Germanium oxide treatment system

Abstract

A germanium oxide processing system is provided, including a calcination furnace, a dross tank, and a collection module. The calcination furnace is configured to heat and dry germanium oxide material in a flowing vacuum oxygen-free environment and discharge water vapor to the collection module, and to heat and calcine the germanium oxide material at a temperature at which the germanium oxide does not sublimate in a flowing vacuum oxygen-free environment with nitrogen gas admitted and discharge water vapor and nitrogen gas to the collection module and dross gas and nitrogen gas to the dross tank. The dross tank is configured to receive the dross gas and nitrogen gas, condense to form a viscous liquid, and discharge the nitrogen gas to the collection module. The collection module is configured to form a flowing vacuum with the calcination furnace, receive and condense and collect the heat and dry water vapor, receive and condense and collect the heat and calcine water vapor and nitrogen gas, receive and cool the nitrogen gas discharged from the dross tank during the heat and calcine.

Description

Technical Field

[0001] This disclosure relates to the field of germanium materials, and more specifically to a germanium oxide treatment system. Background Technology

[0002] Germanium is an important semiconductor material, widely used in semiconductor devices and infrared optical components. Germanium dioxide is an intermediate raw material for the preparation of high-purity germanium. Germanium dioxide is reduced with hydrogen to produce elemental germanium, which is then purified through processes such as zone melting to produce germanium with even higher purity.

[0003] The purity of germanium dioxide has a significant impact on the subsequent preparation of elemental germanium. Germanium dioxide (in powder form), as an intermediate raw material, contains moisture, which is typically removed by baking. For example, patent document CN1614049A, published on May 11, 2005, describes the use of oven baking to remove water and water of crystallization from the germanium dioxide material.

[0004] The oven baking process does not treat the evaporated water in any way, which is detrimental to production safety and resource conservation.

[0005] In addition, oven baking is only for dehydration of germanium dioxide materials, and the oven itself is not suitable for removing other residues (such as oil) contained in germanium dioxide materials.

[0006] Therefore, there is a need to develop germanium dioxide processing equipment to improve the purity of germanium dioxide, adapt to the treatment of water and other sludge (such as oil) contained in germanium dioxide, and improve production safety and resource conservation.

[0007] In addition, both the drying oven and the germanium dioxide processing equipment that needs to be developed need to be further adapted to large-scale production and have improved processing capacity. Summary of the Invention

[0008] In view of the problems existing in the background art, one object of this disclosure is to provide a germanium oxide processing system that can improve the purity of germanium oxide materials.

[0009] In view of the problems existing in the background art, another object of this disclosure is to provide a germanium oxide treatment system that can be adapted to the treatment of water and other slag substances contained in germanium oxide materials.

[0010] In view of the problems existing in the background art, another object of this disclosure is to provide a germanium oxide treatment system that can improve production safety and resource conservation.

[0011] Therefore, a germanium oxide processing system is provided, comprising a roasting furnace, a slag tank, and a collection module. The roasting furnace is used to: heat and dry the germanium oxide material inside in a flow-through vacuum anaerobic environment to decompose the germanium oxide material and discharge water vapor to the collection module; and to roast the germanium oxide material inside in a flow-through vacuum anaerobic environment with nitrogen introduced at a temperature at which germanium oxide does not sublimate, to decompose the germanium oxide material to release water vapor and discharge water vapor and nitrogen to the collection module, and to decompose the germanium oxide material to release slag gas and discharge slag gas and nitrogen to the slag tank. The slag tank is controlled to be connected to the roasting furnace, and is used to: controllably receive the slag gas and nitrogen gas decomposed from the germanium oxide material heated in the roasting furnace, causing the slag gas to condense into a viscous liquid in the slag tank and be collected therein, and to discharge nitrogen gas from the slag tank to the collection module. The collection module is controlled to be connected to the roasting furnace and to the slag tank. The collection module is used to: form a flow-through vacuum with the roasting furnace; receive water vapor from the decomposition of germanium oxide material by heating and drying in the roasting furnace and condense and collect the water vapor; receive water vapor and nitrogen gas from the decomposition of germanium oxide material by heating and roasting in the roasting furnace and condense and collect the water vapor; and receive nitrogen gas discharged through the slag tank when the slag gas is decomposed by heating and roasting germanium oxide material by the roasting furnace and cool the nitrogen gas.

[0012] The beneficial effects of this disclosure are as follows.

[0013] In the germanium oxide processing system disclosed herein, the purity of germanium oxide is improved due to the removal of water and other sludge (e.g., oil) contained in the germanium oxide material.

[0014] In the germanium oxide processing system disclosed herein, the calcining furnace has both drying and calcining functions. That is, drying and calcining will cover a wide temperature range. Within this temperature range, low-temperature drying is used to remove water contained in the germanium oxide material, and high-temperature calcination is used to further remove water contained in the germanium oxide material as well as other slag substances (such as oil) contained in the germanium oxide material. This enables the calcining furnace 1 to achieve functional versatility, that is, the germanium oxide processing system disclosed herein can adapt to the processing of water and other slag substances (such as oil) contained in the germanium oxide material.

[0015] In the germanium oxide treatment system disclosed herein, a slag tank is controlled to be connected to a roasting furnace, and a collection module is controlled to be connected to both the roasting furnace and the slag tank. In other words, the germanium oxide treatment system can operate in a closed flow path, which not only enables the collection of water vapor and slag during the drying and roasting process, but also improves the environmental safety of the production environment in which the germanium oxide treatment system is located (i.e., improves production safety). The collection of water vapor is conducive to recycling and thus saving resources, and the collection of slag is also conducive to its centralized disposal as waste for subsequent recycling or treatment. Attached Figure Description

[0016] Figure 1 This is a schematic plan view of the germanium oxide processing system according to the present disclosure.

[0017] Figure 2 This is a three-dimensional view of the calcination furnace in the germanium oxide treatment system.

[0018] Figure 3 yes Figure 2 Longitudinal section view.

[0019] Figure 4 It is a three-dimensional view of the movable bracket and part of the drive mechanism of the roasting furnace.

[0020] Figure 5 This is a rear view of the movable bracket and part of the drive mechanism of the roasting furnace.

[0021] Figure 6 This is a 3D view of the movable support frame of the roasting oven.

[0022] Figure 7 This is a 3D view of the slag tank of the germanium oxide treatment system.

[0023] Figure 8 yes Figure 7 Partial exploded view, in which the locking element and lifting mechanism are not shown for clarity.

[0024] Figure 9 yes Figure 7 An exploded view of the locking components of a slag tank.

[0025] Figure 10 yes Figure 9 Example of deformation of the locking parts of the slag tank.

[0026] Figure 11 yes Figure 7 An enlarged view of the lifting mechanism of the slag tank.

[0027] Figure 12 Is adopted Figure 10 A top view of a modified slag tank.

[0028] The reference numerals in the attached figures are explained as follows:

[0029] 1000 Germanium Oxide Treatment System 221 Annular Groove

[0030] 1. Calcination furnace 222 disc-shaped protrusion

[0031] L-axis 222a circumferential surface

[0032] D1 First Direction 223 Discharge Pipe

[0033] D2 Second Direction 23 Locking Part

[0034] 10. Outer shell 231. Pivot shaft

[0035] 101 inner cavity 231a shaft

[0036] 102 First end T through hole

[0037] 103 Second end 231b Annular protrusion

[0038] 104 Locking element 232 Pivot arm

[0039] 11 Heating jacket 232a First arm

[0040] 12 Cover V-hole

[0041] 121 Locking recess 232b Second arm

[0042] 13 First Exit 232c Third Arm

[0043] 14 Second outlet S-threaded hole

[0044] 15A First Control Valve 233 Bolt

[0045] 15B Second Control Valve 234 Mounting Component

[0046] 16 Nitrogen Inlet 234a First Plate

[0047] 17 Movable bracket P1 First perforation

[0048] 171 frame 234b second board

[0049] 171a First beam P2 second perforation

[0050] 171b Second beam 234c Third slab

[0051] 171c third beam 235 pin

[0052] 171d fourth beam 236 operating lever

[0053] 171e Fifth Beam 24 Lifting Mechanism

[0054] 171f Sixth Beam 241 Fixing Frame

[0055] 171g seventh beam 242 lifting rod

[0056] 171h Eighth Beam 243 Chuck

[0057] F-shaped rectangular frame 244 claws

[0058] 172 limit switch to 244a connecting arm

[0059] 173 roller 244b hook

[0060] 18 limiting components 25 sealing rings

[0061] 19 Drive mechanism 26 Connecting pipe

[0062] 191 rack 27 bottom port

[0063] 192 connecting frame 3 collection module

[0064] 192a First Connector 31 Connecting Pipe

[0065] 192b Second Connector 32 Water Jet Unit

[0066] 193 rack 321 diffuser tube

[0067] 194 Gears 33 Storage Tanks

[0068] 195 motor 34 pump

[0069] 2 slag hoppers and 4 loading trays

[0070] 21 tanks, 5 cooling modules

[0071] 211 flange 51 condenser

[0072] 211a containment tank 52 first vacuum negative pressure tank

[0073] 22 Top Cover 53 Second Vacuum Negative Pressure Tank

[0074] 54 Pressure Relief Valve Detailed Implementation

[0075] The accompanying drawings illustrate embodiments of this disclosure, and it will be understood that the disclosed embodiments are merely examples of this disclosure, which can be implemented in various forms. Therefore, the specific details disclosed herein should not be construed as limiting, but are intended only as the basis for the claims and as an illustrative basis to teach those skilled in the art how to implement this disclosure in various ways.

[0076] Reference Figure 1 The germanium oxide treatment system 1000 disclosed herein includes a roasting furnace 1, a slag tank 2, and a collection module 3.

[0077] The roasting furnace 1 is used to: heat and dry the germanium oxide material inside it in a flow-through vacuum oxygen-free environment to decompose the germanium oxide material and discharge water vapor to the collection module 3; and to heat and roast the germanium oxide material inside it in a flow-through vacuum oxygen-free environment with nitrogen introduced at a temperature at which germanium oxide does not sublimate, so as to decompose the germanium oxide material to release water vapor and discharge water vapor and nitrogen to the collection module 3, and to decompose the germanium oxide material to release slag gas and discharge slag gas and nitrogen to the slag tank 2.

[0078] The slag tank 2 is connected in a controlled manner to the roasting furnace 1. The slag tank 2 is used to: receive the slag gas and nitrogen gas produced by the decomposition of germanium oxide material by the roasting furnace 1 in a controlled manner, so that the slag gas condenses into a viscous liquid in the slag tank 2 and is collected in the slag tank 2, and so that the nitrogen gas is discharged from the slag tank 2 to the collection module 3.

[0079] The collection module 3 is controlled to be connected to the roasting furnace 1 and to the slag tank 2. The collection module 3 is used to: form a flow-through vacuum with the roasting furnace 1; receive water vapor from the germanium oxide material decomposed by the roasting furnace 1 during heating and drying, and condense and collect the water vapor; receive water vapor and nitrogen gas decomposed by the roasting furnace 1 during heating and roasting of the germanium oxide material, and condense and collect the water vapor; and receive nitrogen gas discharged through the slag tank 2 when the slag gas is decomposed by the roasting furnace 1 during heating and roasting of the germanium oxide material, and cool the nitrogen gas.

[0080] In the germanium oxide processing system 1000 and calcining furnace 1 disclosed herein, the purity of germanium oxide is improved due to the removal of water and other slag substances (e.g., oil) contained in the germanium oxide material.

[0081] In the germanium oxide processing system 1000 of this disclosure, the calcining furnace 1 has both drying and calcining functions. That is, drying and calcining will cover a wide temperature range. Within this temperature range, low-temperature drying is used to remove water contained in the germanium oxide material, and high-temperature calcination is used to further remove water contained in the germanium oxide material as well as other slag substances (such as oil) contained in the germanium oxide material. This enables the calcining furnace 1 to achieve functional versatility, that is, the germanium oxide processing system 1000 and the calcining furnace 1 of this disclosure can be adapted to the processing of water and other slag substances (such as oil) contained in the germanium oxide material.

[0082] In the germanium oxide treatment system 1000 disclosed herein, the slag tank 2 is controlled to be connected to the roasting furnace 1, and the collection module 3 is controlled to be connected to both the roasting furnace 1 and the slag tank 2. In other words, the germanium oxide treatment system 1000 can operate in a closed flow path, which not only enables the collection of water vapor and slag during the drying and roasting process (i.e., it is applicable to the treatment of slag during germanium oxide purification), but also improves the environmental safety of the production environment in which the germanium oxide treatment system 1000 is located (i.e., it improves production safety). The collection of water vapor is conducive to recycling and thus saving resources, and the collection of slag is also conducive to its centralized treatment as waste for subsequent recycling or processing.

[0083] In the germanium oxide processing system 1000 disclosed herein, in actual production, the proportion of both slag and water in the germanium oxide material is relatively small. Due to the adoption of the collection module 3 and the slag tank 2, the collection module 3 and the slag tank 2 can be adapted to the processing scale of germanium oxide material in the calcining furnace 1 (i.e., adaptable to large-scale production), thereby improving the processing capacity.

[0084] In the germanium oxide processing system 1000 disclosed herein, the germanium oxide material is germanium dioxide, but it is not limited to this. The germanium oxide material can be germanium monoxide or germanium dioxide hydrate, as long as it is used for the subsequent preparation of elemental germanium.

[0085] In the germanium oxide treatment system 1000 disclosed herein, because the aforementioned germanium oxide treatment system 1000 can operate in a closed flow path, the oxygen-free environment of the flowing vacuum avoids the oxidation of germanium (and the oxidation of germanium monoxide). The flowing oxygen-free environment is adapted to the dynamic formation and dynamic emission of water vapor generated during drying in the calcination furnace 1 and water vapor and slag gases during the calcination process. Nitrogen gas is introduced only for the calcination process, and no nitrogen gas is needed for the drying process because the drying temperature is lower than that of calcination, and it only targets the water contained in the germanium oxide material.

[0086] In the germanium oxide treatment system 1000 disclosed herein, condensation of the slag tank 2 can be achieved by providing an external cooling water jacket or by providing a circulating cooling water flow path within the peripheral wall of the tank body 21 described later in the slag tank 2.

[0087] In one example, the heating and drying temperature is below 100°C. During heating and drying, the connection between the slag tank 2 and the roasting furnace 1 is closed (i.e., the connection between the slag tank 2 and the collection module 3 is closed), while the connection between the roasting furnace 1 and the collection module 3 is open, and the nitrogen inlet 16 (described later) is closed. In one example, the heating and roasting adopts a three-stage roasting process: the temperature of the first stage of roasting is 200-250°C, the temperature of the second stage of roasting is 300-350°C, and the temperature of the third stage of roasting is 400-450°C. During the three stages of heating and roasting, the connection between the slag tank 2 and the roasting furnace 1 is open (i.e., the connection between the slag tank 2 and the collection module 3 is open), the nitrogen inlet 16 is open, and the connection between the roasting furnace 1 and the collection module 3 is closed. That is, drying and roasting do not overlap in terms of nitrogen supply or the connection between the roasting furnace 1 and the collection module 3. In an alternative embodiment, during the first stage of roasting, the connection between the slag tank 2 and the roasting furnace 1 is closed (i.e., the connection between the slag tank 2 and the collection module 3 is closed), while the connection between the roasting furnace 1 and the collection module 3 is open, and the nitrogen inlet 16 (described later) is closed. During the second and third stages of roasting, the connection between the slag tank 2 and the roasting furnace 1 is open (i.e., the connection between the slag tank 2 and the collection module 3 is open), the nitrogen inlet 16 is open, and the connection between the roasting furnace 1 and the collection module 3 is closed. That is, drying and roasting overlap in terms of nitrogen supply and the connection between the roasting furnace 1 and the collection module 3.

[0088] In addition, the heating and drying time (heating and holding time) and the calcination time (heating and holding time, for example, 20-36 hours) can be set according to the actual production (i.e. the amount of germanium oxide material processed by calcination furnace 1). After the drying and calcination are completed, calcination furnace 1 stops heating and allows the processed germanium oxide material to cool in calcination furnace 1. After cooling to room temperature, the processed germanium oxide material is taken out from calcination furnace 1.

[0089] In actual production, drying and calcination can be performed on the same germanium oxide material, that is, the dried germanium oxide material does not need to be cooled down before being removed from the furnace and can be directly calcined; or the germanium oxide material can be dried and cooled down before being removed from the furnace, and then ball-milled, sieved and loaded into the furnace for calcination. The calcination can be performed in a single state where the three stages of heating and calcination described above are connected, or in the alternative embodiment described above, the first stage of calcination is connected to the second and third stages in a different state.

[0090] Reference Figures 2 to 5 and combined Figure 1 The roasting furnace 1 includes an outer shell 10, a heating jacket 11, a cover 12, a first outlet 13, a second outlet 14, a first control valve 15A, a second control valve 15B, and a nitrogen inlet 16.

[0091] The outer casing 10 has an inner cavity 101, a first end 102 and a second end 103 opposite in axial direction L, the first end 102 being closed and the second end 103 being open. A heating sleeve 11 is disposed inside the outer casing 10, and the heating sleeve 11 heats the inner cavity 101 of the outer casing 10. A cover 12 is movably disposed at the second end 103 of the outer casing 10. The cover 12 is used to: open when germanium oxide material is placed in the inner cavity 101, and close the cover 12 to close the second end 103 after germanium oxide material is placed in the inner cavity 101. A first outlet 13 communicates with the inner cavity 101. A second outlet 14 communicates with the inner cavity 101. A first control valve 15A is disposed between the first outlet 13 and the slag tank 2 to control the communication between the first outlet 13 and the slag tank 2. A second control valve 15B is disposed between the second outlet 14 and the collection module 3 to control the communication between the second outlet 14 and the collection module 3. The nitrogen inlet 16 is connected to the inner cavity 101 and an external nitrogen source (not shown) for receiving nitrogen from the external nitrogen source.

[0092] A first control valve 15A is used to control the connection between the first outlet 13 and the slag tank 2, thereby controlling the connection between the slag tank 2 and the roasting furnace 1. The first control valve 15A can be directly installed at the first outlet 13 or directly installed at the slag tank 2.

[0093] The second control valve 15B is used to be set between the second outlet 14 and the collection module 3 to control the connection between the second outlet 14 and the collection module 3, so that the collection module 3 is controlled to be connected to the roasting furnace 1.

[0094] Of course, in an example not shown, control valves like the second control valve 15B can also be separately installed in the slag tank 2 and the collection module 3, so that the slag tank 2 is controlled to be connected to the collection module 3, that is, control valves are installed upstream and downstream of the slag tank 2.

[0095] The heating jacket 11 can be selected from any suitable type. For example, the heating jacket 11 can be a fiber electric heating jacket, which has excellent high temperature resistance and heat preservation effect. Furthermore, the fiber electric heating jacket can be a ceramic fiber electric heating jacket.

[0096] In one example, refer to Figure 2 and combined Figure 1 , Figures 3 to 5 The first outlet 13 is located at the closed first end 102 of the outer casing 10. The second outlet 14 is located at the cover 12. The nitrogen inlet 16 is located at the outer casing 10.

[0097] In one example, such as Figures 1 to 5 As shown, the axial direction L is horizontal. That is, the calcining furnace 1 is horizontal. Using a horizontal configuration, the germanium oxide material enters and exits the calcining furnace 1 after the cover 12 is opened, which reduces the difficulty of entering and exiting the calcining furnace 1 compared to a vertical configuration. Furthermore, by combining the aforementioned first outlet 13 located at the closed first end 102 of the outer shell 10 and the second outlet 14 located at the cover 12, the first outlet 13 and the second outlet 14 can communicate with the inner cavity 101 of the outer shell 10 in the axial direction L.

[0098] In one example, as shown in Figure 2, the cover 12 is provided with a plurality of locking recesses 121 distributed circumferentially; the outer shell 10 is provided with pivotally distributed locking members 104 circumferentially. The locking members 104 pivot into the locking recesses 121 respectively, locking the cover 12 and the outer shell 10 together. Similarly, as shown in Figure 2... Figure 2 As shown, the first end 102 of the outer casing 10 is closed by locking the cover 12 to the outer casing 10.

[0099] The nitrogen flow rate connected to nitrogen inlet 16 is determined based on actual production conditions, for example, 80-160 L / min.

[0100] Reference Figures 2 to 6 The calcining furnace 1 also includes a movable support 17. The movable support 17 is used to support germanium oxide material and can move in and out of the inner cavity 101 of the calcining furnace 1. The use of the movable support 17 reduces manual labor and improves work efficiency.

[0101] Furthermore, such as Figures 2 to 5 As shown, the movable bracket 17 is connected to the cover 12 so that when the movable bracket 17 enters the inner cavity 101 of the roasting furnace 1, the movable bracket 17 moves the cover 12 together and closes the second end 103 of the outer shell 10; and when the movable bracket 17 moves out of the inner cavity 101 of the roasting furnace 1, the movable bracket 17 moves the cover 12 together and opens the second end 103 of the outer shell 10. The connection between the movable bracket 17 and the cover 12 simplifies the operation of opening and closing the cover 12, reduces manual labor, and improves work efficiency.

[0102] In one example, refer to Figures 2 to 6 The germanium oxide processing system 1000 includes multiple loading trays 4, each of which is enclosed at the bottom and sides but open at the top, and each loading tray 4 is used to hold germanium oxide material. The loading of germanium oxide material on each loading tray 4 can be carried out by a separate feeding mechanism (e.g., vibratory feeder), thereby improving work efficiency and reducing labor.

[0103] The movable bracket 17 includes a frame 171, multiple limiting pairs 172, and multiple rollers 173. The multiple limiting pairs 172 are spaced apart along the axial direction L on the frame 171, each limiting pair 172 for placing a corresponding loading tray 4 on the frame 171, with each limiting pair 172 corresponding to a loading tray 4 on either side of the axial direction L. The multiple rollers 173 are mounted on the bottom of the frame 171. When the movable bracket 17 is located in the inner cavity 101 of the calcining furnace 1, the multiple rollers 173 will roll in contact with the wall of the inner cavity 101 of the calcining furnace 1. The use of the frame 171 facilitates the flow of heat from the heating jacket 11 within the inner cavity 101 of the calcining furnace 1, improving the uniformity of heating the germanium oxide material in the loading tray 4.

[0104] More specifically, refer to Figure 6Frame 171 includes a first beam 171a, a second beam 171b, a third beam 171c, a fourth beam 171d, multiple fifth beams 171e, multiple sixth beams 171f, multiple seventh beams 171g, and multiple eighth beams 171h. The first beam 171a, second beam 171b, third beam 171c, and fourth beam 171d all extend along the axial direction L. The first beam 171a and second beam 171b are opposite, parallel, and spaced apart from each other in a first direction D1 perpendicular to the axial direction L. The third beam 171c and fourth beam 171d are opposite, parallel, and spaced apart from each other in the first direction D1 perpendicular to the axial direction L. The first beam 171a and third beam 171c are opposite, parallel, and spaced apart from each other in a second direction D2 perpendicular to both the axial direction L and the first direction D1. The second beam 171b and fourth beam 171d are opposite, parallel, and spaced apart from each other in the second direction D2 perpendicular to both the axial direction L and the first direction D1. Each fifth beam 171e extends along the second direction D2 and connects to the first beam 171a and the third beam 171c. Multiple fifth beams 171e are parallel to each other and spaced apart along the axial direction L. Each sixth beam 171f extends along the second direction D2 and connects to the second beam 171b and the fourth beam 171d. Multiple sixth beams 171f are parallel to each other and spaced apart along the axial direction L. Each seventh beam 171g extends along the first direction D1 and connects to the first beam 171a and the second beam 171b. Multiple seventh beams 171g are parallel to each other and spaced apart along the axial direction L. Each eighth beam 171h extends along the first direction D1 and connects to the third beam 171c and the fourth beam 171d. Multiple eighth beams 171h are parallel to each other and spaced apart along the axial direction L. The corresponding fifth beams 171e, sixth beams 171f, seventh beams 171g, and eighth beams 171h form a rectangular frame F. A limiting pair 172 is provided on two adjacent rectangular frames F along the axial direction L. Thus, the frame 171 forms a rectangular shape with multiple compartments, thereby matching the length of the axial direction L of the calcining furnace 1 with the frame 171, and thus placing as many charging trays 4 carrying germanium oxide materials as possible within the axial direction L dimension range, thereby improving the calcining furnace 1's processing capacity for germanium oxide materials to adapt to large-scale production.

[0105] like Figure 6 As shown, the limit pair 172 is two L-shaped mirror symmetric pairs.

[0106] like Figure 6 As shown, multiple limiting pairs 172 are arranged in multiple layers along the second direction D2. Correspondingly, the loading tray 4 will also be placed in multiple layers on the frame 171, thereby further improving the processing capacity of the calcining furnace 1 for germanium oxide materials, thus further adapting to large-scale production. The number of layers can be determined based on the volume, length, and height of the inner cavity 101 of the outer shell 10 of the calcining furnace 1 and the volume of the loading tray 4.

[0107] like Figure 6As shown, multiple rollers 173 are arranged in two rows. One row of rollers 173 is installed below the third beam 171c, and the other row of rollers 173 is installed below the fourth beam 171d. This improves the stability of the frame 171 moving in and out of the inner cavity 101 of the outer shell 10 of the roasting furnace 1, as well as the stability of the frame 171 being supported within the inner cavity 101 of the outer shell 10 of the roasting furnace 1. In an alternative embodiment, a sliding pair can be used to achieve the movement of the frame 171 on the inner wall of the inner cavity 101 of the outer shell 10 of the roasting furnace 1.

[0108] Reference Figure 2 and Figure 6 A rectangular frame F at one end of the axial direction L of the frame 171 is fixedly installed on the cover 12.

[0109] Reference Figure 3 The roasting furnace 1 has a limiting member 18 in its inner cavity 101, which is used to stop the other end of the axial direction L of the frame 171.

[0110] In one example, refer to Figure 2 and Figure 3 and combined Figure 4 and Figure 5 The roasting furnace 1 also includes a drive mechanism 19. The drive mechanism 19 is connected to the movable bracket 17 to drive the movable bracket 17 and the cover 12 to reciprocate along the axial direction L. The use of the drive mechanism 19 realizes the automated operation of the movable bracket 17, eliminates manual labor, and improves work efficiency.

[0111] Specifically, such as Figure 3 As shown, the drive mechanism 19 includes a frame 191, a connecting frame 192, a rack 193, a gear 194, and a motor 195. The frame 191 supports the housing 10. The connecting frame 192 includes a first connector 192a and a second connector 192b, which form an L-shape. The first connector 192a connects to the cover 12, and the second connector 192b extends parallel to the axial direction L and is spaced apart from the movable bracket 17 in a second direction D2 perpendicular to the first axial direction L. The rack 193 extends along the axial direction L and is mounted on the second connector 192b. The motor 195 is mounted on the frame 191 and provides rotational motion. Gear 194 is connected to motor 195 to rotate under the rotational motion provided by motor 195. Gear 194 meshes with rack 193 to drive rack 193 together with connecting frame 192, cover 12 and movable bracket 17 when gear 194 rotates.

[0112] In an alternative embodiment not shown, the drive mechanism 19 may be selected from other methods besides rack and pinion transmission, such as cylinder transmission, hydraulic transmission, screw and nut slider transmission, etc.

[0113] Reference Figures 7 to 12 The slag container 2 includes a container body 21, a top cover 22, and multiple locking components 23. The container body 21 has an annular flange 211 protruding radially outward. Each locking component 23 includes a pivot shaft 231, a pivot arm 232, and a bolt 233. The pivot shaft 231 is fixed below the flange 211; the pivot arm 232 is a curved arm, one end of which is pivotally connected to the pivot shaft 231, and the other end of which has a threaded hole S; the bolt 233 is screwed into the threaded hole S, and both axial ends of the bolt 233 protrude from the pivot arm 232. Each locking element 23 is configured such that after the top cover 22 is placed on the flange 211 of the tank body 21, the pivot arm 232 pivots around the pivot arm 232 so that the bolt 233 is above the top cover 22. Then, the bolt 233 is tightened against the top cover 22 so that the bolt 233 presses against the top cover 22 and locks the tank body 21 and the top cover 22. When it is necessary to open the top cover 22, the bolt 233 is tightened in the opposite direction so that the bolt 233 is disengaged from the top cover 22. Then, the pivot arm 232 pivots around the pivot arm 232 so that the pivot arm 232 and the bolt 233 are removed from the top cover 22. Compared with the method of locking and opening the flange 211 of the tank body 21 and the top cover 22 using screws and nuts, the use of each locking element 23, including the pivot shaft 231, the pivot arm 232 and the bolt 233, improves the efficiency of locking and unlocking the flange 211 of the tank body 21 and the top cover 22.

[0114] like Figure 7 and Figure 8 As shown, the top cover 22 has an annular groove 221 for receiving and pressing the bolt 233 against it. The arrangement of the annular groove 221 and the bolt 233 also provides radial restraint on the top cover 22.

[0115] In one example, such as Figure 9 and Figure 10As shown, the pivot shaft 231 has a shaft body 231a and an annular protrusion 231b. One end of the shaft body 231a has a through hole T. The annular protrusion 231b protrudes radially outward from the other end of the shaft body 231a. Each locking member 23 also includes a mounting member 234 and a pin 235. The mounting member 234 has a first plate 234a, a second plate 234b, and a third plate 234c forming a U-shape. The first plate 234a and the second plate 234b are opposite to and spaced apart. The first plate 234a has a first through hole P1, the second plate 234b has a second through hole P2, and the third plate 234c connects one end of the first plate 234a and one end of the second plate 234b. The third plate 234c is used for fixed installation (e.g., by welding) below the flange 211 of the tank body 21. The shaft 231a passes through the first through hole P1 and the second through hole P2, the annular protrusion 231b abuts against the outside of the first plate 234a, the through hole T of the shaft 231a is located outside the second plate 234b, and the pin 235 is inserted into the second through hole P2 and restricts the shaft 231a from coming out of the second through hole P2.

[0116] In one example, such as Figure 9 and Figure 10 As shown, the pivot arm 232 has a first arm 232a, a second arm 232b, and a third arm 232c. The first arm 232a has a through hole V through which the shaft 231a passes, allowing the pivot arm 232 to pivot around the pivot axis 231. The second arm 232b is opposite to and spaced apart from the first arm 232a, and a threaded hole S is formed in the second arm 232b. The third arm 232c connects the first arm 232a and the second arm 232b. The distance between the second arm 232b and the first arm 232a is such that the pivot arm 232's pivoting around the shaft 231a does not interfere with the flange 211 of the top cover 22 and the tank body 21.

[0117] like Figure 10 As shown, each locking component 23 also includes an operating lever 236. The operating lever 236 is transversely fixed to one end of the bolt 233 along its axial direction L. The operating lever 236 is for the operator to grip, allowing the bolt 233 to be tightened toward or away from the top cover 22. Figure 9 Compared to the leverless method shown in Figure 236, Figure 10 The operating lever 236 is equivalent to directly replacing the tool for tightening bolt 233.

[0118] Reference Figure 7 , Figure 8 and Figure 11The top cover 22 has a disc-shaped protrusion 222; the slag tank 2 also includes a lifting mechanism 24. The lifting mechanism 24 includes a fixing frame 241, a lifting rod 242, a chuck 243, and a jaw 244. The fixing frame 241 is fixedly mounted (e.g., by welding) to the outer wall of the tank body 21. The lifting rod 242 is mounted on the fixing frame 241 and provides lifting movement. The chuck 243 is fixedly mounted (e.g., by screws) to the top of the lifting rod 242 and the chuck 243 presses radially against the circumferential surface 222a of the disc-shaped protrusion 222. The chuck 244 has a connecting arm 244a and a hook 244b. One end of the connecting arm 244a is fixedly connected to the top surface of the chuck 243, and the hook 244b is connected to the other end of the connecting arm 244a. The hook 244b hooks onto the circumferential surface 222a of the disc-shaped protrusion 222 on the side opposite to the chuck 243, so that the hook 244b and the chuck 243 clamp the top cover 22. During operation, when the lifting rod 242 rises, it drives the chuck 243, the chuck 244, and the top cover 22 to rise together and move away from the tank body 21; when the lifting rod 242 descends, it drives the chuck 243, the chuck 244, and the top cover 22 to descend together and move closer to the tank body 21. The lifting mechanism 24 facilitates the manual removal of the viscous liquid adhering to the inner wall of the top cover 22 after the lifting rod 242 drives the chuck 243, the jaws 244 and the top cover 22 to rise away from the tank body 21.

[0119] The lifting rod 242 is either an electro-hydraulic rod or an electro-pneumatic rod. Other methods can also be used, such as a screw-nut-slider transmission mechanism.

[0120] Based on the shape of the circumferential surface 222a of the disc-shaped protrusion 222, in one example, the claw 244 is radially fixedly connected to the circumferential surface 222a of the disc-shaped protrusion 222. The fixed connection can be achieved by, but is not limited to, welding.

[0121] like Figure 7 , Figure 11 and Figure 12 As shown, there are multiple jaws 244, which open from the top surface of the chuck 243.

[0122] Reference Figure 8 The flange 211 of the tank body 21 is provided with a receiving groove 211a. The slag tank 2 also includes a sealing ring 25, which is disposed in the receiving groove 211a. The sealing ring 25 is used to seal the top cover 22 and the tank body 21 when the top cover 22 is placed on the tank body 21. Figure 8 In the middle, there are two sealing rings 25 and two receiving grooves 211a. The receiving groove 211a located on the radial outer side is aligned with the annular groove 221 of the top cover 22.

[0123] Reference Figure 1The slag tank 2 also includes a connecting pipe 26, which is disposed in the tank body 21 and is used to connect in a controlled manner to the roasting furnace 1 and the collection module 3 to receive the slag gas and nitrogen gas decomposed from the roasting of germanium oxide material in the roasting furnace 1.

[0124] In addition, refer to Figure 1 , Figure 7 and Figure 8 The slag tank 2 also includes an openable and closable bottom port 27, which is located at the bottom of the tank body 21 and can be opened and closed. In the figure, the bottom port 27 can be closed by screwing on a cover and opened by removing the screws and taking off the cover, so that the viscous liquid inside the tank body 21 can be manually shoveled out.

[0125] exist Figure 1 In this structure, there are three slag canisters 2, which are connected sequentially. The connection between the slag canister 2 closest to the roasting furnace 1 and the roasting furnace 1 is higher than the connection between the slag canister 2 furthest from the roasting furnace 1 and the middle slag canister 2. Conversely, the connection between the slag canister 2 closest to the roasting furnace 1 and the middle slag canister 2 is lower than the connection between the slag canister 2 furthest from the roasting furnace 1 and the middle slag canister 2. This increases the flow path of the slag gas entering each slag canister 2, especially the slag canister 2 closest to the roasting furnace 1 and the middle slag canister 2, allowing the slag gas to be sufficiently cooled into a viscous liquid in the slag canister 2 closest to the roasting furnace 1 and the middle slag canister 2.

[0126] In addition, the top cover 22 of the slag tank 2 furthest from the roasting furnace 1 can be separately equipped with a discharge pipe 223, which connects the interior of the tank body 21 of the slag tank 2 and the collection module 3.

[0127] Reference Figure 1The collection module 3 includes a connecting pipe 31, a hydraulic ejector 32, a storage tank 33, and a pump 34. The slag tank 2 and the roasting furnace 1 are controlled to be connected to the connecting pipe 31. The connecting pipe 31 is connected to the hydraulic ejector 32. The hydraulic ejector 32 has a diffuser 321, which is used to create a vacuum within itself to provide the necessary flow-through vacuum for the introduction of nitrogen into the roasting furnace 1, causing controlled water vapor from the roasting furnace 1 to condense into water, and the nitrogen from the slag tank 2 and the roasting furnace 1 to cool and be discharged via the diffuser 321. The storage tank 33 is used to receive the condensed water and cooled nitrogen discharged from the diffuser 321. The pump 34 is used to supply the condensate in the storage tank 33 to the hydraulic ejector 32. Compared to using a separate vacuum device and a separate condensation device for condensing water vapor, the hydraulic ejector 32 achieves the required flow-through vacuum and water vapor condensation, greatly simplifying the number of components and operation of the collection module 3. Pump 34 supplies condensate from storage tank 33 to hydraulic ejector 32, achieving water supply to hydraulic ejector 32 and recycling of condensate formed from water vapor, thus saving resources and reducing costs. During operation, after germanium oxide material is loaded into calcining furnace 1, hydraulic ejector 32 is activated to create a vacuum in the inner cavity 101 of the outer shell 10 of calcining furnace 1. After drying and calcination are completed, hydraulic ejector 32 and pump 34 cease operation.

[0128] The water jet 32 ​​can be, but is not limited to, the W-100L water jet.

[0129] The storage tank 33 can be made of, but is not limited to, PE material. To prevent the pump 34 from running dry during initial operation, the storage tank 33 can store a certain amount of water sufficient for recycling. After collecting a certain amount of condensate, the storage tank 33 can discharge it into the sewage treatment system for treatment and recycling, thereby achieving resource conservation. In addition, the pressure (due to nitrogen) inside the storage tank 33 can be monitored so that nitrogen, along with the condensate, can be discharged into the sewage treatment system when necessary.

[0130] Pump 34 can be, but is not limited to, a multistage pump 50D8x5.

[0131] In addition, refer to Figure 1The germanium oxide processing system 1000 also includes a cooling module 5. The cooling module 5 includes a condenser 51, a first vacuum negative pressure tank 52, and a second vacuum negative pressure tank 53. The condenser 51 is connected to the calcining furnace 1 and is used to convert the water vapor discharged from the calcining furnace 1 during heating and drying into room-temperature water vapor through heat exchange. The first vacuum negative pressure tank 52 is connected to the condenser 51, and the second vacuum negative pressure tank 53 is connected to both the first vacuum negative pressure tank 52 and the collection module 3. The first vacuum negative pressure tank 52 and the second vacuum negative pressure tank 53 are used to store the room-temperature water vapor from the condenser 51. The use of the cooling module 5 increases the flow path of the water vapor to accommodate the large-scale production of the calcining furnace 1. The condenser 51 cools the water vapor to room temperature, which is then further cooled at the collection module 3. This reduces the load on the collection module 3 (specifically, the water jet 32), improves the cooling capacity of the collection module 3, and enhances the adaptability of the collection module 3 to the large-scale production of the calcining furnace 1.

[0132] In one example, condenser 51 is a horizontal glass condenser. By observing the deposits on the inner surface of the glass, it is possible to visually monitor and provide feedback on whether the drying temperature is appropriate. Compared to a vertical design, the horizontal design better ensures the connectivity between condenser 51 and the first vacuum negative pressure tank 52 and the calcining furnace 1.

[0133] Reference Figure 1 The cooling module 5 also includes a pressure relief valve 54, which is connected to the second vacuum negative pressure tank 53 for pressure relief. The pressure relief valve 54 can be connected to an external pipeline for pressure relief and nitrogen recovery. Furthermore, the first vacuum negative pressure tank 52 can also be equipped with a pressure relief valve 54, thus enabling the first vacuum negative pressure tank 52 and the second vacuum negative pressure tank 53 to operate in a backup configuration, enhancing production safety.

[0134] Furthermore, in the germanium oxide processing system 1000 disclosed herein, a control operation station (not shown) can be set up to control the operation of each component of the entire germanium oxide processing system 1000 (specifically, the operation of nitrogen gas inlet, heating jacket 11, first control valve 15A, second control valve 15B, drive mechanism 19, lifting rod 242, water jet 32, pump 34, condenser 51, pressure relief valve 54, etc.).

[0135] Several exemplary embodiments have been described in detail above, but this document is not intended to limit itself to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined to form several other combinations, which are not shown for simplicity.

Claims

1. A germanium oxide treatment system, characterized in that, The germanium oxide treatment system (1000) includes a roasting furnace (1), a slag tank (2), and a collection module (3); The roasting furnace (1) is used to: heat and dry the germanium oxide material loaded therein in a flow-through vacuum oxygen-free environment to decompose the germanium oxide material and discharge water vapor to the collection module (3), and to heat and roast the germanium oxide material loaded therein in a flow-through vacuum oxygen-free environment with nitrogen introduced at a temperature at which germanium oxide does not sublimate, so as to decompose the germanium oxide material to release water vapor and discharge water vapor and nitrogen to the collection module (3), and to decompose the germanium oxide material to release slag gas and discharge slag gas and nitrogen to the slag tank (2); The slag tank (2) is connected in a controlled manner to the roasting furnace (1). The slag tank (2) is used to: receive the slag gas and nitrogen gas decomposed by the roasting furnace (1) heating germanium oxide material in a controlled manner, so that the slag gas condenses in the slag tank (2) to form a viscous liquid and is collected in the slag tank (2), and so that the nitrogen gas is discharged from the slag tank (2) to the collection module (3). The collection module (3) is controlled to be connected to the roasting furnace (1) and to the slag tank (2). The collection module (3) is used to: form a flow-through vacuum with the roasting furnace (1), receive water vapor from the germanium oxide material decomposed by the roasting furnace (1) and condense and collect the water vapor, receive water vapor and nitrogen gas decomposed by the roasting furnace (1) and condense and collect the water vapor, and receive nitrogen gas discharged through the slag tank (2) when the germanium oxide material decomposes by the roasting furnace (1) and roasts it.

2. The germanium oxide treatment system according to claim 1, characterized in that, The roasting furnace (1) includes an outer shell (10), a heating jacket (11), a cover (12), a first outlet (13), a second outlet (14), a first control valve (15A), a second control valve (15B), and a nitrogen inlet (16). The outer shell (10) has an inner cavity (101), a first end (102) and a second end (103) opposite in the axial direction (L), the first end (102) being closed and the second end (103) being open; The heating sleeve (11) is disposed inside the outer shell (10), and the heating sleeve (11) heats the inner cavity (101) of the outer shell (10); The cover (12) is movably disposed at the second end (103) of the outer shell (10). The cover (12) is used to: when germanium oxide material is placed in the inner cavity (101), when the cover (12) is opened, and after germanium oxide material is placed in the inner cavity (101), close the cover (12) to seal the second end (103). The first outlet (13) is connected to the inner cavity (101); The second outlet (14) is connected to the inner cavity (101); The first control valve (15A) is used to be installed between the first outlet (13) and the slag tank (2) to control the connection between the first outlet (13) and the slag tank (2); The second control valve (15B) is used to be disposed between the second outlet (14) and the collection module (3) to control the connection between the second outlet (14) and the collection module (3); The nitrogen inlet (16) is connected to the inner cavity (101) and the external nitrogen source, and is used to access nitrogen supplied from the external nitrogen source.

3. The germanium oxide treatment system according to claim 2, characterized in that, The roasting oven (1) also includes a movable bracket (17). The movable bracket (17) is used to carry germanium oxide material and can move in and out of the inner cavity (101) of the roasting furnace (1).

4. The germanium oxide treatment system according to claim 3, characterized in that, The movable bracket (17) is connected to the cover (12) so that when the movable bracket (17) enters the inner cavity (101) of the roasting furnace (1), the movable bracket (17) moves the cover (12) together and closes the second end (103) of the outer shell (10) with the cover (12), and when the movable bracket (17) moves out of the inner cavity (101) of the roasting furnace (1), the movable bracket (17) moves the cover (12) together and opens the second end (103) of the outer shell (10) with the cover (12).

5. The germanium oxide treatment system according to claim 1, characterized in that, The collection module (3) includes a connecting pipe (31), a hydraulic jet (32), a storage tank (33) and a pump (34); the slag tank (2) and the roasting furnace (1) are controlled to be connected to the connecting pipe (31); Connecting pipe (31) is connected to water jet (32); The hydraulic jet (32) has a diffuser (321) and is used to create a vacuum therein to provide the required flow-through vacuum for the introduction of nitrogen into the roasting furnace (1), so that the controlled water vapor from the roasting furnace (1) condenses into water and the nitrogen from the slag tank (2) and the roasting furnace (1) is cooled and discharged via the diffuser (321); The storage tank (33) is used to receive the condensed water and cooled nitrogen discharged from the diffuser (321); The pump (34) is used to supply condensate from the storage tank (33) to the hydraulic jet (32).

6. The germanium oxide treatment system according to claim 1, characterized in that, The germanium oxide processing system (1000) also includes a cooling module (5); The cooling module (5) includes a condenser (51), a first vacuum negative pressure tank (52), and a second vacuum negative pressure tank (53). The condenser (51) is connected to the roasting furnace (1) and is used to convert the water vapor discharged from the roasting furnace (1) during heating and drying into room temperature water vapor through heat exchange; The first vacuum negative pressure tank (52) is connected to the condenser (51). The second vacuum negative pressure tank (53) is connected to the first vacuum negative pressure tank (52) and the collection module (3). The first vacuum negative pressure tank (52) and the second vacuum negative pressure tank (53) are used to store room temperature water vapor from the condenser (51).

7. The germanium oxide treatment system according to claim 6, characterized in that, The condenser (51) is a horizontal glass condenser.

8. The germanium oxide treatment system according to claim 6, characterized in that, The collection module (3) also includes a pressure relief valve (54). The pressure relief valve (54) is connected to the second vacuum negative pressure tank (53) and is used to relieve pressure in the second vacuum negative pressure tank (53).

9. The germanium oxide treatment system according to claim 1, characterized in that, There are three slag tanks (2), and the three slag tanks (2) are connected in sequence. The connection between the slag container (2) closest to the roasting furnace (1) and the roasting furnace (1) is higher than the connection between the slag container (2) furthest from the roasting furnace (1) and the middle slag container (2). The connection between the slag container (2) closest to the roasting furnace (1) and the middle slag container (2) is lower than the connection between the slag container (2) furthest from the roasting furnace (1) and the middle slag container (2).

10. The germanium oxide treatment system according to claim 1, characterized in that, Germanium oxide is germanium dioxide; The heating and drying temperature is below 100°C. During heating and drying, the connection between the slag tank (2) and the collection module (3) is closed, the connection between the roasting furnace (1) and the collection module (3) is opened, and the nitrogen inlet (16) is closed. The heating and roasting adopts a three-stage roasting process. The temperature of the first stage of roasting is 200-250°C, the temperature of the second stage of roasting is 300-350°C, and the temperature of the third stage of roasting is 400-450°C. During the three stages of heating and roasting, the connection between the slag tank (2) and the collection module (3) is opened, the nitrogen inlet (16) is opened, and the connection between the roasting furnace (1) and the collection module (3) is closed.

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