A method of using an apparatus for the extraction of metal ions from a molten salt

Abstract

The application provides a metal ion molten salt extraction device, which comprises a piston, a sealed pipe, a fixing part, a rubber hose, a quartz pipe and a filter screen. The sealed pipe is a straight pipe with open ends, one end of which is provided with the piston, and the other end is provided with the fixing part. The rubber hose is internally through and has open ends, one end of which is connected with the sealed pipe through the fixing part, and the other end is connected with the quartz pipe. The quartz pipe is a straight pipe with open ends, one end of which is connected with the rubber hose, and the other end is a molten salt sampling port. The filter screen is arranged at the molten salt sampling port and is used for filtering the metal powder possibly taken during sampling, so as to ensure that the metal ion concentration in the sample is not affected. The application also provides a use method of the device. Through the method of placing preset metal particles and rapidly cooling the sample in the quartz pipe, the chemical equilibrium deviation caused by the disproportionation reaction of metal ions is inhibited, and the accurate and rapid sampling of the multivalent metal ions in the molten salt is realized.

Description

Technical Field

[0001] This invention belongs to the field of electrochemical metallurgy technology, specifically relating to an extraction device for high-temperature molten salt containing multivalent metal ions, and a method for using the device. Background Technology

[0002] Rare metals have garnered significant attention in modern society due to their superior physicochemical properties, such as high-temperature resistance and corrosion resistance. In recent years, with the continuous development of advanced science and technology, the application fields of rare metals with superior properties have been expanding, and demand has been increasing. Molten salt electrolysis is a promising method for preparing rare metals, using high-temperature molten salt as the electrolyte during the electrolysis process. During the electrolytic production of metals, it is crucial to continuously monitor the composition of the molten salt and understand its composition within the electrolytic cell to assess the real-time electrolysis status. However, the high temperature and strong corrosiveness of molten salt make sampling difficult. Furthermore, metal powder generated during electrolysis can easily contaminate the sample, affecting the concentration of the metal ions to be measured. Simultaneously, multivalent metal ions exist in multiple valence states within the molten salt. Ions in different valence states undergo reversible disproportionation / disproportionation reactions, and the reaction equilibrium is influenced by ion concentration. The absence of zero-valence metals in the sample after filtering metal powder can affect the reaction equilibrium, causing changes in the valence state of metal ions and resulting in discrepancies with actual results, thus impacting subsequent testing. Therefore, accurate sampling of multivalent metal ions in molten salt is a critical issue. Summary of the Invention

[0003] The technical problem solved by this invention is that it is currently difficult to sample high-temperature molten salts containing multivalent metal ions, and the metal ions in the sampling results are prone to reaction, affecting the final results.

[0004] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0005] An extraction device for molten metal ions includes a piston, a sealing tube, a fixing component, a rubber hose, a quartz tube, and a filter screen, wherein...

[0006] The sealing tube is a straight tube open at both ends, with a piston at one end and a fixing member at the other end. The fixing member has a through hole in its center, allowing the sealing tube to communicate with the inner cavity of the rubber hose.

[0007] The rubber hose is internally continuous and open at both ends. One end is connected to the sealing tube through a fixing component, and the other end is connected to the quartz tube.

[0008] The quartz tube is a straight tube with openings at both ends; one end is connected to a rubber hose, and the other end is a molten salt sampling port.

[0009] The filter screen is installed at the molten salt sampling port to filter out any metal powder that may be collected during sampling.

[0010] Preferably, the piston is located in the sealing tube and can reciprocate along the axis of the sealing tube, and a handle is installed at the end of the piston away from the fixed part to realize the movement of the piston.

[0011] Preferably, a connecting tube is arranged between the fixed part and the rubber hose, and the connecting tube is a straight tube with two open ends. The connecting tube is a rigid tube, one end of which is clamped with the fixed part, and the other end is in interference fit with the rubber hose, that is, the inner diameter of the rubber hose matches the outer diameter of the connecting tube to realize sealing. Compared with directly connecting the rubber hose with the fixed part, the connecting tube can better realize the connection and sealing between the sealing tube and the rubber hose.

[0012] Preferably, the fixed part is located between the sealing tube and the connecting tube to realize the fixed connection and sealing of the sealing tube and the connecting tube. A through hole is arranged in the center of the fixed part, and the through hole is arranged along the axial direction of the fixed part to realize the communication of the inner cavities of the sealing tube and the connecting tube.

[0013] Preferably, the materials of the sealing tube and the connecting tube are quartz or glass.

[0014] Preferably, a scale is arranged on the quartz tube to control the amount of extracted sample.

[0015] Preferably, the mesh aperture is 500 mesh.

[0016] Preferably, the mesh is built in the quartz tube, and pre-set metal particles are placed on the mesh. The type of the pre-set metal particles is consistent with the corresponding metal of the metal ions to be extracted in the molten salt, which is used to inhibit the disproportionation reaction of the metal ions and avoid the deviation of the chemical equilibrium.

[0017] The description of "the type of the pre-set metal particles is consistent with the corresponding metal of the metal ions to be extracted in the molten salt" is as follows: if the target of the test or analysis after sampling is titanium ions, the pre-set metal particles are titanium particles; if the target of the test or analysis after sampling is vanadium ions, the pre-set metal particles are vanadium particles.

[0018] The amount of the pre-set metal particles added is related to the sampling amount of the molten salt. It is necessary to ensure that enough pre-set metal particles are added to maintain the chemical equilibrium in the molten salt.

[0019] In the present application, the pre-set metal particles placed on the mesh are more important. If there are no pre-set metal particles, the chemical equilibrium of the extracted molten salt will deviate. Taking titanium ions as an example, the chemical equilibrium in the molten salt is 3Ti 2+ = Ti + 2Ti 3+ If there are no pre-set titanium particles on the mesh, the chemical equilibrium will move to the right, so that the divalent titanium ions in the extracted molten salt sample will decrease and the trivalent titanium ions will increase, which will affect the subsequent test results.

[0020] The application also provides a method for using the extraction device of the metal ion molten salt, comprising the following steps:

[0021] S1, placing a sufficient amount of preset metal particles on the filter screen before sampling;

[0022] S2, pressing the handle to move the piston towards the fixed part until the end of the piston contacts the fixed part, and then placing the molten salt sampling end of the quartz tube provided with the filter screen into the high-temperature molten salt;

[0023] S3, pulling the handle to move the piston away from the fixed part, so that the molten salt passes through the filter screen and enters the inside of the quartz tube until the required amount of high-temperature molten salt is obtained;

[0024] S4, sealing the molten salt sampling port by using the cork, and rapidly cooling the quartz tube in water;

[0025] S5, taking out the extraction device after the molten salt is cooled, taking out the molten salt sample, and leaving it for subsequent characterization.

[0026] The function of rapidly cooling the quartz tube in water is to accelerate the solidification of the sample. Since the reaction rate of metal ions between different valence states is extremely low when the molten salt is in a solid state, the rapid cooling method in water is used to accelerate the solidification of the sample, reduce the time of the sample in a liquid state, and better maintain the real distribution of metal ions of different valence states in the sample, thereby ensuring the accuracy of the test results.

[0027] Compared with the prior art, the application has the following beneficial effects:

[0028] 1) The application provides an extraction device of a metal ion molten salt. In the molten salt sampling process, the filter screen can be used to avoid the mixing of metal powder in the molten salt into the sample, thereby ensuring that the concentration of metal ions in the sample is not affected.

[0029] 2) The application also provides a method for using the device, which suppresses the chemical equilibrium deviation caused by the disproportionation reaction of metal ions by placing preset metal particles in the quartz tube and rapidly cooling the sample, thereby realizing accurate and rapid sampling of metal ions of different valence states in the molten salt. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the application, the following will briefly introduce the drawings needed to be used in the embodiment description. Obviously, the drawings in the following description are only some embodiments of the application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0031] Figure 1 Fig. 1 is a structural schematic diagram of the extraction device of the metal ion molten salt of the application;

[0032] Among them, 1-handle, 2-piston, 3-sealing tube, 4-fixing component, 5-connecting tube, 6-rubber hose, 7-quartz tube, 8-pre-placed metal particles, 9-filter screen. Detailed Implementation

[0033] The technical solutions and problems solved by the embodiments of the present invention will be described below with reference to the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them.

[0034] like Figure 1 As shown, an extraction device for molten metal ions according to the present invention includes a piston 2, a sealing tube 3, a fixing member 4, a rubber hose 6, a quartz tube 7, and a filter screen 9, wherein...

[0035] The sealing tube 3 is a straight tube open at both ends. A piston 2 is installed at one end, and a fixing member 4 is installed at the other end. The fixing member 4 has a through hole in its center, so that the sealing tube 3 communicates with the inner cavity of the rubber hose 6.

[0036] The rubber hose 6 is internally continuous and open at both ends. One end is connected to the sealing tube 3 through the fixing member 4, and the other end is connected to the quartz tube 7.

[0037] The quartz tube 7 is a straight tube with openings at both ends. One end is connected to a rubber hose 6, and the other end is a molten salt sampling port for obtaining high-temperature molten salt. The filter screen 9 is set at the molten salt sampling port to filter out metal powder that may be obtained during sampling.

[0038] In one embodiment of the present invention, the piston 2 is located inside the sealing tube 3 and can reciprocate along the axis of the sealing tube 3. A handle 1 is installed at the end of the piston 2 away from the fixing member 4 to realize the piston movement.

[0039] In one embodiment of the present invention, a connecting pipe 5 is provided between the fixing member 4 and the rubber hose 6. The connecting pipe 5 is a straight pipe open at both ends. Since the connecting pipe 5 is a rigid pipe, one end is snapped into the fixing member 4, and the other end is interference-fitted with the rubber hose 6, that is, the inner diameter of the rubber hose 6 matches the outer diameter of the connecting pipe 5 to achieve a seal. Compared with directly connecting the rubber hose 6 to the fixing member 4, using the connecting pipe 5 can better achieve the connection and seal between the sealing pipe and the rubber hose.

[0040] In one embodiment of the present invention, the fixing member 4 is located between the sealing tube 3 and the connecting tube 5 to achieve a fixed connection and seal between the sealing tube 3 and the connecting tube 5. A through hole is provided at the center of the fixing member 4, and the through hole is arranged axially along the fixing member 4 to achieve communication between the inner cavities of the sealing tube 3 and the connecting tube 5.

[0041] In one embodiment of the present application, the material of the sealing tube 3 and the connecting tube 5 is quartz or glass. The quartz tube 7 is provided with a scale, which can control the amount of extracted sample. The aperture of the filter screen 9 is 500 mesh.

[0042] In one embodiment of the present application, the filter screen 9 is built in the quartz tube 7, and the preset metal particles 8 are placed on the filter screen 9. The type of the preset metal particles 8 is consistent with the corresponding metal of the metal ions to be extracted, which is used to inhibit the disproportionation reaction of the metal ions and avoid the deviation of chemical equilibrium.

[0043] Embodiment 1

[0044] The extraction device for metal ion molten salt is used to sample the molten salt, and the titanium ions in the molten salt are sampled and analyzed, and the specific steps are as follows:

[0045] S0, prepare NaCl-KCl-TiCl2 electrolyte according to the molar ratio of 1:1:1, heat the prepared electrolyte in the electrolytic cell under the protection of argon to 900 ℃, and then keep warm for 2 h until the electrolyte is completely melted. When the temperature in the electrolytic cell is uniform, start sampling.

[0046] S1, place a sufficient amount of titanium metal particles on the filter screen, press down the piston, and place the quartz tube provided with the filter screen into the high-temperature molten salt. Pull the piston away from the fixed part, and the molten salt passes through the filter screen into the inside of the quartz tube until the desired amount of high-temperature molten salt is obtained. Then, seal the sampling port with a cork, and place the quartz tube in water for rapid cooling. After the molten salt is cooled, the extraction device is taken out, and the molten salt sample is taken out for subsequent characterization.

[0047] When the above extraction device is used, usually 10 grams of metal is placed in the filter screen. Taking the sampling of 10 grams of molten salt as an example, it is calculated that the divalent titanium ions in the sampled molten salt are 1.90 grams. According to the reaction equation 3Ti 2+ = Ti + 2Ti 3+ , 0.63 grams of titanium metal particles are added to ensure the reaction balance.

[0048] Embodiment 2

[0049] The extraction device for metal ion molten salt is used to sample the molten salt, and the titanium ions in the molten salt are sampled and analyzed, and the specific steps are as follows:

[0050] S0, prepare NaCl-KCl-TiCl2 electrolyte according to the molar ratio of 1:1:1, heat the prepared electrolyte in the electrolytic cell under the protection of argon to 900 ℃, and then keep warm for 2 h until the electrolyte is completely melted. When the temperature in the electrolytic cell is uniform, start sampling.

[0051] S1, a sufficient amount of metal zirconium particles is placed behind the filter screen, the piston is pressed down, the quartz tube provided with the filter screen of the molten salt sampling port is placed into the high-temperature molten salt, the piston is pulled to move away from the fixed part, the molten salt passes through the filter screen into the inside of the quartz tube, until the required amount of high-temperature molten salt is obtained; then the sampling port is sealed by using a cork, and the quartz tube is placed in water for rapid cooling; after the molten salt is cooled, the extraction device is taken out, the molten salt sample is taken out, and is left for subsequent characterization.

[0052] The above is the preferred embodiment of the present application, it should be pointed out that, for those skilled in the art, without departing from the principles of the present application, can also make a number of improvements and refinements, these improvements and refinements should also be considered as the protection scope of the present application.

Claims

1. A method of using a device for extracting molten salt of metal ions, characterized in that, Includes the following steps: S1. Place a sufficient amount of pre-placed metal particles on the filter screen before sampling; S2. Press down the handle to move the piston closer to the fixed part until one end of the piston contacts the fixed part, and then put the molten salt sampling end of the quartz tube with the filter screen into the high temperature molten salt. S3. Pull the handle to move the piston away from the fixed part. The molten salt enters the quartz tube through the filter screen until the required amount of high-temperature molten salt is obtained. S4. Seal the molten salt sampling port with a cork and rapidly cool the quartz tube in water. S5. After the molten salt cools, remove the extraction device and take out the molten salt sample for subsequent characterization. The metal ion molten salt extraction device includes a piston, a sealing tube, a fixing component, a rubber hose, a quartz tube, and a filter screen, wherein... The sealing tube is a straight tube open at both ends, with a piston at one end and a fixing member at the other end. The fixing member has a through hole in its center, allowing the sealing tube to communicate with the inner cavity of the rubber hose. The rubber hose is internally continuous and open at both ends. One end is connected to the sealing tube through a fixing component, and the other end is connected to the quartz tube. The quartz tube is a straight tube with openings at both ends; one end is connected to a rubber hose, and the other end is a molten salt sampling port. The filter screen is installed at the molten salt sampling port and is built into the quartz tube. Pre-placed metal particles are placed on the filter screen, and the type of the pre-placed metal particles is consistent with the metal ions to be sampled in the molten salt.

2. The method of using the metal ion molten salt extraction device according to claim 1, characterized in that, The piston is located inside the sealing tube and can reciprocate along the axis of the sealing tube. A handle is installed at the end of the piston away from the fixed member to realize the piston movement.

3. The method of using the metal ion molten salt extraction device according to claim 1, characterized in that, A connecting pipe is provided between the fixing component and the rubber hose. The connecting pipe is a straight pipe with open ends. One end is snapped into the fixing component, and the other end is interference-fitted with the rubber hose.

4. The method of using the metal ion molten salt extraction device according to claim 3, characterized in that, The fixing component is located between the sealing tube and the connecting tube, and a through hole is provided at the center of the fixing component. The through hole is arranged along the axial direction of the fixing component to realize the communication between the inner cavities of the sealing tube and the connecting tube.

5. The method of using the metal ion molten salt extraction apparatus according to any one of claims 1 to 4, characterized in that, The sealing tube and connecting tube are made of quartz or glass.

6. The method of using the metal ion molten salt extraction apparatus according to any one of claims 1 to 4, characterized in that, The quartz tube has graduations.

Images