A device and method for recovering and preparing metallic tantalum from waste and old tantalum capacitors

Abstract

The application provides a device and method for recovering and preparing metal tantalum from waste tantalum capacitors, relates to the technical field of metal material recovery, and comprises a sulfuration roasting furnace, a mounting plate, a uniform conduction mechanism and a conveying mechanism; the uniform conduction mechanism comprises a guide seat, a rotating shaft and a cam, the rotating shaft is vertically and rotationally connected to the inside of the mounting plate, the top end of the rotating shaft is fixedly connected with the cam, the inside of the guide seat is slidably connected with a reciprocating frame, and the circumferential surface of the right side of the reciprocating frame is sleeved with a spring. According to the scheme, the reciprocating frame drives the push plate to move back and forth through the rotation of the cam and the transmission of the transmission wheel, the push plate is used for knocking the crucible, the material in the crucible is leveled, the thickness of the material is uniform, the uniform material layer thickness can ensure that the diffusion of sulfur steam in the particle gap is smoother, each tantalum particle can fully contact the sulfur source, the sulfuration reaction is more complete and uniform, and the metal tantalum recovery rate is significantly improved.

Description

Technical Field

[0001] This invention relates to the field of metal material recycling technology, and in particular to an apparatus and method for recovering and preparing tantalum metal from waste tantalum capacitors. Background Technology

[0002] Tantalum is a rare metal with unique physical and chemical properties, widely used in industry, electronics, and medicine. Tantalum capacitors account for approximately 60% of global tantalum consumption, but their short lifespan leads to a large amount of tantalum-containing waste. Traditional landfill or incineration methods not only waste resources but also cause heavy metal pollution. Recovering tantalum from tantalum capacitors is not only a technological solution to alleviate resource shortages but also an inevitable choice to reshape the global strategic resource landscape.

[0003] In related technologies, when recovering tantalum metal from tantalum capacitors, the selective separation of tantalum from impurity metals via sulfidation roasting is the core step in recovering high-purity tantalum. However, some existing sulfidation roasting equipment does not easily ensure a uniform thickness of material within the crucible during tantalum extraction, leading to uneven heat conduction during the reaction and incomplete sulfidation. This results in a reduced tantalum metal recovery rate. Furthermore, excessively thin local areas can cause over-reaction, generating difficult-to-treat byproducts and increasing the difficulty of purification.

[0004] Therefore, it is necessary to provide an apparatus and method for recovering and preparing metallic tantalum from waste tantalum capacitors to solve the above-mentioned technical problems. Summary of the Invention

[0005] This invention provides an apparatus and method for recovering and preparing metallic tantalum from waste tantalum capacitors, which solves the technical problem in some existing sulfidation roasting equipment that is not convenient to ensure the uniform thickness of the material in the crucible when extracting metallic tantalum.

[0006] To solve the above-mentioned technical problems, the equipment for recovering and preparing metallic tantalum from waste tantalum capacitors provided by the present invention includes a sulfidation roasting furnace, a mounting plate, a uniform conduction mechanism, and a conveying mechanism;

[0007] The uniform transmission mechanism includes a guide seat, a rotating shaft, and a cam. The rotating shaft is vertically rotatably connected to the inside of the mounting plate. The top end of the rotating shaft is fixedly connected to the cam. A reciprocating frame is slidably connected inside the guide seat. A spring is sleeved on the circumferential side of the right side of the reciprocating frame. A transmission wheel is rotatably connected to the inner side of the right side of the reciprocating frame. A push plate is fixedly provided on the left side of the reciprocating frame. A drive motor for driving the rotating shaft to rotate is provided at the bottom of the mounting plate. A crucible is provided on the left side of the push plate.

[0008] The conveying mechanism is located on the top of the mounting plate and is used to adjust the working position of the crucible back and forth.

[0009] Preferably, the conveying mechanism includes two guide rails fixed on both sides of the top of the mounting plate, a placement seat slidably connected to the surface of the two guide rails, a screw block fixed to the bottom of the placement seat, a bidirectional threaded screw threaded to the inner side of the screw block, a conveying motor for driving the bidirectional threaded screw to rotate is provided on the front side of the mounting plate, the rear end of the bidirectional threaded screw is rotatably connected to the front of the vulcanization roasting furnace, and the crucible is placed on the top of the placement seat.

[0010] Preferably, two uprights are fixedly provided on the left side of the top of the placement seat, and a reset frame is slidably connected to the inner side of each of the two uprights. A reset spring is sleeved on the surface of each of the two reset frames and on the right side of each of the two uprights. The right side of each of the two reset frames is in contact with the outer surface of the crucible.

[0011] Preferably, a mixing mechanism is fixed on one side of the two guide rails that are separated from each other. The mixing mechanism includes two mounting brackets fixed on the two guide rails that are separated from each other. A mixing shaft is rotatably connected to the inner side of the right mounting bracket. A mixing cylinder is rotatably connected to the surface of the mixing shaft. Multiple mixing frames are provided on the surface of the mixing shaft and inside the mixing cylinder. A mixing motor for driving the mixing shaft to rotate is provided on the right side of the right mounting bracket.

[0012] Preferably, a switching mechanism is fixedly provided on the left side of the placement seat. The switching mechanism includes a switching gear plate fixedly provided on the left side of the placement seat. The mounting bracket on the left side is rotatably connected to a drive shaft and a rotating rod from top to bottom. A switching gear is fixedly provided on the surface of the rotating rod. The switching gear meshes with the switching gear plate. Synchronous pulleys are fixedly provided on the surfaces of the rotating rod and the drive shaft. Synchronous belts are sleeved on the surfaces of the two synchronous pulleys. The right end of the drive shaft is fixedly connected to the mixing cylinder.

[0013] Preferably, a driving mechanism is fixedly provided on the right side of the vulcanizing roasting furnace. The driving mechanism includes a sliding seat fixedly provided on the right side of the vulcanizing roasting furnace. A slider is slidably connected to the inner side of the sliding seat. A compression spring is provided inside the sliding seat and located behind the slider. A driving tooth plate is fixedly provided on the top of the slider. A driving shaft is rotatably connected inside the vulcanizing roasting furnace. A driving gear is fixedly provided at the right end of the driving shaft. The driving gear meshes with the driving tooth plate. A connecting frame is provided on the rear side of the bottom of the placement seat. A trigger rod is threadedly connected to the inner side of the connecting frame.

[0014] Preferably, a protective mechanism is fixedly provided at the left end of the drive shaft. The protective mechanism includes a drive wheel fixedly provided at the left end of the drive shaft. A mounting seat is rotatably connected to the surface of the drive shaft. The right side of the mounting seat is fixedly connected to the inner wall of the vulcanization roasting furnace. Two slide rails are fixedly provided on the left side of the mounting seat. A connecting bracket is slidably connected to the surface of each of the two slide rails. The left side of each of the two connecting brackets is located inside the drive wheel. A high-temperature protective shell is fixedly provided on the opposite side of each of the two connecting brackets. A gas detector is provided on the inner side of the bottom high-temperature protective shell.

[0015] Preferably, an argon gas protection mechanism is provided on the left side of the vulcanizing roasting furnace, and a pipe is connected to the top of the argon gas protection mechanism. The pipe is connected to the vulcanizing roasting furnace. An alarm is provided on the top of the vulcanizing roasting furnace. A support frame is fixedly provided at the bottom of the mounting plate, and the back of the support frame is fixedly connected to the front of the vulcanizing roasting furnace.

[0016] A method for recovering and preparing metallic tantalum from waste tantalum capacitors includes the following steps:

[0017] Step S1: Place the waste tantalum capacitors in a quartz tube furnace for pyrolysis and collect the pyrolysis residue;

[0018] Step S2: Crush the pyrolysis residue, and then use ultrasonic sieving to remove most of the silica and residual carbon to obtain metal enrichment.

[0019] Step S3: Remove the iron-nickel alloy from the metal concentrate by magnetic separation to obtain tantalum-rich metal powder;

[0020] Step S4: Mix tantalum-rich metal powder and a certain amount of sulfur, then sulfide-roast to obtain the sulfide-roasted product.

[0021] Step S5: Use nitric acid to leach and remove impurities from the sulfurized roasting product;

[0022] Step S6: Use dilute hydrofluoric acid to acid leaching and calcining the product to remove residual trace amounts of silica, then filter, wash and dry to obtain tantalum oxide powder.

[0023] Step S7: The obtained tantalum oxide powder is mixed with metallic sodium in a certain proportion and placed in an inert atmosphere sealed reactor for reduction reaction. After cooling, the product is taken out, washed with dilute hydrochloric acid to remove the byproduct Na2O, washed with deionized water until neutral, and vacuum dried to obtain metallic tantalum.

[0024] Compared with related technologies, the equipment and method for recovering and preparing metallic tantalum from waste tantalum capacitors provided by the present invention have the following advantages:

[0025] The cam rotates, and under the action of the transfer wheel, the reciprocating frame drives the pusher plate to move back and forth. The pusher plate taps the crucible, leveling the material inside and achieving uniform material thickness. The uniform material layer thickness ensures smoother diffusion of sulfur vapor between particles, allowing each tantalum particle to fully contact the sulfur source, ensuring a more complete and uniform sulfidation reaction, and significantly improving the recovery rate of tantalum metal. At the same time, the uniform material thickness can inhibit over-sulfidation during the tantalum reaction, thereby reducing the probability of hydrolysis to form insoluble tantalum oxides. This can reduce side reactions and impurities, and improve the purity of tantalum metal products. Compared with manual material leveling, this equipment can achieve standardized operation, with more consistent material thickness and porosity for each batch. This makes it easier to control parameters such as temperature distribution and reaction time during sulfidation roasting, reducing batch-to-batch deviations in recovery rate and purity. Attached Figure Description

[0026] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.

[0027] Figure 1 The optimal structural schematic diagram provided for this invention;

[0028] Figure 2 This is a schematic diagram of the structure of the sulfidation roasting furnace provided by the present invention (left view).

[0029] Figure 3 A schematic diagram of the uniform conduction mechanism and conveying mechanism provided by the present invention;

[0030] Figure 4 for Figure 3 The enlarged structural diagram at point A is shown below;

[0031] Figure 5 for Figure 4 The diagram shows the structure of the placement base;

[0032] Figure 6 A schematic diagram showing the state of the rotating shaft driving the cam to rotate, provided by the present invention.

[0033] Figure 7 A schematic diagram of the structure of the mixing mechanism and the switching mechanism provided by the present invention;

[0034] Figure 8 for Figure 7 The enlarged structural diagram at point B is shown below;

[0035] Figure 9 for Figure 7 The diagram shows a cross-sectional view of the mixing cylinder.

[0036] Figure 10 A schematic diagram showing the state in which the placement seat of the present invention drives the switching gear plate to move forward, causing the switching gear to rotate.

[0037] Figure 11 for Figure 10 The diagram shown illustrates the state in which the placement seat continuously drives the switching gear plate to move forward, causing the switching gear to rotate.

[0038] Figure 12 Schematic diagram of the drive mechanism and protection mechanism provided by the present invention;

[0039] Figure 13 for Figure 12 The diagram shows the structure of the protective mechanism.

[0040] Figure 14 for Figure 13 The diagram shows the structure of the drive wheel;

[0041] Figure 15 A flowchart illustrating the method for recycling and preparing tantalum metal provided by this invention.

[0042] Explanation of icon numbers:

[0043] 1. Vulcanizing roasting furnace; 2. Mounting plate;

[0044] 3. Uniform transmission mechanism; 31. Guide seat; 32. Rotating shaft; 33. Cam; 34. Reciprocating frame; 35. Spring; 36. Transmission wheel; 37. Push plate; 38. Drive motor;

[0045] 4. Conveying mechanism; 41. Guide rail; 42. Placement seat; 43. Screw block; 44. Double-sided threaded screw; 45. Conveying motor;

[0046] 5. Crucible; 6. Stand; 7. Reset bracket; 8. Reset spring;

[0047] 9. Mixing mechanism; 91. Mounting bracket; 92. Mixing shaft; 93. Mixing cylinder; 94. Mixing frame; 95. Mixing motor;

[0048] 10. Switching mechanism; 101. Switching gear plate; 102. Drive shaft; 103. Rotating rod; 104. Switching gear; 105. Synchronous pulley; 106. Synchronous belt;

[0049] 11. Drive mechanism; 111. Sliding seat; 112. Slider; 113. Compression spring; 114. Drive gear plate; 115. Drive shaft; 116. Drive gear; 117. Connecting frame; 118. Trigger rod;

[0050] 12. Protective mechanism; 121. Drive wheel; 122. Mounting base; 123. Slide rail; 124. Connecting bracket; 125. High-temperature protective shell; 126. Gas detector;

[0051] 13. Argon protection mechanism; 14. Pipeline; 15. Alarm; 16. Support frame.

[0052] The realization of the objective, functional features and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0053] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not 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 effort are within the scope of protection of the present invention.

[0054] This invention provides an apparatus and method for recovering and preparing metallic tantalum from waste tantalum capacitors.

[0055] First embodiment:

[0056] Please see Figures 1 to 6 A device for recycling tantalum metal from waste tantalum capacitors, comprising a sulfidation roasting furnace 1, a mounting plate 2, a uniform conduction mechanism 3, and a conveying mechanism 4;

[0057] The uniform transmission mechanism 3 includes a guide seat 31, a rotating shaft 32, and a cam 33. The rotating shaft 32 is vertically rotatably connected to the inside of the mounting plate 2. The top end of the rotating shaft 32 is fixedly connected to the cam 33. A reciprocating frame 34 is slidably connected inside the guide seat 31. A spring 35 is sleeved on the circumferential side of the right side of the reciprocating frame 34. A transmission wheel 36 is rotatably connected to the inner side of the right side of the reciprocating frame 34. A push plate 37 is fixedly provided on the left side of the reciprocating frame 34. A drive motor 38 for driving the rotating shaft 32 to rotate is provided at the bottom of the mounting plate 2. A crucible 5 is provided on the left side of the push plate 37.

[0058] Please combine Figure 3 , Figure 4 and Figure 6 : Start the drive motor 38. The drive motor 38 rotates and drives the rotating shaft 32 to rotate. The rotating shaft 32 rotates and drives the cam 33 to rotate. The rotating cam 33 rotates and then drives the reciprocating frame 34 to move back and forth through the transmission wheel 36. The reciprocating frame 34 drives the push plate 37 to move back and forth left and right. The push plate 37 moves back and forth left and right, thereby striking the crucible 5, so that the material in the crucible 5 becomes uniform in thickness due to vibration.

[0059] The conveying mechanism 4 is located on the top of the mounting plate 2 and is used to adjust the working position of the crucible 5 back and forth.

[0060] The conveying mechanism 4 includes two guide rails 41 fixed on both sides of the top of the mounting plate 2. The surfaces of the two guide rails 41 are slidably connected to a placement seat 42. A screw block 43 is fixed at the bottom of the placement seat 42. A bidirectional threaded screw 44 is threadedly connected to the inner side of the screw block 43. A conveying motor 45 for driving the bidirectional threaded screw 44 to rotate is provided on the front side of the mounting plate 2. The rear end of the bidirectional threaded screw 44 is rotatably connected to the front side of the vulcanization roasting furnace 1. The crucible 5 is placed on the top of the placement seat 42.

[0061] Please combine Figure 3 and Figure 5 Start the conveyor motor 45. The conveyor motor 45 rotates and drives the bidirectional threaded screw 44 to rotate. The bidirectional threaded screw 44 rotates through the screw block 43 and drives the placement seat 42 to move. By rotating the conveyor motor 45 in both directions, the placement seat 42 can slide back and forth on the surface of the guide rail 41.

[0062] Two uprights 6 are fixedly provided on the left side of the top of the placement base 42. The inner sides of the two uprights 6 are slidably connected to the reset frame 7. The surfaces of the two reset frames 7 and the right sides of the two uprights 6 are fitted with reset springs 8. The right sides of the two reset frames 7 are in contact with the outer surface of the crucible 5.

[0063] Please combine Figure 3 and Figure 6 When the crucible 5 moves to the left, the two reset frames 7 slide to the left inside the stand 6, and the two reset springs 8 contract. When the reciprocating frame 34 resets to the right, the two reset frames 7 slide to the right inside the stand 6 through the expansion of the reset springs 8, thereby resetting the position of the crucible 5.

[0064] In this embodiment, the cam 33 rotates, and under the action of the transfer wheel 36, the reciprocating frame 34 drives the push plate 37 to move back and forth. The push plate 37 taps the crucible 5 to level the material inside the crucible 5, achieving uniform material thickness. The uniform material layer thickness ensures smoother diffusion of sulfur vapor between particles, allowing each tantalum particle to fully contact the sulfur source, ensuring a more complete and uniform sulfidation reaction, and significantly improving the recovery rate of tantalum metal. At the same time, the uniform material thickness can inhibit excessive sulfidation during the tantalum reaction, thereby reducing the probability of hydrolysis to form insoluble tantalum oxides, reducing side reactions and impurities, and improving the purity of tantalum metal products. Compared with manual scraping of materials, this equipment can achieve standardized operation, with more consistent material thickness and porosity for each batch, making it easier to control parameters such as the temperature distribution and reaction time of sulfidation roasting, and reducing batch-to-batch deviations in recovery rate and purity.

[0065] Second embodiment:

[0066] Please see Figures 7 to 11 A mixing mechanism 9 is fixedly provided on one side of the two guide rails 41 that are separated from each other. The mixing mechanism 9 includes two mounting brackets 91 fixedly provided on the one side of the two guide rails 41 that are separated from each other. A mixing shaft 92 is rotatably connected to the inner side of the right mounting bracket 91. A mixing cylinder 93 is rotatably connected to the surface of the mixing shaft 92. Multiple sets of mixing frames 94 are provided on the surface of the mixing shaft 92 and inside the mixing cylinder 93. A mixing motor 95 for driving the mixing shaft 92 to rotate is provided on the right side of the right mounting bracket 91.

[0067] Please combine Figure 7 and Figure 9 Tantalum-rich metal powder and a measured amount of sulfur are added into the mixing cylinder 93. Then, the mixing motor 95 is started. The rotation of the mixing motor 95 drives the mixing shaft 92 to rotate, which in turn drives multiple sets of mixing frames 94 to rotate, thereby mixing the tantalum-rich metal powder and the measured amount of sulfur.

[0068] A switching mechanism 10 is fixedly provided on the left side of the placement seat 42. The switching mechanism 10 includes a switching toothed plate 101 fixedly provided on the left side of the placement seat 42. The mounting bracket 91 on the left side is rotatably connected to a drive shaft 102 and a rotating rod 103 from top to bottom. A switching gear 104 is fixedly provided on the surface of the rotating rod 103. The switching gear 104 meshes with the switching toothed plate 101. Synchronous pulleys 105 are fixedly provided on the surfaces of both the rotating rod 103 and the drive shaft 102. A synchronous belt 106 is sleeved on the surfaces of the two synchronous pulleys 105. The right end of the drive shaft 102 is fixedly connected to the mixing cylinder 93.

[0069] Please combine Figure 7 , Figure 8 , Figure 11 and Figure 12 The rotation of the bidirectional threaded screw 44 drives the screw block 43 and the placement seat 42 to move back and forth. The back and forth movement of the placement seat 42 in turn drives the switching gear plate 101 to move back and forth. The back and forth movement of the switching gear plate 101 drives the switching gear 104 to reciprocate. The reciprocating rotation of the switching gear 104 drives the transmission shaft 102 to reciprocate through the synchronous pulley 105 and the synchronous belt 106. The reciprocating rotation of the transmission shaft 102 drives the mixing cylinder 93 to oscillate back and forth, thereby improving the mixing effect of the mixing frame 94.

[0070] Furthermore, the rotation of the bidirectional threaded screw 44 drives the screw block 43 and the placement seat 42 to move forward continuously. The placement seat 42 then drives the switching gear plate 101 to move forward continuously. The switching gear plate 101 then drives the switching gear 104 to rotate clockwise. The switching gear 104 drives the transmission shaft 102 to rotate through the rotating rod 103, the synchronous wheel 105 and the synchronous belt 106. The transmission shaft 102 then drives the mixing cylinder 93 to rotate clockwise, thereby slowly pouring the material in the mixing cylinder 93 into the crucible 5.

[0071] In this embodiment, the mixing motor 95 drives multiple mixing racks 94 to rotate, directly mixing the materials, breaking up powder agglomerates, and making the sulfur particles evenly dispersed in the metal powder. While mixing, the mixing cylinder 93 reciprocates through the transmission shaft 102, switching gear 104, and switching tooth plate 101, causing the materials to tumble inside the mixing cylinder 93, thereby filling the dead corners of the mixing and avoiding local sulfur enrichment or deficiency. The placement seat 42 continuously drives the crucible 5 forward, so that the materials in the mixing cylinder 93 can be slowly poured into the crucible 5. While pouring the materials, the placement seat 42 is controlled to drive the crucible 5 to move back and forth, so that the materials in the mixing cylinder 93 can be evenly poured into different positions, avoiding the phenomenon of local accumulation of materials.

[0072] Third embodiment:

[0073] Please see Figure 1 , Figure 2 , Figures 12 to 14 A driving mechanism 11 is fixedly provided on the right side of the vulcanizing roasting furnace 1. The driving mechanism 11 includes a sliding seat 111 fixedly provided on the right side of the vulcanizing roasting furnace 1. A slider 112 is slidably connected to the inner side of the sliding seat 111. A compression spring 113 is provided inside the sliding seat 111 and located behind the slider 112. A driving tooth plate 114 is fixedly provided on the top of the slider 112. A driving shaft 115 is rotatably connected inside the vulcanizing roasting furnace 1. A driving gear 116 is fixedly provided at the right end of the driving shaft 115. The driving gear 116 meshes with the driving tooth plate 114. A connecting frame 117 is provided on the rear side of the bottom of the placement seat 42. A trigger rod 118 is threadedly connected to the inner side of the connecting frame 117.

[0074] Please combine Figure 12 When the placement seat 42 drives the connecting frame 117 and the trigger rod 118 to move backward continuously, the trigger rod 118 will contact the drive gear plate 114 and push the drive gear plate 114 backward. The drive gear plate 114 moves backward and drives the drive gear 116 to rotate. The slider 112 slides backward on the inner side of the sliding seat 111, and the compression spring 113 is compressed.

[0075] Furthermore, when the trigger rod 118 releases the pressure on the drive gear plate 114, the expansion force of the compression spring 113 causes the slider 112 to slide on the front side of the inner side of the sliding seat 111. The slider 112 moves forward, causing the drive gear plate 114 to move forward, thereby resetting the position of the drive gear 116.

[0076] Preferably, the connecting frame 117 has a through groove, and the connecting frame 117 can be disassembled by unscrewing the bolts. The contact time between the trigger rod 118 and the drive tooth plate 114 can be adjusted by rotating the trigger rod 118.

[0077] A protective mechanism 12 is fixedly provided at the left end of the drive shaft 115. The protective mechanism 12 includes a drive wheel 121 fixedly provided at the left end of the drive shaft 115. A mounting base 122 is rotatably connected to the surface of the drive shaft 115. The right side of the mounting base 122 is fixedly connected to the inner wall of the vulcanization roasting furnace 1. Two slide rails 123 are fixedly provided on the left side of the mounting base 122. A connecting bracket 124 is slidably connected to the surface of each of the two slide rails 123. The left side of each of the two connecting brackets 124 is located inside the drive wheel 121. A high-temperature protective shell 125 is fixedly provided on the opposite side of each of the two connecting brackets 124. A gas detector 126 is provided on the inner side of the bottom high-temperature protective shell 125.

[0078] Please combine Figure 13 and Figure 14 The drive gear 116 rotates and drives the drive wheel 121 to rotate via the drive shaft 115. The rotation of the drive wheel 121 causes the two connecting brackets 124 to slide on the surface of the slide rail 123 to move to a different side. The movement of the two connecting brackets 124 causes the two high-temperature protective shells 125 to move to a different side, thereby exposing the gas detector 126 for detection of the internal gas.

[0079] Preferably, the inner side of the drive wheel 121 is provided with a through groove that cooperates with the connecting bracket 124. By rotating the drive wheel 121, the two connecting brackets 124 can be moved to opposite sides under the limit of the slide rail 123.

[0080] An argon gas protection mechanism 13 is provided on the left side of the vulcanizing roasting furnace 1. A pipe 14 is connected to the top of the argon gas protection mechanism 13. The pipe 14 is connected to the vulcanizing roasting furnace 1. An alarm 15 is provided on the top of the vulcanizing roasting furnace 1. A support frame 16 is fixedly provided at the bottom of the mounting plate 2. The back of the support frame 16 is fixedly connected to the front of the vulcanizing roasting furnace 1.

[0081] Preferably, after placing the crucible 5 into the sulfurization roasting furnace 1, the opening of the sulfurization roasting furnace 1 is closed first, and then argon gas is continuously introduced through the argon gas protection mechanism 13 and the pipeline 14. The purpose is to exhaust the air in the sulfurization roasting furnace 1. This process needs to be continued for a period of time to avoid the metal or sulfur reacting with oxygen during roasting.

[0082] In this embodiment, when the placement seat 42 moves backward, it simultaneously drives the connecting frame 117 and the trigger rod 118 to move backward. The backward movement of the trigger rod 118 pushes the drive gear plate 114 backward, causing the drive gear 116 to drive the drive wheel 121 to rotate. The rotation of the drive wheel 121 opens the high-temperature protective shell 125 through the connecting bracket 124, exposing the gas detector 126 to directly contact the gas inside the furnace for detection. In the non-detection state, the two high-temperature protective shells 125 are tightly closed, forming a closed space to enclose the gas detector 126, isolating it from high-temperature radiation and corrosive gas corrosion inside the furnace, and preventing the gas detector 126 from degrading in performance due to long-term exposure.

[0083] Fourth embodiment:

[0084] Please see Figure 15 A method for recovering and preparing metallic tantalum from waste tantalum capacitors includes the following steps:

[0085] Step S1: Place the waste tantalum capacitors in a quartz tube furnace for pyrolysis and collect the pyrolysis residue;

[0086] Preferably, the pyrolysis conditions are: argon atmosphere, nitrogen flow rate of 100 mL / min, pyrolysis temperature of 500-700℃, and pyrolysis time of 0.5-2 h;

[0087] Step S2: Crush the pyrolysis residue, and then use ultrasonic sieving to remove most of the silica and residual carbon to obtain metal enrichment.

[0088] Step S3: Remove the iron-nickel alloy from the metal concentrate by magnetic separation to obtain tantalum-rich metal powder;

[0089] Step S4: Mix tantalum-rich metal powder and a certain amount of sulfur, then sulfide-roast to obtain the sulfide-roasted product.

[0090] Preferably, the mass ratio of sulfur to tantalum-rich metal powder is 0.2-1:1, the calcination atmosphere is argon, the calcination temperature is 900-1100℃, and the calcination time is 0.5-1h.

[0091] Step S5: Use nitric acid to leach and remove impurities from the sulfurized roasting product;

[0092] Preferably, the nitric acid concentration is 1-5 mol / L, the liquid-to-solid ratio is 3-5:1, the acid leaching temperature is 40-80℃, the acid leaching time is 4-8h, and the stirring speed is 200 r / min;

[0093] Step S6: Use dilute hydrofluoric acid to acid leaching and calcining the product to remove residual trace amounts of silica, then filter, wash and dry to obtain tantalum oxide powder.

[0094] Preferably, the concentration of dilute hydrofluoric acid is 4-10%, the liquid-to-solid ratio is 1-3:1, the acid leaching is carried out at room temperature for 10-30 minutes, the stirring rate is 200 r / min, the washing method is water washing, and the drying temperature is 180℃.

[0095] Step S7: The obtained tantalum oxide powder is mixed with metallic sodium in a certain proportion and placed in an inert atmosphere sealed reactor for reduction reaction. After cooling, the product is taken out, washed with dilute hydrochloric acid to remove the byproduct Na2O, washed with deionized water until neutral, and vacuum dried to obtain metallic tantalum.

[0096] In this embodiment, resource intensification is achieved by recycling waste tantalum capacitors. The residual carbon that is not completely separated is removed by sulfidation roasting and the insoluble manganese is converted into manganese sulfide that is easily dissolved by acid, thereby obtaining purer tantalum oxide. Metallic tantalum is obtained by sodium thermal reduction. This effectively alleviates the dependence of the high-tech new materials industry on raw materials of primary tantalum ore and simultaneously recovers high-value-added nickel-iron electrode materials, forming a multi-dimensional resource recycling system.

[0097] Please refer to the reference again. Figures 1 to 14 The working principle of the equipment for recovering and preparing metallic tantalum from waste tantalum capacitors provided by the present invention is as follows:

[0098] Step S1: Tantalum-rich metal powder and a measured amount of sulfur are added into the mixing cylinder 93, and then the mixing motor 95 is started. The mixing motor 95 rotates, driving the mixing shaft 92 to rotate. The rotation of the mixing shaft 92 drives multiple sets of mixing frames 94 to rotate, thus mixing the tantalum-rich metal powder and the measured amount of sulfur.

[0099] Step S2: Start the conveyor motor 45. The double-sided screw 44 rotates, causing the screw block 43 and the placement seat 42 to move back and forth. The back and forth movement of the placement seat 42 causes the switching gear plate 101 to move back and forth. The back and forth movement of the switching gear plate 101 causes the switching gear 104 to reciprocate. The reciprocating rotation of the switching gear 104 drives the transmission shaft 102 to reciprocate through the synchronous pulley 105 and the synchronous belt 106. The reciprocating rotation of the transmission shaft 102 causes the mixing cylinder 93 to oscillate back and forth, thereby improving the mixing effect of the mixing frame 94.

[0100] In step S3, after the materials in the mixing cylinder 93 are mixed, the screw block 43 and the placement seat 42 are moved forward continuously by the rotation of the bidirectional threaded screw 44. The placement seat 42 then drives the switching gear plate 101 to move forward continuously. The switching gear plate 101 drives the switching gear 104 to rotate clockwise. The switching gear 104 drives the transmission shaft 102 to rotate through the rotating rod 103, the synchronous wheel 105 and the synchronous belt 106. The transmission shaft 102 then drives the mixing cylinder 93 to rotate clockwise, thereby slowly pouring the materials in the mixing cylinder 93 into the crucible 5.

[0101] In step S4, the screw block 43, the placement seat 42, and the crucible 5 are moved backward by rotating the bidirectional threaded screw 44. When the crucible 5 moves to the working position, the drive motor 38 is started. The drive motor 38 rotates and drives the rotating shaft 32 to rotate. The rotating shaft 32 rotates and drives the cam 33 to rotate. The rotation of the cam 33 causes the reciprocating frame 34 to move back and forth left and right through the transmission wheel 36. The reciprocating frame 34 drives the push plate 37 to move back and forth left and right. The reciprocating movement of the push plate 37 knocks on the crucible 5, so that the material in the crucible 5 becomes uniform in thickness due to vibration.

[0102] Step S5: Place the processed crucible 5 into the sulfurization roasting furnace 1. After the crucible 5 is placed into the sulfurization roasting furnace 1, first close the opening of the sulfurization roasting furnace 1, and then use the argon protection mechanism 13 and the pipeline 14 to continuously introduce argon gas to exhaust the air in the sulfurization roasting furnace 1.

[0103] The bidirectional threaded screw 44 drives the placement seat 42, connecting bracket 117 and trigger rod 118 to move backward continuously. When the trigger rod 118 contacts the drive gear plate 114, it pushes the drive gear plate 114 backward. The drive gear plate 114 moves backward and drives the drive gear 116 to rotate. The slider 112 slides backward on the inner side of the sliding seat 111, and the compression spring 113 contracts. The rotation of the drive gear 116 drives the drive wheel 121 to rotate through the drive shaft 115. The rotation of the drive wheel 121 causes the two connecting brackets 124 to slide on the surface of the slide rail 123 to move to the opposite side. The movement of the two connecting brackets 124 causes the two high-temperature protective shells 125 to move to the opposite side, thereby exposing the gas detector 126 and detecting the internal gas.

[0104] The above description is only a preferred embodiment of the present invention and does not limit the patent scope of the present invention. All equivalent structural transformations made under the concept of the present invention using the contents of the present invention specification and drawings, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.

Claims

1. A calcination apparatus for recovering and preparing metallic tantalum from waste tantalum capacitors, characterized in that, Includes a vulcanization roasting furnace, mounting plate, uniform conduction mechanism, and conveying mechanism; The uniform transmission mechanism includes a guide seat, a rotating shaft, and a cam. The rotating shaft is vertically rotatably connected to the inside of the mounting plate. The top end of the rotating shaft is fixedly connected to the cam. A reciprocating frame is slidably connected inside the guide seat. A spring is sleeved on the circumferential side of the right side of the reciprocating frame. A transmission wheel is rotatably connected to the inner side of the right side of the reciprocating frame. A push plate is fixedly provided on the left side of the reciprocating frame. A drive motor for driving the rotating shaft to rotate is provided at the bottom of the mounting plate. A crucible is provided on the left side of the push plate. The conveying mechanism is located on the top of the mounting plate and is used to adjust the working position of the crucible back and forth. A support frame is fixedly mounted on the bottom of the mounting plate, and the back of the support frame is fixedly connected to the front of the vulcanization roasting furnace.

2. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 1, characterized in that, The conveying mechanism includes two guide rails fixed on both sides of the top of the mounting plate. A placement seat is slidably connected to the surface of the two guide rails. A screw block is fixed to the bottom of the placement seat. A bidirectional threaded screw is threaded to the inner side of the screw block. A conveying motor for driving the bidirectional threaded screw to rotate is provided on the front side of the mounting plate. The rear end of the bidirectional threaded screw is rotatably connected to the front side of the vulcanization roasting furnace. The crucible is placed on the top of the placement seat.

3. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 2, characterized in that, Two uprights are fixedly mounted on the left side of the top of the placement base. The inner sides of the two uprights are slidably connected to reset frames. The surfaces of the two reset frames and the right sides of the two uprights are fitted with reset springs. The right sides of the two reset frames are in contact with the outer surface of the crucible.

4. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 2, characterized in that, A mixing mechanism is fixed on one side of the two guide rails that are separated from each other. The mixing mechanism includes two mounting brackets fixed on the two guide rails that are separated from each other. A mixing shaft is rotatably connected to the inner side of the right mounting bracket. A mixing cylinder is rotatably connected to the surface of the mixing shaft. Multiple mixing frames are arranged on the surface of the mixing shaft and inside the mixing cylinder. A mixing motor for driving the mixing shaft to rotate is arranged on the right side of the right mounting bracket.

5. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 4, characterized in that, A switching mechanism is fixedly provided on the left side of the placement seat. The switching mechanism includes a switching gear plate fixedly provided on the left side of the placement seat. The mounting bracket on the left side is rotatably connected to a drive shaft and a rotating rod from top to bottom. A switching gear is fixedly provided on the surface of the rotating rod. The switching gear meshes with the switching gear plate. Synchronous pulleys are fixedly provided on the surfaces of the rotating rod and the drive shaft. Synchronous belts are sleeved on the surfaces of the two synchronous pulleys. The right end of the drive shaft is fixedly connected to the mixing cylinder.

6. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 2, characterized in that, A driving mechanism is fixedly installed on the right side of the vulcanizing roasting furnace. The driving mechanism includes a sliding seat fixedly installed on the right side of the vulcanizing roasting furnace. A slider is slidably connected to the inner side of the sliding seat. A compression spring is installed inside the sliding seat and behind the slider. A driving tooth plate is fixedly installed on the top of the slider. A driving shaft is rotatably connected inside the vulcanizing roasting furnace. A driving gear is fixedly installed at the right end of the driving shaft. The driving gear meshes with the driving tooth plate. A connecting frame is installed on the rear side of the bottom of the placement seat. A trigger rod is threadedly connected to the inner side of the connecting frame.

7. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 6, characterized in that, A protective mechanism is fixed to the left end of the drive shaft. The protective mechanism includes a drive wheel fixed to the left end of the drive shaft. A mounting base is rotatably connected to the surface of the drive shaft. The right side of the mounting base is fixedly connected to the inner wall of the vulcanization roasting furnace. Two slide rails are fixed to the left side of the mounting base. Connecting brackets are slidably connected to the surfaces of the two slide rails. The left sides of the two connecting brackets are located inside the drive wheel. High-temperature protective shells are fixed to the opposite sides of the two connecting brackets. A gas detector is provided inside the bottom high-temperature protective shell.

8. The calcination equipment for recovering and preparing metallic tantalum from waste tantalum capacitors according to claim 1, characterized in that, An argon gas protection mechanism is installed on the left side of the vulcanization roasting furnace. A pipe is connected to the top of the argon gas protection mechanism and is connected to the vulcanization roasting furnace. An alarm is installed on the top of the vulcanization roasting furnace.

9. A method for recovering and preparing metallic tantalum from waste tantalum capacitors, characterized in that, The method for recycling and preparing tantalum metal includes the calcination equipment and the steps described in any one of claims 1-8: Step S1: Place the waste tantalum capacitors in a quartz tube furnace for pyrolysis and collect the pyrolysis residue; Step S2: Crush the pyrolysis residue, and then use ultrasonic sieving to remove most of the silica and residual carbon to obtain metal enrichment. Step S3: Remove the iron-nickel alloy from the metal concentrate by magnetic separation to obtain tantalum-rich metal powder; Step S4: After mixing tantalum-rich metal powder with a certain amount of sulfur, the mixture is fed into a calcination device for sulfurization and calcination to obtain the sulfurized calcination product. Step S5: Use nitric acid to leach and remove impurities from the sulfurized roasting product; Step S6: Use dilute hydrofluoric acid to acid leaching and calcining the product to remove residual trace amounts of silica, then filter, wash and dry to obtain tantalum oxide powder. Step S7: The obtained tantalum oxide powder is mixed with metallic sodium in a certain proportion and placed in an inert atmosphere sealed reactor for reduction reaction. After cooling, the product is taken out, washed with dilute hydrochloric acid to remove the byproduct Na2O, washed with deionized water until neutral, and vacuum dried to obtain metallic tantalum.

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