Method for preparing alkali metal material from halogenated alkali metal salt and high-calcium sodium

Abstract

The invention discloses a method for preparing an alkali metal material from halogenated alkali metal salt and high-calcium sodium, and relates to the technical field of alkali metal recovery and preparation. The halogenated alkali metal salt is dried and dewatered through drying and dewatering equipment; crushing or dissociating the high-calcium sodium through sodium slag crushing equipment; introducing the halogenated alkali metal salt in the step S100 and the high-calcium sodium in the step S200 into a high-temperature vacuum furnace, and carrying out a replacement reaction under the protection of inert gas; the alkali metal material serving as a replacement reaction product is guided into a storage tank in a distillation mode to be stored; compared with the prior art, the method has the technical advantages that the high-calcium sodium obtained by electrolyzing sodium chloride is relatively thoroughly treated and subjected to impurity removal through the replacement reaction of the halogenated alkali metal salt and the high-calcium sodium, the sodium is purified for subsequent application, the calcium accounting for the second position by mass is also treated, the post-treatment process is reduced, and the economical efficiency is further improved; equipment and energy required by the method are appropriate in cost, high in pertinence and safe to operate.

Description

Technical Field

[0001] The present application relates to the technical field of alkali metal recovery and preparation, and in particular to a method for preparing alkali metal materials from halogenated alkali metal salts and high calcium sodium. Background Art

[0002] During the sodium chloride molten electrolysis process to produce metallic sodium, a certain amount of electrolytic tailings, commonly known as high-calcium sodium or secondary sodium, remains after the metallic sodium is separated from the electrolytic cell. High-calcium sodium accounts for approximately 3% of the metallic sodium output, with 60-80% sodium and 10-40% calcium. The remaining residual molten salts include sodium chloride, calcium chloride, and oxide impurities such as sodium oxide and calcium oxide. High-calcium sodium is difficult to handle, and long-term storage poses a safety hazard. Extracting metallic sodium from high-calcium sodium not only improves economic efficiency but also allows for the recycling and reuse of hazardous waste, eliminating safety hazards and environmental pollution.

[0003] The current methods for treating metallic high calcium sodium in industrial production include the extrusion method mentioned in CN2846437Y and CN2846436Y; the vacuum distillation method proposed in CN104294054A and CN102634671A; the sub-boiling distillation of thermal radiation synergistic distillation in CN103757435A and CN203700465U; the vacuum distillation in CN103667708A, CN111363922A and CN212560390U; The molten salt heating method of 07574318A; the molten electrolysis method mentioned in CN108048872B, CN203700555U, CN108624913A and "Research on the Purification of Metallic Sodium by Na•β-Al_2O_3 Diaphragm"; the direct heating filtration method adopted by patents CN206188863U, CN109136579B, and CN208378965U; in addition, there are other treatment methods such as heated solvent filtration method, cold trap method, chemical treatment method, sedimentation method, etc. Some of the products obtained by these methods are not completely free of impurities, some introduce new substances that need to be separated, and the required equipment cost and energy consumption are high; in addition, these methods do not solve the treatment of calcium slag, which accounts for the second largest proportion by mass in high-calcium sodium. Because the calcium slag has a high hardness and is relatively active, in addition to vacuum distillation, which places certain requirements on the equipment, it is difficult to collect high-purity calcium products. In order to thoroughly treat high-calcium sodium, there is an urgent need for a method that can conveniently recycle both sodium and calcium in high-calcium sodium; when drying and pretreating the halogenated alkali metal salt, it is necessary to regularly stir the material and collect temperature and humidity. After the halogenated alkali metal salt material is stirred evenly, a thermometer and hygrometer are manually inserted, which is difficult to do manually during high-temperature operations. Alternatively, a thermometer and hygrometer are directly embedded, but the embedded height is fixed, resulting in inaccurate collected data, and the thermometer and hygrometer are easily damaged when exposed to a high-temperature environment for a long time. How to achieve a reasonable linkage between the stirring structure and the temperature and humidity collection has also become a technical problem to be solved by those skilled in the art. Summary of the Invention

[0004] In response to the shortcomings of the prior art, the present invention provides a method for preparing an alkali metal material from a halogenated alkali metal salt and high-calcium sodium. This method solves the technical problems in the prior art of difficulty in reasonably recovering and fully utilizing high-calcium sodium and generating secondary slag waste. The method can also synthesize high-value alkali metals to increase the added value of the product. Specific implementation methods are as follows: A method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium comprises the following steps: S100, drying and removing water from the halogenated alkali metal salt by a drying and water removal device; S200, crushing or dissociating high calcium sodium through sodium slag crushing equipment; S300, introducing the alkali metal halide in step S100 and the high calcium sodium in step S200 into a high-temperature vacuum furnace, and performing a replacement reaction under the protection of an inert gas; The reaction principle of the replacement reaction in step S400 and step S300 is: Na+Ca+MX→NaX+CaX2+M Ca + Na2O → CaO + Na Wherein, M refers to one or more of lithium, sodium, potassium, rubidium, and cesium, and X refers to halogen, which is one or both of chlorine and fluorine; S500, introducing the alkali metal material as the displacement reaction product into a storage tank by distillation for storage.

[0005] Preferably, the halogenated alkali metal salt is one or more fluorinated or chlorinated alkali metal salts; the main components of the high calcium sodium are: 60-80% sodium, 10-40% calcium, and the remaining small amount of residual molten salt such as sodium chloride, calcium chloride, oxide impurities such as sodium oxide, calcium oxide, etc.

[0006] Preferably, the alkali metal material is one or more alkali metal elements or alkali metal alloys; the alkali metal is one or more of lithium, sodium, potassium, rubidium, and cesium; the alkali metal alloy is an alkali metal alloy composed of a mixture of one or more alkali metals among lithium, potassium, rubidium, and cesium and sodium in an appropriate proportion.

[0007] Based on the above technical solution, a more thorough impurity removal process can be achieved through the replacement reaction of halogenated alkali metal salts with the high-calcium sodium obtained by electrolysis of sodium chloride. This process not only purifies sodium for subsequent applications, but also simultaneously treats calcium, the second most abundant element, effectively shortening the post-processing process. This technical approach not only improves sodium purity but also further enhances overall economic efficiency by simplifying the process chain.

[0008] Preferably, the ratio of the halogenated alkali metal salt to the high calcium sodium is 0.5-10:1.

[0009] Preferably, in step S100, calcium chloride is further added to the drying and dehydration equipment to form a mixed salt with the halogenated alkali metal salt as a reaction substrate to reduce the melting point of the desired mixture.

[0010] Preferably, the high calcium sodium in step S200 is crushed and dissociated under an inert gas environment, and the inert gas in step S200 and step S300 is argon.

[0011] Based on the above technical solutions, the method for removing water from the halogenated alkali metal salt can be selected from one or more of vacuum high-temperature dehydration, microwave drying, azeotropic distillation, vibrating fluidized bed drying, membrane separation and the like.

[0012] Preferably, the sodium slag crushing equipment in step S200 adopts a method of adding a solvent after heating and performing layered filtration and separation by utilizing the difference in density and degree of complexation, wherein the solvent is one or more density gradient liquids such as thermal silicone oil, 2-methylnaphthalene, high-boiling point saturated aliphatic hydrocarbons or aromatic hydrocarbons, ionic liquids, esters, and ethers.

[0013] Based on the above technical solution, the high calcium sodium crushing and dissociation method can also be selected to use one or more of a double spiral belt crushing device, a hammer type, and a toothed disc crusher in an inert gas environment to crush by mechanical force.

[0014] Preferably, the temperature of the replacement reaction in step S300 is 600-900° C., the holding time is 3-12 h, and the pressure in the furnace is 0.05-0.5 MPa.

[0015] Preferably, in step S600, by-product separation is performed by vacuum distillation or hot filtration, and the by-product is a mixture of calcium chloride and sodium chloride composite salts used for preparing deicing agent.

[0016] Based on the above technical solution, after the required alkali metal or alkali metal alloy is prepared, the product and by-products need to be separated by vacuum distillation or hot filtration. The resulting by-products, such as a mixture of complex salts such as calcium chloride and sodium chloride, can be further prepared into the main component of a de-icing agent or processed in other ways.

[0017] A device for preparing an alkali metal material from a halogenated alkali metal salt and high-calcium sodium includes a drying and dehydration device used for vacuum high-heat dehydration in step S100. The drying and dehydration device includes a drying box and a heating base. A square isolation box is provided in the drying box, and the halogenated alkali metal salt is filled in a C shape in the drying box.

[0018] The square isolation box is equipped with a linkage component, which includes a vertical closed-loop conveyor belt. Temperature and humidity probes and flip plates are respectively provided at the high and low positions on both sides of the conveyor belt. The overall outline of the flip plate is consistent with the C-shaped layout of the drying box. A second opening is opened at the low position of the square isolation box, and the temperature and humidity probe is connected to the second opening when it is at the low end.

[0019] A lifting component is also vertically provided in the square isolation box. The output end of the lifting component is connected to the flip plate. The lifting and lowering of the flip plate is transmitted to the temperature and humidity probe through the linkage component, and the lifting and lowering directions of the flip plate and the temperature and humidity probe are opposite.

[0020] Based on the above technical solution, when the halogenated alkali metal salt is pretreated in a high-temperature vacuum furnace, moisture can be effectively removed through the drying process. When testing the degree of dryness, the temperature and humidity probe and the flip plate adopt a linkage design: after the flip plate completes flipping the material, the temperature and humidity probe is exposed for testing. This linkage mechanism not only ensures the uniformity of the test sample, but also protects the temperature and humidity probe during the material flipping process, achieving dual optimization of process reliability and detection accuracy.

[0021] In summary, this application has the following beneficial technical effects: 1. The present invention uses a replacement reaction between a halogenated alkali metal salt and high-calcium sodium to thoroughly remove impurities from the high-calcium sodium obtained by electrolysis of sodium chloride. Not only is the sodium purified for subsequent applications, but the calcium, which accounts for the second largest proportion by mass, is also processed, thereby reducing the post-processing process and further improving economic efficiency. 2. The equipment and energy costs required by the present invention are reasonable, the process is simple, the targeting is strong and the operation is safe; 3. The present invention has a simple structure. By pre-treating the halogenated alkali metal salt in a high-temperature vacuum furnace, water can be effectively removed through drying. When the temperature and humidity probe is used to detect the dryness, a flip plate is linked to the temperature and humidity probe. After the flip plate flips the material, the temperature and humidity probe is exposed for testing. This not only improves the uniformity of the test sample, but also protects the temperature and humidity probe. 4. The flip plate in the present invention can be linked with the temperature and humidity probe, and can also perform an independent material flipping effect, reducing the exposure frequency of the temperature and humidity probe before drying is completed, and further improving the durability of the temperature and humidity probe. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the process flow of the present invention; Figure 2 It is a structural schematic diagram of the present invention; Figure 3 It is a schematic diagram of the explosion structure of the present invention; Figure 4 This is a cross-sectional view of the present invention after the cooling structure is added; Figure 5 This is a cross-section of the structure of the present invention Figure 1 ; Figure 6 This is a cross-section of the structure of the present invention Figure 2 ; Figure 7 This is a cross-section of the structure of the present invention Figure 3 ; Figure 8 It is a schematic diagram of the explosion structure of the drying box in the present invention; Figure 9 This is a schematic diagram of the structure of the linkage assembly and the flip plate in the present invention. Figure 1 ; Figure 10 In the present invention Figure 9 An enlarged schematic diagram of Figure 11 It is a cross section of the linkage assembly and the flap structure of the present invention; Figure 12 This is a schematic diagram of the structure of the linkage assembly and the flip plate in the present invention. Figure 2 .

[0023] Description of reference numerals: 1. Drying oven, 2. Linkage assembly, 3. Flip plate, 4. Temperature and humidity probe, 5. Locking assembly, 6. Square isolation box, 7. Lifting seat, 8. Cooling tower, 9. Cooling unit, 10. Heating base, 11. Thermal liquid tank, 12. Liquid pipeline, 13. Opening and closing valve, 14. Temperature sensor, 15. Water pump, 16. Lifting assembly, 101. Feeding port, 102. Top cover, 103. Bulk material conical head, 201, conveyor belt, 202, partition plate, 203, elastic expansion member, 204, guide wheel, 205, vertical guide groove, 206, serrated, 207, side plate, 301, mounting seat, 302, angled bulk plate, 303, transverse plate, 501, handle, 502, gear, 503, synchronization block, 504, locking wheel, 601, first opening, 602, second opening. DETAILED DESCRIPTION

[0024] The specific implementation of the present invention is described below with reference to the accompanying drawings and embodiments: It should be noted that the structures, proportions, sizes, etc. illustrated in the drawings of this specification are only used to match the contents disclosed in the specification for people familiar with this technology to understand and read, and are not used to limit the conditions under which the present invention can be implemented. Any structural modification, change in proportional relationship or adjustment of size should still fall within the scope of the technical content disclosed in the present invention without affecting the efficacy and purpose that can be achieved by the present invention.

[0025] At the same time, the terms such as "upper", "lower", "left", "right", "middle" and "one" quoted in this specification are only for the convenience of description and are not used to limit the scope of implementation of the present invention. Changes or adjustments to their relative relationships should be regarded as the scope of implementation of the present invention without substantially changing the technical content.

[0026] The following is combined with Figure 1-12 This application is described in further detail.

[0027] The present application discloses a method for preparing an alkali metal material using a halogenated alkali metal salt and high calcium sodium.

[0028] Example 1, with reference to Figure 1 This embodiment discloses a method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium. The method is used to prepare refined sodium, comprising the following steps: The first step is to place 100 kg of high calcium sodium in a high calcium sodium melting tank, start argon protection, and slowly heat it to above 120 ° C. After the high calcium sodium is initially dissociated, start stirring to accelerate the dissociation. The stirring speed gradually increases from slow to fast depending on the degree of dissociation, and is maintained at 50-300 rpm to obtain molten high calcium sodium; In the second step, 105 kg of sodium chloride solid and 160 kg of calcium chloride solid are placed in a high-temperature resistance furnace for vacuum high-temperature dehydration at 200 ° C for 2 hours under 10-100 Pa to make the water content no more than 0.1%.

[0029] In the third step, the molten high-calcium sodium and dry sodium chloride and calcium chloride solids are placed in a high-temperature vacuum furnace at 600-800°C through pipelines and a feeding device for a replacement reaction. Under the protection of argon, metallic sodium and calcium chloride are gradually formed.

[0030] In the fourth step, the replacement reaction ends when the temperature stabilizes and no longer rises significantly or drops slightly, and the detector detects that the amount of sodium vapor no longer changes and continues to maintain for two hours. After the replacement reaction is completed, the formed metallic sodium is distilled into a sodium storage tank under a low vacuum of 0.1-1 Pa to obtain about 99.4 kg of sodium with a content of about 99.9%. The final sodium is die-cast into a silver-white cylindrical sodium ingot with a diameter of about 30 mm, a length of about 500 mm, and a weight of about 35 kg.

[0031] In the fifth step, after the reaction is completed, the by-products remaining in the high-temperature vacuum furnace are cooled and taken out through the liftable furnace and rotating arm, resulting in a white solid mixture of approximately 243 kg of calcium chloride and 17 kg of sodium chloride, which also contains a very small amount of sodium oxide, calcium oxide and other small impurities, which can be used in the preparation of snow melting agents.

[0032] Example 2, reference Figure 1 Different from the above embodiment, this embodiment further discloses a method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium. The method is used to prepare a sodium-potassium alloy, comprising the following steps: In the first step, 100kg of high-calcium sodium is crushed in an inert atmosphere using a twin-helix belt crusher. The crusher's blades are made of highly wear-resistant stainless steel alloy, with staggered spiral cutters or toothed rollers. During operation, the two spiral shafts rotate relative to each other. Once the high-calcium sodium enters the crushing chamber, it is broken down into particles ranging from 10 to 50mm by the shear and tearing forces of the spiral belt cutters.

[0033] In the second step, 150 kg of potassium chloride solid and 100 kg of calcium chloride solid were placed in a vibrating fluidized bed for high-temperature dehydration under the conditions of 150°C inlet air temperature, 0.5 m / s wind speed, 1 mm amplitude, and 30 min residence time, so that the moisture content was no more than 0.1%.

[0034] In the third step, the high-calcium sodium particles and dry potassium chloride and calcium chloride solids are placed in a high-temperature vacuum furnace at 600-800°C through pipelines and a feeding device for a replacement reaction. Under the protection of argon, a metallic sodium-potassium alloy and calcium chloride and sodium chloride are gradually formed.

[0035] In the fourth step, the replacement reaction ends when the temperature stabilizes and no longer rises significantly or decreases slightly, and the sodium vapor volume detected by the detector remains constant for two hours. After the replacement reaction is complete, the resulting metallic sodium-potassium alloy is distilled under a low vacuum of 0.1-1 Pa into an alloy storage tank, yielding approximately 137.5 kg of a 99.9% sodium-potassium alloy, of which approximately 58.9 kg (42.8%) contains sodium, and approximately 78.6 kg (57.2%) contains potassium. The resulting sodium-potassium alloy has a melting point of approximately 19°C and a density of 0.89.

[0036] In the fifth step, after the reaction is completed, the by-products remaining in the high-temperature vacuum furnace are cooled and taken out through the liftable furnace and rotating arm, obtaining a white solid mixture of approximately 197.1 kg of calcium chloride and 58.5 kg of sodium chloride, which also contains a small amount of impurities such as a very small amount of calcium oxide. This can be used to prepare snow-melting agents later.

[0037] Example 3, reference Figure 1 Different from the above embodiment, this embodiment further discloses a method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium. The method is used to prepare metallic potassium, comprising the following steps: In the first step, add 100kg of sodium calcium sulfate and 300kg of 2-methylnaphthalene to a stirred tank, slowly heat to above 150°C, and gradually stir from slow to fast at a speed of 10-300rpm. After the sodium calcium sulfate is completely dissociated, vacuum filter to obtain the crushed sodium calcium sulfate. In the second step, 350 kg of potassium chloride solid and 150 kg of calcium chloride solid are subjected to microwave infrared drying with a microwave power of 18 kW, a frequency of 2450 MHZ, an operating temperature of 120°C, a material layer thickness of 10 mm, a conveying speed of 1 m / min, an exhaust volume of 2000 m3 / h, a 3-10 μm far infrared band, and a processing time of 6 hours, so that the moisture content is no more than 0.2%.

[0038] In the third step, the crushed high-calcium sodium and dried potassium chloride and calcium chloride solids are placed in a high-temperature vacuum furnace at 600-800°C through pipelines and a feeding device for a replacement reaction. Under the protection of argon, metallic potassium, calcium chloride, and sodium chloride are gradually formed.

[0039] In the fourth step, the replacement reaction ends when the temperature stabilizes and no longer rises significantly or decreases slightly, and the detector detects that the amount of sodium vapor no longer changes and continues to maintain for two hours. After the replacement reaction is completed, the formed metallic potassium is distilled into a potassium storage tank under a low vacuum of 0.1-1 Pa to obtain about 178.5 kg of potassium with a content of about 99.9%. The final potassium is die-cast into a silver-white cylindrical potassium ingot with a diameter of about 30 mm, a length of about 500 mm, and a weight of about 30 kg.

[0040] In the fifth step, after the reaction is completed, the by-products remaining in the high-temperature vacuum furnace are cooled and taken out through the liftable furnace and rotating arm to obtain a mixed white solid of approximately 247.1 kg of calcium chloride, 165.3 kg of sodium chloride and 9.1 kg of potassium chloride, which also contains a small amount of impurities such as a very small amount of calcium oxide. It can be used in the preparation of snow melting agent later.

[0041] Example 4, reference Figures 2 to 12The present embodiment discloses a drying and dehydrating device for preparing alkali metal materials from halogenated alkali metal salts and high calcium sodium. The drying and dehydrating device comprises a drying box 1 and a heating base 10. A square isolation box 6 is provided in the drying box 1, and the halogenated alkali metal salt is filled in a C shape in the drying box 1. The square isolation box 6 is equipped with a linkage component 2. The linkage component 2 comprises a vertical closed-loop conveyor belt 201. Temperature and humidity probes 4 and a flip plate 3 are respectively provided at the high and low positions on both sides of the conveyor belt 201. The overall outline of the flip plate 3 is consistent with the C-shaped layout of the drying box 1. A second opening 602 is provided at the lower position of the box 6, and the temperature and humidity probe 4 is communicated with the second opening 602 when it is at the lower end. In this structure, a lifting component 16 is also vertically provided in the square isolation box 6, and the output end of the lifting component 16 is connected to the flip plate 3. The lifting and lowering of the flip plate 3 is transmitted to the temperature and humidity probe 4 through the linkage component 2, and the lifting and lowering directions of the flip plate 3 and the temperature and humidity probe 4 are opposite; a wiping sponge can be built into the top of the square isolation box 6. After the temperature and humidity probe 4 is lifted up and hidden, it can be cleaned by wiping the sponge to improve the sensitivity and accuracy of subsequent detection.

[0042] The linkage assembly 2 further includes a baffle plate 202 and a side plate 207 arranged on both sides, both of which have a vertical guide groove 205 on the inner side. A lifting seat 7 is slidably provided on the vertical guide groove 205, and the lifting seat 7 is connected to the temperature and humidity probe 4.

[0043] A top cover 102 with a feed port 101 is provided on the top of the drying box 1, and a bulk cone head 103 is provided inside the feed port 101. In this structure, the halogenated alkali metal salt is pre-broken through the tip of the bulk cone head 103 to improve the subsequent drying quality.

[0044] The flip plate 3 includes a mounting seat 301 connected to the conveyor belt 201. The mounting seat 301 is provided with a folded bulk plate 302 downward through the horizontal plate 303. The folded bulk plate 302 is horizontally arranged to be necked and hollowed from the inside to the outside. A first opening 601 is provided on the side of the square isolation box 6 away from the second opening 602. The height of the first opening 601 is greater than the second opening 602. The second opening 602 is used for vertical sliding of the mounting seat 301, and a telescopic plate for sealing is provided between the mounting seat 301 and the second opening 602 to prevent material from being introduced from the gap of the second opening 602. A corresponding telescopic plate can also be arranged between the first opening 601 and the temperature and humidity probe 4, so that the conveyor belt 201 is completely built into the square isolation box 6, thereby improving the isolation effect.

[0045] The specific implementation process is as follows: the halogenated alkali metal salt is introduced from the feed port 101, and under the action of the bulk conical head 103, the halogenated alkali metal salt is initially broken up; when temperature and humidity detection is required, the lifting component 16 as the cylinder moves the flip plate 3 upward, and the upward movement of the flip plate 3 causes the halogenated alkali metal salt to flip; when the flip plate 3 moves upward, the conveyor belt 201 causes the temperature and humidity probe 4 to move downward, and after the first opening 601 coincides with the temperature and humidity probe 4, the temperature and humidity probe 4 is exposed to start the detection of drying results.

[0046] Example 5, with reference to Figure 4 Based on Example 4, this embodiment discloses a drying and dewatering device for preparing alkali metal materials from halogenated alkali metal salts and high calcium sodium, including a heat-conducting liquid tank 11 arranged on the side of a drying box 1, a liquid pipeline 12 is provided between the high and low positions of the heat-conducting liquid tank 11, the inlet and outlet of the liquid pipeline 12 are provided with an opening and closing valve 13, and a temperature sensor 14, a water pump 15 and a cooling unit 9 are connected in series to the liquid pipeline 12. In this structure, the cooling unit 9 is connected to the cooling tower 8. In the heat-insulating and drying state, the two opening and closing valves 13 are closed, and the heat-conducting liquid tank 11 provides a heat-insulating effect; when the drying box 1 needs to be quickly cooled after drying, the two opening and closing valves 13 are opened, and the liquid in the liquid pipeline 12 is extracted from the top, and after being cooled by the cooling unit 9, it returns to the drying box 1 from the bottom. The liquid with a higher temperature at the top is preferentially extracted from the heat-conducting liquid tank 11, which can improve the heat dissipation efficiency.

[0047] Example 6, reference Figures 8 to 12 Based on Example 4, this embodiment discloses a drying and dehydration device for preparing alkali metal materials from halogenated alkali metal salts and high calcium sodium. The linkage component 2 also includes a guide wheel 204 and a serrated shape 206 arranged on the vertical guide groove 205. Each guide wheel 204 supports the conveyor belt 201 as a square frame, and an elastic telescopic part 203 is vertically provided in the middle section of the conveyor belt 201. The elastic telescopic part 203 is preferably a spring.

[0048] The locking assembly 5 includes a gear 502 and a locking wheel 504 which are respectively rotatably arranged on the lifting base 7. The gear 502 is engaged with the serrated 206 on both sides. In this structure, the gear 502 is coaxially connected to the synchronization block 503. The synchronization block 503 is provided with a plurality of arc surfaces equidistantly along its circumference. The locking wheel 504 is coaxially connected to the handle 501. The locking wheel 504 can also be coaxially connected to the drive motor. A notch is provided on the locking wheel 504. The notch in the locking wheel 504 interacts with the arc surface of the synchronization block 503.

[0049] The specific implementation process is as follows: the flip plate 3 needs to be flipped up and down multiple times during drying, and the number of detections by the temperature and humidity probe 4 is less than the flipping frequency of the flip plate 3; when the flip plate 3 is flipped in the early stage, the temperature and humidity probe 4 needs to be locked; the locking wheel 504 is flipped so that the non-notch part on the locking wheel 504 is stuck in the arc surface on the synchronization block 503, and at this time the gear 502 is locked on the vertical guide groove 205; the lifting assembly 16 drives the flip plate 3 to move up and down to complete the vertical stirring of the halogenated alkali metal salt, and the elastic telescopic part 203 is deformed to adapt to the position locking of the gear 502.

[0050] Comparative Example 1: Referring to CN103757435A, this comparative example relates to a method for purifying metallic sodium, wherein a solid raw material metallic sodium with a purity of 99.5% is placed in a distillation kettle body, fixed and sealed with bolts, assembled and placed on a heating furnace, and the solid sodium is heated by an infrared radiation lamp and a focusing tube. Then, under the conditions of temperature control at 240°C to 260°C, vacuum degree ≤10Pa, heating time of 2h, and two passes of high-purity argon gas carrying impurities in the middle, the solid sodium is melted into a liquid state, and the volatile impurities contained in the liquid metallic sodium are evaporated and separated from the liquid metallic sodium. The volatile impurities are extracted with a vacuum pump, and then the liquid sodium is heated in a heating furnace to a temperature of 400°C. Circulating cooling water is then introduced into the condenser, and radiation is added to assist distillation. The thermal radiation increases the liquid surface temperature and accelerates the evaporation rate of the sodium on the liquid surface. The sodium vapor is rapidly condensed into sodium solid when it encounters the condenser, thereby realizing the thermal radiation-assisted distillation purification of metallic sodium. In this case, the required raw material content is high, and the impurities are not processed thoroughly. Only low-boiling point impurities can be processed, and the remaining sodium slag cannot be completely processed.

[0051] Comparative Example 2: Referring to CN107574318A, this comparative example relates to a sodium slag purification and separation method and a purification device used therein. The method comprises configuring a molten salt in a molten salt melting furnace, which is a mixed molten salt of sodium chloride, potassium chloride, and calcium chloride, and heating the mixture to 600°C to melt the mixture. Sodium slag having a sodium content of 65wt% and a calcium content of 24wt% is slowly added to the sodium slag melting tank in batches. After the sodium slag temperature rises to the melting point, the sodium slag flows into the molten salt melting furnace through a descending pipe. After being buffered, the sodium slag enters the molten salt melt. Through the separation effect of the molten salt melt, the separated sodium floats to the upper liquid surface of the molten salt melt and is collected into a sodium collection device through a sodium recovery pipe. This example uses a mixed molten salt as a solvent to heat the sodium slag, but in essence, it still does not solve the problem of calcium recovery in the sodium slag.

[0052] Comparative Example 3: Referring to CN108624913A, this comparative example relates to a process for purifying industrial sodium by melting electrolysis to obtain high-purity sodium, wherein a small refined sodium tank is filled with sodium seed, and when the argon pressure in the electrolytic cell is 0.1 kPa, the small refined sodium tank is connected to the cathode tube; the electrolytic cell is heated to 180°C, and the ceramic diaphragm tube is preheated by heat preservation, and then the small refined sodium tank and the cathode tube are heated and kept at 180°C, and all the sodium seed is injected into the ceramic diaphragm tube; the industrial sodium tank, the industrial sodium transition tank and the electrolytic cell are heated to 180°C, kept warm, and argon is introduced, and then the industrial sodium tank is heated to 180°C, the industrial sodium transition tank and the electrolytic cell are heated, the argon gas ... industrial sodium tank is heated, the industrial sodium transition tank and the electrolytic cell are heated, the industrial sodium tank is heated, the industrial sodium transition tank and the Sodium is injected into the industrial sodium transition tank and then into the electrolytic cell; when the industrial sodium in the electrolytic cell reaches a specified amount, the injection is stopped; when the industrial sodium transition tank is full of industrial sodium, the injection is stopped, and finally the industrial sodium transition tank is heated to 260° C. and kept warm; after a period of insulation, the electrolysis current is set at 10A and electrolysis is started, and the current is increased after a period of electrolysis; when the refined sodium output in the ceramic diaphragm tube reaches a specified amount, the electrolysis is stopped, and the refined sodium in the ceramic diaphragm tube is pressed into the refined sodium tank through the refined sodium pipeline by utilizing the argon pressure difference between the electrolytic cell and the refined sodium tank; When the sodium is discharged, electrolysis is restarted; after multiple sodium discharges, the industrial sodium in the industrial sodium transition tank is injected into the electrolytic cell to replenish the industrial sodium, and then the industrial sodium in the industrial sodium tank is injected into the industrial sodium transition tank, and the injection is stopped after it is full; when the refined sodium in the refined sodium tank reaches the specified amount, the refined sodium in the refined sodium tank is discharged into a refined sodium storage tank that has been evacuated and heated to 110°C. The equipment used in this method is complex, the cost is high, and it cannot solve the problem of recycling sodium slag calcium.

[0053] Many other changes and modifications can be made without departing from the spirit and scope of the present invention. It should be understood that the present invention is not limited to the specific embodiments, and the scope of the present invention is defined by the appended claims.

Claims

1. A method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium, characterized in that: The following steps are involved: S100, drying and removing water from the halogenated alkali metal salt by a drying and water removal device; S200, crushing or dissociating high calcium sodium through sodium slag crushing equipment; S300, introducing the alkali metal halide in step S100 and the high calcium sodium in step S200 into a high-temperature vacuum furnace, and performing a replacement reaction under the protection of an inert gas; The reaction principle of the replacement reaction in step S400 and step S300 is: Na+Ca+MX→NaX+CaX2+M Ca + Na2O → CaO + Na Wherein, M refers to one or more of lithium, sodium, potassium, rubidium, and cesium, and X refers to halogen, which is one or both of chlorine and fluorine; S500, introducing the alkali metal material as the displacement reaction product into a storage tank by distillation for storage.

2. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 1, characterized in that: The halogenated alkali metal salt is one or more fluorinated or chlorinated alkali metal salts.

3. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 2, characterized in that: The alkali metal material is one or more of an alkali metal element or an alkali metal alloy; The alkali metal is one or more of lithium, sodium, potassium, rubidium, and cesium; The alkali metal alloy is an alkali metal alloy composed of a mixture of one or more alkali metals selected from lithium, potassium, rubidium, and cesium and sodium in an appropriate proportion.

4. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 1, characterized in that: The usage ratio of the halogenated alkali metal salt to the high calcium sodium is 0.5-10:

1.

5. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 1, characterized in that: In step S100, calcium chloride is further added to the drying and dehydration equipment to form a mixed salt with the halogenated alkali metal salt as a reaction substrate to reduce the melting point of the required mixture.

6. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 1, characterized in that: In step S200, the high calcium sodium is crushed and dissociated under an inert gas environment.

7. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 6, characterized in that: The inert gas in step S200 is nitrogen or argon, and the inert gas in step S300 is argon.

8. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 1, characterized in that: In step S300 , the temperature of the replacement reaction is 600-900° C., the holding time is 3-12 hours, and the pressure in the furnace is 0.05-0.5 MPa.

9. The method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium according to claim 1, characterized in that: In step S600, by-products are separated by vacuum distillation or hot filtration, and the by-products are a mixture of calcium chloride and sodium chloride composite salts used for preparing deicing agents.

10. A method for preparing an alkali metal material from a halogenated alkali metal salt and high calcium sodium, characterized in that: The invention comprises a drying and dehydrating device used in step S100, the drying and dehydrating device comprising a drying box (1) and a heating base (10), a square isolation box (6) being provided in the drying box (1), and a halogenated alkali metal salt being filled in a C-shape in the drying box (1); The square isolation box (6) is equipped with a linkage assembly (2), the linkage assembly (2) comprising a vertical closed-loop conveyor belt (201), a temperature and humidity probe (4) and a flip plate (3) respectively provided at the high and low positions on both sides of the conveyor belt (201), the overall profile of the flip plate (3) being consistent with the C-shaped layout of the drying box (1), a second opening (602) is provided at the low position of the square isolation box (6), and the temperature and humidity probe (4) is in communication with the second opening (602) when at the low end; A lifting assembly (16) is also vertically provided in the square isolation box (6). The output end of the lifting assembly (16) is connected to the flip plate (3). The lifting and lowering of the flip plate (3) is transmitted to the temperature and humidity probe (4) through the linkage assembly (2), and the lifting and lowering directions of the flip plate (3) and the temperature and humidity probe (4) are opposite.

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