CN114561670A - High-purity indium electrolysis device and electrolysis method thereof - Google Patents
High-purity indium electrolysis device and electrolysis method thereof Download PDFInfo
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Abstract
A high-purity indium electrolysis device and an electrolysis method thereof are disclosed, wherein the electrolysis device comprises an electrolytic bath (1), a sedimentation tank (2), an anode copper bar (17), a cathode copper bar (18), an anode plate (10), a cathode plate (11), an electrolysis power supply (3), an electrolytic bath cover plate (12) and a temperature-controllable circulating system connected with the electrolytic bath and the sedimentation tank; the anode plate is an indium plate, and the cathode plate is a titanium plate; the temperature-controllable circulating system comprises a circulating pipeline, a speed-adjustable circulating pump (6) and a filter (9), a heater (7) and a cooler (8), a filtrate pipe (13) and a valve, wherein the two ends of the circulating pipeline are respectively connected with a liquid outlet and a liquid inlet of the electrolytic cell, the speed-adjustable circulating pump and the filter (9) are arranged on the circulating pipeline, the heater (7) and the cooler (8) are arranged between the speed-adjustable circulating pump and the filter in parallel through pipelines, the filtrate pipe (13) is connected with the speed-adjustable circulating pump and the sedimentation tank, and the valve is arranged on the pipeline. The invention can realize automatic control of electrolysis environment and process parameters, effectively remove impurities and precipitates in the electrolyte and improve the quality and stability of the electrolysis product.
Description
Technical Field
The invention belongs to the technical field of electrolysis, and particularly relates to an electrolysis device and an electrolysis method for high-purity indium.
Background
The high-purity indium is a product with the indium content of more than 99.999 percent, is widely applied to the fields of electronic industry, aerospace, alloy manufacturing, solar cells, national defense and military industry, nuclear industry, modern information industry and the like, and mainly comprises manufacturing Indium Tin Oxide (ITO) thin film materials, semiconductor compound materials, copper indium selenium polycrystalline thin film solar cells, indium-containing brazing filler metals, indium-based brazing filler metals and the like. At present, the high-purity indium purification technology mainly comprises methods such as electrolytic refining, vacuum distillation, zone melting and the like. The electrolytic refining purification is a key link in the production of high-purity indium, and the control of the electrolysis environment and the process parameters in the electrolysis process has important influence on the quality of the high-purity indium.
Based on the technical scheme, the invention provides the high-purity indium electrolysis device and the electrolysis method thereof, which can effectively control the electrolysis environment and the process parameters, so that the electrolysis efficiency is effectively improved, the impurity content is reduced, and the quality of high-purity indium is improved.
Disclosure of Invention
The invention aims to provide a high-purity indium electrolysis device and an electrolysis method thereof, which can effectively improve electrolysis efficiency, reduce impurity content and improve high-purity indium quality.
The technical scheme adopted by the invention is as follows:
a high-purity indium electrolysis device comprises an electrolytic bath, a sedimentation tank arranged at the bottom of the electrolytic bath, an anode copper bar and a cathode copper bar which are arranged on the top surface of the electrolytic bath, an anode plate and a cathode plate which are respectively hung on the anode copper bar and the cathode copper bar and are arranged in the electrolytic bath, an electrolysis power supply connected with the anode copper bar and the cathode copper bar, a cover plate covered on the top surface of the electrolytic bath and provided with a ventilation device, and a controllable temperature circulation system connected with the electrolytic bath and the sedimentation tank; the anode plate is an indium plate, and the cathode plate is a titanium plate; the temperature-controllable circulating system comprises a circulating pipeline, a speed-adjustable circulating pump, a filter, a heater, a cooler, a filtrate pipe and valves, wherein the two ends of the circulating pipeline are respectively connected with a liquid outlet and a liquid inlet of the electrolytic cell, the speed-adjustable circulating pump is arranged on the circulating pipeline and is close to one end of the liquid outlet, the filter is arranged on the circulating pipeline and is close to one end of the liquid inlet, the heater and the cooler are arranged between the speed-adjustable circulating pump and the filter in parallel through pipelines, the filtrate pipe is connected with the speed-adjustable circulating pump and the sedimentation tank, and the valves are respectively arranged on the filtrate pipe, the heater liquid inlet pipeline and the cooler liquid inlet pipeline.
Furthermore, a temperature sensor and a pH sensor are arranged on the electrolytic bath.
Furthermore, the anode copper bar consists of a copper core and a protective layer coated outside the copper core, contact grooves are uniformly distributed on the protective layer, and the hanging lugs on the top of the anode plate are hung in the contact grooves. The cathode copper bar is also composed of a copper core and a protective layer coated outside the copper core, contact grooves are uniformly distributed on the protective layer, and the hanging lugs at the top of the cathode plate are hung in the contact grooves.
Further, the purity of indium of the anode plate is 99.9% -99.995%, and the thickness of the anode plate is 5-35 mm; the purity of the titanium plate of the cathode plate is 99.9-99.99%, the thickness of the cathode plate is 1.5-5mm, and the surface roughness Ra is 0.2-1.6.
Furthermore, the anode plate is cast by indium molten metal, a casting mold for casting the anode plate is composed of two half molds which are closed, a pouring gate and a pouring channel leading to a cavity from the bottom of the pouring gate are arranged at the top end of the parting surface of the two half molds, a cooling water channel and an anode plate ejection mechanism are arranged on each half mold, the cooling water channel is a rotary water channel with the lower part arranged closely and the middle part and the upper part arranged gradually sparsely, cooling water enters from a water inlet of the cooling water channel and is discharged from a water outlet, the anode plate ejection mechanism is a group of ejector rods transversely penetrating through the half molds, the inner ends of the ejector rods are positioned on the wall surface of the cavity, and the outer ends of the ejector rods are higher than the outer surfaces of the half molds.
The electrolysis method of the high-purity indium electrolysis device comprises the following steps:
s1, preparing In with the concentration of 50-150g/L2(SO4)3Adding the solution into an electrolytic cell, and then adding NaCl and an additive; closing the upper cover plate, and opening a valve on a filtrate pipe of the temperature-controllable circulating system, the speed-adjustable circulating pump, a valve on a liquid inlet pipeline of the heater and the heater; setting the heater temperature at 60-100 deg.C, circulating for 30-180min, and waiting for additive and In2(SO4)3Stopping heating after the solution is completely mixed, at the moment, closing a valve on a liquid inlet pipeline of the heater, opening a valve on a liquid inlet pipeline of the cooler, starting the cooler, setting the temperature of the cooler to be 5-10 ℃, cooling the electrolyte, and adjusting the pH value of the electrolyte to be 1.6-2.5; after the electrolyte is cooled to room temperature, the cooler and the speed-adjustable circulating pump are closed, the cover plate is opened, the anode copper bar and the cathode copper bar are placed into the cover plate, the distance between the anode copper bar and the cathode copper bar is adjusted to be 35-120mm, and then the anode copper bar and the cathode copper bar are respectively connected with the anode and the cathode of the electrolytic power supply;
s2, placing the anode plate into an electrolytic cell, and hanging a top-end hanging lug in a contact groove of an anode copper bar; placing the cathode plate into an electrolytic cell, and hanging a top hanging lug in a contact groove of a cathode copper bar;
s3, closing the cover plate, turning on an electrolytic power supply and setting the current density to be 50-100A/m2The voltage of the tank is 0.5-1.2V, electrolysis is started, and the temperature of the electrolyte is kept constant between 20-28 ℃ by a temperature-controllable circulating system; when the first period of electrolysis is finished, the cathode plate is taken out and stripped and then put into the electrolytic tank againPerforming the following steps; supplementing additives and adjusting pH to the electrolyte according to the method of the step S1, wherein part of anode mud, impurities and other precipitates generated by electrolysis are precipitated in a precipitation tank and part of the anode mud, the impurities and other precipitates are filtered and removed by a filter in the circulation process, so that the purity and the stability of the electrolyte are maintained;
and S4, after the electrolysis is completed, adding a precipitator, adjusting the temperature of the electrolyte to precipitate impurity elements in the electrolyte in a sedimentation tank, pumping the electrolyte out through a speed-adjustable circulating pump, cleaning waste residues in the sedimentation tank, cleaning an electrolytic bath, and uniformly recovering and treating the generated waste residues and waste liquid.
Further, in the above method, the concentration of NaCl in the electrolyte is 60-150 g/L.
Further, in the method, the additive is one or more of gelatin, beta-naphthoic acid, thioether, mercaptan and lignosulfonate, and the concentration of the additive is 0.1-0.5 g/L.
Further, in the method, the precipitator is one or more of barium carbonate, barium chloride, ammonia water and gelatin, and the addition amount of the precipitator is 0.01-2% of the mass of the electrolyte.
The invention has the following beneficial effects:
(1) the electrolysis device is provided with the temperature-controllable circulating system, can realize automatic control of electrolysis environment and technological parameters, dynamically adjusts the temperature of the electrolyte, and is convenient for regulating and controlling the components of the electrolyte and keeping the temperature of the electrolyte constant in the electrolysis process. Meanwhile, the sedimentation tank and the filter can effectively remove impurities and sediments in the electrolyte in the circulating process, and the purity and cleanness of the electrolyte are ensured, so that the quality and stability of an electrolytic product are improved. And the generated waste gas, waste liquid and waste residue are easy to collect and treat, so that the labor intensity of workers can be reduced.
(2) The anode plate casting mold is provided with the water channels which are distributed in a rotary type, dense at the bottom and loose at the top in a stepped manner, so that the mold has positive temperature gradient distribution from bottom to top, and the anode plate is sequentially solidified from bottom to top, thereby ensuring that the anode plate has no casting defect, refining the grain size of the anode plate, enriching some impurity elements near hangers and reducing the content of the impurity elements in the effective area of the anode plate. The ejector rod and the coating in the casting mould are beneficial to demoulding, thereby ensuring that the anode plate is not deformed when being taken out. The die can be applied to large-scale automatic production of the polar plate, and ensures the stable and reliable quality of the polar plate.
(3) The electrolysis method has the advantages of simple process, cleanness, environmental protection, high production efficiency and good quality and product stability of the produced electrolytic high-purity indium.
Drawings
FIG. 1 is a schematic view of an electrolysis apparatus according to the present invention;
FIG. 2 is a schematic view of an anode copper bar;
FIG. 3 is a cross-sectional view taken along line A-A of FIG. 2;
FIG. 4 is a schematic view of a cathode copper bar;
FIG. 5 is a schematic view of a casting mold for an anode plate;
FIG. 6 is a cross-sectional view taken along line B-B of FIG. 5;
FIG. 7 shows the grain comparison of the anode plate (b) cast by the anode plate casting mold of the present invention with the normal anode plate (a);
FIG. 8 is a structural diagram of cathode indium after electrolysis according to the present invention.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, but the scope of the invention is not limited thereto.
As shown in figure 1, the high-purity indium electrolysis device comprises an electrolytic bath 1, a sedimentation tank 2 arranged at the bottom of the electrolytic bath, an anode copper bar 17 and a cathode copper bar 18 arranged on the top surface of the electrolytic bath, an anode plate 10 and a cathode plate 11 respectively hung on the anode copper bar and the cathode copper bar and arranged in the electrolytic bath, an electrolysis power supply 3 connected with the anode copper bar and the cathode copper bar, a cover plate 12 covered on the top surface of the electrolytic bath and provided with an air interchanger, and a temperature-controllable circulating system connected with the electrolytic bath and the sedimentation tank. The anode plate 10 is an indium plate, and the cathode plate 11 is a titanium plate. The temperature-controllable circulating system comprises a circulating pipeline, a speed-adjustable circulating pump 6, a filter 9, a heater 7 and a cooler 8, a filtrate pipe 13 and valves, wherein the two ends of the circulating pipeline are respectively connected with a liquid outlet 5 and a liquid inlet 16 of the electrolytic cell, the speed-adjustable circulating pump 6 is installed on the circulating pipeline and is close to one end of the liquid outlet 5, the filter 9 is installed on the circulating pipeline and is close to one end of the liquid inlet 16, the heater 7 and the cooler 8 are arranged between the speed-adjustable circulating pump and the filter in parallel through pipelines, the filtrate pipe 13 is connected with the speed-adjustable circulating pump and the sedimentation tank, and the valves are respectively arranged on the filtrate pipe 13, the heater liquid inlet pipeline 14 and the cooler liquid inlet pipeline 15. The electrolytic cell is provided with a temperature sensor 4a and a pH sensor 4 b. The electrolytic bath is made of acid and alkali resistant materials such as polytetrafluoroethylene, polymethyl methacrylate and the like. As shown in fig. 2 and 3, the anode copper bar 17 is composed of a copper core 20 and a protective layer 19 coated outside the copper core, contact grooves 21 are uniformly distributed on the protective layer, and a hanging lug on the top of the anode plate 10 is hung in the contact groove 21. The cathode copper bar 18 is also composed of a copper core and a protective layer coated outside the copper core, as shown in fig. 4, contact grooves are uniformly distributed on the protective layer of the cathode copper bar, and the hanging lugs on the top of the cathode plate 11 are hung in the contact grooves. The copper bar protective layer is made of insulating acid and alkali resistant materials such as polytetrafluoroethylene or rubber. The purity of the indium of the anode plate 10 is 99.9-99.995%, and the thickness of the anode plate is 5-35 mm; the purity of the titanium plate of the cathode plate 11 is 99.9-99.99%, the thickness of the cathode plate is 1.5-5mm, and the surface roughness Ra is 0.2-1.6.
The anode plate of the invention can be cast by using a casting mold as shown in figures 5 and 6. The casting mold consists of two half molds 23 which are closed, a pouring gate 24 and a pouring gate 25 leading to a cavity from the bottom of the pouring gate are arranged at the top end of the parting surface of the two half molds, a cooling water channel 22 and an anode plate ejection mechanism 26 are arranged on each half mold, the cooling water channel is a rotary water channel with the lower part arranged tightly and the middle part and the upper part arranged sparsely, and cooling water enters from a water inlet 27 of the cooling water channel and is discharged through a water outlet 28. The anode plate ejection mechanism 26 is a group of ejector rods transversely penetrating through the half mold, the inner ends of the ejector rods are positioned on the wall surface of the cavity, and the outer ends of the ejector rods are higher than the outer surface of the half mold. The casting mould is made of stainless steel, the surface of the cavity is plated with a layer of titanium with the thickness of 0.5-2mm, and the surface roughness Ra of the cavity is 0.2-0.8.
When the anode plate is poured, the two half moulds are closed and fixed, cooling water is connected, and the temperature of the cooling water is controlled to be 10-30 ℃. Heating indium ingot containing 99.9-99.995 wt.% indium to 180-240 ℃ for melting, keeping the temperature for 10-30min, removing surface oxidation slag, and pouring into a mold from a pouring gate 24. And (3) opening the mold after the molten metal is solidified, ejecting the anode plate molded by casting inwards by using an ejection mechanism 26, and cutting off a casting head. The crystal grains of the anode plate obtained by casting are shown in figure 7(b), and compared with the crystal grains of the common anode plate (a), the crystal grains of the anode plate cast by the die are small in size and uniform in distribution.
The electrolysis method of the high-purity indium electrolysis device comprises the following steps:
s1, preparing In with the concentration of 50-150g/L2(SO4)3Adding the solution into an electrolytic bath, and then adding 60-150g/L NaCl and an additive, wherein the additive can be one or more of gelatin, beta-naphthoic acid, thioether, mercaptan and lignosulfonate, and the concentration of the additive is 0.1-0.5 g/L;
closing the upper cover plate 12, and opening a valve on a filtrate pipe 13 of the temperature-controllable circulating system, the speed-adjustable circulating pump 6, a valve on a heater liquid inlet pipeline 14 and the heater 7; setting the heater temperature at 60-100 deg.C, circulating for 30-180min, and waiting for additive and In2(SO4)3Stopping heating after the solution is completely mixed, at the moment, closing a valve on a heater liquid inlet pipeline 14, opening a valve on a cooler liquid inlet pipeline 15, starting a cooler 8, setting the temperature of the cooler to be 5-10 ℃, cooling the electrolyte, and adjusting the pH value of the electrolyte to be 1.6-2.5; after the electrolyte is cooled to room temperature, the cooler and the speed-adjustable circulating pump 6 are closed, the cover plate 12 is opened, the anode copper bar 17 and the cathode copper bar 18 are placed, the distance between the poles is adjusted to be 35-120mm, and then the anode copper bar and the cathode copper bar are respectively connected with the anode and the cathode of the electrolytic power supply 3;
s2, placing the anode plate which is poured in advance into an electrolytic bath, and hanging a top hanging lug in a contact groove of an anode copper bar; placing the cathode plate into an electrolytic cell, and hanging a top hanging lug in a contact groove of a cathode copper bar;
s3, closing the cover plate, turning on an electrolytic power supply and setting the current density to be 50-100A/m2The voltage of the tank is 0.5-1.2V, electrolysis is started, and the temperature of the electrolyte is kept constant between 20-28 ℃ by a temperature-controllable circulating system; when the first period of electrolysis is finished, taking out the cathode plate, stripping the cathode plate, and putting the cathode plate into the electrolytic cell again; adding additives and adjusting pH to the electrolyte as in step S1Part of anode mud, impurities and other precipitates generated by decomposition are precipitated in the sedimentation tank 2 in the circulation process, and the other part of the precipitates are filtered and removed by the filter 9, so that the purity and the stability of the electrolyte are kept;
and S4, after the electrolysis is completed, adding a precipitator, adjusting the temperature of the electrolyte to precipitate impurity elements in the electrolyte in a sedimentation tank, pumping the electrolyte out through a speed-adjustable circulating pump (6), cleaning waste residues in the sedimentation tank, cleaning the electrolytic tank, and uniformly recovering and treating the generated waste residues and waste liquid. The precipitant can be one or more of barium carbonate, barium chloride, ammonia water and gelatin, and the addition amount is 0.01-2% of the electrolyte mass.
One specific example is as follows:
(1) configuring 100g/L of In2(SO4)3Pouring the solution into an electrolytic cell, filling 2/3 of the electrolytic cell with the solution, and adding additives of NaCl and gelatin, wherein the concentration of NaCl is 80g/L, and the concentration of gelatin is 0.25 g/L. Closing the upper cover plate 12, sequentially opening the valve on the filtrate pipe 13, the speed-adjustable circulating pump 6, the valve on the heater liquid inlet pipeline 14 and the heater 7, setting the temperature of the heater of the electrolytic cell to 80 ℃, circulating for 120min, and waiting for the additive and In2(SO4)3The solution was mixed thoroughly and heating was stopped. At this time, the valve on the heater liquid inlet pipeline 14 is closed, the valve on the cooler liquid inlet pipeline 15 is opened, the cooler 8 is opened, the temperature of the cooler is set to 5 ℃, the temperature of the electrolyte is reduced, and the pH of the electrolyte is adjusted to 2.0. After the solution is cooled to room temperature, the cooler and the temperature-controllable circulating system are closed, the cover plate is opened, the anode copper bar and the cathode copper bar are placed in the cooler, and then the anode copper bar and the cathode copper bar are respectively connected with the anode and the cathode of the electrolytic power supply;
(2) cleaning a prepared anode plate and a prepared cathode plate, putting the anode plate and the cathode plate into an electrolytic bath, and respectively hanging the anode plate and the cathode plate on an anode copper bar and a cathode copper bar;
(3) closing the cover plate, turning on the electrolysis power supply, and setting the current density at 70A/m2And the voltage of the tank is 0.8V, the electrolysis is started, and the temperature of the electrolyte is kept constant between 22 ℃ by a temperature-controllable circulating system. When one period of electrolysis is finished, the cathode plate is taken out and stripped, and then the cathode plate is put into the cell againIn the solution tank. Supplementing additives and adjusting pH to the electrolyte, wherein part of anode mud, impurities or other precipitates generated by electrolysis partially precipitate in a sedimentation tank and part of the anode mud, the impurities or other precipitates are filtered and removed in the circulation process;
(4) after the electrolysis is completed, adding a precipitator barium carbonate with the concentration of 0.1g/L, adjusting the temperature of the electrolyte to 40 ℃ to precipitate impurity elements such as Pb in the electrolyte, pumping the electrolyte out through a circulating system to clean waste residues in a bottom precipitation tank, cleaning an electrolytic bath, and uniformly recovering and treating the generated waste residues and waste liquid.
The product obtained by electrolysis in this example has a dense structure without defects, as shown in FIG. 8.
Claims (9)
1. A high-purity indium electrolysis device is characterized by comprising an electrolytic bath (1), a sedimentation tank (2) arranged at the bottom of the electrolytic bath, an anode copper bar (17) and a cathode copper bar (18) arranged on the top surface of the electrolytic bath, an anode plate (10) and a cathode plate (11) which are respectively hung on the anode copper bar and the cathode copper bar and are arranged in the electrolytic bath, an electrolysis power supply (3) connected with the anode copper bar and the cathode copper bar, a cover plate (12) covered on the top surface of the electrolytic bath and provided with a ventilation device, and a temperature-controllable circulating system connected with the electrolytic bath and the sedimentation tank; the anode plate (10) is an indium plate, and the cathode plate (11) is a titanium plate; the temperature-controllable circulating system comprises a circulating pipeline, a speed-adjustable circulating pump (6) and a filter (9), wherein two ends of the circulating pipeline are respectively connected with a liquid outlet (5) and a liquid inlet (16) of an electrolytic cell, the speed-adjustable circulating pump (6) is installed on the circulating pipeline and is close to one end of the liquid outlet (5), the filter (9) is installed on the circulating pipeline and is close to one end of the liquid inlet (16), a heater (7) and a cooler (8) are arranged between the speed-adjustable circulating pump and the filter in parallel through pipelines, a filtrate pipe (13) is connected with the speed-adjustable circulating pump and the sedimentation tank, and valves are respectively arranged on the filtrate pipe (13), a heater liquid inlet pipeline (14) and a cooler liquid inlet pipeline (15).
2. A high purity indium electrolysis apparatus according to claim 1, wherein a temperature sensor (4a) and a pH sensor (4b) are provided on the electrolysis cell.
3. The high-purity indium electrolysis device according to claim 1 or 2, wherein the anode copper bar (17) is composed of a copper core (20) and a protective layer (19) coated outside the copper core, contact grooves (21) are uniformly distributed on the protective layer, and the hanging lugs on the top of the anode plate (10) are hung in the contact grooves (21); the cathode copper bar (18) is also composed of a copper core and a protective layer coated outside the copper core, contact grooves are uniformly distributed on the protective layer, and the hanging lugs at the top of the cathode plate (11) are hung in the contact grooves.
4. A high purity indium electrolysis apparatus according to claim 1, wherein the purity of indium of the anode plate (10) is 99.9-99.995%, and the anode plate thickness is 5-35 mm; the purity of the titanium plate of the cathode plate (11) is 99.9-99.99%, the thickness of the cathode plate is 1.5-5mm, and the surface roughness Ra is 0.2-1.6.
5. The high-purity indium electrolyzing device according to claim 1 or 4, wherein the anode plate (10) is cast by indium metal liquid, the casting mold for casting the anode plate is composed of two half molds (23) which are closed, a pouring gate (24) and a pouring gate (25) leading from the bottom of the pouring gate to the cavity are arranged at the top end of the parting surface of the two half molds, each half mold is provided with a cooling water channel (22) and an anode plate ejection mechanism (26), the cooling water channel is a convoluted water channel with tightly arranged lower part and gradually sparse arrangement in the middle part and upper part, cooling water enters from a water inlet (27) of the cooling water channel and is discharged through a water outlet (28), the anode plate ejection mechanism (26) is a group of ejector rods transversely penetrating through the half molds, the inner ends of the ejector rods are positioned on the wall surface of the cavity, and the outer ends of the ejector rods are higher than the outer surface of the half molds.
6. The electrolysis method of the high-purity indium electrolysis device according to claim 1, characterized by comprising the following steps:
s1, preparing In with the concentration of 50-150g/L2(SO4)3Adding the solution into an electrolytic cell, and then adding NaCl and an additive; closing the upper cover plate (12), opening the valve on the filtrate pipe (13) of the temperature-controllable circulating system, the speed-adjustable circulating pump (6), the valve on the liquid inlet pipeline (14) of the heater and the heater(7) (ii) a Setting the heater temperature at 60-100 deg.C, circulating for 30-180min, and waiting for additive and In2(SO4)3Stopping heating after the solution is completely mixed, at the moment, closing a valve on a heater liquid inlet pipeline (14), opening a valve on a cooler liquid inlet pipeline (15), starting a cooler (8), setting the temperature of the cooler to be 5-10 ℃, cooling the electrolyte, and adjusting the pH value of the electrolyte to be 1.6-2.5; after the electrolyte is cooled to room temperature, the cooler and the speed-adjustable circulating pump (6) are closed, the cover plate (12) is opened, the anode copper bar (17) and the cathode copper bar (18) are placed, the distance between the electrodes is adjusted to be 35-120mm, and then the anode copper bar and the cathode copper bar are respectively connected with the anode and the cathode of the electrolytic power supply (3);
s2, placing the anode plate into an electrolytic cell, and hanging a top-end hanging lug in a contact groove of an anode copper bar; placing the cathode plate into an electrolytic cell, and hanging a top hanging lug in a contact groove of a cathode copper bar;
s3, closing the cover plate, turning on an electrolytic power supply and setting the current density to be 50-100A/m2The voltage of the cell is 0.5-1.2V, electrolysis is started, and the temperature of the electrolyte is kept constant between 20-28 ℃ by a temperature-controllable circulating system; when the first period of electrolysis is finished, taking out the cathode plate, stripping the cathode plate, and putting the cathode plate into the electrolytic cell again; supplementing additives and adjusting pH to the electrolyte according to the method of the step S1, wherein part of anode mud, impurities and other precipitates generated by electrolysis are precipitated in the sedimentation tank (2) in the circulation process, and the other part of the anode mud, the impurities and the other precipitates are filtered and removed by the filter (9), so that the purity and the stability of the electrolyte are maintained;
and S4, after the electrolysis is completed, adding a precipitator, adjusting the temperature of the electrolyte to precipitate impurity elements in the electrolyte in a sedimentation tank, pumping the electrolyte out through a speed-adjustable circulating pump (6), cleaning waste residues in the sedimentation tank, cleaning the electrolytic tank, and uniformly recovering and treating the generated waste residues and waste liquid.
7. The electrolytic process of claim 6, wherein the concentration of NaCl in the electrolyte is 60 to 150 g/L.
8. The electrolysis method according to claim 6, wherein the additive is one or more of gelatin, β -naphthoic acid, thioether, thiol, lignosulfonate, and additive concentration is 0.1-0.5 g/L.
9. The electrolysis method according to claim 6, wherein the precipitant is one or more of barium carbonate, barium chloride, ammonia water and gelatin, and the addition amount is 0.01-2% of the electrolyte mass.
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