Foam breaking rectifying tower for preparing high-purity electronic-grade molybdenum hexafluoride and control method

Abstract

The invention relates to a bubble breaking rectifying tower for preparing high-purity electronic grade molybdenum hexafluoride and a control method, the bubble breaking rectifying tower comprises a plurality of bubble stretching and thinning mechanisms, each bubble stretching and thinning mechanism comprises a gas flow guide frame body, a fixed plate body and a bubble attachment plate, the gas flow guide frame bodies and the fixed plate bodies are arranged on a first mounting bracket at intervals, and the gas flow guide frame bodies and the fixed plate bodies are arranged on a second mounting bracket at intervals; the middle part of the bubble attachment plate is transversely hinged to the top end of the fixed plate body, the bubble attachment plate shields an opening of the gas guide frame body in an unstressed state, and the gas guide frame body and the bubble attachment plate are arranged at an interval; the liquid driving devices are arranged on the second mounting support and used for outputting liquid towards the top of the bubble attachment plate, the bubble attachment plate stretches and thinns a contact line between the foam corresponding fixing plate body and the bubble attachment plate in the rapid swinging process, and after the bubble attachment plate and the gas flow guide frame body are opened, the bubble attachment plate and the gas flow guide frame body are separated from each other. And the bubble attachment plate drives air to flow into the opening so as to break the stretched and thinned part.

Description

Technical Field

[0001] The present invention relates to the field of molybdenum hexafluoride distillation, and in particular to a bubble-breaking distillation tower and a control method for preparing high-purity electronic-grade molybdenum hexafluoride. Background Art

[0002] Molybdenum hexafluoride can be produced by the reaction of molybdenum powder and fluorine gas. The resulting crude molybdenum hexafluoride gas contains other impurities. After the crude molybdenum hexafluoride gas is condensed and filtered to remove some solid impurities, a crude molybdenum hexafluoride liquid is obtained. The impurities include liquid molybdenum tetrafluoride, molybdenum pentafluoride, molybdenum oxyfluoride, etc. The boiling points of these impurities are higher than that of molybdenum hexafluoride. Therefore, the crude molybdenum hexafluoride liquid needs to be purified by distillation in a distillation tower to obtain high-purity molybdenum hexafluoride.

[0003] The boiling point of molybdenum hexafluoride is around 34°C, while the boiling points of other impurities are much higher than that of molybdenum hexafluoride. Furthermore, during the purification process, the distillation tower uses low-temperature distillation, and the bottom temperature of the distillation tower is generally controlled at around 40°C, resulting in a slow heating rate. Furthermore, during the distillation process, a large amount of molybdenum hexafluoride accumulates at the top of the distillation tower, 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. The pressure inside these bubbles slowly rises, and after they burst, the high-pressure gas inside them is ejected outward. This ejection process easily ejects impurities from the bottom liquid, thereby introducing them into the gas phase and reducing the distillation efficiency of the distillation tower. In the prior art, defoaming devices or filter plates are generally used to reduce bubbles. However, these devices and filter plates are ineffective for bubbles that slowly grow and become viscous at low temperatures.

[0004] In view of the above problems existing in the prior art, the purpose of the present invention is to design a bubble-breaking distillation tower and a control method for preparing high-purity electronic grade molybdenum hexafluoride. Summary of the Invention

[0005] In response to the problems existing in the above-mentioned prior art, the present invention provides a bubble-breaking distillation tower and a control method for preparing 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 bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride, comprising: 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.

[0007] 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, and a movable plug is provided in the liquid receiving chamber, and the movable plug is driven by a corresponding movable plug driving cylinder.

[0008] Furthermore, the liquid receiving port is arranged on the second mounting bracket close to the inner wall of the distillation tower body, and the nozzle is arranged on the second mounting bracket away from the inner wall of the distillation tower body. After the movable plug is away from the nozzle, the liquid receiving port is connected to the liquid receiving cavity.

[0009] Furthermore, 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 the blocking ball has a liquid channel opened 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.

[0010] Further, the upper portion of the bubble attachment plate is coated with an oleophobic layer.

[0011] Furthermore, the gas guide frame and the bubble attachment plate are respectively provided with serrated edges.

[0012] Furthermore, the serrated edge is a sharp-angled serration, and the serrated edge of the gas guide frame and the serrated edge of the bubble attachment plate are complementary serrations.

[0013] Furthermore, the width of the gas guide frame is greater than the thickness of the bubble attachment plate.

[0014] Furthermore, an oleophilic layer is provided on the lower surface of the first mounting bracket.

[0015] A control method for a bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride is further provided, based on a bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride, comprising the following steps: Every first distillation time, executing: controlling the liquid driving device to centrally spray liquid toward the top of the bubble attachment plate, thereby driving the bubble attachment plate to swing and burst the bubbles; Every second distillation time, executing: controlling the liquid driving device to output liquid in a scattered manner to flush the surface of the bubble stretching and thinning mechanism, and the second distillation time is greater than the first distillation time.

[0016] Therefore, the present invention provides the following effects and / or advantages: 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 easily and slowly produces 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.

[0017] The present application sets a blocking sphere structure on the nozzle, so that the nozzle can spray in a straight line or in an umbrella shape. The bubble attachment plate can be driven by the straight line spraying, and the bubble stretching and thinning mechanism can be cleaned by the umbrella shape spraying.

[0018] The bubble attachment plate of the present application is provided with an oleophobic layer, which can prevent the oil phase inside the bubbles from spreading easily on the surface of the bubble attachment plate, and is conducive to maintaining the spherical shape of the bubbles on the bubble attachment plate.

[0019] 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.

[0020] 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

[0021] Figure 1 Schematic diagram of the structure of an embodiment of the present invention.

[0022] Figure 2 is a cross-sectional view of an embodiment of the present invention.

[0023] Figure 3 for Figure 2 A partial enlarged schematic diagram of part B.

[0024] Figure 4 Schematic diagram of the structure of the bubble stretching and thinning mechanism and the liquid driving device.

[0025] Figure 5 Schematic diagram of the nozzle structure.

[0026] Figure 6 Schematic diagram of the working state when the blocking ball of the nozzle has not left the opening.

[0027] Figure 7 Schematic diagram of the working state of the nozzle when the blocking ball leaves the opening.

[0028] Description of reference numerals: Distillation tower body 41, heavy component reflux port 411, steam return port 412, light component reflux port 413, steam outlet 414, guide plate 415, first mounting bracket 416, bubble rising hole 4161, second mounting bracket 417, distillation tower condenser 42, reflux tank 43, reboiler 44, bubble stretching and thinning mechanism 45, gas guide frame 451, fixed plate 452, bubble attachment plate 453, liquid driving device 46, liquid receiving chamber 461, liquid receiving port 462, nozzle 464, movable plug 465, movable plug driving cylinder 466, liquid channel 467, blocking ball 468, and contraction spring 469. DETAILED DESCRIPTION

[0029] 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 1-5 , a bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride, comprising: 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.

[0030] 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.

[0031] 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.

[0032] 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.

[0033] 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.

[0034] 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.

[0035] 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.

[0036] 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.

[0037] 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. refer to Figure 6 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; refer to Figure 7When 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 around under the action of the blocking ball 468.

[0038] 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.

[0039] Furthermore, the upper portion of the bubble attachment plate 453 is coated with an oleophobic layer.

[0040] 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.

[0041] Furthermore, the gas guide frame 451 and the bubble attachment plate 453 are respectively provided with serrated edges.

[0042] 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.

[0043] 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.

[0044] Furthermore, the width of the gas guide frame 451 is greater than the thickness of the bubble attachment plate 453 .

[0045] 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.

[0046] Furthermore, an oleophilic layer is provided on the lower surface of the first mounting bracket 416 .

[0047] 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 .

[0048] A control method for a bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride is further provided. The control method comprises the following steps based on the bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride: 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.

[0049] 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.

[0050] 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.

[0051] 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.

[0052] 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.

[0053] 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 bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride, characterized by: include: 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.

2. A bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 1, 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), 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).

3. A bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 2, characterized in that: 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 communicated with the liquid receiving chamber (461).

4. A bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 2, characterized in that: 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).

5. The bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: The upper portion of the bubble attachment plate (453) is coated with an oleophobic layer.

6. The bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: The gas guide frame (451) and the bubble attachment plate (453) are respectively provided with serrated edges.

7. The bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 6, characterized in that: The serrated edge is a sharp-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.

8. The bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: The width of the gas guide frame (451) is greater than the thickness of the bubble attachment plate (453).

9. The bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 1, characterized in that: The lower surface of the first mounting bracket (416) is provided with an oleophilic layer.

10. A method for controlling a bubble-breaking distillation column for preparing high-purity electronic-grade molybdenum hexafluoride, characterized in that: A bubble-breaking distillation tower for preparing high-purity electronic-grade molybdenum hexafluoride according to claim 4 comprises 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, executing: controlling the liquid driving device (46) to output liquid in a manner of spreading outwards, thereby flushing the surface of the bubble stretching and thinning mechanism (45), wherein the second distillation time is greater than the first distillation time.

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