CN219526748U - Silver-containing etching waste liquid recycling silver recovery device - Google Patents
Silver-containing etching waste liquid recycling silver recovery device Download PDFInfo
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- CN219526748U CN219526748U CN202320462593.8U CN202320462593U CN219526748U CN 219526748 U CN219526748 U CN 219526748U CN 202320462593 U CN202320462593 U CN 202320462593U CN 219526748 U CN219526748 U CN 219526748U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The utility model relates to a device for recycling silver-containing etching waste liquid, which is characterized in that: comprises a silver etching waste liquid storage tank, a precipitation tank, a first dosing tank, a first centrifugal machine, a reduction reaction tank, a second centrifugal machine, a cleaning tank, a high-temperature casting furnace, a cooling tank and an electrolytic tank which are connected in sequence; the sedimentation tank top is connected with first dosing tank, is connected with the solid dosing tank and the liquid dosing tank that respectively arrange alone on the reduction reaction tank, and the waste liquid collecting tank is connected to the liquid discharge port of first centrifuge, and the waste gas treatment tower is connected to the gas discharge port of electrolysis trough, adds reducing iron powder in the solid dosing tank, adds dilute sulfuric acid in the liquid dosing tank, adds the additive in the first dosing tank. Is a treatment device for silver etching waste liquid generated by silver etching technology in the semiconductor industry.
Description
Technical Field
The utility model relates to the technical field of hazardous waste treatment, in particular to a device for recycling silver-containing etching waste liquid.
Background
The silver series products are widely applied to the fields of chemical industry, electronic plating, materials, industrial catalysis and the like. Various silver-containing waste solutions are generated in various industries involving silver, such as directly discharging the silver-containing waste solution into the environment, which not only pollutes the environment, but also causes waste of silver resources. Therefore, the recovery of silver from the silver-containing waste liquid has important significance.
In recent years, with the rise of the semiconductor industry, the yield of waste etching liquid containing noble metals is also increased. In which silver etchant yields have increased year by year. Common system methods for silver etching solutions include nitric acid systems, sodium persulfate-sulfuric acid systems, hydrogen peroxide-sulfuric acid systems, and the like, and the resulting etching solution liquid contains more noble metal silver and also contains more acid. If the waste liquid is directly discharged into the environment, on one hand, the price of the silver-containing reagent is low, and the silver ions are directly discarded to cause huge waste, and on the other hand, after the silver ions reenter the water circulation system of the river, tap water is possibly polluted, so that personal safety and health are endangered.
Disclosure of Invention
In order to solve the problems in the background technology, the utility model provides a device for recycling silver from silver-containing etching waste liquid, which is a treatment device for silver etching waste liquid generated by silver etching technology in the semiconductor industry.
In order to solve the problems, the utility model adopts the following technical scheme: the utility model provides a silver-containing etching waste liquid recycling device that retrieves silver which characterized in that: comprises a silver etching waste liquid storage tank, a precipitation tank, a first dosing tank, a first centrifugal machine, a reduction reaction tank, a second centrifugal machine, a cleaning tank, a high-temperature casting furnace, a cooling tank and an electrolytic tank which are connected in sequence; the sedimentation tank top is connected with first dosing tank, is connected with the solid dosing tank and the liquid dosing tank that respectively arrange alone on the reduction reaction tank, and the waste liquid collecting tank is connected to the liquid discharge port of first centrifuge, and the waste gas treatment tower is connected to the gas discharge port of electrolysis trough, adds reducing iron powder in the solid dosing tank, adds dilute sulfuric acid in the liquid dosing tank, adds the additive in the first dosing tank.
Further, stirring devices are arranged in the silver etching waste liquid storage tank and the precipitation tank.
Further, a washing liquid adding tank is arranged in the washing tank, and an adding device, a stirring device and a solid-liquid separation device are arranged in the washing tank.
Still further, silver etching waste liquid holding tank be linked together through conveying line and precipitation tank, precipitation tank bottom links to each other through pipeline and first centrifuge, first centrifuge's discharge gate passes through the pipeline and is connected with reduction reaction tank feed inlet, the solid is conveyed to reduction reaction tank from first centrifuge's solid discharge gate, reduction reaction tank's discharge gate is connected through pipeline and second centrifuge feed inlet, the second centrifuge discharge gate is connected through pipeline and washing tank, the discharge gate of washing tank is connected with high temperature casting furnace feed inlet, washing tank discharge gate and high temperature casting furnace feed inlet are connected through the conveyer belt, high temperature casting furnace discharge gate is connected through conveyer belt and cooling tank, the cooling tank discharge gate passes through the conveyer belt and links to each other with the electrolysis trough.
Still further, a 50 ℃ circulating liquid device is arranged at the lower part of the cleaning tank 7.
Still further, set up the exhaust hood above the electrolysis trough, exhaust hood is connected with the exhaust-gas treatment tower.
The utility model has the beneficial effects that: the utility model provides a device for recycling silver-containing etching waste liquid, which is a treatment device for silver etching waste liquid generated by silver etching technology in the semiconductor industry. Firstly, silver chloride sediment is generated by adopting a chemical precipitation method, and then solid-liquid separation is carried out in a centrifugal way.
Drawings
The utility model will be further described with reference to the drawings and examples.
Fig. 1 is a structural diagram of the present utility model.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The utility model provides a device for recycling silver-containing etching waste liquid, which is a treatment device for silver etching waste liquid generated by silver etching technology in the semiconductor industry. Firstly, silver chloride sediment is generated by adopting a chemical precipitation method, and then solid-liquid separation is carried out in a centrifugal way.
And reducing the generated silver chloride solid precipitate by using iron powder, further washing the obtained crude silver, removing impurities at high temperature, casting ingots, and finally further purifying the crude silver by electrolysis. The method can recycle the noble metal silver in the silver etching solution by using the chemical precipitation, reduction and electrolysis process methods, and obtain high-purity silver metal.
Specifically, the technical scheme of the utility model comprises the following steps: the device for recycling silver-containing etching waste liquid comprises a silver etching waste liquid storage tank 1, a precipitation tank 2, a first dosing tank 3, a first centrifugal machine 4, a reduction reaction tank 5, a second centrifugal machine 6, a cleaning tank 7, a high-temperature casting furnace 8, a cooling tank 9 and an electrolytic tank 10.
The silver etching waste liquid storage tank 1 is communicated with the precipitation tank 2 through a conveying pipeline. Valves are respectively arranged on all the conveying pipelines. A first dosing tank 3 is arranged above the sedimentation tank 2, and an electromagnetic valve is preferably arranged on a connecting pipeline of the first dosing tank and the sedimentation tank. The bottom of the precipitation tank 2 is connected with a first centrifugal machine 4 through a pipeline, a discharge hole of the first centrifugal machine 4 is connected with a feed inlet of a reduction reaction tank 5 through a pipeline, and two independent second and third dosing tanks, namely a solid dosing tank 5a and a liquid dosing tank 5b, are arranged on the reduction reaction tank 5. The discharge gate of reduction reaction tank 5 is connected through the pipeline with the feed inlet of second centrifuge 6, and the discharge gate of second centrifuge 6 is connected through pipeline and washing tank 7, and the discharge gate of washing tank 7 is connected with the feed inlet of high temperature casting furnace 8, and the discharge gate of high temperature casting furnace 8 communicates with each other through conveyer belt and cooling tank 9, and the discharge gate of cooling tank 9 passes through conveyer belt and electrolysis (cell anode) groove 10 and links to each other.
Further stated, the silver etching waste liquid storage (storage) tank 1 is communicated with the precipitation tank 2 through a conveying pipeline, a first dosing tank 3 is arranged above the precipitation tank 2, the bottom of the precipitation tank 2 is connected with the first centrifugal machine 4 through a pipeline, electromagnetic valves are respectively arranged on each connected conveying pipeline, the volume of the waste liquid of the (silver etching waste liquid) storage tank 1 flowing into the precipitation tank 2 can be controlled, and accordingly the addition according to the calculated proportion is achieved, and stirring devices are arranged in the (silver etching waste liquid) storage tank 1 and the precipitation tank 2.
Still further, the additive of the first dosing tank 3 is mainly silver ion precipitant (sodium chloride), so that silver ions in the etching solution generate precipitate silver chloride.
Ag + +Cl - AgCl (precipitation)
Still further describing, the reaction solution after silver ion precipitation is pumped into the first centrifugal machine 4 for solid-liquid separation, the solid is conveyed to the reduction reaction tank 5 from the solid discharge port of the first centrifugal machine 4, the liquid is discharged from the first centrifugal machine 4 and is singly collected into the waste liquid collecting tank 11, and the discharged reaches the standard after advanced treatment.
Further, after silver chloride precipitation was carried out in the reduction reaction tank 5, a reducing iron powder was added from the upper solid charging tank 5a, and an iron powder having a mesh of more than 100 mesh was selected, and at the same time, a proper amount of 10% dilute sulfuric acid was added from the liquid charging tank 5b, and the mixture was allowed to stand for 8 hours without stirring.
2AgCl+Fe→2Ag+FeCl 2
After the reaction is completed, carrying out solid-liquid separation on the silver powder, wherein the silver powder containing impurities is obtained through solid. The liquid is collected independently, and can be recycled after test and preparation.
Further describing, the crude silver containing impurities obtained after solid-liquid separation is cleaned and decontaminated, the cleaning solution in the cleaning tank 7 is 5% dilute sulfuric acid, an adding device, a stirring device and a solid-liquid separation device are arranged in the cleaning tank (cleaning tank 7), the temperature of the cleaning solution is ensured to be stable at about 50 ℃ (a 50 ℃ circulating liquid device is arranged at the lower part of the cleaning tank 7), and the residual iron powder in the crude silver is mainly removed.
Further to explain, the discharge opening of the cleaning tank 7 and the feed opening of the high temperature casting furnace 8 are connected through a conveyor belt, the crude silver is subjected to impurity removal and recasting in the high temperature casting furnace 8, and the new shape of the casting is equivalent to that of an electrolytic (cell anode) tank 10.
Further, the re-cast crude silver is cooled by the cooling tank 9, and the cooling water is tap water for recycling.
As a further illustration, the recast crude silver is transferred to the electrolytic cell 10 with the anode as the anode, the cathode being a stainless steel plate, and the electrolyte being AgNO 3 、HNO 3 、KNO 3 The mixed solution (to improve the conductivity of the electrolyte and adjust the pH of the electrolyte, an appropriate amount of HNO is added respectively 3 And KNO 3 )。
Anode end reaction: ag-e - →Ag + ；
Cathode end reaction: ag (silver) + +e - →Ag
Further describing, the specific operation process of silver electrolysis is as follows: the anode silver plate is hung on the anode rod, the stainless steel plate is hung on the cathode rod, the anode and the cathode are respectively connected to the anode and the cathode of the direct current rectifier, and the power supply is connected to start electrolysis. The silver simple substance in the anode silver plate loses electrons and becomes silver ions to enter the electrolyte, and the silver ions at the cathode obtain electrons and become silver simple substances to be separated out on the cathode stainless steel plate. The stirring rod is adopted to make reciprocating motion between the anode and the cathode, so that electrolytic silver powder precipitated on the cathode stainless steel plate is scraped off, and meanwhile, short circuit between the anode and the cathode is avoided. When the temperature of the electrolyte is higher, the solution can generate acid gas, and the acid gas is collected by an exhaust hood on the electrolytic tank 10 and then directly connected into the waste gas treatment tower 12 for treatment.
The utility model effectively recovers silver in the silver etching waste liquid, and is a device capable of recycling silver for the silver-containing etching waste liquid. And precipitating silver ions in the etching solution by a precipitation method, reducing silver salt to obtain crude silver containing impurities, further removing impurities by washing, and finally obtaining the metal silver with higher purity by high-temperature casting and electrolytic purification. The three wastes of the system are effectively collected and treated in the whole reaction process, so as to achieve the aim of safely and efficiently recovering the metallic silver.
The utility model provides a device for effectively recycling silver in silver etching waste liquid, which can recycle silver in silver etching waste liquid. And precipitating silver ions in the etching solution by a precipitation method, reducing silver salt to obtain crude silver containing impurities, further removing impurities by washing, and finally obtaining the metal silver with higher purity by high-temperature casting and electrolytic purification. The three wastes of the system are effectively collected and treated in the whole reaction process, so as to achieve the aim of safely and efficiently recovering the metallic silver.
The process for recycling silver from the silver-containing etching waste liquid based on the device comprises the following steps of:
1) Chemical precipitation: the silver etching waste liquid storage (storage) tank 1 is pumped into the precipitation tank 2 through an electromagnetic valve, silver ion precipitant (sodium chloride) is added through the first dosing tank 3 according to the amount of the pumped silver etching waste liquid, and the built-in stirrer is started in the process of adding the waste liquid (silver etching waste liquid) storage tank 1 and the precipitation tank 2. Silver ions in the sedimentation tank generate sediment silver chloride:
ag++ Cl- →AgCl (precipitate)
2) And (3) centrifugal solid-liquid separation: the reaction solution after silver ion precipitation is pumped into a first centrifugal machine 4 for solid-liquid separation, the solid is conveyed to a reduction reaction tank 5 from a solid discharge port of the first centrifugal machine 4, and the liquid is discharged from the first centrifugal machine 4 and is separately collected into a waste liquid collecting tank 11 for disposal.
3) And (3) reduction: the solid after the treatment of the step 2) is conveyed into a reduction (reaction) tank 5, the reducing iron powder is added from a solid dosing tank 5a above, the iron powder with the mesh number of more than 100 meshes is selected, meanwhile, a proper amount of 10% dilute sulfuric acid is added from a liquid dosing tank 5b, and the mixture is kept stand for 8 hours, so that stirring is not started.
2AgCl+Fe→2Ag+FeCl 2
After the reaction is completed, carrying out solid-liquid separation on the silver powder, wherein the silver powder containing impurities is obtained through solid. The liquid is collected independently, and can be recycled after test and preparation.
4) High temperature impurity removal casting: the discharge port of the cleaning tank 7 is connected with the feed port of the high-temperature casting furnace 8 through a conveyor belt, the crude silver is subjected to impurity removal and re-casting in the high-temperature casting furnace 8, and the new shape of the casting is equivalent to that of an electrolysis (cell anode) tank 10.
5) Electrolytic purification: the recast crude silver is transferred to the electrolytic cell 10 with the anode as anode, the cathode being a stainless steel plate, and the electrolyte being AgNO 3 、HNO 3 、KNO 3 The mixed solution (to improve the conductivity of the electrolyte and adjust the pH of the electrolyte, an appropriate amount of HNO is added respectively 3 And KNO 3 )。
Anode end reaction: ag-e - →Ag + ；
Cathode end reaction: ag (silver) + +e - →Ag
6) Waste collection: the harmful gases produced by electrolysis are treated by an exhaust gas treatment system (i.e., an exhaust gas treatment tower 12).
The foregoing description of the preferred embodiments of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the utility model.
The foregoing description of the preferred embodiments of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the utility model.
Claims (6)
1. The utility model provides a silver-containing etching waste liquid recycling device that retrieves silver which characterized in that: comprises a silver etching waste liquid storage tank (1), a precipitation tank (2), a first dosing tank (3), a first centrifugal machine (4), a reduction reaction tank (5), a second centrifugal machine (6), a cleaning tank (7), a high-temperature casting furnace (8), a cooling tank (9) and an electrolytic tank (10) which are connected in sequence; the sedimentation tank (2) top is connected with first dosing tank (3), is connected with solid dosing tank (5 a) and liquid dosing tank (5 b) that respectively arrange alone on reduction reaction tank (5), and waste liquid collecting tank (11) is connected to the liquid discharge port of first centrifuge (4), and waste gas treatment tower (12) is connected to the gas discharge port of electrolysis trough (10), adds reducing iron powder in solid dosing tank (5 a), adds dilute sulfuric acid in liquid dosing tank (5 b), adds the additive in first dosing tank (3).
2. The device for recycling silver from silver-containing etching waste liquid according to claim 1, wherein the device comprises: stirring devices are arranged in the silver etching waste liquid storage tank (1) and the precipitation tank (2).
3. The device for recycling silver from silver-containing etching waste liquid according to claim 1, wherein the device comprises: the cleaning tank (7) is internally provided with a cleaning solution adding tank, and the cleaning tank (7) is internally provided with an adding device, a stirring device and a solid-liquid separation device.
4. A device for recycling silver from silver-containing etching waste liquid according to claim 1, 2 or 3, characterized in that: silver etching waste liquid holding vessel (1) be linked together through pipeline and precipitation tank (2), precipitation tank (2) bottom is linked together through pipeline and first centrifuge (4), the discharge gate of first centrifuge (4) is connected through pipeline and reduction reaction tank (5) feed inlet, solid is passed to reduction reaction tank (5) from the solid discharge gate of first centrifuge (4), the discharge gate of reduction reaction tank (5) is connected through pipeline and second centrifuge (6) feed inlet, the discharge gate of second centrifuge (6) is connected through pipeline and washing tank (7), the discharge gate of washing tank (7) is connected with high temperature casting furnace (8) feed inlet, washing tank (7) discharge gate and high temperature casting furnace (8) feed inlet are connected through the conveyer belt, high temperature casting furnace (8) discharge gate is communicated with cooling tank (9) through the conveyer belt, cooling tank (9) discharge gate is connected with electrolysis tank (10) through the conveyer belt.
5. The device for recycling silver from silver-containing etching waste liquid according to claim 3, wherein the device comprises: the lower part of the cleaning tank (7) is provided with a 50 ℃ circulating liquid device.
6. The device for recycling silver from silver-containing etching waste liquid according to claim 4, wherein the device comprises: an exhaust hood is arranged on the electrolytic tank (10) and is connected with an exhaust gas treatment tower (12).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320462593.8U CN219526748U (en) | 2023-03-07 | 2023-03-07 | Silver-containing etching waste liquid recycling silver recovery device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320462593.8U CN219526748U (en) | 2023-03-07 | 2023-03-07 | Silver-containing etching waste liquid recycling silver recovery device |
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| Publication Number | Publication Date |
|---|---|
| CN219526748U true CN219526748U (en) | 2023-08-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202320462593.8U Active CN219526748U (en) | 2023-03-07 | 2023-03-07 | Silver-containing etching waste liquid recycling silver recovery device |
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- 2023-03-07 CN CN202320462593.8U patent/CN219526748U/en active Active
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