Method for extracting tungsten in black tungsten filament alkali washing waste liquid

Abstract

A method for extracting tungsten in black tungsten wire alkali washing waste liquid relates to the technical field of tungsten extraction, and comprises the following steps: S1, alkali washing: converting a black tungsten wire into a white tungsten wire through electrolysis of an alkali washing tank so as to carry out electroplating production of a tungsten wire diamond wire, and then recovering the tungsten-containing alkali washing liquid; s2, acid-base reaction: enabling the tungsten-containing alkali washing solution to react with concentrated hydrochloric acid to generate tungstic acid, so as to obtain a reaction solution A; s3, filtering: adding water into the reaction solution A to circulate, enabling the solution to be neutral, and then carrying out solid-liquid separation on the circulating solution to obtain wet tungsten oxide B; and S4, drying: evaporating moisture in the wet tungsten oxide B. According to the method for extracting the tungsten in the black tungsten wire alkali washing waste liquid, the tungsten in the black tungsten wire alkali washing waste liquid can be extracted, so that the production cost of a company is reduced, powder is periodically activated through mechanical oscillation, WOO agglomeration is broken, the ball milling quality is improved, and the method is suitable for industrial production. Powder materials can be collected without shutdown, and therefore the production efficiency is improved.

Description

Technical Field

[0001] The invention relates to the technical field of tungsten extraction, in particular to a method for extracting tungsten from black tungsten wire alkali washing waste liquid. Background Art

[0002] With the booming semiconductor industry and the widespread application of photovoltaics, the demand for hard and brittle materials is increasing, and the performance parameters of these materials after processing are gradually narrowing. This is particularly true for silicon wafers, where precision cutting is particularly demanding. Currently, the rapid development of diamond wire in China has brought diamond wire prices close to parity. As silicon wafers become thinner, and diamond wire is a core consumable for achieving this thinning, the requirements for diamond wire specifications are becoming more stringent. Leading industry scientists believe that the four main directions for future diamond wire development are: thinner wire, efficient cutting, thinner wire conservation, and low Total Thickness Variation (TTV). With these four rapid developments, the development of tungsten diamond wire has become a top priority. For diamond wire manufacturers, using black tungsten wire, which offers the best value, is the fastest way to achieve cost reduction and efficiency gains.

[0003] However, black tungsten wire itself cannot be directly used for production. It needs to undergo surface treatment to clean the graphite on the surface and convert it into white tungsten wire for production. However, during the cleaning process, some tungsten is incorporated into the alkaline washing solution. Therefore, the tungsten in the solution is extracted and converted into tungsten oxide, which can reduce the company's production costs and the discharge of tungsten-containing wastewater. To this end, we have proposed a method for extracting tungsten from the alkaline washing wastewater of black tungsten wire. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to overcome the existing defects and provide a method for extracting tungsten from the alkali washing waste liquid of black tungsten wire. The method can extract tungsten from the alkali washing waste liquid of black tungsten wire, thereby reducing the company's production costs. The method periodically activates the powder through mechanical vibration, breaks the WO3 agglomeration, thereby improving the quality of ball milling. The method can collect the powder material without stopping the machine, thereby improving production efficiency and effectively solving the problems in the background technology.

[0005] In order to achieve the above-mentioned purpose, the present invention adopts the following technical solutions: A method for extracting tungsten from black tungsten wire alkali washing wastewater comprises the following steps: S1. Alkali washing: The black tungsten wire is electrolyzed into white tungsten wire in an alkali washing tank, so as to carry out the electroplating production of tungsten wire and diamond wire, and then the tungsten-containing alkaline washing solution is recovered; S2. Acid-base reaction: reacting the tungsten-containing alkaline washing solution with concentrated hydrochloric acid to generate tungstic acid to obtain reaction solution A; S3. Filtration: Add water to the reaction solution A for circulation to make the solution neutral, and then perform solid-liquid separation on the circulating solution to obtain wet tungsten oxide B; S4. Drying: Evaporate the water in the wet tungsten oxide B, and decompose the tungstic acid into water and tungsten oxide at high temperature to obtain a bulk sample of tungsten oxide C. S5. Ball milling: The bulk sample tungsten oxide C is ball milled into powder. During the operation, an appropriate amount of water and alcohol are added to the ball mill to remove impurities from tungsten oxide C to obtain tungsten oxide D. S6, Second Drying: Evaporating the water in tungsten oxide D to obtain relatively pure tungsten oxide E; S7. Second ball milling: ball mill the tungsten oxide E using a ball milling device to obtain a powder product.

[0006] Furthermore, the ball milling device includes a ball milling jar, a PLC controller is installed on the side of the ball milling jar, a barrel is rotatably connected to the ball milling jar through a bearing, ball milling grooves are evenly opened on the inner side of the barrel, the inner side of the ball milling grooves is filled with grinding balls, and filter holes are evenly opened on the ball milling grooves, a feed pipe is connected and fixed to the top of the ball milling jar, a conveying unit is installed on the feed pipe, and a hopper is connected and fixed on the feed pipe, a driving mechanism for driving the barrel to rotate is installed on the side of the ball milling jar, a powder collection unit for collecting filtered powder in the ball milling groove is installed on the side of the ball milling jar, a ball milling auxiliary unit is installed at the bottom of the ball milling jar, and the PLC controller is electrically connected to an external power supply.

[0007] Furthermore, the conveying unit includes a spiral blade and a stepper motor, the stepper motor is installed at the end of the feeding tube, the spiral blade is fixed on the output shaft of the stepper motor, the spiral blade is arranged on the inner side of the feeding tube, and the stepper motor is electrically connected to the PLC controller.

[0008] Furthermore, the driving mechanism includes a servo motor, a worm and a worm wheel. The worm wheel is fixed at the end of the barrel. The worm is rotatably installed on the inner side of the stand of the ball mill. The worm is engaged with the worm wheel. The servo motor is installed on the side of the stand of the ball mill. The output shaft of the servo motor is fixedly connected to the end of the worm. The servo motor is electrically connected to the PLC controller.

[0009] Furthermore, the ball mill auxiliary unit includes an ultrasonic generator and a transducer. The transducer is installed at the bottom of the ball mill jar, and the ultrasonic generator is installed on the transducer. Both the ultrasonic generator and the transducer are electrically connected to the PLC controller.

[0010] Furthermore, the powder collection unit includes a dust collector and a collection pipe. The dust collector is installed on the side of the ball mill. The dust collector is connected to the inside of the barrel through the collection pipe. The end of the collection pipe is rotatably connected to the barrel. The dust collector is electrically connected to the PLC controller.

[0011] Furthermore, the powder collecting unit further comprises a rotary joint, and the end of the collecting tube is rotatably connected to the barrel via the rotary joint.

[0012] Compared with the prior art, the present invention has the following advantages: 1. It can extract tungsten from the black tungsten wire alkaline washing waste liquid, thereby reducing the company's production costs.

[0013] 2. It activates the powder periodically through mechanical vibration, breaks up WO3 agglomeration, and thus improves the quality of ball milling. It can collect the powder material without stopping the machine, thereby improving production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention; Figure 2 It is a schematic diagram of the three-dimensional side structure of the present invention; Figure 3 It is a schematic diagram of the three-dimensional first cross-sectional structure of the present invention; Figure 4 It is a schematic diagram of the second three-dimensional cross-sectional structure of the present invention.

[0015] In the figure: 1-ball mill, 2-PLC controller, 3-driving mechanism, 31-servo motor, 32-worm, 33-worm gear, 4-powder collecting unit, 41-vacuum cleaner, 42-rotary joint, 43-collecting pipe, 5-conveying unit, 51-spiral blade, 52-stepping motor, 6-ball mill auxiliary unit, 61-ultrasonic generator, 62-transducer, 7-barrel, 8-bearing, 9-feeding pipe, 10-hopper, 11-ball mill tank, 12-grinding balls, 13-filter hole. DETAILED DESCRIPTION

[0016] The present invention is explained in detail by the following examples, the purpose of which is to protect all technical improvements within the scope of the present invention.

[0017] See also Figure 1-4 This embodiment provides a technical solution: a method for extracting tungsten from black tungsten wire alkali washing wastewater, comprising the following steps: S1. Alkali washing: The black tungsten wire is electrolyzed into white tungsten wire in an alkali washing tank, so as to carry out the electroplating production of tungsten wire and diamond wire, and then the tungsten-containing alkaline washing solution is recovered; S2. Acid-base reaction: reacting the tungsten-containing alkaline washing solution with concentrated hydrochloric acid to generate tungstic acid to obtain reaction solution A; S3. Filtration: Add water to the reaction solution A for circulation to make the solution neutral, and then perform solid-liquid separation on the circulating solution to obtain wet tungsten oxide B; S4. Drying: Evaporate the water in the wet tungsten oxide B, and decompose the tungstic acid into water and tungsten oxide at high temperature to obtain a bulk sample of tungsten oxide C. S5. Ball milling: The bulk sample tungsten oxide C is ball milled into powder. During the operation, an appropriate amount of water and alcohol are added to the ball mill to remove impurities from tungsten oxide C to obtain tungsten oxide D. S6, Second Drying: Evaporating the water in tungsten oxide D to obtain relatively pure tungsten oxide E; S7. Second ball milling: ball mill the tungsten oxide E using a ball milling device to obtain a powder product.

[0018] It can extract tungsten from the black tungsten wire alkaline washing wastewater, thereby reducing the company's production costs.

[0019] The ball milling device includes a ball milling jar 1, a PLC controller 2 is installed on the side of the ball milling jar 1, a barrel 7 is rotatably connected to the ball milling jar 1 through a bearing 8, ball milling grooves 11 are evenly opened on the inner side of the barrel 7, the inner side of the ball milling grooves 11 is filled with grinding balls 12, and filter holes 13 are evenly opened on the ball milling grooves 11, a feeding pipe 9 is connected and fixed to the top of the ball milling jar 1, a conveying unit 5 is installed on the feeding pipe 9, and a hopper 10 is connected and fixed to the feeding pipe 9, a driving mechanism 3 for driving the barrel 7 to rotate is installed on the side of the ball milling jar 1, a powder collection unit 4 for collecting filtered powder in the ball milling groove 11 is installed on the side of the ball milling jar 1, a ball milling auxiliary unit 6 is installed at the bottom of the ball milling jar 1, and the PLC controller 2 is electrically connected to an external power supply.

[0020] The conveying unit 5 includes a spiral blade 51 and a stepper motor 52. The stepper motor 52 is installed at the end of the feeding tube 9. The spiral blade 51 is fixed on the output shaft of the stepper motor 52. The spiral blade 51 is arranged on the inner side of the feeding tube 9. The stepper motor 52 is electrically connected to the PLC controller 2. Tungsten oxide E is added to the hopper 10. Then, the output shaft of the stepper motor 52 drives the spiral blade 51 to rotate, and the material body is conveyed to the ball mill trough 11 through the spiral blade 51. It can evenly convey the material body, thereby reducing the burden of subsequent ball milling of the material body.

[0021] The driving mechanism 3 includes a servo motor 31, a worm 32 and a worm wheel 33. The worm wheel 33 is fixed to the end of the barrel 7. The worm 32 is rotatably installed on the inner side of the stand of the ball mill 1. The worm 32 is engaged with the worm wheel 33. The servo motor 31 is installed on the side of the stand of the ball mill 1. The output shaft of the servo motor 31 is fixedly connected to the end of the worm 32. The servo motor 31 is electrically connected to the PLC controller 2. The output shaft of the servo motor 31 drives the worm 32 to rotate. The worm 32 is engaged with the worm wheel 33. The worm wheel 33 drives the barrel 7 to rotate. The material body is ground by the grinding balls 12 in the ball mill groove 11 on the barrel 7. Then, the ground material body enters the barrel 7 through the filter hole 13. It can discharge qualified powder material while grinding, thereby improving production efficiency.

[0022] The ball milling auxiliary unit 6 includes an ultrasonic generator 61 and a transducer 62. The transducer 62 is installed at the bottom of the ball mill 1, and the ultrasonic generator 61 is installed on the transducer 62. The ultrasonic generator 61 and the transducer 62 are electrically connected to the PLC controller 2. During the ball milling process, the ultrasonic generator 61 emits an ultrasonic signal, and the transducer 62 converts the ultrasonic signal into mechanical vibration. The mechanical vibration periodically activates the powder and breaks the WO3 agglomeration, thereby improving the quality of the ball milling.

[0023] The powder collection unit 4 includes a dust collector 41 and a collection pipe 43. The dust collector 41 is installed on the side of the ball mill 1. The dust collector 41 is connected to the inside of the barrel 7 through the collection pipe 43. The end of the collection pipe 43 is rotatably connected to the barrel 7. The dust collector 41 is electrically connected to the PLC controller 2. The powder collection unit 4 also includes a rotary joint 42. The end of the collection pipe 43 is rotatably connected to the barrel 7 through the rotary joint 42. The ground material enters the inside of the barrel 7 through the filter hole 13. Then, the dust collector 41 collects the powder material in the barrel 7 through the collection pipe 43. It can collect the powder material without stopping the machine, thereby improving production efficiency.

[0024] The working principle of a ball milling device provided by the present invention is as follows: tungsten oxide E is added to the hopper 10, and then the output shaft of the stepper motor 52 drives the spiral blade 51 to rotate, and the material body is transported into the ball milling tank 11 through the spiral blade 51. Then, the output shaft of the servo motor 31 drives the worm 32 to rotate, the worm 32 engages with the worm gear 33, and the worm gear 33 drives the barrel 7 to rotate, and the grinding balls 12 in the ball milling tank 11 on the barrel 7 grind the material body. Then, the ground material body enters the barrel 7 through the filter hole 13. Then, the dust collector 41 collects the powder material body in the barrel 7 through the collection pipe 43. During the ball milling process, the ultrasonic generator 61 emits an ultrasonic signal, and the transducer 62 converts the ultrasonic signal into mechanical vibration. The mechanical vibration periodically activates the powder to break the WO3 agglomeration.

[0025] It is worth noting that the components disclosed in the above embodiments are all universal standard parts or components known to those skilled in the art, and their structures and principles are all known to those skilled in the art through technical manuals or conventional experimental methods. The PLC controller 2 controls the stepper motor 52, the servo motor 31, the ultrasonic generator 61, the transducer 62 and the vacuum cleaner 41 using methods commonly used in the prior art. The PLC controller 2, the stepper motor 52, the servo motor 31, the ultrasonic generator 61, the transducer 62 and the vacuum cleaner 41 are all products currently available on the market, and their structures and principles belong to the well-known technology. This scheme only explains the role they play in this scheme and the technical effects to be produced.

[0026] In the present invention, unless otherwise expressly specified or limited, the terms "installed," "connected," "connected," "fixed," etc. should be understood in a broad sense. For example, the terms "installed," "connected," "connected," "fixed," etc. should be understood in a broad sense. For example, the terms "connected" can refer to fixed connections, detachable connections, or integration; mechanical connections, electrical connections; direct connections, or indirect connections through an intermediate medium; internal communication between two elements, or interaction between two elements, unless otherwise expressly limited. A person skilled in the art will be able to understand the specific meanings of the above terms in the present invention based on the specific circumstances. For example, a rotational connection can refer to a rotational connection via a bearing.

[0027] The parts of the present invention that are not described in detail are prior art. Although the present invention is specifically demonstrated and introduced in conjunction with the preferred embodiments, there are many methods and approaches to implement the technical solution. The above is only a preferred embodiment of the present invention. However, those skilled in the art should understand that various changes can be made to the present invention in form and details without departing from the spirit and scope of the present invention as defined by the appended claims, and all of these are within the scope of protection of the present invention.

Claims

1. A method for extracting tungsten from black tungsten wire alkali washing wastewater, characterized by: The following steps are involved: S1. Alkali washing: The black tungsten wire is electrolyzed into white tungsten wire in an alkali washing tank, so as to carry out the electroplating production of tungsten wire and diamond wire, and then the tungsten-containing alkaline washing solution is recovered; S2. Acid-base reaction: reacting the tungsten-containing alkaline washing solution with concentrated hydrochloric acid to generate tungstic acid to obtain reaction solution A; S3. Filtration: Add water to the reaction solution A for circulation to make the solution neutral, and then perform solid-liquid separation on the circulating solution to obtain wet tungsten oxide B; S4. Drying: Evaporate the water in the wet tungsten oxide B, and decompose the tungstic acid into water and tungsten oxide at high temperature to obtain a bulk sample of tungsten oxide C; S5. Ball milling: The bulk sample tungsten oxide C is ball milled into powder. During the operation, an appropriate amount of water and alcohol are added to the ball mill to remove impurities from tungsten oxide C to obtain tungsten oxide D. S6, Second Drying: Evaporating the water in tungsten oxide D to obtain relatively pure tungsten oxide E; S7. Second ball milling: ball mill the tungsten oxide E using a ball milling device to obtain a powder product.

2. The method for extracting tungsten from black tungsten wire alkali washing wastewater according to claim 1, characterized in that: The ball milling device comprises a ball milling jar (1), a PLC controller (2) is installed on the side of the ball milling jar (1), a barrel (7) is rotatably connected to the ball milling jar (1) via a bearing (8), a ball milling groove (11) is evenly provided on the inner side of the barrel (7), the inner side of the ball milling groove (11) is filled with grinding balls (12), and filtering holes (13) are evenly provided on the ball milling groove (11), a feeding pipe (9) is connected and fixed to the top of the ball milling jar (1), a conveying unit (5) is installed on the feeding pipe (9), and a hopper (10) is connected and fixed to the feeding pipe (9), a driving mechanism (3) for driving the barrel (7) to rotate is installed on the side of the ball milling jar (1), a powder collecting unit (4) for collecting filtered powder in the ball milling groove (11) is installed on the side of the ball milling jar (1), a ball milling auxiliary unit (6) is installed at the bottom of the ball milling jar (1), and the PLC controller (2) is electrically connected to an external power supply.

3. The method for extracting tungsten from black tungsten wire alkali washing wastewater according to claim 2, characterized in that: The conveying unit (5) includes a spiral blade (51) and a stepper motor (52), wherein the stepper motor (52) is mounted at the end of the feeding tube (9), the spiral blade (51) is fixed on the output shaft of the stepper motor (52), and the spiral blade (51) is arranged on the inner side of the feeding tube (9). The stepper motor (52) is electrically connected to the PLC controller (2).

4. The method for extracting tungsten from black tungsten wire alkali washing wastewater according to claim 2, characterized in that: The driving mechanism (3) includes a servo motor (31), a worm (32) and a worm wheel (33), wherein the worm wheel (33) is fixed to the end of the barrel (7), the worm (32) is rotatably mounted on the inner side of the stand of the ball mill (1), the worm (32) is meshed with the worm wheel (33), the servo motor (31) is mounted on the side of the stand of the ball mill (1), the output shaft of the servo motor (31) is fixedly connected to the end of the worm (32), and the servo motor (31) is electrically connected to the PLC controller (2).

5. The method for extracting tungsten from black tungsten wire alkali washing wastewater according to claim 2, characterized in that: The ball mill auxiliary unit (6) includes an ultrasonic generator (61) and a transducer (62), wherein the transducer (62) is mounted on the bottom of the ball mill jar (1), and the ultrasonic generator (61) is mounted on the transducer (62). Both the ultrasonic generator (61) and the transducer (62) are electrically connected to the PLC controller (2).

6. The method for extracting tungsten from black tungsten wire alkali washing wastewater according to claim 2, characterized in that: The powder collecting unit (4) includes a dust collector (41) and a collecting pipe (43). The dust collector (41) is installed on the side of the ball mill (1). The dust collector (41) is connected to the inside of the barrel (7) through the collecting pipe (43). The end of the collecting pipe (43) is rotatably connected to the barrel (7). The dust collector (41) is electrically connected to the PLC controller (2).

7. The method for extracting tungsten from black tungsten wire alkali washing wastewater according to claim 6, characterized in that: The powder collecting unit (4) further comprises a rotary joint (42), and the end of the collecting tube (43) is rotatably connected to the barrel (7) via the rotary joint (42).

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