Metallic gallium extraction device and extraction method thereof

By designing an extraction device that links the mixing rod and the cleaning plate, the problems of inconvenience in water phase treatment and pipeline blockage during the gallium metal extraction process are solved, and the stability and efficiency of the extraction effect are improved.

CN120350253AActive Publication Date: 2025-07-22JIANGXI JIULING LITHIUM CO LTD

Patent Information

Application Number
CN202510584562.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-07
Publication Date
2025-07-22
Estimated Expiration
2045-05-07

AI Technical Summary

Technical Problem

In the prior art, the treatment of the aqueous phase during the gallium metal extraction process is inconvenient, which can easily affect the subsequent extraction effect and can easily block the pipeline.

Method used

A metal gallium extraction device is designed, including an extraction tank, base and extraction mechanism. The coordinated rotation of the stirring rod and cleaning plate is used to ensure that the water phase is evenly stirred and the clarification is cleaned simultaneously to avoid clogging.

Benefits of technology

Effectively clean the clear content inside the extraction tank to ensure the subsequent extraction effect and stability, avoid water washing operations caused by blockage, and improve the extraction efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a metal gallium extraction device and an extraction method thereof. The gallium extraction device comprises an extraction tank, a base and an extraction mechanism, a top plate is hermetically mounted at the top of the extraction tank through bolts, a mounting cover is mounted at the top of the top plate through bolts, a feeding pipe is mounted on the inner wall of the mounting cover, a recycling pipe is mounted at the bottom end of the extraction tank, a suction pipe is fixedly arranged on the side wall of the extraction tank, and the extraction mechanism comprises a mounting plate fixedly arranged on the inner wall of the extraction tank; according to the scheme, the cleaning plate designed in a special shape is used for controlling the screw rod to rotate in a linkage manner, so that water-phase clarified matters are synchronously treated in the process of discharging a water phase, the interior of the extraction tank can be well and finely cleaned, and meanwhile, the clarified matters are centrally treated, so that the blockage of a recovery pipe can be avoided; therefore, the top plate does not need to be opened for washing, clarified impurities in the extraction tank can be effectively reduced, and the subsequent extraction effect and the extraction stability are ensured.
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Description

Technical Field

[0001] The present invention relates to the technical field of gallium extraction, and particularly to a metal gallium extraction device and an extraction method thereof. Background Art

[0002] Gallium is an important rare and dispersed metal, which is widely used in the fields of semiconductors, optoelectronic materials, and new energy. Gallium usually exists in an associated form in bauxite, zinc ore, and lithium-containing silicate minerals (such as lepidolite and spodumene). Traditional gallium extraction methods mainly rely on the bayer process of bauxite or by-products of zinc smelting, but these methods have low extraction efficiency for gallium in lithium-containing silicate minerals. Therefore, it is of great significance to develop an efficient and environmentally friendly technology for extracting gallium from lithium-containing silicate minerals, and the solvent extraction method is the most applicable.

[0003] Bauxite, zinc ore, and lithium-containing silicate minerals (such as lepidolite and spodumene) all contain gallium metal. Secondly, some waste electronic waste, such as semiconductors, optoelectronic materials, and new energy devices, also contain gallium metal elements. The solvent extraction method can extract all materials containing gallium metal, and the compatibility of raw materials is stronger. Whether it is various types of waste ores or electronic waste, gallium metal can be recovered from them by solvent extraction.

[0004] However, in the prior art, during the extraction process of gallium metal, a clarification section will form for static stratification. The gallium-rich organic phase enters the stripping process, and the aqueous phase (raffinate) is returned to leaching or discarded. The organic phase will be on the upper side, and the aqueous phase will be on the lower side. The aqueous phase will contain extraction impurities. When the organic phase enters the stripping stage, the impurities in the aqueous phase will still exist in the extraction tank, which is likely to affect subsequent extraction use and is also likely to block the pipeline.

[0005] Therefore, it is necessary to provide a metal gallium extraction device and an extraction method thereof to solve the above technical problems. Summary of the Invention

[0006] The present invention provides a metal gallium extraction device and an extraction method thereof, which solve the technical problems in the related art that it is inconvenient to treat the aqueous phase, which is likely to affect subsequent extraction and is also likely to block the pipeline.

[0007] To solve the above technical problems, a metal gallium extraction device provided by the present invention includes an extraction tank, a base, and an extraction mechanism;

[0008] The top of the extraction tank is hermetically installed with a top plate by bolts. The top of the top plate is installed with a mounting cover by bolts. The inner wall of the mounting cover is installed with a feed pipe. The bottom end of the extraction tank is installed with a recovery pipe. The side wall of the extraction tank is fixedly provided with a suction pipe;

[0009] The extraction mechanism includes a mounting plate fixedly arranged on the inner wall of the extraction tank. An extraction motor is installed on the upper surface of the top plate and inside the mounting cover by bolts. The output shaft of the extraction motor is keyed to a key rod. The bottom end of the key rod is integrally provided with a stirring rod. The middle position inside the mounting plate is rotatably connected with a turntable. A connecting rod is fixedly arranged on the side wall of the turntable. The bottom end of the connecting rod is fixedly provided with a cleaning plate. A ratchet wheel is keyed to the outer wall of the key rod and inside the turntable. On both sides of the ratchet wheel inside the turntable, ratchet teeth are rotatably installed through torsion springs.

[0010] A positioning plate is installed inside the cleaning plate by bolts. A screw rod is installed inside the recovery pipe and on one side of the positioning plate by bolts.

[0011] Preferably, the outlet end of the feed pipe penetrates inside the mounting cover and extends into the top plate. The periphery of the extraction tank is installed on the base by bolts.

[0012] Preferably, the ratchet wheel and the ratchet teeth are meshed with each other. The outer wall of the screw rod fits with the inner wall of the recovery pipe.

[0013] Preferably, the long end outer wall of the cleaning plate contacts the inner wall of the extraction tank. The cleaning plate is designed with a shape that is higher on the outside and gradually lower towards the inside.

[0014] Preferably, it further includes a high-temperature furnace, and a blanking mechanism and a protection mechanism are installed outside the high-temperature furnace;

[0015] The blanking mechanism includes a blanking cylinder fixedly arranged on the inner wall of the high-temperature furnace. A blanking motor is installed on the outer wall of the high-temperature furnace by bolts. A spiral rod is keyed to the inside of the blanking motor and inside the blanking cylinder. A half gear is keyed to the outer wall of the output shaft of the blanking motor and on one side of the blanking cylinder. A rack reciprocating ring is meshed and installed on the outer wall of the half gear. A blanking frame is installed through the top of the blanking cylinder in a sealed manner.

[0016] The protection mechanism includes a mounting frame installed on the side wall of the high-temperature furnace and on one side of the blanking motor. A sliding rod is fixedly arranged on the side wall of the rack reciprocating ring, and the number of sliding rods is two. A sleeve is installed inside the mounting frame, and the number of sleeves is two. A piston plate is slidably connected inside each of the two sleeves. A first one-way valve and a second one-way valve are installed on one side of the piston plate inside each of the two sleeves. An intake pipe is installed at the inlet end of the first one-way valve.

[0017] Preferably, one end of the spiral rod is rotatably connected to the axis of the blanking cylinder through a bearing. The axes of the two sliding rods are fixedly connected to the axes of the two piston plates;

[0018] The air outlet ends of two of the second one-way valves are both hermetically installed with a high-temperature furnace and an extraction tank through hoses.

[0019] Preferably, it further includes an exhaust mechanism. A linkage disk is connected to the outer wall of the key rod through a keyway above the mounting plate, and a convex block is fixedly arranged on the top of the linkage disk.

[0020] The exhaust mechanism includes an exhaust pipe fixedly arranged inside the top plate and the mounting cover. A limiting plate is fixedly arranged at the middle position of the exhaust pipe. A lifting rod is slidably connected to the axis of the limiting plate. Through holes are arranged in the limiting plate in an equidistant annular distribution. A guide wheel is installed at the bottom end of the lifting rod, and a blocking plate is fixedly arranged at the top end of the lifting rod.

[0021] Preferably, the bottom of the guide wheel is in contact with the upper surface of the linkage disk, and the blocking plate is designed in a tapered shape with a wider upper part and a narrower lower part.

[0022] A method for extracting gallium from metal, comprising the following steps:

[0023] S1: Material pretreatment;

[0024] Crush and grind lithium-containing silicate minerals (such as lepidolite and spodumene), not limited to minerals, all materials containing gallium elements can be used (such as waste electronic devices or recycled products containing gallium elements) to 200 mesh and above 50% to improve the reaction activity.

[0025] S2: High-temperature roasting;

[0026] Mix the ground material with sulfates (such as sodium sulfate and potassium sulfate) evenly according to a mass ratio of 1:1 - 1:3.

[0027] Place the mixture in a high-temperature furnace 2 and heat it at 600 - 900 °C for 1 - 3 hours. At high temperature, the sulfate decomposes to generate SO3, which reacts with gallium in the mineral to generate gallium sulfate (Ga2(SO4)3):

[0028] Ga2O3 + 3SO3 → Ga2(SO4)3;

[0029] S3: Water immersion and concentration;

[0030] Cool the product after the high-temperature reaction to room temperature, add water for leaching. Gallium sulfate is easily soluble in water and enters the solution. After the solution is evaporated and concentrated multiple times, other insoluble impurities (such as SiO2) remain in the residue. Filter and separate the leaching solution and the residue to obtain a gallium-containing solution.

[0031] S4: Solvent extraction, and the extraction process is all carried out in an extraction tank.

[0032] Selectively extract gallium from gallium-containing solution using organic extractants (such as Kelex 100, LIX series); the extraction conditions are as follows:

[0033] pH value: 2–3

[0034] Concentration of extractant: 5–10%

[0035] Phase ratio (organic phase: aqueous phase) is 1:1–1:3

[0036] Strip the gallium-loaded organic phase with an acidic solution (such as 1–2 mol / L HCl) to obtain a high-concentration gallium-containing solution;

[0037] Mixing section: The leachate is mixed with the organic phase (extractant + diluent) at a volume ratio of 1:3 to 1:5 for 5–10 minutes;

[0038] Clarification section: Let it stand for layering. The gallium-rich organic phase enters the stripping process, the aqueous phase (raffinate) is returned to leaching or discarded, the organic phase is sucked in through the suction pipe and enters the stripping process, and the aqueous phase is discharged from the recovery pipe;

[0039] S5: Recovery of gallium;

[0040] Electrolyze or chemically reduce the high-concentration gallium-containing solution to obtain metallic gallium;

[0041] Electrolysis conditions: Current density 200–500 A / m 2 , voltage 3–5 V, temperature 25–50 °C.

[0042] Compared with the related technologies, the metallic gallium extraction device and its extraction method provided by the present invention have the following

[0043] Beneficial effects:

[0044] The stirring rod agitates the aqueous phase to first ensure the uniformity of the aqueous phase and avoid uneven distribution of the lower and upper layers of the aqueous phase. At the same time, the cleaning plate will also rotate at the bottom of the extraction tank following the rotation of the stirring rod. One side of the cleaning plate structure is a vertical surface, and the other side is an inclined surface. During the counterclockwise rotation, the inclined surface end of the cleaning plate will scrape the aqueous phase clarifying substances at the bottom of the extraction tank onto the inclined surface. Secondly, the outside of the cleaning plate is high, so the clarifying substances remaining on the inclined surface of the cleaning plate will flow from high to low towards the position of the recovery pipe. When the aqueous phase clarifying substances are concentrated at the port of the recovery pipe, the counterclockwise rotating screw forms a spiral conveyor to quickly clean the clarifying substances;

[0045] The cleaning plate with a special shape design drives the control screw to rotate. While ensuring that the aqueous phase can be discharged, the aqueous phase clarifier is processed synchronously, which can clean the inside of the extraction tank in detail. At the same time, the clarifier is centrally processed, which can avoid the blockage of the recovery pipe. In this way, when the extraction tank is used for subsequent extraction, it is not necessary to open the top plate for water washing, which can effectively reduce the clarified impurities in the extraction tank and ensure the subsequent extraction effect and the stability of extraction. BRIEF DESCRIPTION OF THE DRAWINGS

[0046] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on the structures shown in these drawings.

[0047] Figure 1 The best structural schematic diagram provided by the present invention;

[0048] Figure 2 is Figure 1 The external structural schematic diagram of the extraction tank shown;

[0049] Figure 3 is Figure 2 The sectional structural schematic diagram of the installation cover shown;

[0050] Figure 4 is Figure 3 The internal sectional structural schematic diagram of the extraction tank shown;

[0051] Figure 5 is Figure 4 The structural schematic diagram of the extraction mechanism shown;

[0052] Figure 6 is Figure 5 The connection structural schematic diagram of the cleaning plate and the recovery pipe shown;

[0053] Figure 7 is Figure 6 The enlarged structural schematic diagram at A shown;

[0054] Figure 8 is Figure 5 The split structural schematic diagram of the ratchet and the turntable shown;

[0055] Figure 9 is Figure 1 The structural schematic diagram of the blanking mechanism and the protection mechanism shown;

[0056] Figure 10 is Figure 9 The enlarged structural schematic diagram at B shown;

[0057] Figure 11 is Figure 4 a schematic diagram of the internal structure of the exhaust mechanism shown

[0058] Figure 12 is a schematic diagram of the working process of the exhaust mechanism, where (a) is a schematic diagram of the exhaust mechanism in the blocked state, and (b) is a schematic diagram of the exhaust state of the exhaust mechanism controlled by the cam contacting the guide wheel

[0059] Explanation of the reference numerals in the drawings

[0060] 1. Extraction tank

[0061] 2. High-temperature furnace, 3. Recovery pipe, 4. Suction pipe, 5. Base

[0062] 6. Extraction mechanism, 61. Extraction motor, 62. Mounting plate, 63. Key rod, 64. Turntable, 65. Connecting rod, 66. Cleaning plate, 67. Stirring rod, 68. Positioning plate, 69. Screw, 610. Ratchet, 611. Ratchet teeth

[0063] 7. Feeding mechanism, 71. Feeding cylinder, 72. Feeding motor, 73. Half gear, 74. Screw rod, 75. Rack reciprocating ring, 76. Feeding frame

[0064] 8. Protection mechanism, 81. Mounting frame, 82. Slide bar, 83. Sleeve, 84. First one-way valve, 85. Second one-way valve, 86. Inlet pipe, 87. Piston plate

[0065] 9. Exhaust mechanism, 91. Exhaust pipe, 92. Limiting plate, 93. Through hole, 94. Lifting rod, 95. Sealing plate, 96. Guide wheel

[0066] 10. Top plate, 11. Mounting cover, 12. Feed pipe

[0067] 13. Linkage disk, 14. Protrusion Specific implementation manners

[0068] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention

[0069] The present invention provides a metal gallium extraction device and its extraction method

[0070] First embodiment

[0071] A metal gallium extraction method includes the following steps

[0072] S1: Material pretreatment;

[0073] Crush and grind lithium-containing silicate minerals (such as lepidolite and spodumene), not limited to minerals, and all materials containing gallium elements (such as waste electronic devices or recycled products containing gallium elements) to more than 50% passing 200 mesh to improve the reaction activity;

[0074] S2: High-temperature roasting;

[0075] Mix the ground material with sulfates (such as sodium sulfate and potassium sulfate) evenly at a mass ratio of 1:1 - 1:3;

[0076] Place the mixture in high-temperature furnace 2 and heat it at 600 - 900 °C for 1 - 3 hours. At high temperature, the sulfate decomposes to generate SO3, which reacts with gallium in the mineral to form gallium sulfate (Ga2(SO4)3):

[0077] Ga2O3 + 3SO3 → Ga2(SO4)3;

[0078] S3: Water leaching and concentration;

[0079] Cool the product after high-temperature reaction to room temperature, add water for leaching. Gallium sulfate is easily soluble in water and enters the solution. After the solution is evaporated and concentrated multiple times, other insoluble impurities (such as SiO2) remain in the residue. Filter to separate the leaching solution and the residue to obtain a gallium-containing solution;

[0080] S4: Solvent extraction, and the extraction process is all carried out in extraction tank 1;

[0081] Use an organic extractant (such as Kelex100, LIX series) to selectively extract gallium from the gallium-containing solution; the extraction conditions are as follows:

[0082] pH value: 2 - 3

[0083] Extractant concentration: 5 - 10%

[0084] Phase ratio (organic phase: aqueous phase) is 1:1 - 1:3

[0085] Strip the gallium-loaded organic phase with an acidic solution (such as 1 - 2 mol / L HCl) to obtain a high-concentration gallium-containing solution;

[0086] Mixing section: Mix the leaching solution and the organic phase (extractant + diluent) at a volume ratio of 1:3 - 1:5 for 5 - 10 minutes;

[0087] Clarification section: Let it stand for layering. The gallium-rich organic phase enters the stripping process, the aqueous phase (raffinate) is returned to leaching or discarded, the organic phase is sucked in through the suction pipe to enter the stripping process, and the aqueous phase is discharged from the recovery pipe;

[0088] S5: Recovery of gallium;

[0089] Electrolyze or chemically reduce the high-concentration gallium-containing solution to obtain metallic gallium;

[0090] Electrolysis conditions: current density 200–500 A / m 2 , voltage 3–5 V, temperature 25–50 °C.

[0091] In this embodiment: By mixing the lithium-containing silicate mineral with sulfates (such as sodium sulfate, potassium sulfate) and heating, gallium is converted into water-soluble gallium sulfate (Ga2(SO4)3), and then gallium is efficiently extracted from the solution by solvent extraction. This method has the characteristics of simple process, high gallium recovery rate, environmental friendliness, etc., and is suitable for comprehensively recovering gallium resources from lithium-containing silicate minerals such as lepidolite and spodumene;

[0092] On the one hand, gallium resources can be recovered from a variety of ores without the need to classify the ores for treatment. Secondly, some small waste ores can also be directly crushed without classification, which is conducive to the integrated utilization of resources;

[0093] On the other hand, for recycling materials such as semiconductors, optoelectronic materials and new energy devices, this method can also be used. Through solvent extraction, the internal gallium metal materials can be recycled. Therefore, this method has a wide range of applicability and is conducive to resource integration and material recycling.

[0094] Second embodiment:

[0095] Please refer to Figures 1 to 8 , a metal gallium extraction device, including an extraction tank 1, a base 5 and an extraction mechanism 6;

[0096] The top of the extraction tank 1 is sealed and installed with a top plate 10 by bolts. The top of the top plate 10 is installed with a mounting cover 11 by bolts. The inner wall of the mounting cover 11 is installed with a feed pipe 12. The bottom end of the extraction tank 1 is installed with a recovery pipe 3. A suction pipe 4 is fixedly arranged on the side wall of the extraction tank 1;

[0097] The extraction mechanism 6 includes a mounting plate 62 fixedly arranged on the inner wall of the extraction tank 1. An extraction motor 61 is installed on the upper surface of the top plate 10 and inside the mounting cover 11 by bolts. The output shaft of the extraction motor 61 is keyed to a key rod 63. The bottom end of the key rod 63 is integrally provided with a stirring rod 67. The middle position inside the mounting plate 62 is rotatably connected with a turntable 64. A connecting rod 65 is fixedly arranged on the side wall of the turntable 64. The bottom end of the connecting rod 65 is fixedly provided with a cleaning plate 66. A ratchet 610 is keyed on the outer wall of the key rod 63 and inside the turntable 64. On both sides of the ratchet 610 inside the turntable 64, ratchet teeth 611 are rotatably installed through torsion springs;

[0098] A positioning plate 68 is installed inside the cleaning plate 66 by means of bolts, and a screw rod 69 is installed inside the recovery pipe 3 and on one side of the positioning plate 68 by means of bolts.

[0099] See also Figure 1 and Figure 2 : In the working process of the first embodiment, S4: solvent extraction, the extraction process is all carried out in the extraction tank;

[0100] The gallium-containing solution enters the extraction tank 1 through the feed pipe 12. During extraction, the mounting cover 11 needs to be sealed with the top plate 10, and the top plate 10 needs to be sealed with the extraction tank 1.

[0101] See also Figure 5 and Figure 8 : The extraction motor 61 can be started to rotate forward and reversely. When the extraction motor 61 rotates clockwise, the output shaft of the extraction motor 61 drives the key rod 63 and the stirring rod 67 at the bottom to rotate clockwise. The rotation of the stirring rod 67 mixes and stirs the gallium-containing solution, organic extractant and other solvents in the extraction tank 1 to ensure sufficient extraction;

[0102] When the key rod 63 rotates clockwise, the ratchet 610 will also rotate clockwise. The clockwise rotating ratchet 610 will form a rotation avoidance with the ratchet teeth 611 on both sides, so the clockwise rotating ratchet 610 will not affect the ratchet teeth 611 and the rotating disk 64.

[0103] See also Figure 4 : After extraction, the extraction motor 61 needs to be stopped to ensure that the extraction tank 1 is stationary. The organic phase and the aqueous phase after extraction will form a clear layer in the extraction tank 1. The organic phase will be discharged through the suction pipe 4 to enter the stripping stage in the first embodiment, and the aqueous phase will be discharged through the recovery pipe 3 for waste liquid treatment and recycling;

[0104] See also Figure 4 , Figure 5 and Figure 8 : When all the organic phase is discharged, the user needs to start the extraction motor 61 to rotate counterclockwise. The extraction motor 61 can control the key rod 63 to make the ratchet 610 rotate counterclockwise. The counterclockwise rotating ratchet 610 will affect the ratchet teeth 611 on both sides, thereby controlling the entire turntable 64 to drive the connecting rod 65 to realize the counterclockwise rotation of the cleaning plate 66 at the bottom of the extraction tank 1. At the same time, the stirring rod 67 will also rotate during the rotation of the ratchet 610;

[0105] See also Figure 6 and Figure 7 When the cleaning plate 66 rotates counterclockwise, the cleaning plate 66 will also synchronously drive the positioning plate 68 to control the screw 69 to rotate counterclockwise in the recovery pipe 3.

[0106] Working principle of this embodiment: When all the gallium-containing solution enters the extraction tank 1, first start the extraction motor 61 to rotate clockwise. The output shaft of the extraction motor 61 drives the key rod 63 and the stirring rod 67 at the bottom to rotate clockwise. The rotation of the stirring rod 67 stirs the solvents such as the gallium-containing solution and the organic extractant in the extraction tank 1 to ensure sufficient extraction.

[0107] After extraction, a clear layer separation is formed. First, the organic phase is discharged through the suction pipe 4 and enters the stripping stage.

[0108] Then start the extraction motor 61 to rotate counterclockwise. At this time, the cleaning plate 66, the stirring rod 67 and the screw 69 will all rotate counterclockwise. The stirring rod 67 agitates the water phase water body environment, and then the recovery pipe 3 extracts the water phase in the extraction tank 1.

[0109] The outlet end of the feed pipe 12 penetrates through the inside of the mounting cover 11 and extends into the inside of the top plate 10. The periphery of the extraction tank 1 is installed on the base 5 through bolts.

[0110] The ratchet 610 and the ratchet teeth 611 are meshed with each other. The outer wall of the screw 69 is in mutual fit with the inner wall of the recovery pipe 3.

[0111] The outer long end wall of the cleaning plate 66 is in contact with the inner wall of the extraction tank 1. The cleaning plate 66 is designed with a shape that is high on the outside and gradually becomes lower towards the inside.

[0112] In this embodiment: When in the extraction stage, the clockwise rotation of the extraction motor 61 can only affect the rotation of the stirring rod 67 for sufficient extraction. When the extraction is completed and a clear layer separation is formed, the organic phase can be discharged for stripping first. Then, when the extraction motor 61 is started to rotate counterclockwise, it can drive the linkage rotation of the stirring rod 67, the cleaning plate 66 and the screw 69.

[0113] The stirring rod 67 agitates the water phase to first ensure the uniformity of the water phase and avoid uneven distribution of the lower and upper layers of the water phase. At the same time, the cleaning plate 66 will also rotate at the bottom of the extraction tank 1 following the rotation of the stirring rod 67. One side of the structure of the cleaning plate 66 is a vertical surface and the other side is an inclined surface. During the counterclockwise rotation, the inclined surface end of the cleaning plate 66 will scrape the water phase clarifying substances at the bottom of the extraction tank 1 onto the inclined surface. Secondly, the outside of the cleaning plate 66 is high. Therefore, the clarifying substances remaining on the inclined surface of the cleaning plate 66 will flow from high to low towards the position of the recovery pipe 3. When the water phase clarifying substances are concentrated at the port of the recovery pipe 3, the counterclockwise rotating screw 69 forms a spiral conveyor to quickly clean the clarifying substances.

[0114] The rotation of the control screw 69 is linked by the cleaning plate 66 with a special shape design. While ensuring that the aqueous phase can be discharged, the aqueous phase clarifier is processed synchronously, which can clean the inside of the extraction tank 1 in detail. At the same time, the clarifier is centrally processed, which can prevent the recovery pipe 3 from being blocked. In this way, when the extraction tank 1 is used for subsequent extraction, it is not necessary to open the top plate 10 for water washing, which can effectively reduce the clarified impurities in the extraction tank 1 and ensure the subsequent extraction effect and the stability of extraction.

[0115] Third Embodiment:

[0116] Please refer to Figure 1 、 Figure 9 and Figure 10 and, it further includes a high-temperature furnace 2, and the outside of the high-temperature furnace 2 is installed on a feeding mechanism 7 and a protection mechanism 8;

[0117] The feeding mechanism 7 includes a feeding cylinder 71 fixed on the inner wall of the high-temperature furnace 2. A feeding motor 72 is installed on the outer wall of the high-temperature furnace 2 through bolts. A screw rod 74 is key-connected inside the feeding motor 72 and located inside the feeding cylinder 71. A semi-gear 73 is key-connected to the outer wall of the output shaft of the feeding motor 72 and located on one side of the feeding cylinder 71. A rack reciprocating ring 75 is meshed and installed on the outer wall of the semi-gear 73. A feeding frame 76 is installed through the top of the feeding cylinder 71 in a sealed manner;

[0118] The protection mechanism 8 includes a mounting frame 81 installed on the side wall of the high-temperature furnace 2 and located on one side of the feeding motor 72. A sliding rod 82 is fixed on the side wall of the rack reciprocating ring 75, and the number of the sliding rods 82 is two. A sleeve 83 is installed inside the mounting frame 81, and the number of the sleeves 83 is two. A piston plate 87 is slidably connected inside each of the two sleeves 83. A first one-way valve 84 and a second one-way valve 85 are installed inside each of the two sleeves 83 and located on one side of the piston plate 87. An air inlet pipe 86 is installed at the inlet end of the first one-way valve 84.

[0119] Please refer to Figure 1 and Figure 9 : During the working process of the first embodiment, in the S1 and S2 stages, the pulverized powder needs to be put into the feeding cylinder 71 from the feeding frame 76, and then the user starts the feeding motor 72 to control the screw rod 74 to rotate inside the feeding cylinder 71, and the powder is put into the high-temperature furnace 2 for roasting by means of screw conveying;

[0120] It can be understood that: the feeding frame 76 can be externally provided with a pipeline for fully sealed powder conveying.

[0121] Please refer to Figure 9 and Figure 10: When the unloading motor 72 drives the screw rod 74 to rotate and unload, the half gear 73 on the output shaft of the unloading motor 72 will continue to rotate, and the continuous rotation of the half gear 73 can mesh with the control rack reciprocating ring 75 to perform horizontal reciprocating motion along the rotation trajectory of the half gear 73;

[0122] The reciprocating motion of the rack reciprocating ring 75 can synchronously drive the two slide rods 82 to reciprocate, and the slide rod 82 is fixedly connected to the piston plate 87. When the piston plate 87 retreats, the gas will be drawn into the sleeve 83 through the first one-way valve 84 and the air intake pipe 86. When the piston plate 87 is pushed, the gas in the sleeve 83 can be pushed out from the second one-way valve 85.

[0123] One end of the spiral rod 74 is rotatably connected to the axis of the lower barrel 71 through a bearing, and the axis of the two slide rods 82 is fixedly connected to the axis of the two piston plates 87;

[0124] The gas outlet ends of the two second one-way valves 85 are sealed and installed with the high-temperature furnace 2 and the extraction tank 1 through hoses.

[0125] See also Figure 1 and Figure 9 : The hoses installed outside the two second one-way valves 85 are installed with the high-temperature furnace 2 and the extraction tank 1 respectively. The first one-way valve 84 only allows one-way transportation from the outside to the inside, and the second one-way valve 85 only allows one-way transportation from the inside to the outside. Therefore, when the piston plate 87 retreats, suction is formed, and when the piston plate 87 moves forward, thrust is formed.

[0126] In this embodiment, the powder is transported in a fully sealed environment by using a rotating screw rod 74, ensuring that the powder can be stably transported inside the high-temperature furnace 2. Secondly, when the screw rod 74 is rotating and transporting, it can be linked to control the rack reciprocating ring 75 to synchronously drive the slide bar 82 to control the piston plate 87 to form a reciprocating push-pull stroke in the sleeve 83, thereby assisting the air intake and exhaust. Secondly, the high-temperature furnace 2 and the extraction tank 1 are sealed and installed through two sealing tubes. The sealing tube connecting the high-temperature furnace 2 and the air intake pipe 86 can be equipped with an external nitrogen tank. By entering nitrogen to cooperate with the powder transportation, the powder transportation environment can be guaranteed to be safer, especially in the environment of the high-temperature furnace 2, to avoid the explosion of powder.

[0127] Secondly, the sealing tube and the air inlet pipe 86 connected to the extraction tank 1 can preferably be transported by argon gas. The inert gas enters the interior of the extraction tank 1, which can ensure a more stable extraction environment on the one hand, and prevent the oxidation of the extractant and solvent on the other hand, further improving the extraction effect.

[0128] Third embodiment:

[0129] See also Figure 1, Figure 4 , Figures 11 to 12 , further comprising an exhaust mechanism 9, the outer wall of the key rod 63 and the key groove located above the mounting plate 62 are connected with a linkage disk 13, and a protrusion 14 is fixed on the top of the linkage disk 13;

[0130] The exhaust mechanism 9 includes an exhaust pipe 91 fixedly mounted inside the top plate 10 and the mounting cover 11, a limit plate 92 is fixedly mounted in the middle of the exhaust pipe 91, a lifting rod 94 is slidably connected to the axis of the limit plate 92, and through holes 93 equidistantly distributed in an annular pattern are formed inside the limit plate 92, a guide wheel 96 is mounted on the bottom end of the lifting rod 94, and a sealing plate 95 is fixedly mounted on the top end of the lifting rod 94.

[0131] The bottom of the guide wheel 96 contacts the upper surface of the linkage disk 13, and the blocking plate 95 adopts a conical design that is wide at the top and narrow at the bottom.

[0132] See also Figure 4 : In the process of the first embodiment, whether the extraction motor 61 rotates clockwise or counterclockwise, it will drive the linkage disk 13 to rotate;

[0133] See also Figure 11 and Figure 12 (a): When the exhaust mechanism 9 is in the initial state, the guide wheel 96 will fit with the upper surface of the linkage disk 13. At this time, affected by gravity, the blocking plate 95 will block the top of the exhaust pipe 91. At this time, the internal environment of the entire extraction tank 1 is a sealed environment. During the operation of the second embodiment, the incoming argon gas will exist in the internal environment of the extraction tank 1 to perform gas protection extraction;

[0134] See also Figure 11 and Figure 12 (b) in the figure: When the linkage disk 13 rotates clockwise or counterclockwise, when the inclined surface of the protrusion 14 on the linkage disk 13 rotates to the position of the guide wheel 96, it will resist the guide wheel 96 upward. The guide wheel 96 drives the lifting rod 94 to rise along the limit plate 92, thereby controlling the sealing plate 95 to separate from the top of the exhaust pipe 91. The gas in the extraction tank 1 will enter the exhaust pipe 91 and pass through the through hole 93 in the limit plate 92, and finally be exhausted from the top of the exhaust pipe 91.

[0135] See also Figure 3 and Figure 4 The entire exhaust mechanism 9 is installed in a through-type manner inside the top plate 10 and the mounting cover 11, so that the gas can be directly discharged to the outside, and according to actual usage, gas treatment equipment, such as activated carbon adsorption devices, can be independently installed outside the exhaust mechanism 9.

[0136] This embodiment: During the working processes of the first and second embodiments, first, during the working process of the first embodiment, the linkage disk 13 can rotate synchronously with the clockwise rotation of the extraction motor 61. The continuously rotating linkage disk 13 drives the convex block 14 to rotate to achieve intermittent control of the opening and blocking of the exhaust mechanism 9. In this way, during the extraction process, intermittent exhaust can be realized, which can not only ensure the stable pressure state during the extraction process of the extraction tank 1, but also avoid excessive loss of argon gas inside the extraction tank 1, ensuring stable extraction effect while achieving safe pressure stabilization;

[0137] When the extraction motor 61 rotates counterclockwise to process the aqueous phase, the linkage disk 13 can still rotate to drive the convex block 14 to control the opening of the exhaust mechanism 9 for exhaust. And during the processing of the aqueous phase, the convex block 14 can be maintained in the open state of the exhaust mechanism 9 all the time, so that all the gas in the extraction tank 1 can be discharged completely, facilitating the user for subsequent extraction and making the internal and external gas media the same.

[0138] The above are only the preferred embodiments of the present invention, and do not limit the patent scope of the present invention accordingly. Any equivalent structural transformation made under the concept of the present invention by using the content of the specification and drawings of the present invention, or directly / indirectly applied in other related technical fields, is included in the patent protection scope of the present invention.

Claims

1. A gallium metal extraction device, characterized in that, It includes an extraction tank, a base, and an extraction mechanism; The top of the extraction tank is sealed and installed with a top plate through bolts. The top of the top plate is installed with a mounting cover through bolts. The inner wall of the mounting cover is installed with a feed pipe. The bottom end of the extraction tank is installed with a recovery pipe. The side wall of the extraction tank is fixedly provided with a suction pipe; The extraction mechanism includes a mounting plate fixedly arranged on the inner wall of the extraction tank. On the upper surface of the top plate and inside the mounting cover, an extraction motor is installed through bolts. The output shaft of the extraction motor is keyed to a key rod. The bottom end of the key rod is integrally provided with a stirring rod. The middle position inside the mounting plate is rotatably connected with a turntable. The side wall of the turntable is fixedly provided with a connecting rod. The bottom end of the connecting rod is fixedly provided with a cleaning plate. The outer wall of the key rod and inside the turntable is keyed to a ratchet wheel. On both sides of the ratchet wheel inside the turntable, ratchet teeth are rotatably installed through torsion springs; Inside the cleaning plate, a positioning plate is installed through bolts. Inside the recovery pipe and on one side of the positioning plate, a screw rod is installed through bolts.

2. The gallium metal extraction device according to claim 1, wherein The outlet end of the feed pipe penetrates through the inside of the mounting cover and extends to the inside of the top plate. The periphery of the extraction tank is installed on the base through bolts.

3. The gallium metal extraction device according to claim 1, wherein The ratchet wheel and the ratchet teeth are meshed with each other. The outer wall of the screw rod fits with the inner wall of the recovery pipe.

4. The gallium metal extraction device according to claim 1, characterized in that, The long end outer wall of the cleaning plate is in contact with the inner wall of the extraction tank. The cleaning plate is designed in a shape where the outside is high and gradually becomes lower towards the inside.

5. The gallium metal extraction device according to claim 1, characterized in that, It also includes a high-temperature furnace, and a blanking mechanism and a protection mechanism are installed outside the high-temperature furnace; The blanking mechanism includes a blanking cylinder fixedly arranged on the inner wall of the high-temperature furnace. The outer wall of the high-temperature furnace is installed with a blanking motor through bolts. Inside the blanking motor and inside the blanking cylinder, a spiral rod is keyed. On the outer wall of the output shaft of the blanking motor and on one side of the blanking cylinder, a half gear is keyed. A rack reciprocating ring is meshed and installed on the outer wall of the half gear. The top of the blanking cylinder is hermetically installed with a blanking frame through penetration; The protection mechanism includes a mounting frame installed on the side wall of the high-temperature furnace and on one side of the blanking motor. The side wall of the rack reciprocating ring is fixedly provided with sliding rods, and the number of sliding rods is two. Inside the mounting frame, sleeves are installed, and the number of sleeves is two. Inside both sleeves, piston plates are slidably connected. Inside both sleeves and on one side of the piston plates, a first one-way valve and a second one-way valve are installed. The inlet end of the first one-way valve is installed with an intake pipe.

6. The gallium metal extraction device according to claim 5, characterized in that, One end of the spiral rod is rotatably connected to the axis of the blanking cylinder through a bearing. The axes of the two sliding rods are fixedly connected to the axes of the two piston plates; Among them, the outlet ends of the two second one-way valves are hermetically installed with the high-temperature furnace and the extraction tank through hoses.

7. The gallium metal extraction device according to claim 5, characterized in that, It also includes an exhaust mechanism. Above the mounting plate on the outer wall of the key rod, a linkage disk is keyed. On the top of the linkage disk, a convex block is fixedly provided; The exhaust mechanism includes an exhaust pipe fixedly arranged inside the top plate and the mounting cover. A limiting plate is fixedly arranged at the middle position of the exhaust pipe. A lifting rod is slidably connected to the axis of the limiting plate. Through holes evenly distributed in an annular shape are formed inside the limiting plate. A guide wheel is installed at the bottom end of the lifting rod, and a sealing plate is fixedly arranged at the top end of the lifting rod.

8. The gallium metal extraction device according to claim 7, wherein The bottom of the guide wheel is in contact with the upper surface of the linkage disc. The sealing plate is designed in a tapered shape with a wider upper part and a narrower lower part.

9. A method for extracting gallium metal, characterized in that, The method for extracting gallium metal is used for the gallium metal extraction device as described in any one of claims 1-8, and includes the following steps: S1: Material pretreatment; Lithium-containing silicate minerals (such as lepidolite and spodumene), not limited to minerals, all materials containing gallium element can be used (such as waste electronic devices or recycled products containing gallium element, etc.) are crushed and ground to more than 50% of 200 mesh to improve the reaction activity. S2: High-temperature roasting; The ground material is mixed evenly with sulfates (such as sodium sulfate and potassium sulfate) in a mass ratio of 1:1–1:

3. The mixture is placed in a high-temperature furnace 2 and heated at 600–900 °C for 1–3 hours. At high temperature, the sulfate decomposes to generate SO3, which reacts with gallium in the mineral to generate gallium sulfate (Ga2(SO4)3): Ga2O3 + 3SO3 → Ga2(SO4)3; S3: Water leaching and concentration; The product after the high-temperature reaction is cooled to room temperature, and water is added for leaching. Gallium sulfate is easily soluble in water and enters the solution. After the solution is evaporated and concentrated multiple times, other insoluble impurities (such as SiO2) remain in the residue. The leaching solution and the residue are separated by filtration to obtain a gallium-containing solution. S4: Solvent extraction, and the extraction process is all carried out in an extraction tank; An organic extractant (such as Kelex100, LIX series) is used to selectively extract gallium from the gallium-containing solution; the extraction conditions are as follows: pH value: 2–3 Concentration of extractant: 5–10% Phase ratio (organic phase: aqueous phase) is 1:1–1:3 The gallium-loaded organic phase is back-extracted with an acidic solution (such as 1–2 mol / L HCl) to obtain a high-concentration gallium-containing solution; Mixing section: The leaching solution and the organic phase (extractant + diluent) are mixed at a volume ratio of 1:3–1:5 for 5–10 minutes; Clarification section: Stand for layering. The gallium-rich organic phase enters the back-extraction process. The aqueous phase (raffinate) is returned to leaching or discarded. The organic phase is sucked in from the suction pipe and enters the back-extraction process. The aqueous phase is discharged from the recovery pipe; S5: Recovery of gallium; The high-concentration gallium-containing solution is electrolyzed or chemically reduced to obtain gallium metal; Electrolysis conditions: current density 200–500 A / m 2 , voltage 3–5 V, temperature 25–50 °C.

Citation Information

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