A device and method for recovering germanium by continuous distillation

Abstract

The invention relates to the field of germanium distillation and recovery, and in particular to a device and method for continuously distilling and recovering germanium. The device comprises: a tank body, wherein a feed port is provided on the top of the tank body. The device distills germanium waste liquid through two groups of distillation boxes and sequentially transports the waste liquid to a working distillation box through a one-way electromagnetic valve. During the distillation and heating process, a stirring rod can stir the waste liquid germanium, and a delivery water pump is used to transport the high-temperature waste liquid through the interior of the waste liquid germanium for preheating, thereby improving the utilization rate of thermal energy, improving the distillation and heating efficiency of the waste liquid in the later stage, and reducing the heat of the high-temperature waste liquid. The waste liquid is cooled for a second time by a condensation water pump and condensed and transported to a first connecting chamber and a second connecting chamber, wherein the steam is condensed, and the waste liquid is cooled, thereby improving the efficiency of the waste liquid treatment in the later stage, improving the continuous distillation efficiency of the equipment and the utilization rate of the waste liquid, and simultaneously driving multiple groups of bolts to disengage from threaded holes by rotating an external hexagonal sleeve, thereby improving the replacement efficiency of the pipeline.

Description

Technical Field

[0001] The invention relates to the field of germanium distillation recovery, and in particular to a device and a method for continuously distilling and recovering germanium. Background Art

[0002] Germanium is an important rare and dispersed metal and the most important semiconductor material besides silicon. Germanium products are widely used in the semiconductor industry, aerospace, fiber optic communications, chemical catalysts, infrared optics, solar cells, health care and medicine and other fields.

[0003] Existing germanium recovery methods are divided into two types: physical recovery and chemical recovery. The physical recovery process is generally divided into three steps: melting, separation and purification. Chemical recovery usually involves fusing germanium materials with chemical materials to produce a reaction, and then distilling the resulting substances for purification. During the recovery process, a large amount of low-concentration waste liquid is generated. This waste liquid also contains a certain amount of extractable germanium elements, and requires more refined distillation for extraction and recovery. In order to recycle germanium and avoid resource waste, the existing extraction of low-concentration germanium waste liquid still has the following defects:

[0004] 1. During the extraction process, since the amount of this low-concentration germanium waste liquid is generally large, the existing extraction method is to extract through two distillations. In the first step, the gas after the waste liquid distillation is fused and absorbed with a hydrochloric acid solution, and then sent to a distillation device for a second extraction to obtain a germanium product that meets the standards. However, during the extraction process, this method requires the extraction material to be transported back and forth between the still and the distillation device, and the material cannot be continuously distilled and extracted. Moreover, since both materials are extracted by distillation and heating, the material needs to be heated twice after transportation, which reduces the efficiency of heating and extraction.

[0005] 2. After the existing waste liquid distillation extraction, a large amount of waste liquid will still be generated. This waste liquid has no extraction value and is toxic and harmful. However, the large amount of heat generated by the internal steam heating cannot be used as domestic heat energy after natural cooling. It can only be discharged into the treatment pool for centralized treatment, resulting in a waste of heat energy. In addition, since the waste liquid cannot be chemically treated when the temperature is high, it takes a long time to cool naturally. If external force is used to cool the waste liquid before treatment, it will cause a waste of resources.

[0006] 3. A lot of chemical reagents need to be added during distillation, most of which are corrosive. Although the existing equipment has done a lot of anti-corrosion treatment, pipeline corrosion is inevitable. In order to prevent the distilled gas from leaking and causing harm to the human body, the pipeline needs to be replaced in time. Most of the existing pipelines are welded and flanged. The above traditional connection methods make the pipeline extremely inconvenient during replacement.

[0007] Therefore, it is necessary to invent a device and a method for continuously distilling and recovering germanium to solve the above problems. Summary of the Invention

[0008] The purpose of the present invention is to provide a device and method for continuously distilling and recovering germanium. Through two groups of distillation boxes, the germanium waste liquid can be continuously distilled and the high-temperature waste liquid can be circulated by a water pump to preheat the germanium waste liquid, and the waste liquid can be condensed and circulated by a condensing water pump to condense the steam, so as to solve the problems in the prior art that the equipment cannot be continuously distilled, the heating efficiency is low, the heat energy of the high-temperature waste liquid is wasted, and the natural cooling treatment efficiency is low.

[0009] To achieve the above-mentioned object, the present invention provides the following technical solution: A device for continuously distilling and recovering germanium, comprising: a tank body, a feed inlet being provided at the top of the tank body, support legs being installed at the bottom of the tank body, a first partition being installed at the top of the inner wall of the tank body, the first partition isolating the top of the tank body to form a sealed storage space, a third partition being fixedly connected at the bottom of the inner wall of the tank body, the third partition isolating the bottom of the tank body to form a sealed storage space, a second partition being provided between the first and third partitions, a distillation box being installed at the top of the second partition, and a group of distillation boxes being symmetrically installed at the top of the third partition;

[0010] A first steam pipe is connected through the top of the distillation box, and a steam heater is connected through the bottom of the first steam pipe. The steam heater is placed on one side of the tank body.

[0011] As a preferred solution of the present invention, a feed pipe is connected to the top of the distillation box, a solenoid valve is connected to one side of the feed pipe, and the solenoid valve is connected to the first partition above, so that the solenoid valve is connected to the sealed storage space formed above. A set of feed pipes and solenoid valves are also installed in the distillation box above the third partition, and are connected to the sealed storage space above. A first connecting pipe is connected to one side of the distillation box, and a first sleeve is sleeved on the first connecting pipe.

[0012] As a preferred solution of the present invention, a first connecting chamber is opened inside the first sleeve, a first pipe is connected to the top of the first connecting chamber, a second pipe is connected to the bottom of the first connecting chamber, a one-way solenoid valve is connected to the first connecting pipe on the side away from the connection with the distillation box, a distillation box is installed above the third partition, the top of the distillation box is connected to the second partition, the one-way solenoid valve is connected to the distillation box, a feeding pipe is connected to one side of the distillation box, a one-way solenoid valve is also installed in the feeding pipe, and the distillation box installed above the third partition is connected to the distillation box in the same way as the distillation box installed above the second partition, and the second pipe is connected to the first connecting chamber inside the first sleeve installed below.

[0013] As a preferred solution of the present invention, a second steam pipe is connected through the top of the distillation box, the second steam pipe is connected through the steam heater, a discharge pipe is connected through one side of the distillation box, a docking ring is fixedly connected to one side of the discharge pipe, a through hole is provided on one side of the docking ring, six groups of through holes are provided in a ring shape on one side of the docking ring, a first annular groove is provided on the inner wall of the through hole, a positioning block is slidably connected in the first annular groove, a bolt is connected through the through hole, and the bolt is fixedly connected to the positioning block.

[0014] As a preferred solution of the present invention, one side of the bolt is fixedly connected to a gear, one side of the gear is meshedly connected to a gear ring, a second annular groove is provided on the outside of the docking ring, a limiting block is slidably connected in the second annular groove, an inner wall of an outer hexagonal sleeve is fixedly connected above the limiting block, the inner wall of the outer hexagonal sleeve is fixedly connected to the gear ring, a docking tube is connected through the docking ring, a sealing gasket is sleeved on the docking tube, a fixing ring is fitted on one side of the sealing gasket, the fixing ring is fixedly connected to the docking tube, a threaded hole is provided on one side of the fixing ring, and the threaded hole is threadedly connected to the bolt.

[0015] As a preferred solution of the present invention, the fixing ring is fixedly connected to a second connecting pipe on the side away from the connection with the docking tube, a second sleeve is sleeved on the second connecting pipe, a second connecting cavity is opened inside the second sleeve, the second connecting cavity is connected to the first pipe above, a third connecting pipe is connected to the bottom of the second connecting cavity, a condensate pump is connected to the bottom of the third connecting pipe, and the condensate pump is placed on one side of the tank body.

[0016] As a preferred solution of the present invention, the third partition is isolated below the tank body to form a sealed storage space, and an insulation board is installed inside the sealed storage space, so that the insulation board forms two symmetrical sealed spaces on the left and right sides of the sealed storage space. The condensate pump is connected to the right sealed storage space formed by the insulation board through a pipeline, and a discharge pipe is connected to one side of the distillation box, and the discharge pipe is connected to the left sealed storage space formed by the insulation board. The distillation box and the distillation box above the third partition are both connected to the left sealed storage space through a discharge pipe, and a fourth connecting pipe is connected below the first connecting cavity inside the first sleeve installed on one side of the distillation box above the third partition, and the fourth connecting pipe is connected to the right sealed storage space, and a one-way solenoid valve is installed in each group of discharge pipes.

[0017] As a preferred solution of the present invention, a first circulation pipe is connected to the bottom of the left sealed storage space formed by the insulation board, a water delivery pump is connected to the bottom of the first circulation pipe, the water delivery pump is placed at the bottom of the tank body, a second circulation pipe is connected to one side of the water delivery pump, a protective rubber sleeve is sleeved on the second circulation pipe, a serpentine pipe is connected to the top of the second circulation pipe, the serpentine pipe is installed in the sealed storage space formed by isolation of the first partition board, a third circulation pipe is connected to one side of the serpentine pipe, the third circulation pipe is connected to the right sealed storage space formed by the insulation board on the side away from the serpentine pipe connection, and a discharge port is provided below the right sealed storage space formed by the insulation board.

[0018] As a preferred solution of the present invention, the second connecting pipe is connected to a finished product box on the side away from the connection with the discharge pipe, and the finished product box is placed on one side of the tank body. A protective box is installed above the second partition, and a motor is installed in the protective box. The output end of the motor is fixedly connected to the first bevel gear, and one side of the first bevel gear is meshed with the second bevel gear. The second bevel gear is meshed with three groups on one side of the first bevel gear. One side of the second bevel gear is axially connected to the third bevel gear, and one side of the third bevel gear is meshed with the fourth bevel gear. A stirring rod is rotatably connected inside the distillation box, and the stirring rod is installed in both groups of distillation boxes. A first bevel gear is also installed above the stirring rod, and one side of the first bevel gear is also meshed with a second bevel gear, and this second bevel gear is axially connected to the fourth bevel gear. The stirring rods inside the two groups of distillation boxes are connected to the other two groups of second bevel gears using this structure.

[0019] A method for recovering germanium by continuous distillation includes the above-mentioned device for recovering germanium by continuous distillation, and the specific processing steps are as follows:

[0020] Step 1: The germanium waste liquid is transported to a sealed space formed by isolation of a first partition, and then transported to a distillation box through a feed pipe, and heated by a steam heater through a first steam pipe. When the germanium waste liquid is distilled, waste liquid with no extraction and processing significance is generated. At this time, the germanium waste liquid is transported to a left sealed storage space formed by isolation of a lower insulation board through a discharge pipe;

[0021] Step 2: At this time, the boiling waste liquid is transported to the serpentine tube by the delivery water pump, and the germanium waste liquid inside the sealed space formed by the first partition is preheated. During this process, the germanium waste liquid will be cooled and transported to the right sealed storage space formed by the insulation board through the third circulation pipe. At this time, the completely cooled waste liquid is transported to the second connecting cavity by the condensation water pump and then to the first connecting cavity through the first pipeline. Finally, it returns to the right sealed storage space formed by the insulation board, and is then transported to the treatment pool for centralized treatment through the discharge port;

[0022] Step 3: At this time, the one-way solenoid valve is opened, and the steam generated by heating the germanium waste liquid passes through the first connecting pipe, which will form a condensation effect and be transported to the inside of the distillation box. At this time, the distillation box repeats the distillation effect of steps 1 and 2, and transports the extracted germanium through the second connecting pipe to the finished product box.

[0023] In the above technical solution, compared with the prior art, the technical effects and advantages provided by the present invention are as follows:

[0024] The germanium waste liquid is distilled through two groups of distillation boxes and can be transported to the inside of the working distillation box in sequence through the action of the one-way solenoid valve. During the distillation and heating process, the germanium waste liquid can be stirred by the stirring rod, and the high-temperature waste liquid is transported through the inside of the germanium waste liquid by the delivery water pump for preheating, thereby improving the utilization rate of thermal energy, so that the efficiency of the later distillation heating of the germanium waste liquid can be improved, while reducing the heat of the high-temperature waste liquid. The waste liquid is cooled for a second time by the condensing water pump and condensed and transported to the first connecting chamber and the second connecting chamber, and the steam is condensed. After the waste liquid is cooled, the efficiency of the later treatment of the waste liquid is improved, the continuous distillation efficiency of the equipment and the utilization rate of the waste liquid are improved, and by rotating the external hexagonal socket, multiple groups of bolts can be driven to disengage from the threaded holes at the same time, thereby improving the replacement efficiency of the pipeline. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments described in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0026] Figure 1It is a schematic diagram of the overall structure of the present invention;

[0027] Figure 2 It is a schematic diagram of the overall cross-sectional structure of the present invention;

[0028] Figure 3 This is a schematic cross-sectional view of the distillation box of the present invention;

[0029] Figure 4 This is a schematic diagram of the overall layout structure of the tank body of the present invention;

[0030] Figure 5 Schematic diagram of the serpentine tube structure of the present invention;

[0031] Figure 6 It is a schematic diagram of the through-hole layout structure of the present invention;

[0032] Figure 7 This is a schematic diagram of the cross-sectional structure of the second sleeve of the present invention;

[0033] Figure 8 For the present invention Figure 1 A in the middle is an enlarged structural diagram;

[0034] Figure 9 For the present invention Figure 1 The enlarged structural diagram at B in the middle;

[0035] Figure 10 For the present invention Figure 1 The enlarged structural diagram at C in the middle;

[0036] Figure 11 For the present invention Figure 2 Enlarged structural diagram at point D in the middle.

[0037] Description of reference numerals:

[0038] 1. Tank; 2. First baffle; 3. Second baffle; 4. Third baffle; 5. Distillation box; 6. First steam pipe; 7. Steam heater; 8. Feed pipe; 9. Solenoid valve; 10. First connecting pipe; 11. First sleeve; 12. First connecting chamber; 13. First pipe; 14. Second pipe; 15. Rectification box; 16. One-way solenoid valve; 17. Docking ring; 18. Through hole; 19. First annular groove; 20. Positioning block; 21. Bolt; 22. Gear; 23. Gear ring; 24. Second annular groove; 25. Stopper; 26. Hexagonal sleeve; 27. Docking sleeve; 28. Sealing gasket; 29. ​​Retaining ring; 30. Threaded hole; 31 , second connecting pipe; 32, second sleeve; 33, second connecting chamber; 34, third connecting pipe; 35, condensate pump; 36, insulation board; 37, discharge pipe; 38, fourth connecting pipe; 39, first circulation pipe; 40, water delivery pump; 41, second circulation pipe; 42, protective rubber sleeve; 43, serpentine pipe; 44, third circulation pipe; 45, second steam pipe; 46, finished product box; 47, protective box; 48, motor; 49, first bevel gear; 50, second bevel gear; 51, third bevel gear; 52, fourth bevel gear; 53, stirring rod; 54, feeding pipe; 55, discharge pipe; 56, feed port; 57, support leg; 58, discharge port. DETAILED DESCRIPTION

[0039] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0040] The present invention provides Figure 1-11 The device for continuous distillation and recovery of germanium is shown, comprising: a tank body 1, a feed inlet 56 being defined above the tank body 1, support legs 57 being mounted below the tank body 1, a first baffle 2 being mounted above the inner wall of the tank body 1, the first baffle 2 isolating the upper portion of the tank body 1 to form a sealed storage space, a third baffle 4 being fixedly connected below the inner wall of the tank body 1, the third baffle 4 isolating the lower portion of the tank body 1 to form a sealed storage space, a second baffle 3 being disposed between the first baffle 2 and the third baffle 4, a distillation box 5 being mounted above the second baffle 3, and a set of distillation boxes 5 being symmetrically mounted above the third baffle 4;

[0041] A first steam pipe 6 is connected through the top of the distillation box 5 , and a steam heater 7 is connected through the bottom of the first steam pipe 6 . The steam heater 7 is placed on one side of the tank body 1 .

[0042] In the above structure, the interior of the tank body 1 is divided into four parts by the arrangement of the first partition 2 , the second partition 3 and the third partition 4 , and the steam heater 7 can perform steam heating on the two groups of distillation boxes 5 through the first steam pipe 6 .

[0043] like Figure 1 、 Figure 2 、 Figure 9 and Figure 11 As shown, a feed pipe 8 is connected to the top of the distillation box 5, and a solenoid valve 9 is connected to one side of the feed pipe 8. The top of the solenoid valve 9 is connected to the first partition 2, so that the solenoid valve 9 is connected to the sealed storage space formed above. A set of feed pipes 8 and solenoid valves 9 are also installed in the distillation box 5 above the third partition 4, and are connected to the sealed storage space above. A first connecting pipe 10 is connected to one side of the distillation box 5, and a first sleeve 11 is sleeved on the first connecting pipe 10.

[0044] In the above structure, the germanium waste liquid in the sealed storage space formed by the isolation of the first partition plate 2 can be transported to the two groups of distillation boxes 5 through the feed pipe 8 by opening the solenoid valve 9 .

[0045] like Figure 1 、 Figure 2 、 Figure 9 and Figure 11 As shown, a first connecting chamber 12 is opened inside the first sleeve 11, a first pipe 13 is connected to the top of the first connecting chamber 12, a second pipe 14 is connected to the bottom of the first connecting chamber 12, the first connecting pipe 10 is connected to a one-way solenoid valve 16 on the side away from the connection with the distillation box 5, a distillation box 15 is installed above the third partition 4, the distillation box 15 is connected to the second partition 3 above, the one-way solenoid valve 16 is connected to the distillation box 15, a feeding pipe 54 is connected to one side of the distillation box 15, a one-way solenoid valve 16 is also installed in the feeding pipe 54, and the distillation box 5 installed above the third partition 4 is connected to the distillation box 5 in the same way as the distillation box 5 installed above the second partition 3, and the second pipe 14 is connected to the first connecting chamber 12 inside the first sleeve 11 installed below.

[0046] In the above structure, the steam inside the distillation box 5 can be transported to the inside of the distillation box 15 through the first connecting pipe 10 by opening the one-way solenoid valve 16, and due to the action of the one-way solenoid valve 16, the steam inside the distillation box 15 will not flow back.

[0047] like Figure 1 、 Figure 2 、 Figure 6 、 Figure 9 and Figure 11 As shown, a second steam pipe 45 is connected through the top of the distillation box 15, and the second steam pipe 45 is connected through the steam heater 7. A discharge pipe 55 is connected through one side of the distillation box 15, and a docking ring 17 is fixedly connected to one side of the discharge pipe 55. A through hole 18 is provided on one side of the docking ring 17. Six groups of through holes 18 are provided in a ring shape on one side of the docking ring 17. A first annular groove 19 is provided on the inner wall of the through hole 18. A positioning block 20 is slidably connected in the first annular groove 19. A bolt 21 is connected through the through hole 18, and the bolt 21 is fixedly connected to the positioning block 20.

[0048] In the above structure, the steam heater 7 can transport steam to the interior of the distillation box 15 through the second steam pipe 45 , and due to the cooperation between the positioning block 20 and the first annular groove 19 , the bolt 21 can be positioned and rotated in the through hole 18 .

[0049] like Figure 6 and Figure 9 As shown, a gear 22 is fixedly connected to one side of the bolt 21, and a gear ring 23 is meshedly connected to one side of the gear 22. A second annular groove 24 is provided on the outer side of the docking ring 17, and a limit block 25 is slidably connected in the second annular groove 24. The inner wall of the outer hexagonal sleeve 26 is fixedly connected above the limit block 25, and the inner wall of the outer hexagonal sleeve 26 is fixedly connected to the gear ring 23. A docking tube 27 is connected through the docking ring 17, and a sealing gasket 28 is sleeved on the docking tube 27. A fixing ring 29 is fitted on one side of the sealing gasket 28, and the fixing ring 29 is fixedly connected to the docking tube 27. A threaded hole 30 is provided on one side of the fixing ring 29, and the threaded hole 30 is threadedly connected to the bolt 21.

[0050] In the above structure, the outer hexagonal socket 26 is rotated by a tool, so that the outer hexagonal socket 26 drives the multiple sets of gears 22 to rotate through the gear ring 23, thereby driving the bolt 21 to move along the threaded hole 30, causing the docking sleeve 27 to move into the docking ring 17 and squeeze the sealing gasket 28, and the bolt 21 can also be disengaged from the threaded hole 30.

[0051] like Figure 1 、 Figure 2 、 Figure 6 、 Figure 7 and Figure 10 As shown, the fixing ring 29 is fixedly connected to a second connecting pipe 31 on the side away from the connection with the docking tube 27, and a second sleeve 32 is sleeved on the second connecting pipe 31. A second connecting cavity 33 is opened inside the second sleeve 32. The second connecting cavity 33 is connected to the first pipe 13 above, and the second connecting cavity 33 is connected to a third connecting pipe 34 below. The third connecting pipe 34 is connected to a condensate pump 35 below, and the condensate pump 35 is placed on one side of the tank body 1.

[0052] In the above structure, the condensate pump 35 can cool the liquid and transport it to the second connecting chamber 33 through the third connecting pipe 34, and transport it to the first connecting chamber 12 through the first pipe 13, and then transport it to another group of first sleeves 11 below through the second pipe 14, thereby completing the condensation of the steam inside the two groups of first connecting pipes 10 and the second connecting pipe 31.

[0053] like Figure 1 and Figure 2As shown, the third partition 4 is isolated below the tank body 1 to form a sealed storage space, and an insulation board 36 is installed inside the sealed storage space, so that the insulation board 36 forms two symmetrical sealed spaces on the left and right sides of the sealed storage space. The condensate pump 35 is connected to the right sealed storage space formed by the insulation board 36 through the pipeline, and a discharge pipe 37 is connected to one side of the distillation box 5. The discharge pipe 37 is connected to the left sealed storage space formed by the insulation board 36, and the distillation box 5 and the distillation box 15 above the third partition 4 are both connected to the left sealed storage space through the discharge pipe 37, and the first connecting cavity 12 inside the first sleeve 11 installed on one side of the distillation box 5 above the third partition 4 is connected to the fourth connecting pipe 38 below, and the fourth connecting pipe 38 is connected to the right sealed storage space, and a one-way solenoid valve 16 is installed in each group of discharge pipes 37.

[0054] In the above structure, the waste liquid inside the two groups of distillation boxes 5 and the distillation box 15 can be transported to the left sealed storage space formed by the insulation board 36 through the discharge pipe 37, and the first connecting cavity 12 inside the first sleeve 11 installed on one side of the distillation box 5 above the third partition board 4 can transport the internal liquid to the right sealed storage space formed by the insulation board 36.

[0055] like Figure 1 、 Figure 2 and Figure 5 As shown, a first circulation pipe 39 is connected to the bottom of the left sealed storage space formed by the heat insulation board 36, and a water delivery pump 40 is connected to the bottom of the first circulation pipe 39. The water delivery pump 40 is placed at the bottom of the tank body 1, and a second circulation pipe 41 is connected to one side of the water delivery pump 40. A protective rubber sleeve 42 is sleeved on the second circulation pipe 41, and a serpentine pipe 43 is connected to the top of the second circulation pipe 41. The serpentine pipe 43 is installed in the sealed storage space isolated by the first partition 2, and a third circulation pipe 44 is connected to one side of the serpentine pipe 43. The third circulation pipe 44 is connected to the right sealed storage space formed by the heat insulation board 36 on the side away from the connection with the serpentine pipe 43, and a discharge port 58 is provided below the right sealed storage space formed by the heat insulation board 36.

[0056] In the above structure, the hot waste liquid inside the left sealed storage space formed by the insulation board 36 can be transported to the second circulation pipe 41 and then to the serpentine pipe 43 through the water delivery pump 40, and the waste liquid inside the sealed storage space isolated by the first partition 2 is preheated. The protective rubber sleeve 42 can ensure that the heat loss of the hot waste liquid is reduced during the transportation process, and can prevent the staff from being scalded. The material of the protective rubber sleeve 42 is high-temperature resistant organic silicone HN-203, but is not limited to this material.

[0057] like Figure 1 、 Figure 2 、 Figure 3 and Figure 11As shown, the second connecting pipe 31 is connected to the side connected to the discharge pipe 55 through a finished product box 46, and the finished product box 46 is placed on one side of the tank body 1. A protective box 47 is installed above the second partition 3, and a motor 48 is installed in the protective box 47. The output end of the motor 48 is fixedly connected to a first bevel gear 49, and one side of the first bevel gear 49 is meshed with a second bevel gear 50. The second bevel gear 50 is meshed with three groups on one side of the first bevel gear 49. One side of the second bevel gear 50 is axially connected to a third bevel gear 51, and one side of the third bevel gear 51 is meshed with a fourth bevel gear 52. A stirring rod 53 is rotatably connected inside the distillation box 15, and the stirring rod 53 is installed in both groups of distillation boxes 5. A first bevel gear 49 is also installed above the stirring rod 53, and one side of the first bevel gear 49 is also meshed with a second bevel gear 50, and this second bevel gear 50 is axially connected to the fourth bevel gear 52. The stirring rods 53 inside the two groups of distillation boxes 5 are connected to the other two groups of second bevel gears 50 using this structure.

[0058] In the above structure, the extracted germanium can be transported to the finished product box 46 through the second connecting pipe 31, and the first bevel gear 49 and the second bevel gear 50 are driven to rotate by the motor 48, so that the second bevel gear 50 drives the third bevel gear 51 and the fourth bevel gear 52 to rotate, and the stirring rod 53 is driven to rotate by the fourth bevel gear 52, so that the stirring rods 53 inside the two groups of distillation boxes 5 and the distillation box 15 stir the material.

[0059] A method for recovering germanium by continuous distillation includes the above-mentioned device for recovering germanium by continuous distillation, and the specific processing steps are as follows:

[0060] Step 1: The germanium waste liquid is transported to the sealed space formed by the isolation of the first partition plate 2, and then transported to the distillation box 5 through the feed pipe 8. The steam heater 7 heats the germanium waste liquid in the distillation box 5 through the first steam pipe 6. When the germanium waste liquid is distilled, waste liquid with no extraction and processing significance is generated. At this time, the germanium waste liquid is transported to the left sealed storage space formed by the isolation of the lower insulation board 36 through the discharge pipe 37;

[0061] Step 2: At this time, the boiling waste liquid is transported to the serpentine pipe 43 by the delivery water pump 40, and the germanium waste liquid inside the sealed space isolated by the first partition 2 is preheated. During this process, the germanium waste liquid will be cooled and transported to the right sealed storage space isolated by the insulation board 36 through the third circulation pipe 44. At this time, the completely cooled waste liquid is transported to the second connecting chamber 33 by the condensation water pump 35 and then to the first connecting chamber 12 through the first pipe 13. Finally, it returns to the right sealed storage space isolated by the insulation board 36, and then is transported to the treatment tank for centralized treatment through the discharge port 58;

[0062] Step 3: At this time, the one-way solenoid valve 16 is opened, and the steam generated by the heating of the germanium waste liquid passes through the first connecting pipe 10, which will form a condensation effect and be transported to the inside of the distillation box 15. At this time, the distillation box 15 repeats the distillation effect of steps 1 and 2, and transports the extracted germanium to the finished product box 46 through the second connecting pipe 31.

[0063] The specific embodiments of the present invention are as follows: Figure 1-11As shown: the germanium waste liquid is transported to the sealed space formed by the isolation of the first partition 2 through the feed port 56. At this time, the solenoid valve 9 is opened to transport the germanium waste liquid to the two groups of distillation boxes 5 through the feed pipe 8. At this time, the first bevel gear 49 is driven to rotate by the motor 48, and the first bevel gear 49 drives the second bevel gear 50 and the third bevel gear 51 to rotate, so that the third bevel gear 51 drives the fourth bevel gear 52 to rotate and drives the stirring rod 53 to rotate, so that the three groups of stirring rods 53 stir the germanium waste liquid at the same time. At this time, steam heating is performed on one group of distillation boxes 5 through the first steam pipe 6. After the distillation inside the distillation box 5 is completed, steam heating is performed on the other group of distillation boxes 5. At this time, there will be high-temperature waste liquid with no extraction value inside the distillation box 5. At this time, it is transported to the left sealed storage space formed by the insulation board 36 through the discharge pipe 37. At this time, the delivery water pump 40 transports the high-temperature waste liquid to the second circulation pipe 41 and then to the serpentine pipe 43 through the first circulation pipe 39. Due to the shape of the serpentine pipe 43, the high-temperature waste liquid needs to be transported for a period of time in the sealed space formed by the first partition 2. At this time, the high temperature in the waste liquid can preheat the germanium waste liquid inside the sealed space formed by the first partition 2, so that the heating efficiency is improved when it enters the distillation box 5 next time, and the waste liquid is transported to the right sealed storage space formed by the insulation board 36 through the third circulation pipe 44. At this time, the waste liquid is cooled and condensed by the condensation water pump 35, and is connected to the third The pipe 34 is transported to the second connecting chamber 33 and passes through the first connecting chamber 12 of the first pipe 13 above, and then enters the first pipe 13 set below through the second pipe 14, and finally returns to the right sealed storage space formed by the insulation board 36 through the fourth connecting pipe 38, completing a cycle and completing the condensation work of the first connecting pipe 10 and the second connecting pipe 31. At this time, the one-way solenoid valve 16 is opened to allow the first connecting pipe 10 to condense the steam inside the distillation box 5 and transport it to the distillation box 15. At this time, the chemical agent is added to the distillation box 15 through the feeding pipe 54, and then the steam heater 7 is transported to the distillation box 15 for distillation through the second steam pipe 45. Finally, the steam is transported to the distillation box 15 through the second connecting pipe 31. The germanium vapor inside the distillation box 15 is condensed and transported to the finished product box 46. The distillation time difference between the two groups of distillation boxes 5 can make the distillation box 15 work differently. Due to the function of the one-way solenoid valve 16, the distillation box 15 can continuously add germanium waste liquid to the interior during operation. By preheating and stirring the germanium waste liquid and recycling the high-temperature waste liquid, the equipment can continue to distill and improve the efficiency of distillation heating. By cooling and condensing the waste liquid and circulating it, the steam inside the two groups of first connecting pipes 10 and second connecting pipes 31 is condensed, which can improve the utilization rate of the waste liquid and quickly cool the waste liquid, so that the waste liquid can be quickly processed, thereby improving the continuity of the distillation of the equipment.

[0064] 2. By using a tool to rotate the outer hexagonal sleeve 26, the limit block 25 slides along the second annular groove 24, so that the outer hexagonal sleeve 26 drives the gear ring 23 to rotate, the gear ring 23 drives the gear 22 to rotate, the gear 22 drives the bolt 21 to rotate, and the bolt 21 drives the positioning block 20 to slide in the first annular groove 19, so that the bolt 21 is disengaged from the threaded hole 30, and the docking sleeve 27 is disengaged from the docking ring 17. Due to the fit between the docking sleeve 27 and the docking ring 17, the sealing gasket 28 is squeezed to ensure the sealing of the docking. In this way, multiple groups of bolts 21 can be driven to be disassembled and installed at the same time, thereby improving the replacement efficiency of the second connecting pipe 31 and ensuring the safety of equipment operation.

[0065] The above description is merely illustrative of certain exemplary embodiments of the present invention. It goes without saying that those skilled in the art will be able to modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and description are illustrative in nature and should not be construed as limiting the scope of protection of the claims.

Claims

1. A device for continuous distillation recovery of germanium, comprising: A tank body (1), characterized in that: a feed port (56) is provided on the top of the tank body (1), a support leg (57) is installed below the tank body (1), a first partition (2) is installed above the inner wall of the tank body (1), the first partition (2) isolates the top of the tank body (1) to form a sealed storage space, a third partition (4) is fixedly connected to the bottom of the inner wall of the tank body (1), the third partition (4) isolates the bottom of the tank body (1) to form a sealed storage space, a second partition (3) is provided between the first partition (2) and the third partition (4), a distillation box (5) is installed above the second partition (3), and a group of distillation boxes (5) are also symmetrically installed above the third partition (4); A first steam pipe (6) is connected through the top of the distillation box (5), and a steam heater (7) is connected through the bottom of the first steam pipe (6). The steam heater (7) is placed on one side of the tank body (1); A feed pipe (8) is connected through the top of the distillation box (5), and a solenoid valve (9) is connected through one side of the feed pipe (8). The solenoid valve (9) is connected through the top of the first partition (2), so that the solenoid valve (9) is connected through the sealed storage space formed above. The feed pipe (8) and the solenoid valve (9) are also installed in a set on the distillation box (5) above the third partition (4), and are connected through the sealed storage space above. A first connecting pipe (10) is connected through one side of the distillation box (5), and a first sleeve (11) is sleeved on the first connecting pipe (10); A first connecting chamber (12) is provided inside the first sleeve (11), a first pipe (13) is connected through the top of the first connecting chamber (12), a second pipe (14) is connected through the bottom of the first connecting chamber (12), a one-way solenoid valve (16) is connected through the first connecting pipe (10) on the side away from the connection with the distillation box (5), a rectification box (15) is installed above the third partition (4), and the rectification box (15) is connected through the top with the second partition (3). The one-way solenoid valve (16) is connected to the distillation box (15), and a feeding pipe (54) is connected to one side of the distillation box (15). The one-way solenoid valve (16) is also installed in the feeding pipe (54). The distillation box (5) installed above the third partition (4) is connected to the distillation box (5) in the same manner as the distillation box (5) installed above the second partition (3). The second pipe (14) is connected to the first connecting cavity (12) inside the first sleeve (11) installed below. The high-temperature waste liquid is transported through the interior of the germanium waste liquid by a water delivery pump (40) for preheating; The waste liquid is cooled for a second time and condensed and transported by the condensate pump (35), and the steam is condensed to cool the waste liquid.

2. A device for recovering germanium by continuous distillation according to claim 1, characterized in that: A second steam pipe (45) is connected through the top of the distillation box (15), and the second steam pipe (45) is connected through the steam heater (7). A discharge pipe (55) is connected through one side of the distillation box (15), and a docking ring (17) is fixedly connected to one side of the discharge pipe (55). A through hole (18) is provided on one side of the docking ring (17). Six groups of through holes (18) are provided in a ring shape on one side of the docking ring (17). A first annular groove (19) is provided on the inner wall of the through hole (18). A positioning block (20) is slidably connected in the first annular groove (19). A bolt (21) is connected through the through hole (18), and the bolt (21) is fixedly connected to the positioning block (20).

3. A device for recovering germanium by continuous distillation according to claim 2, characterized in that: One side of the bolt (21) is fixedly connected to a gear (22), and one side of the gear (22) is meshedly connected to a gear ring (23). A second annular groove (24) is provided on the outer side of the docking ring (17), and a limit block (25) is slidably connected in the second annular groove (24). The upper side of the limit block (25) is fixedly connected to the inner wall of an outer hexagonal sleeve (26), and the inner wall of the outer hexagonal sleeve (26) is fixedly connected to the gear ring (23). A docking tube (27) is connected through the docking ring (17), and a sealing gasket (28) is sleeved on the docking tube (27). One side of the sealing gasket (28) is fitted with a fixing ring (29), and the fixing ring (29) is fixedly connected to the docking tube (27). A threaded hole (30) is provided on one side of the fixing ring (29), and the threaded hole (30) is threadedly connected to the bolt (21).

4. A device for recovering germanium by continuous distillation according to claim 3, characterized in that: The fixing ring (29) is fixedly connected to a second connecting pipe (31) on a side away from the connection with the docking sleeve (27); a second sleeve (32) is sleeved on the second connecting pipe (31); a second connecting cavity (33) is provided inside the second sleeve (32); the upper portion of the second connecting cavity (33) is connected to the first pipe (13); the lower portion of the second connecting cavity (33) is connected to a third connecting pipe (34); the lower portion of the third connecting pipe (34) is connected to a condensate pump (35); and the condensate pump (35) is placed on one side of the tank body (1).

5. A device for recovering germanium by continuous distillation according to claim 4, characterized in that: The third partition (4) is isolated below the tank body (1) to form a sealed storage space, and an insulation board (36) is installed inside the sealed storage space, so that the insulation board (36) forms two symmetrical sealed spaces on the left and right sides of the sealed storage space. The condensate pump (35) is connected to the right sealed storage space formed by the insulation board (36) through a pipeline. A discharge pipe (37) is connected to one side of the distillation box (5). The discharge pipe (37) is connected to the left sealed storage space formed by the insulation board (36). The distillation box (5) and the rectification box (15) above the third partition (4) are both connected to the left sealed storage space through the discharge pipe (37). The first connecting cavity (12) inside the first sleeve (11) installed on one side of the distillation box (5) above the third partition (4) is connected to the bottom through a fourth connecting pipe (38). The fourth connecting pipe (38) is connected to the right sealed storage space, and a one-way solenoid valve (16) is installed in each group of discharge pipes (37).

6. A device for continuous distillation recovery of germanium according to claim 5, characterized in that: A first circulation pipe (39) is connected to the bottom of the left sealed storage space formed by the heat insulation board (36), and a water delivery pump (40) is connected to the bottom of the first circulation pipe (39). The water delivery pump (40) is placed at the bottom of the tank body (1). A second circulation pipe (41) is connected to one side of the water delivery pump (40). A protective rubber sleeve (42) is sleeved on the second circulation pipe (41). A serpentine pipe (43) is connected to the top of the second circulation pipe (41). The serpentine pipe (43) is installed in the sealed storage space isolated by the first partition board (2). A third circulation pipe (44) is connected to one side of the serpentine pipe (43). The third circulation pipe (44) is connected to the right sealed storage space formed by the heat insulation board (36) on the side away from the serpentine pipe (43). A discharge port (58) is provided below the right sealed storage space formed by the heat insulation board (36).

7. A device for continuous distillation recovery of germanium according to claim 4, characterized in that: The second connecting pipe (31) is connected to a finished product box (46) on the side away from the discharge pipe (55), and the finished product box (46) is placed on one side of the tank body (1). A protective box (47) is installed above the second partition (3), and a motor (48) is installed in the protective box (47). The output end of the motor (48) is fixedly connected to a first bevel gear (49), and one side of the first bevel gear (49) is meshed with a second bevel gear (50). The second bevel gear (50) is meshed with three groups of rings on one side of the first bevel gear (49), and one side of the second bevel gear (50) is axially connected to a third bevel gear (49). Gear (51), one side of the third bevel gear (51) is meshed with a fourth bevel gear (52), and a stirring rod (53) is rotatably connected inside the distillation box (15). The stirring rod (53) is installed in both groups of distillation boxes (5). A first bevel gear (49) is also installed above the stirring rod (53). One side of the first bevel gear (49) is also meshed with a second bevel gear (50), and the second bevel gear (50) is axially connected to the fourth bevel gear (52). The stirring rods (53) inside the two groups of distillation boxes (5) are connected to the other two groups of second bevel gears (50) using this structure.

8. A method for recovering germanium by continuous distillation, comprising the apparatus for recovering germanium by continuous distillation according to claim 7, characterized in that: The processing steps are as follows: Step 1: The germanium waste liquid is transported to a sealed space formed by isolation by the first partition (2), and then the germanium waste liquid is transported to the distillation box (5) through the feed pipe (8), and the steam heater (7) heats the germanium waste liquid in the distillation box (5) through the first steam pipe (6). When the germanium waste liquid is distilled, waste liquid with no extraction and processing significance is generated. At this time, the germanium waste liquid is transported to the left sealed storage space formed by isolation by the lower insulation board (36) through the discharge pipe (37); Step 2: At this time, the hot waste liquid is transported to the serpentine tube (43) through the water delivery pump (40), and the germanium waste liquid inside the sealed space isolated by the first partition (2) is preheated. During this process, the germanium waste liquid will be cooled and transported to the right sealed storage space isolated by the heat insulation board (36) through the third circulation pipe (44). At this time, the completely cooled waste liquid is transported to the second connecting chamber (33) through the condensation water pump (35) and then transported to the first connecting chamber (12) through the first pipe (13). Finally, it returns to the right sealed storage space isolated by the heat insulation board (36) and is then transported to the treatment pool for centralized treatment through the discharge port (58); Step 3: At this time, the one-way solenoid valve (16) is opened, and the steam generated by the heating of the germanium waste liquid passes through the first connecting pipe (10), forming a condensation effect and being transported to the inside of the distillation box (15). At this time, the distillation box (15) repeats the distillation effect of steps 1 and 2, and transports the extracted germanium through the second connecting pipe (31) to the finished product box (46).

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