation column body 41, with the second mounting bracket 417 positioned above the first mounting bracket 416.

[0148] The distillation column condenser 42 is connected to the steam outlet 414 and is used to condense the gaseous stream at the top of the distillation column body 41 to form reflux liquid.

[0149] The reflux tank 43 is connected between the distillation column condenser 42 and the light component reflux port 413, and is used to store and reflux the reflux liquid;

[0150] The reboiler 44 is connected between the heavy component reflux port 411 and the vapor return port, and is used to heat and vaporize the heavy component liquid at the bottom of the distillation column body 41.

[0151] In this embodiment, the distillation column body 41, distillation column condenser 42, reflux tank 43, and reboiler 44 are directly adopted from existing technologies. The principle in this embodiment is to continuously heat and vaporize the liquid at the bottom of the column using the reboiler 44, causing the liquid to vaporize and flow towards the top of the column. The distillation column condenser 42 condenses the vapor stream from the top of the column to form reflux liquid, which then returns to the top of the column through the light component reflux port 413 and flows downwards from the top. During the downward flow of the reflux liquid, it comes into contact with the vapor stream generated by the reboiler 44, exchanging energy. Part of the energy in the vapor stream is transferred to the reflux liquid, causing part of the reflux liquid to vaporize during the downward flow and part of the vapor stream to liquefy during the upward flow. By continuously repeating the above process, the lighter and lower boiling point components in the liquid at the bottom of the column can be separated to the top of the column and condensed and stored in the reflux tank 43, thereby achieving a purification effect.

[0152] A number of bubble stretching and thinning mechanisms 45 are provided. Each bubble stretching and thinning mechanism 45 includes a gas guiding frame 451, a fixed plate 452, and a bubble attachment plate 453. A first mounting bracket 416 is provided with a number of bubble rising through holes 4161. The gas guiding frame 451 and the fixed plate 452 are spaced apart on the first mounting bracket 416. The middle part 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 force, it blocks the opening of the gas guiding frame 451. The gas guiding frame 451 and the bubble attachment plate 453 are spaced apart.

[0153] In this embodiment, the bottom liquid is a viscous, high-concentration impurity composed of molybdenum tetrafluoride, molybdenum pentafluoride, and molybdenum oxyfluoride, while the top liquid is a liquid with a low boiling point, molybdenum hexafluoride. Bubbles generated in the bottom liquid slowly expand upwards. A bubble rising through-hole 4161 provides a pathway for the upward expansion of these bubbles. After expansion, the gas guide frame 451 and the fixed plate 452 are spaced apart, allowing the expanded bubbles to extend into the space between them and adhere to the space between them. The gas guide frame 451 and the fixed plate 452 are also spaced apart, creating a contact line at their interface. During the oscillation of the bubble attachment plate 453, a shearing and tensile force is generated at the contact line of the bubbles.

[0154] Several liquid driving devices 46 are disposed 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 452. During the rapid swinging process, the bubble attachment plate 453 stretches and thins the contact line between the foam and the fixed plate 452 and the bubble attachment plate 453. After the bubble attachment plate 453 and the gas guide frame 451 form an opening, the bubble attachment plate 453 drives air to flow into the opening, thereby breaking the stretched and thinned part.

[0155] The above describes how, after a bubble adheres to the gas guide frame 451 and the bubble attachment plate 453, a contact line is formed at the interface. At this time, the liquid driving 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, and the contact line of the bubble is stretched, causing the viscous liquid in the contact line to thin out. Furthermore, since the bubble is attached between the bubble attachment plate 453 and the fixed plate 452, its volume can be considered constant at the moment of stretching. As the bubble attachment plate 453 swings outward, the distance between it and the gas guide frame 451 increases, and the air inside the bubble is guided into the increased space created by the swinging of the bubble attachment plate 453. Then, after the bubble attachment plate 453 and the gas guide frame 451 form an opening, the air inside the bubble is guided to the opening of the bubble attachment plate 453 and the gas guide frame 451. The internal air breaks through the contact line and is stretched to cover the part at the opening, so that the bubble can rupture when the internal pressure is low. Therefore, the bubble can rupture under low pressure, preventing the high pressure inside the bubble from causing the ejection effect after rupture, and preventing other impurities from being ejected outward to form gaseous impurities.

[0156] Furthermore, the liquid driving device 46 includes a liquid receiving cavity 461, with a liquid receiving port 462 at the top and a nozzle 464 at the bottom, the nozzle 464 facing the upper end of one of the bubble attachment plates 453. A movable plug 465 is provided inside the liquid receiving cavity 461, and the movable plug 465 is driven by a corresponding movable plug driving cylinder 466.

[0157] 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 located at the top of the liquid receiving chamber 461. During the distillation process, the liquid phase flows downward from the top of the distillation column body 41 and enters the liquid receiving chamber 461 through the liquid receiving port 462, where it is temporarily stored.

[0158] Furthermore, the liquid receiving port 462 is located on the second mounting bracket 417 near the inner wall of the distillation column body 41, and the nozzle 464 is located on the second mounting bracket 417 away from the inner wall of the distillation column body 41. After the movable plug 465 moves away from the nozzle 464, the liquid receiving port 462 communicates with the liquid receiving cavity 461.

[0159] 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 cavity 461 after the movable plug 465 retracts from the position of the liquid receiving port 462. At the same time, the drive cylinder extends into the liquid receiving cavity 461 and connects with the movable plug 465 through a sealed connection, thereby preventing the internal liquid from flowing out.

[0160] Furthermore, a blocking ball 468 is provided at the opening of the nozzle 464 by means of 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 facing the upper end of one of the bubble attachment plates 453.

[0161] When the movable plug drive 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 onto the upper end of the bubble attachment plate 453 through the liquid channel 467, thereby driving the bubble attachment plate 453 to swing.

[0162] When the movable plug drive cylinder 466 drives the movable plug 465 to move at high speed, the liquid in the liquid receiving cavity 461 pushes 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 outward under the action of the blocking ball 468.

[0163] In this embodiment, the flow pattern of liquid from nozzle 464 can be controlled by controlling the moving speed of the movable plug 465. A blocking ball 468 is installed at the opening of nozzle 464 via a contraction spring 469. When the movable plug 465 moves at low speed, the liquid pressure is insufficient to force the blocking ball 468 out of the nozzle 464 opening, allowing liquid to spray out from the liquid channel 467 of the blocking ball 468, forming a long, high-speed liquid stream that can spray the top of the bubble attachment plate 453, causing the bubble attachment plate 453 to oscillate. When the movable plug 465 moves at high speed, the liquid pressure forces the blocking ball 468 out of the nozzle 464 opening. At this time, the liquid flowing out of nozzle 464 is dispersed into an umbrella-like structure by the surface of the blocking ball 468 and sprayed outwards at a relatively large flow rate. In this state, nozzle 464 can flush the bubble stretching and thinning mechanism 45 with the dispersed liquid, preventing the viscous bottom liquid from continuously adhering to the surface of the bubble stretching and thinning mechanism 45 and affecting its working effect.

[0164] Furthermore, the upper portion of the bubble attachment plate 453 is coated with an oleophobic layer.

[0165] In this embodiment, the oleophobic layer can prevent bubbles from adhering 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 beneficial to maintaining the stability of the spherical shape of the bubbles between the bubble attachment plate 453 and the gas guide frame 451.

[0166] Furthermore, the gas guide frame 451 and the bubble attachment plate 453 are respectively provided with serrated edges.

[0167] 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.

[0168] In this embodiment, the serrated edge can increase the local curvature of the bubble at the contact line, restricting the spread of the bubble at the structural edges of the gas guide frame 451 and the bubble attachment plate 453, thereby forming a situation where the corresponding edge of the bubble will break when the bubble attachment plate 453 swings rapidly.

[0169] Furthermore, the width of the gas guiding frame 451 is greater than the thickness of the bubble attachment plate 453.

[0170] In this embodiment, the width of the gas guiding frame 451 is relatively large. In the initial stage of the bubble attachment plate 453 swinging, the movement of the bubble attachment plate 453 can drive the air inside the bubble to flow into the gas guiding frame 451 and the bubble attachment plate 453, forming a vortex. In the latter half of the swinging stage of the bubble attachment plate 453, a part of the bubble attachment plate 453 leaves the guiding frame, at which time an opening is generated. Gas rushes into the opening to form a transient vortex and breaks through the bubble sidewall corresponding to the opening, which is more conducive to bubble rupture.

[0171] Furthermore, the lower surface of the first mounting bracket 416 is provided with an oleophilic layer.

[0172] In this embodiment, the oleophilic layer provided on the first mounting bracket 416 can attract the bubbles generated by the bottom liquid to the area below the first mounting bracket 416, and through the gradual expansion of the bubbles, the bubbles can be concentrated more in the bubble stretching and thinning mechanism 45.

[0173] A further method for controlling a distillation apparatus for preparing high-purity electronic-grade molybdenum hexafluoride is provided, comprising the following steps based on the aforementioned distillation apparatus for preparing high-purity electronic-grade molybdenum hexafluoride:

[0174] Every first distillation time, the following is performed: control the liquid driving device 46 to concentrate the liquid spray towards the top of the bubble attachment plate 453, thereby driving the bubble attachment plate 453 to swing and cause the bubbles to burst.

[0175] Every second distillation time, the liquid driving device 46 is controlled to output liquid in a manner that disperses in all directions, thereby rinsing the surface of the bubble stretching and thinning mechanism 45, wherein the second distillation time is longer than the first distillation time.

[0176] In this embodiment, by lifting and switching the liquid output mode of the liquid driving device 46, the device can periodically switch between driving the bubble attachment plate 453 to swing and rinsing the surface of the bubble stretching and thinning mechanism 45, thereby achieving the cleaning effect on the bubble attachment plate 453.

[0177] It should be noted that any reference signs placed between parentheses in the claims should not be construed as limiting the claims. The word "comprising" does not exclude the presence of components or steps not listed in the claims. 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 the same item of hardware. The use of the words first, second, and third, etc., does not indicate any order. These words can be interpreted as names.

[0178] Although preferred embodiments of the invention have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of the invention.

[0179] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0180] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms should not be construed as necessarily referring to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

Claims

1. A preparation process for high-purity electronic-grade molybdenum hexafluoride, characterized in that: Includes the following steps: S1, molybdenum powder and fluorine gas are reacted at 150-250℃ to generate molybdenum hexafluoride primordial gas; S2, perform gas-solid separation on the original molybdenum hexafluoride gas to obtain crude molybdenum hexafluoride gas; S3, the crude molybdenum hexafluoride gas is condensed to obtain condensate and solid impurities. After filtering the solid impurities, crude molybdenum hexafluoride liquid is obtained. S4, removing light components from the crude molybdenum hexafluoride liquid; S5, the crude molybdenum hexafluoride is purified by liquid distillation to obtain electronic-grade molybdenum hexafluoride.

2. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: Step S1 is achieved via a molybdenum hexafluoride reactor (1), which includes: Reactor body (11); Top cover (12), 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); Gas delivery pipe (14) is located on reactor body (11). A circular hole is provided on the outside of reactor body (11), and the inner wall of the circular hole is fixedly connected to the outside of gas delivery pipe (14). Feed pipe (15), the feed pipe (15) is located on top cover (12), the top cover (12) has an opening on the outside, the inner wall of the opening is fixedly connected to the outside of the feed pipe (15), a screw rod (111) is provided inside the feed pipe (15), a motor (112) is fixedly connected to the outside of the feed pipe (15), the output end of the motor (112) is connected to one end of the screw rod (111) through a coupling, and a feeding hopper (16) is provided on the feed pipe (15); The heating element (110) is located inside the reactor body (11); Waste heat recovery and utilization module (17), the waste heat recovery and utilization module (17) is located on the reactor body (11), the waste heat recovery and utilization module (17) is used to recover and reuse the heat contained in the molybdenum hexafluoride gas generated by the reactor; The reaction enhancement module (18) is located inside the reactor body (11) and is used to increase the contact area between fluorine gas and molybdenum powder in the reactor.

3. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: Step S3 is achieved through a pressure swing condenser filter (3), which includes: The tank (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 inside the tank (31). A condenser pipe (32) is connected between the gas phase inlet (313) and the liquid phase outlet (314), and the condenser pipe (32) is immersed in the low temperature cavity; The heat exchange controllable layer (33) is made of a number of elastic and flexible materials. The condensation pipe (32) has several through holes in the middle and rear section of the gas path. The heat exchange controllable layer (33) covers the through holes respectively. A press-formed component (34) is disposed inside the condensation pipe (32) and spaced apart from the heat exchange controllable layer (33); A pressurizing component (35) is disposed in the tank body (31). After the pressurizing component (35) pressurizes the tank body (31), the heat exchange controllable layer (33) expands into the condensation pipe (32) and approaches the compression molding component (34). After the heat exchange controllable layer (33) expands, the heat exchange efficiency is improved, and the semi-solid molybdenum pentafluoride adhering to the inner wall of the heat exchange controllable layer (33) fills the space between the compression molding component (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 component (35) depressurizes the tank body (31), the heat exchange controllable layer (33) shrinks and the molybdenum pentafluoride block crystals fall off. A filter plate (37) is disposed on the side of the condensing pipe (32) near the liquid phase outlet (314). The filter plate (37) is used to intercept molybdenum pentafluoride block crystals and filter the fine molybdenum pentafluoride crystals generated by condensation in the latter part of the condensing pipe (32) through the molybdenum pentafluoride block crystals.

4. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 3, characterized in that: The condensation pipe (32) has through holes in the area corresponding to an internal temperature of 60°C-67°C.

5. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 3, characterized in that: The compression molding part (34) has an arc-shaped concave structure. The side of the compression molding part (34) near the heat exchange controllable layer (33) is provided with a number of protrusions (341). The protrusions (341) give the formed molybdenum pentafluoride block crystals a number of fragile holes. After the heat exchange controllable layer (33) shrinks, the molybdenum pentafluoride block crystals break through the fragile holes. The pressurizing component (35) includes a connecting cylinder (351) that connects to the tank (31). A piston (352) is provided inside the connecting cylinder (351). The piston (352) is driven by a corresponding piston drive cylinder (353). When the piston (352) moves inside the connecting cylinder (351) toward the inside of the tank (31), it pressurizes the inside of the tank (31).

6. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 3, characterized in that: The outer surface of the heat exchange controllable layer (33) is provided with movable fins (36). 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 condenser pipe (32). When the heat exchange controllable layer (33) is in an expanded state, the movable fins (36) are away from the condenser pipe (32).

7. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 3, characterized in that: The working process of the pressure swing condenser filter (3) includes the following steps: S31, cold water is filled into the tank (31), and crude molybdenum hexafluoride gas is introduced into the condensation pipe (32) to condense the crude molybdenum hexafluoride in the condensation pipe (32); S32, executed every first time interval: control the pressurizing component (35) to pressurize the tank (31) and maintain it for a second time, so that the heat exchange controllable layer (33) expands into the condensation pipe (32) and approaches the compression molding component (34), so that the semi-solid molybdenum pentafluoride is cooled and solidified into molybdenum pentafluoride block crystals, and then control the pressurizing component (35) to depressurize the tank (31), so that the heat exchange controllable layer (33) contracts and the molybdenum pentafluoride block crystals fall off.

8. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: Step S5 is performed in a defoaming distillation column (4), which includes: The distillation column body (41) is provided with a heavy component reflux port (411) and a steam return port (412) at the bottom end, and a light component reflux port (413) and a steam outlet (414) at the top end. Several guide plates (415) are provided inside the distillation column body (41). A first mounting bracket (416) and a second mounting bracket (417) are provided at the bottom of the distillation column body (41), and the second mounting bracket (417) is located above the first mounting bracket (416). A distillation column condenser (42) is connected to the steam outlet (414) and is used to condense the gaseous stream at the top of the distillation column body (41) to form reflux liquid; A reflux tank (43) is connected between the distillation column condenser (42) and the light component reflux port (413) for storing and refluxing the reflux liquid; A reboiler (44) is connected between the heavy component reflux port (411) and the vapor return port, and is used to heat and vaporize the heavy component liquid at the bottom of the distillation column body (41); A bubble stretching and thinning mechanism (45) is provided in several parts. The bubble stretching and thinning mechanism (45) includes a gas guide frame (451), a fixed plate (452), and a bubble attachment plate (453). The first mounting bracket (416) is provided with several bubble rising through holes (4161). The gas guide frame (451) and the fixed plate (452) are arranged at intervals on the first mounting bracket (416). The middle part of the bubble attachment plate (453) is horizontally hinged to the top of the fixed plate (452). The bubble attachment plate (453) blocks the opening of the gas guide frame (451) when it is not under force. The gas guide frame (451) and the bubble attachment plate (453) are separated by a gap. A number of liquid driving devices (46) are disposed on the second mounting bracket (417). The liquid driving device (46) is 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 (452). During the rapid swinging process, the bubble attachment plate (453) stretches and thins the contact line between the fixed plate (452) and the bubble attachment plate (453) corresponding to the foam. After the bubble attachment plate (453) and the gas guide frame (451) have an opening, the bubble attachment plate (453) drives air to flow into the opening, thereby breaking the stretched and thinned part.

9. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 8, characterized in that: The liquid drive device (46) includes a liquid receiving cavity (461), a liquid receiving port (462) is provided at the top of the liquid receiving cavity (461), a nozzle (464) is provided at the bottom of the liquid receiving cavity (461), the nozzle (464) faces the upper end of one of the bubble attachment plates (453), and a movable plug (465) is provided in the liquid receiving cavity (461), the movable plug (465) is driven by a corresponding movable plug drive cylinder (466); The liquid receiving port (462) is located on the second mounting bracket (417) near the inner wall of the distillation column body (41), and the nozzle (464) is located on the second mounting bracket (417) away from the inner wall of the distillation column body (41). After the movable plug (465) moves away from the nozzle (464), the liquid receiving port (462) communicates with the liquid receiving cavity (461). The nozzle (464) has a blocking ball (468) provided at its opening by a compression 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) facing the upper end of one of the bubble attachment plates (453). When the movable plug drive 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 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 high speed, the liquid in the liquid receiving cavity (461) pushes 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 outward under the action of the blocking ball (468).

10. The preparation process of high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: In step S4, light components are removed under conditions of 20–100°C and normal pressure; In step S5, the sample is purified by distillation at 40–80°C and atmospheric pressure.

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