A molten salt distillation method zirconium and hafnium separation device and its use method

Abstract

The present invention provides a zirconium-hafnium separation device by molten salt distillation method and a method for using the same, and belongs to the field of metallurgical technology. It includes a storage tank and a distillation tower, the bottom of the distillation tower is fixedly connected with a bottom tank, the bottom of the bottom tank is fixedly connected with a molten salt pump, the top of the distillation tower is fixedly connected with a condenser, one side of the bottom tank is fixedly connected with a reboiling tower, and one side of the distillation tower is fixedly connected with a feeding tower; the top of the storage tank is fixedly connected with two feeding tanks, the top of the feeding tank is fixedly connected with a distribution tank, a control valve is installed on the distribution tank, and the top of the distribution tank is fixedly connected with a feeding hopper; a feeding mechanism is used to assist operators in feeding the device, and the feeding mechanism is connected to the feeding hopper. The present invention is provided with a feeding mechanism, and zirconium tetrachloride and molten salt are simultaneously fed by means of the same group of structures, and the feeding process is simple to operate, high in safety, and improves the efficiency of feeding in the process of reducing production costs.

Description

Technical Field

[0001] The invention relates to the technical field of metallurgy, and in particular to a zirconium-hafnium separation device using a molten salt distillation method and a use method thereof. Background Art

[0002] Industrial molten salt distillation is a technology used to separate zirconium and hafnium. Its basic principle is to use the different boiling points of certain compounds of zirconium and hafnium to separate the two through distillation. The process of industrial molten salt distillation for separating zirconium and hafnium is divided into three steps: loading, distillation and condensation.

[0003] In order to ensure the sealing of zirconium tetrachloride during storage, zirconium tetrachloride is generally stored in a metal container. Molten salt is generally stored in a polyethylene-lined and plastic-outer woven bag. Therefore, different feeding channels are required for the two during the feeding process. In addition, due to the high hardness of the metal container, it is more difficult for operators to open the lid of the metal container, resulting in a slow overall feeding speed. In addition, zirconium tetrachloride is granular under normal conditions, and operators must be fully armed during the feeding process. Zirconium tetrachloride can cause respiratory irritation after inhalation and is highly irritating to the eyes. Direct skin contact with the liquid is highly irritating and can cause burns. Therefore, in order to improve the safety of the device during the feeding process and the feeding efficiency, the present invention provides a zirconium-hafnium separation device using a molten salt distillation method to meet the needs. Summary of the invention

[0004] The technical problem to be solved by the present invention is to provide a zirconium-hafnium separation device by a molten salt distillation method and a method for using the same structure. By setting a feeding mechanism, zirconium tetrachloride and molten salt are simultaneously fed and processed with the help of the same group of structures. The feeding process is simple to operate and has high safety. The feeding efficiency is improved while reducing production costs. The above setting can solve the problem of low feeding efficiency and poor safety of the separation device at this stage.

[0005] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0006] A zirconium-hafnium separation device using a molten salt distillation method comprises a storage tank and a distillation tower, wherein a bottom tank is fixedly connected to the bottom of the distillation tower, a molten salt pump is fixedly connected to the bottom of the bottom tank, a condenser is fixedly connected to the top of the distillation tower, a reboiling tower is fixedly connected to one side of the bottom tank, a feeding tower is fixedly connected to one side of the distillation tower, and a reflux tank is connected to one side of the condenser through a pipeline; two feeding tanks are fixedly connected to the top of the storage tank, a distribution tank is fixedly connected to the top of the feeding tank, a control valve is installed on the distribution tank, and a feeding hopper is fixedly connected to the top of the distribution tank; a feeding mechanism is used to assist an operator in feeding the device, and the feeding mechanism is connected to the feeding hopper; the feeding mechanism comprises a lower positioning plate, a lifting mechanism and an upper positioning plate, the lower positioning plate is rotatably connected to the feeding hopper, the lifting mechanism is fixedly connected to one side of the feeding hopper, the upper positioning plate is fixedly connected to the lifting mechanism, and the lifting mechanism is a linear lifting device driven by a screw and a servo motor.

[0007] Optionally, a hydraulic telescopic rod is rotatably connected to the inner wall of the feeding hopper, and both ends of the hydraulic telescopic rod are respectively connected to the feeding hopper and the lower positioning plate, and one side of the lower positioning plate is rotatably connected to a rotating shaft, and the lower positioning plate and the feeding hopper are connected via the rotating shaft.

[0008] Optionally, an arc-shaped recessed contour is provided on the outer side wall of the lower positioning plate, and an arc-shaped plate is fixedly connected to the middle position of the lower positioning plate, the arc-shaped plate has a downward curvature, and a leakage hole is opened on the arc-shaped plate.

[0009] Optionally, an inner clip is fixedly connected to the inner wall of the lower positioning plate, the inner clip has a trapezoidal profile, an inwardly inclined inclined plate is fixedly connected to one side of the inner clip, a weakening groove is provided on the other side of the inner clip, an electromagnet matching the profile of the inner clip is inserted into the inner clip, and the inner clip and the lower positioning plate are an integrally manufactured structure.

[0010] Optionally, a lifting plate is fixedly connected to the lifting mechanism, the upper positioning plate and the lifting mechanism are connected via the lifting plate, and the lifting plate and the upper positioning plate are fixed via screws.

[0011] Optionally, a first extrusion portion is fixedly connected to the outer wall of the upper positioning plate, a second extrusion portion is fixedly connected to the inner wall of the upper positioning plate, a support portion is fixedly connected inside the upper positioning plate, the support portion is located between the first extrusion portion and the second extrusion portion, and the top inner wall of the upper positioning plate has a slope inclined toward the middle.

[0012] Optionally, the first extrusion portion and the second extrusion portion both have an arc-shaped profile facing away from the supporting portion, and the first extrusion portion and the second extrusion portion are both elastic structures.

[0013] Optionally, the bottom of the lifting plate is rotatably connected to a first rotating rod, one end of the first rotating rod is rotatably connected to a second rotating rod, one end of the second rotating rod is rotatably connected to a plunger, one end of the plunger is fixedly connected to a pull rod, a pull groove is provided at one end of the second rotating rod close to the pull rod, a clamping block is fixedly connected in the pull groove, and a buckle is fixedly connected to the bottom of the lifting plate, and the buckle is a C-shaped elastic structure.

[0014] Optionally, a metal cover is installed at the bottom of the metal container, and an outward-turned portion is provided at the end of the metal cover, and the outward-turned portion has an outwardly curved profile. The metal container and the metal cover are both made of metal materials that can be adsorbed by magnets, and a thermocouple sensor, a temperature sensor and a pressure sensor are installed on the reboiling tower.

[0015] The present invention also provides a method for using a zirconium-hafnium separation device using a molten salt distillation method, comprising the following steps:

[0016] Step 1, loading: when zirconium tetrachloride needs to be added, insert the metal container into the upper positioning plate and let it be upside down on the top of the lower positioning plate. After the metal container is placed, energize the electromagnet to allow the lower positioning plate to absorb the metal cover. At the same time, the lifting mechanism drives the upper positioning plate to move toward the metal cover. During the movement of the upper positioning plate, its inner wall will squeeze the outer wall of the metal container, so that the upper positioning plate and the metal container are clamped and fixed together under the action of friction. The bottom of the upper positioning plate will squeeze the outward turning part on the metal cover and let the metal cover separate from the metal container. When the metal cover is separated from the metal container, the lifting mechanism drives the upper positioning plate to move in the opposite direction. During the reverse movement of the upper positioning plate, the metal container will be driven away from the metal cover. At the same time, the hydraulic telescopic rod drives the lower positioning plate to move in the opposite direction. The positioning disk rotates, and the metal cover will also rotate under the adsorption of the electromagnet during the rotation of the lower positioning disk. At this time, the zirconium tetrachloride in the metal container will enter the distribution tank; when molten salt needs to be added, first adjust the control valve on the distribution tank to allow the material dropped from the feeding hopper to enter another feeding tank, then rotate the first rotating rod and the second rotating rod to make the knife parallel to the lower positioning disk, and then pull the pull rod to rotate the knife downward 90 degrees, so that the knife and the lower positioning disk are perpendicular to each other, place the molten salt bag on the top of the lower positioning disk, and then let the lifting mechanism drive the knife to move toward the molten salt bag. After the knife moves to the position of the molten salt bag, it will cut a hole in the molten salt bag. At this time, the molten salt in the molten salt bag will leak into the distribution tank from the leakage hole on the arc plate along the hole;

[0017] Step 2, distillation, open the valve bodies on the two feed tanks in turn, let the zirconium tetrachloride and molten salt in the feed tank enter the storage tank, a spiral feeding structure is installed in the storage tank, the zirconium tetrachloride and molten salt in the storage tank are transported to the bottom tank through the spiral feeding structure, the reboiling tower heats the material in the bottom tank to boiling, the steam generated by the boiling material will pass upward through the tower plate of the distillation tower to form an ascending steam flow, the steam at the top of the distillation tower is cooled into liquid by the condenser to form a reflux liquid, the reflux liquid will flow downward along the tower plate or filler and meet the rising steam to exchange heat and mass, the low boiling point component continues to rise, and the high boiling point component is brought back to the bottom of the distillation tower by the reflux liquid, so that the material is separated into products by continuous operation.

[0018] Compared with the prior art, the present invention has at least the following beneficial effects:

[0019] In the above scheme, by installing sensors on the device and cooperating with the control effect of the control computer group, by accurately controlling various process parameters, the efficiency and purity of zirconium and hafnium separation can be significantly improved, the stability of product quality can be ensured, labor intensity can be reduced, manual intervention can be reduced, the labor intensity of operators can be reduced, and control parameters can be adjusted in time to cope with various interferences and changes, thereby improving the stability and reliability of the system and reducing the probability of failure.

[0020] By setting up a feeding mechanism, zirconium tetrachloride and molten salt can be fed simultaneously with the help of the same group of structures, and the feeding process is simple to operate and highly safe, thereby improving the feeding efficiency while reducing production costs.

[0021] By setting up the upper positioning plate and the lower positioning plate, not only can the upper positioning plate clamp and fix the metal container with the help of its own gravity, but also the stability of the metal container can be improved with the help of the structural adaptation between the lower positioning plate and the metal cover. In the process of unloading the metal container, all unloading operations can be completed by starting the lifting structure and the hydraulic telescopic rod. Such a setting can replace manpower, thereby improving the loading efficiency and safety during the loading process.

[0022] By setting the upper positioning plate and the lower positioning plate, the molten salt bag can be opened, so that the molten salt in the molten salt bag will leak into the distribution tank through the leakage holes on the arc plate along the opening, and by setting the buckle, the efficiency of the knife deployment and storage process can be greatly improved, and the operating burden of the operator can be reduced. By setting the arc plate, since the arc plate has a downward curvature, the material falling from the plastic woven bag will fall accurately into the feeding hopper under the guidance of its arc structure without side leakage. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The accompanying drawings, which are incorporated herein and constitute a part of the specification, illustrate embodiments of the invention and, together with the description, further serve to explain the principles of the invention and to enable those skilled in the relevant art to make and use the invention.

[0024] Figure 1 It is a schematic diagram of the three-dimensional structure of the zirconium-hafnium separation device by the molten salt distillation method from the first perspective;

[0025] Figure 2 It is a schematic diagram of the stereoscopic structure of the zirconium-hafnium separation device by the molten salt distillation method from the second viewing angle;

[0026] Figure 3 It is an enlarged three-dimensional structural diagram of the storage tank, feeding tank and loading mechanism;

[0027] Figure 4 It is an enlarged three-dimensional structural diagram of the material distribution tank, the feeding hopper and the loading mechanism;

[0028] Figure 5 It is a schematic diagram of the three-dimensional structure of the feeding hopper and the loading mechanism in a cutaway first-person perspective;

[0029] Figure 6 It is a schematic diagram of the three-dimensional structure of the feeding hopper and the loading mechanism in a cutaway second viewing angle;

[0030] Figure 7 It is a schematic diagram of the sectional three-dimensional structure of the feeding hopper and the lower positioning plate;

[0031] Figure 8 for Figure 7 A in the middle is an enlarged schematic diagram of the three-dimensional structure;

[0032] Fig. 9 It is a schematic diagram of the three-dimensional structure of the feeding mechanism and the metal container in a cutaway first-person perspective;

[0033] Fig.10 It is a schematic diagram of the three-dimensional structure of the feeding mechanism and the metal container in a cutaway second viewing angle;

[0034] Fig.11 for Fig.10 The enlarged three-dimensional structure diagram at B in the middle;

[0035] Fig.12 It is a schematic diagram of the sectional three-dimensional structure of the upper positioning plate and the metal cover;

[0036] Fig.13 for Fig.12 The enlarged three-dimensional structure diagram at C in the middle;

[0037] Fig.14 This is a schematic diagram of the three-dimensional structure of the upper positioning plate in cross section from the first perspective;

[0038] Fig.15for Fig.14 The enlarged three-dimensional structure diagram at D in the middle;

[0039] Fig.16 This is a schematic diagram of the three-dimensional structure of the upper positioning plate in section from a second viewing angle;

[0040] Fig.17 It is an enlarged three-dimensional structural diagram of the feeding mechanism and the molten salt bag;

[0041] Fig.18 It is a schematic diagram of an enlarged three-dimensional structure of the first rotating rod, the second rotating rod and the inserting knife before being unfolded;

[0042] Fig.19 It is a schematic diagram of an enlarged three-dimensional structure of the first rotating rod, the second rotating rod and the inserting knife after being unfolded;

[0043] Fig. 20 for Fig.19 The enlarged schematic diagram of the three-dimensional structure at E in the middle.

[0044] Reference numerals:

[0045] 1. Storage tank; 2. Feed tank; 201. Distribution tank; 202. Control valve; 203. Feed hopper; 3. Bottom tank; 4. Reboiling tower; 5. Distillation tower; 6. Condenser; 7. Feed tower; 8. Molten salt pump; 9. Reflux tank; 10. Lower positioning plate; 11. Lifting mechanism; 12. Upper positioning plate; 13. Hydraulic telescopic rod; 14. Inner clamp; 15. Inclined plate; 16. Weakening groove; 17. Electromagnet; 18. Arc plate; 19. Leak hole; 20. Lifting plate; 21. First extrusion part; 22. Second extrusion part; 23. Support part; 24. Metal container; 25. Metal cover; 26. Outward turning part; 27. First rotating rod; 28. Second rotating rod; 29. ​​Insert knife; 30. Buckle; 31. Pull rod; 32. Block; 33. Pull groove.

[0046] As shown in the figure, in order to clearly implement the structure of the embodiment of the present invention, specific structures and devices are marked in the figure, but this is only for illustrative purposes and is not intended to limit the present invention to the specific structure, device and environment. According to specific needs, ordinary technicians in this field can adjust or modify these devices and environments. DETAILED DESCRIPTION

[0047] The following is a detailed description of a molten salt distillation zirconium-hafnium separation device and its use method provided by the present invention in combination with the accompanying drawings and specific embodiments. At the same time, it is explained here that in order to make the embodiments more detailed, the following embodiments are the best and preferred embodiments, and those skilled in the art may also adopt other alternative methods to implement some known technologies; and the accompanying drawings are only for a more specific description of the embodiments, and are not intended to specifically limit the present invention.

[0048] It should be noted that the references to "one embodiment", "embodiment", "exemplary embodiments", "some embodiments" and the like in the specification indicate that the embodiments described may include specific features, structures or characteristics, but not every embodiment may include the specific features, structures or characteristics. In addition, when a specific feature, structure or characteristic is described in conjunction with an embodiment, it should be within the knowledge of a person skilled in the art to implement such feature, structure or characteristic in conjunction with other embodiments (whether or not explicitly described).

[0049] In general, a term can be understood, at least in part, from its use in context. For example, depending, at least in part, on the context, the term "one or more" as used herein can be used to describe any feature, structure, or characteristic in the singular sense, or can be used to describe a combination of features, structures, or characteristics in the plural sense. Additionally, the term "based on" can be understood as not necessarily intended to convey an exclusive set of factors, but can instead, depending, at least in part, on the context, allow for the presence of other factors that are not necessarily explicitly described.

[0050] It will be understood that the meanings of “on,” “over,” and “above” in the present invention should be interpreted in the broadest manner, so that “on” not only means “directly on” something, but also includes the meaning of being “on” something with intervening features or layers therebetween, and “on” or “over” not only means “on” or “above” something, but also includes the meaning of being “on” or “above” something with no intervening features or layers therebetween.

[0051] Additionally, spatially relative terms such as "under," "beneath," "lower," "above," "upper," and the like may be used herein for descriptive convenience to describe the relationship of one element or feature to another element or features, as shown in the accompanying drawings. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the accompanying drawings. The device may be oriented in other ways, and the spatially relative descriptors used herein may be similarly interpreted accordingly.

[0052] like Figures 1 to 4As shown, an embodiment of the present invention provides a zirconium-hafnium separation device by a molten salt distillation method, comprising a storage tank 1 and a distillation tower 5, the bottom of the distillation tower 5 is fixedly connected to a bottom tank 3, the bottom of the bottom tank 3 is fixedly connected to a molten salt pump 8, the top of the distillation tower 5 is fixedly connected to a condenser 6, one side of the bottom tank 3 is fixedly connected to a reboiling tower 4, one side of the distillation tower 5 is fixedly connected to a feed tower 7, and one side of the condenser 6 is connected to a reflux tank 9 through a pipeline; the top of the storage tank 1 is fixedly connected to two feeding tanks 2, the top of the feeding tank 2 is fixedly connected to a distribution tank 201, the distribution tank 201 is installed with a control valve 202, and the top of the distribution tank 201 is fixedly connected to a feeding tank 9. Bucket 203, a galvanic sensor, a temperature sensor and a pressure sensor are installed on the reboiling tower 4. Compared with the existing separation device, the present device is provided with a galvanic sensor and a pressure sensor, and the control of the device is realized through an external control computer group. Specifically, the galvanic sensor can measure the temperature of each section of the connecting pipe between the distillation tower 5 and the bottom tank 3 in real time, and automatically feed back to the control computer group, and heat is performed in real time according to the feedback temperature to prevent the loss caused by cooling of the liquid molten salt in the pipeline, and when the reduction temperature is higher than the set upper limit, the cooling fan and the air inlet valve are automatically started to cool the reactor, and the frequency of the cooling fan is automatically adjusted as the temperature decreases.

[0053] Furthermore, before the system is started, the operator sets the target flow rate, pressure, temperature and other parameters for transporting molten salt through the control computer group. After the system is started, the temperature sensor and pressure sensor will monitor the temperature and pressure data of the molten salt in real time and transmit these data to the control computer group. At the same time, the sensor for measuring the speed and flow rate of the molten salt pump 8 will also transmit the corresponding data to the control computer group. After receiving these data, the control computer group will compare them with the preset target values. If the current temperature, pressure or flow rate does not meet the set requirements, the control computer group will calculate the adjustment instructions according to the preset control algorithm. If the flow rate is lower than the target value, the control computer group will calculate the adjustment instructions according to the preset control algorithm. The computer group will send instructions to the frequency converter to increase the motor speed of the molten salt pump 8, thereby increasing the flow rate. Conversely, if the flow rate is too high, the controller will reduce the motor speed to reduce the flow rate. During the transportation process, the system will continue to monitor and adjust to ensure that the molten salt is always transported in a stable and satisfactory state. If an abnormal situation occurs, such as excessive temperature, excessive pressure or equipment failure, the system will trigger an alarm and take corresponding protective measures, such as emergency shutdown, to avoid accidents. During the entire transportation process, the operator can monitor the system's operating status, parameter changes and historical data in real time through the control computer group, so as to evaluate the system operation and make necessary interventions.

[0054] Optionally, temperature sensors, pressure sensors, flow sensors, etc. are installed at key positions of the condenser 6 to collect data such as temperature, pressure, cooling medium flow, hot fluid flow, etc. in the condenser 6 in real time, and transmit the data to the control computer group. The control computer group compares and analyzes the received data with preset process parameters and control targets, and then generates corresponding control instructions. The control instructions are sent to the actuator, and the actuator adjusts the working state according to the instructions to change the working conditions of the condenser 6. The control computer group can also have an alarm function. When the monitoring parameters exceed the safety range or a fault occurs, an alarm is promptly issued to notify the operator to handle it. At the same time, the system can also record and store operating data for subsequent analysis and optimization.

[0055] In summary, the solution provided by the present application, by installing sensors on the device and cooperating with the control effect of the control computer group, can significantly improve the efficiency and purity of zirconium and hafnium separation by accurately controlling various process parameters, ensure the stability of product quality, reduce labor intensity, reduce manual intervention, reduce the labor intensity of operators, and timely adjust control parameters to cope with various interferences and changes, thereby improving the stability and reliability of the system and reducing the probability of failure.

[0056] In this embodiment, if Figures 9 to 11 As shown, a metal cover 25 is installed at the bottom of the metal container 24, and an outward-turned portion 26 is provided at the end of the metal cover 25. The outward-turned portion 26 has an outwardly curved profile. The metal container 24 and the metal cover 25 are both made of metal that can be adsorbed by magnets. At present, zirconium tetrachloride is generally transported and stored in metal containers 24 on the market. The metal container 24 provided in this application is the most common container on the market. Here, the metal container 24 and the metal cover 25 are disclosed as prior art, so they are not described in detail.

[0057] As an implementation method in this embodiment, Figures 3 to 6As shown, the feeding mechanism is used to assist the operator in feeding the device, and the feeding mechanism is connected to the feeding hopper 203; the feeding mechanism includes a lower positioning plate 10, a lifting mechanism 11 and an upper positioning plate 12, the lower positioning plate 10 is rotatably connected to the feeding hopper 203, the lifting mechanism 11 is fixedly connected to one side of the feeding hopper 203, the upper positioning plate 12 is fixedly connected to the lifting mechanism 11, and the lifting mechanism 11 is a linear lifting device driven by a screw and a servo motor. A hydraulic telescopic rod 13 is rotatably connected to the inner wall of the feeding hopper 203, and the two ends of the hydraulic telescopic rod 13 are respectively connected to the feeding hopper 203 and the lower positioning plate 10, and one side of the lower positioning plate 10 is rotatably connected with a rotating shaft, and the lower positioning plate 10 and the feeding hopper 203 are connected by a rotating shaft, and the top of the storage tank 1 A total of two feeding tanks 2 are installed, and the same distribution tank 201 is installed on the top of these two feeding tanks 2. Switch valves are set at the connection positions of the two feeding tanks 2 and the storage tank 1. The switch valve is used to control the connection state between the feeding tank 2 and the storage tank 1. A control valve 202 is installed on the distribution tank 201. The control valve 202 is used to control the specific direction of the material falling from the feeding hopper 203. By adjusting the control valve 202, the material can fall into different feeding tanks 2. This arrangement makes it possible to simultaneously load two different distribution tanks 201 through only one feeding hopper 203, thereby reducing costs while improving loading efficiency. In this application, the control valve 202 and the switch valve are disclosed as prior art, so the working principles of the two are not described in detail.

[0058] In the feeding mechanism, the lower positioning plate 10 and the upper positioning plate 12 are used to position the metal cover 25 and the metal container 24 respectively. One side of the lower positioning plate 10 is rotatably connected to the feeding hopper 203 through a rotating shaft, and a hydraulic telescopic rod 13 is also installed at the bottom of the lower positioning plate 10. Therefore, the relative position between the lower positioning plate 10 and the feeding hopper 203 can be adjusted by controlling the hydraulic telescopic rod 13. When the telescopic end of the hydraulic telescopic rod 13 contracts, it will drive the lower positioning plate 10 to rotate about the rotating shaft. During the rotation, the lower positioning plate 10 is received in the feeding hopper 203.

[0059] In this embodiment, if Figures 3 to 13As shown, the outer wall of the lower positioning plate 10 is provided with an arc-shaped concave profile, the inner wall of the lower positioning plate 10 is fixedly connected with an inner clip 14, the inner clip 14 has a trapezoidal profile, one side of the inner clip 14 is fixedly connected with an inwardly inclined inclined plate 15, the other side of the inner clip 14 is provided with a weakening groove 16, the inner clip 14 is plugged with an electromagnet 17 that matches the profile of the inner clip 14, the inner clip 14 and the lower positioning plate 10 are an integrally manufactured structure, the lifting mechanism 11 is fixedly connected with a lifting plate 20, the upper positioning plate 12 and the lifting mechanism 11 are fixedly connected with a lifting plate 20, and the upper positioning plate 12 and the lifting mechanism 11 are fixedly connected with an inwardly inclined inclined plate 15. The mechanisms 11 are connected by a lifting plate 20, and the lifting plate 20 and the upper positioning plate 12 are fixed by screws. A first extrusion portion 21 is fixedly connected to the outer wall of the upper positioning plate 12, and a second extrusion portion 22 is fixedly connected to the inner wall of the upper positioning plate 12. A support portion 23 is fixedly connected inside the upper positioning plate 12, and the support portion 23 is located between the first extrusion portion 21 and the second extrusion portion 22. The first extrusion portion 21 and the second extrusion portion 22 both have an arc-shaped profile facing away from the support portion 23. The first extrusion portion 21 and the second extrusion portion 22 are fixedly connected to the outer wall of the upper positioning plate 12. 22 are all elastic structures. When the zirconium tetrachloride is loaded, the metal container 24 is first inserted into the upper positioning plate 12. The top inner wall of the upper positioning plate 12 has an inclined surface inclined toward the middle. The setting of the inclined surface allows the user to use the inclined surface for auxiliary guidance during the process of inserting the metal container 24 into the upper positioning plate 12, thereby improving the success rate and efficiency of placing the metal container 24 in the upper positioning plate 12. A second extrusion portion 22 is provided on the inner wall of the upper positioning plate 12. The second extrusion portion 22 has an inclined surface inclined toward the middle. The arc-shaped contour in the direction of the part 23 is set so that when the user inserts the metal container 24 into the upper positioning plate 12, the metal container 24 will squeeze the arc-shaped contour on the surface of the second extrusion part 22. During the extrusion process, the second extrusion part 22 will deform toward the supporting part 23, and apply a reverse elastic force to the metal container 24 during the deformation process. Under the action of the elastic force, the friction between the upper positioning plate 12 and the metal container 24 can be increased, thereby using the gravity of the metal container 24 to achieve the clamping and fixing effect of the metal container 24.

[0060] Furthermore, when the user inserts the metal container 24 into the upper positioning plate 12, the metal container 24 will slide to the top of the lower positioning plate 10 under the action of its own gravity. Since an arc-shaped concave profile is provided on the outer wall of the lower positioning plate 10, the arc-shaped concave profile matches the curved surface profile on the metal cover 25. Therefore, when the metal cover 25 slides down to the top of the lower positioning plate 10, it will adapt to the structure of the lower positioning plate 10, thereby achieving the positioning effect of the metal cover 25 and improving the stability of the metal container 24 and the metal cover 25. In addition, an inner clip 14 with a trapezoidal profile is installed on the inner wall of the lower positioning plate 10, and one side of the inner clip 14 has an inwardly inclined inclined plate 15. The arrangement of the inclined plate 15 This makes one side of the inner clip 14 elastically clamped inward, so the user can use the elastic force of the inclined plate 15 to fix the electromagnet 17. The top of the inclined plate 15 is non-contacting with the lower positioning plate 10. This arrangement allows the user to deform the inner clip 14 at the position of the weakened groove 16 by bending the inclined plate 15 outward. After the inner clip 14 is deformed, the user can take the electromagnet 17 out of the inner clip 14. This installation method is not only simple in structure but also easy to operate. Since the metal cover 25 is made of metal that can be adsorbed by a magnet, when the electromagnet 17 is energized, the metal cover 25 can be adsorbed, so that the metal cover 25 is firmly fixed in the lower positioning plate 10.

[0061] After the metal container 24 is placed, the lifting mechanism 11 is started, and the lifting mechanism 11 drives the upper positioning plate 12 to move toward the metal cover 25. The first extrusion portion 21 is installed on the outer wall of the upper positioning plate 12. Since the first extrusion portion 21 has an arc-shaped profile facing away from the support portion 23, when the first extrusion portion 21 moves to the position of the outer turning portion 26 of the metal cover 25, it will be inserted into the outer turning portion 26 and squeeze the outer turning portion 26 outward. During the squeezing process, the outer turning portion 26 will be deformed and separated from the metal container 24, so that the metal cover 25 and the metal container 24 are separated from the limit. The metal cover 25 of the metal container 24 can be opened by driving the hydraulic telescopic rod 13 to rotate the lower positioning plate 10, and the material in the metal container 24 can also fall into the feeding hopper 203. At this time, the user can slide the lifting mechanism 11 upward, and drive the upper positioning plate 12 to move the metal container 24 upward until all the materials in the metal container 24 are dumped. The user removes the metal container 24 from the upper positioning plate 12 from bottom to top, and removes the metal cover 25 from the lower positioning plate 10 when the electromagnet 17 is powered off. The metal container 24 and the metal cover 25 can be disinfected and reused.

[0062] To sum up, by setting up the upper positioning plate 12 and the lower positioning plate 10, not only can the upper positioning plate 12 clamp and fix the metal container 24 by utilizing its own gravity, but also the stability of the metal container 24 can be improved by utilizing the structural adaptation between the lower positioning plate 10 and the metal cover 25. During the unloading process of the metal container 24, all unloading operations can be completed by simply starting the lifting structure and the hydraulic telescopic rod 13. Such a setting can replace manpower, thereby improving the loading efficiency and safety during the loading process.

[0063] In this embodiment, if Figures 16 to 20 As shown, the bottom of the lifting plate 20 is rotatably connected to a first rotating rod 27, one end of the first rotating rod 27 is rotatably connected to a second rotating rod 28, one end of the second rotating rod 28 is rotatably connected to a plunger 29, one end of the plunger 29 is fixedly connected to a pull rod 31, and a groove 33 is provided at one end of the second rotating rod 28 close to the pull rod 31, and a block 32 is fixedly connected in the groove 33. The bottom of the lifting plate 20 is fixedly connected to a buckle 30, and the buckle 30 is a C-shaped elastic structure. The middle position of the lower positioning plate 10 is fixedly connected to an arc plate 18, and the arc plate 18 has an arc that is bent downward. The arc plate 18 is provided with a leak hole 19. When the molten salt is fed, a woven bag lined with polyethylene and covered with plastic is placed on the top of the upper positioning plate 12, and the first rotating rod 27 and the second rotating rod 28 are rotated to make the plunger 29 parallel to the lower positioning plate 10, and then the pull rod 31 is pulled to rotate the plunger 29 downward by 90 degrees, so that the plunger 29 and the lower positioning plate 10 are perpendicular to each other. At this time, the lifting mechanism 11 drives the plunger 29 to move toward the molten salt bag. After the plunger 29 moves to the position of the molten salt bag, it will cut a hole in the molten salt bag. At this time, the molten salt in the molten salt bag will flow along the molten salt bag. The opening leaks into the material distribution tank 201 from the leakage hole 19 on the arc plate 18. During the rotation of the plunger 29, the pull rod 31 will slide in the groove 33. When the plunger 29 rotates ninety degrees, the pull rod 31 just hits the end of the groove 33. At this time, the block 32 in the groove 33 will block and limit the pull rod 31, thereby preventing the plunger 29 from being misplaced during the lifting process. When the first rotating rod 27 and the second rotating rod 28 are not rotated, they are hidden and stored at the bottom of the lifting plate 20 and limited by the buckle 30. The buckle 30 is a C-shaped elastic structure and hits the first rotating rod 27. At one end, the first rotating rod 27 can be blocked and limited by means of its C-shaped structure. Since the buckle 30 is an elastic structure, when the user pulls down the first rotating rod 27, the buckle 30 will deform and avoid the first rotating rod 27. Through such a setting, the efficiency of the expansion and storage of the inserting knife 29 can be greatly improved, and the operating burden of the operator can be reduced. Since the arc plate 18 has a downward curvature, the material falling from the plastic woven bag will fall accurately into the feeding hopper 203 under the guidance of its arc structure without side leakage.

[0064] The present invention also provides a method for using a zirconium-hafnium separation device using a molten salt distillation method, comprising the following steps:

[0065] Step 1, loading: when zirconium tetrachloride needs to be added, the metal container 24 is inserted into the upper positioning plate 12 and placed upside down on the top of the lower positioning plate 10. After the metal container 24 is placed, the electromagnet 17 is energized to allow the lower positioning plate 10 to absorb the metal cover 25. At the same time, the lifting mechanism 11 drives the upper positioning plate 12 to move toward the metal cover 25. During the movement of the upper positioning plate 12, its inner wall will squeeze the outer wall of the metal container 24, so that the upper positioning plate 12 and the metal container 24 are clamped and fixed together under the action of friction. The bottom of the upper positioning plate 12 will squeeze the outward turning part 26 on the metal cover 25 and let the metal cover 25 separate from the metal container 24. When the metal cover 25 is separated from the metal container 24, the lifting mechanism 11 drives the upper positioning plate 12 to move in the opposite direction. During the reverse movement of the upper positioning plate 12, the metal container 24 will be driven away from the metal cover 25. At the same time, the hydraulic telescopic rod 13 drives the lower positioning plate The positioning disk 10 rotates, and the metal cover 25 also rotates under the adsorption action of the electromagnet 17 during the rotation of the lower positioning disk 10. At this time, the zirconium tetrachloride in the metal container 24 will enter the distribution tank 201; when molten salt needs to be added, first adjust the control valve 202 on the distribution tank 201 to allow the material dropped from the feeding hopper 203 to enter another feeding tank 2, and then rotate the first rotating rod 27 and the second rotating rod 28 to make the plunger 29 at an angle parallel to the lower positioning disk 10, and then pull the pull rod 31 to rotate the plunger 29 downward by ninety degrees, so that the plunger 29 and the lower positioning disk 10 are perpendicular to each other, and the molten salt bag is placed on the top of the lower positioning disk 10, and then the lifting mechanism 11 drives the plunger 29 to move toward the molten salt bag. After the plunger 29 moves to the position of the molten salt bag, it will cut a hole in the molten salt bag. At this time, the molten salt in the molten salt bag will leak into the distribution tank 201 from the leakage hole 19 on the arc plate 18 along the hole;

[0066] Step 2, distillation, open the valve bodies on the two feeding tanks 2 in turn, let the zirconium tetrachloride and molten salt in the feeding tank 2 enter the storage tank 1, a spiral feeding structure is installed in the storage tank 1, and the zirconium tetrachloride and molten salt in the storage tank 1 are transported to the bottom tank 3 through the spiral feeding structure, and the reboiling tower 4 heats the material in the bottom tank 3 to boiling, and the steam generated by the boiling material will pass upward through the tower plate of the distillation tower 5 to form an ascending steam flow, and the steam at the top of the distillation tower 5 is cooled by the condenser 6 into a liquid to form a reflux liquid, and the reflux liquid will flow downward along the tower plate or filler to meet the rising steam for heat and mass exchange, and the low boiling point component continues to rise, while the high boiling point component is brought back to the bottom of the distillation tower 5 by the reflux liquid, so as to continuously operate and separate the materials into products.

[0067] The working principle of the technical solution provided by the present invention is as follows:

[0068] When feeding zirconium tetrachloride, the metal container 24 is first inserted into the upper positioning plate 12. The top inner wall of the upper positioning plate 12 has an inclined surface inclined toward the middle. The setting of the inclined surface allows the user to use the inclined surface for auxiliary guidance during the process of inserting the metal container 24 into the upper positioning plate 12, thereby improving the success rate and efficiency of placing the metal container 24 in the upper positioning plate 12. A second extrusion portion 22 is provided on the inner wall of the upper positioning plate 12. The second extrusion portion 22 has an arc-shaped profile facing away from the support portion 23. The setting of the arc-shaped profile allows the metal container 24 to squeeze the arc-shaped profile on the surface of the second extrusion portion 22 when the user inserts the metal container 24 into the upper positioning plate 12. During the extrusion process, the second extrusion portion 22 will face the support portion 23. 23 is deformed, and in the process of deformation, a reverse elastic force is applied to the metal container 24, under the action of the elastic force, the friction between the upper positioning plate 12 and the metal container 24 can be increased, so that the metal container 24 can be clamped and fixed by means of the gravity of the metal container 24 itself. When the user inserts the metal container 24 into the upper positioning plate 12, the metal container 24 will slide to the top of the lower positioning plate 10 under the action of its own gravity. Since an arc-shaped concave profile is provided on the outer wall of the lower positioning plate 10, the arc-shaped concave profile is consistent with the curved surface profile on the metal cover 25, so when the metal cover 25 slides down to the top of the lower positioning plate 10, it will adapt to the structure of the lower positioning plate 10, thereby achieving the positioning effect of the metal cover 25, and improving the metal container 24 and To ensure the stability of the metal cover 25, an inner clip 14 with a trapezoidal profile is installed on the inner wall of the lower positioning plate 10, and one side of the inner clip 14 is provided with an inwardly inclined inclined plate 15. The setting of the inclined plate 15 allows one side of the inner clip 14 to be elastically clamped inward, so the user can use the elastic force of the inclined plate 15 to achieve a fixing effect on the electromagnet 17. Since the metal cover 25 is made of a metal material that can be adsorbed by a magnet, the electromagnet 17 can achieve an adsorption effect on the metal cover 25 when it is energized, so that the metal cover 25 is firmly fixed in the lower positioning plate 10. After the metal container 24 is placed, the lifting mechanism 11 is started, and the lifting mechanism 11 drives the upper positioning plate 12 to move toward the metal cover 25. The first extrusion portion 21 is installed on the outer wall of the upper positioning plate 12. Since the first extrusion portion 21 has an arc-shaped profile facing away from the support portion 23, when the first extrusion portion 21 moves to the position of the outward turning portion 26 of the metal cover 25, it will be inserted into the outward turning portion 26 and squeeze the outward turning portion 26 outward. During the squeezing process, the outward turning portion 26 will be deformed and detached from the metal container 24, so that the metal cover 25 and the metal container 24 are out of the limit. At this time, the hydraulic telescopic rod 13 drives the lower positioning plate 10 to rotate to open the metal cover 25 of the metal container 24, and the material in the metal container 24 will also fall into the feeding hopper 203. At this time, the user can let the lifting mechanism 11 slide upward, and let the upper positioning plate 12 drive the metal container 24 to move upward together until all the materials in the metal container 24 are dumped.The user removes the metal container 24 from the upper positioning plate 12 from bottom to top, and removes the metal cover 25 from the lower positioning plate 10 when the electromagnet 17 is powered off. The metal container 24 and the metal cover 25 can be reused after being sterilized.

[0069] When loading the molten salt, the molten salt bag is placed on the top of the upper positioning disk 12, the first rotating rod 27 and the second rotating rod 28 are rotated to make the plunger 29 parallel to the lower positioning disk 10, and then the pull rod 31 is pulled downward by ninety degrees to rotate the plunger 29 so that the plunger 29 and the lower positioning disk 10 are perpendicular to each other. At this time, the lifting mechanism 11 drives the plunger 29 to move toward the molten salt bag. After the plunger 29 moves to the position of the molten salt bag, it will cut a hole in the molten salt bag. At this time, the molten salt in the molten salt bag will leak into the distributing tank 201 from the leakage hole 19 on the arc plate 18 along the hole. During the rotation of the plunger 29, the pull rod 31 will slide in the groove 33. When the plunger 29 is rotated ninety degrees, the pull rod 31 just hits the end of the groove 33. At this time, the block 32 in the groove 33 will block and limit the pull rod 31, thereby preventing the plunger 2 In the process of lifting and lowering, there is a phenomenon of misalignment. When the first rotating rod 27 and the second rotating rod 28 are not rotating, they are hidden and stored at the bottom of the lifting plate 20, and are limited by the buckle 30. The buckle 30 is a C-shaped elastic structure and contacts one end of the first rotating rod 27. With the help of its C-shaped structure, the first rotating rod 27 can be blocked and limited. Since the buckle 30 is an elastic structure, when the user pulls down the first rotating rod 27, the buckle 30 will deform and avoid the first rotating rod 27. Through such a setting, the efficiency of the expansion and storage of the inserting knife 29 can be greatly improved, and the operating burden of the operator can be reduced. Since the arc plate 18 has a downward curvature, the material falling from the plastic woven bag will fall accurately into the feeding hopper 203 under the guidance of its arc structure without side leakage.

[0070] When the material is subjected to distillation and separation treatment, the reboiling tower 4 provides heat to the bottom of the distillation tower 5, so that the bottom part of the mixed molten salt solution in the bottom of the distillation tower 5 is vaporized and rises, and the vaporized steam rises and meets the molten salt pumped to the top of the distillation tower 5 by the molten salt pump 8 and the molten salt liquid pumped into the distillation tower 5 by the molten salt pump 8. During the rising process, the composition of the steam is constantly changing due to changes in temperature and pressure, and the downstream molten salt liquid is mainly a mixture rich in potassium chloroaluminate. Therefore, when the steam contacts the molten salt liquid, the saturated vapor pressure of hafnium tetrachloride is relatively low, and it is more easily absorbed by the molten salt liquid, thereby remaining in the liquid phase, while the saturated vapor pressure of zirconium tetrachloride is relatively high, and it is more inclined to remain in the gas phase during the gas-liquid exchange process and continue to rise, among which the continuously rising A small amount of hafnium tetrachloride is still left in the steam, which is recovered into the reflux tank 9 through a valve and continues to participate in the distillation process of the distillation tower 5. The molten salt flowing downward continuously exchanges with the zirconium tetrachloride dissolved in the molten salt, which promotes the continuous enrichment of hafnium tetrachloride at the top of the tower. The time and temperature required for each stage of distillation can be input through the control computer group, and the galvanic sensor can feedback the current temperature data in real time. When the air pressure at the top of the tower and the concentration of hafnium tetrachloride reach a certain level, hafnium tetrachloride comes out from the top of the tower and is cooled down through the condenser 6. As a raw material for extracting hafnium, the bottom tank 3 is connected to the bottom end of the feed tower 7 to separate the distilled hafnium tetrachloride from potassium chloroaluminate, and the atomic-level zirconium tetrachloride is transported to the condenser 6 for cooling with nitrogen. The entire molten salt distillation process is strictly controlled by the control computer group.

[0071] The present invention covers any substitution, modification, equivalent method and scheme made on the essence and scope of the present invention. In order to make the public have a thorough understanding of the present invention, specific details are described in detail in the following preferred embodiments of the present invention, but those skilled in the art can fully understand the present invention without the description of these details. In addition, in order to avoid unnecessary confusion about the essence of the present invention, well-known methods, processes, procedures, components and circuits are not described in detail.

[0072] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A zirconium-hafnium separation device using a molten salt distillation method, comprising a storage tank and a distillation tower, characterized in that: The bottom of the distillation tower is fixedly connected to a bottom tank, the bottom of the bottom tank is fixedly connected to a molten salt pump, the top of the distillation tower is fixedly connected to a condenser, one side of the bottom tank is fixedly connected to a reboiler, one side of the distillation tower is fixedly connected to a feed tower, and one side of the condenser is connected to a reflux tank through a pipeline; Two feeding tanks are fixedly connected to the top of the storage tank, a distribution tank is fixedly connected to the top of the feeding tank, a control valve is installed on the distribution tank, and a feeding hopper is fixedly connected to the top of the distribution tank; A feeding mechanism, which is used to assist an operator in feeding the device, and is connected to the feeding hopper; The feeding mechanism includes a lower positioning plate, a lifting mechanism and an upper positioning plate, wherein the lower positioning plate is rotatably connected to the feeding hopper, the lifting mechanism is fixedly connected to one side of the feeding hopper, and the upper positioning plate is fixedly connected to the lifting mechanism, and the lifting mechanism is a linear lifting device driven by a screw and a servo motor; An arc-shaped concave contour is provided on the outer side wall of the lower positioning plate, and an arc-shaped plate is fixedly connected to the middle position of the lower positioning plate, the arc-shaped plate has an arc that bends downward, and a leakage hole is opened on the arc-shaped plate; An inner clip is fixedly connected to the inner wall of the lower positioning plate, the inner clip has a trapezoidal profile, an inwardly inclined inclined plate is fixedly connected to one side of the inner clip, a weakening groove is provided on the other side of the inner clip, an electromagnet matching the profile of the inner clip is inserted into the inner clip, and the inner clip and the lower positioning plate are an integrally manufactured structure; A first extrusion portion is fixedly connected to the outer wall of the upper positioning plate, a second extrusion portion is fixedly connected to the inner wall of the upper positioning plate, a support portion is fixedly connected inside the upper positioning plate, the support portion is located between the first extrusion portion and the second extrusion portion, and the top inner wall of the upper positioning plate has an inclined surface inclined toward the middle; The first extrusion portion and the second extrusion portion both have an arc-shaped profile facing away from the support portion, and the first extrusion portion and the second extrusion portion are both elastic structures.

2. The zirconium-hafnium separation device using the molten salt distillation method according to claim 1, characterized in that: A hydraulic telescopic rod is rotatably connected to the inner wall of the feeding hopper, and both ends of the hydraulic telescopic rod are respectively connected to the feeding hopper and the lower positioning plate. One side of the lower positioning plate is rotatably connected to a rotating shaft, and the lower positioning plate and the feeding hopper are connected via the rotating shaft.

3. The zirconium-hafnium separation device using the molten salt distillation method according to claim 1, characterized in that: A lifting plate is fixedly connected to the lifting mechanism, the upper positioning plate and the lifting mechanism are connected via the lifting plate, and the lifting plate and the upper positioning plate are fixed via screws.

4. The zirconium-hafnium separation device using the molten salt distillation method according to claim 3, characterized in that: The bottom of the lifting plate is rotatably connected to a first rotating rod, one end of the first rotating rod is rotatably connected to a second rotating rod, one end of the second rotating rod is rotatably connected to a plunger, one end of the plunger is fixedly connected to a pull rod, a pull groove is provided at one end of the second rotating rod close to the pull rod, a clamping block is fixedly connected in the pull groove, and a buckle is fixedly connected to the bottom of the lifting plate, and the buckle is a C-shaped elastic structure.

5. The zirconium-hafnium separation device using the molten salt distillation method according to claim 1, characterized in that: A metal cover is installed at the bottom of the metal container, and an outward-turned portion is provided at the end of the metal cover. The outward-turned portion has an outwardly curved profile. The metal container and the metal cover are both made of metal materials that can be adsorbed by magnets. A thermocouple sensor, a temperature sensor and a pressure sensor are installed on the reboiling tower.

6. The method for using the zirconium-hafnium separation device by molten salt distillation method according to any one of claims 1 to 5, characterized in that: The following steps are involved: Step 1, loading: when zirconium tetrachloride needs to be added, insert the metal container into the upper positioning plate and let it be upside down on the top of the lower positioning plate. After the metal container is placed, energize the electromagnet to allow the lower positioning plate to absorb the metal cover. At the same time, the lifting mechanism drives the upper positioning plate to move toward the metal cover. During the movement of the upper positioning plate, its inner wall will squeeze the outer wall of the metal container, so that the upper positioning plate and the metal container are clamped and fixed together under the action of friction. The bottom of the upper positioning plate will squeeze the outward turning part on the metal cover and let the metal cover separate from the metal container. When the metal cover is separated from the metal container, the lifting mechanism drives the upper positioning plate to move in the opposite direction. During the reverse movement of the upper positioning plate, the metal container will be driven away from the metal cover. At the same time, the hydraulic telescopic rod drives the lower positioning plate to move in the opposite direction. The positioning disk rotates, and the metal cover will also rotate under the adsorption of the electromagnet during the rotation of the lower positioning disk. At this time, the zirconium tetrachloride in the metal container will enter the distribution tank; when molten salt needs to be added, first adjust the control valve on the distribution tank to allow the material dropped from the feeding hopper to enter another feeding tank, then rotate the first rotating rod and the second rotating rod to make the knife parallel to the lower positioning disk, and then pull the pull rod to rotate the knife downward 90 degrees, so that the knife and the lower positioning disk are perpendicular to each other, place the molten salt bag on the top of the lower positioning disk, and then let the lifting mechanism drive the knife to move toward the molten salt bag. After the knife moves to the position of the molten salt bag, it will cut a hole in the molten salt bag. At this time, the molten salt in the molten salt bag will leak into the distribution tank from the leakage hole on the arc plate along the hole; Step 2, distillation, open the valve bodies on the two feed tanks in turn, let the zirconium tetrachloride and molten salt in the feed tank enter the storage tank, a spiral feeding structure is installed in the storage tank, the zirconium tetrachloride and molten salt in the storage tank are transported to the bottom tank through the spiral feeding structure, the reboiling tower heats the material in the bottom tank to boiling, the steam generated by the boiling material will pass upward through the tower plate of the distillation tower to form an ascending steam flow, the steam at the top of the distillation tower is cooled into liquid by the condenser to form a reflux liquid, the reflux liquid will flow downward along the tower plate or filler and meet the rising steam to exchange heat and mass, the low boiling point component continues to rise, and the high boiling point component is brought back to the bottom of the distillation tower by the reflux liquid, so that the material is separated into products by continuous operation.

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