CN111809050A - Method for recycling ITO waste target - Google Patents
Method for recycling ITO waste target Download PDFInfo
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- CN111809050A CN111809050A CN202010451276.7A CN202010451276A CN111809050A CN 111809050 A CN111809050 A CN 111809050A CN 202010451276 A CN202010451276 A CN 202010451276A CN 111809050 A CN111809050 A CN 111809050A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a method for recycling an ITO waste target, which comprises the following steps: and (3) taking the ITO waste target as a cathode and deionized water as cathode tank electrolyte, generating a reduction waste target after electrolysis in a cathode area, taking the reduction waste target as an anode and a potassium hydroxide solution as anode tank electrolyte, and obtaining a potassium stannate solution and indium hydroxide precipitate after electrolysis in an anode area. The cathode is an ITO waste target, the anode is a reduction waste target after the electrolysis of the cathode ITO waste target, the anode tank and the cathode tank are connected through a salt bridge to form an electrolysis loop for coupled electrolysis, indium hydroxide generated in the anode tank is roasted to prepare indium oxide, a potassium stannate solution in the anode tank reacts with hydrogen chloride to obtain tin hydroxide, and the tin hydroxide is roasted to prepare tin oxide, the residual potassium chloride solution can be used for preparing the salt bridge, so that inorganic waste liquid is not generated in the whole electrolysis process, the maximum utilization of reactants is realized in the whole process, the anion anode tank is not required to be separated by an ion diaphragm, the indium tin ion separation effect is good, and the ITO waste target is recovered at the lowest electrolysis cost.
Description
Technical Field
The invention relates to the technical field of inorganic material preparation, in particular to a method for recycling an ITO (indium tin oxide) waste target.
Background
In recent years, indium-tin oxide (In)2O3-SnO2Commonly known as ITO) sputtering targets for transparent conduction in liquid crystal display devicesMany electronic components such as thin films and gas sensors are widely used, and in the application of ITO, a thin film of a conductive oxide is formed on a substrate by a sputtering method called sputtering coating, in which a target material is not uniformly consumed but a part of the target material is intensively consumed, called an etching part, and the etching part continues a sputtering operation until a backing plate supporting the target is exposed, and the target material cannot be used any more and needs to be replaced with a new one.
Therefore, many non-etched portions, that is, unused target portions remain in the sputtering target after the sputtering is completed, and all of these portions become a waste target. In addition, when a sputtering target made of these conductive oxides is manufactured, a waste target (scrap) is also generated from the abrasive powder and the cutting powder. Since sputtering target materials formed from these conductive oxides are expensive due to the use of high-purity materials, valuable metals are generally recovered from such waste target materials and reused.
In the prior art, valuable metals are recovered by one or a combination of a plurality of methods such as an acid dissolution method, an ion exchange method, a solvent extraction method, a high-temperature reduction method, a molten salt electrolysis method and the like, and with the deep research on the recovery of the valuable metals and the continuous updating and demand of people, a plurality of novel recovery methods are developed, for example, the valuable metals are recovered from ITO waste targets by adopting an electrolysis method. In the prior art, inorganic acid is mostly adopted as electrolyte in the method for recovering the ITO waste target by adopting an electrolytic method, inorganic waste liquid is generated, and when an anode-cathode tank is separated by an ion diaphragm, the separation effect of indium and tin ions is poor, the structure of the electrolytic tank is complex, and the cost is increased.
Aiming at the defects of the technology for recovering valuable metals from the ITO waste target in the prior art, the invention overcomes the technical problem and provides a method for recovering the ITO waste target.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recycling an ITO waste target.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a method for recycling an ITO waste target, which is characterized by comprising the following steps of: the method comprises the steps of taking an ITO waste target as a cathode and deionized water as cathode tank electrolyte, generating a reduction waste target after electrolysis in a cathode area, taking the reduction waste target as an anode and a potassium hydroxide solution as anode tank electrolyte, connecting the anode tank and the cathode tank through a salt bridge to form an electrolysis loop for coupling electrolysis, and obtaining a potassium stannate solution and an indium hydroxide precipitate after electrolysis in the anode area.
As a further improvement of the invention, after the step of obtaining the potassium stannate solution and the indium hydroxide precipitate after the anode area electrolysis, the method further comprises the following steps: and (3) precipitating the indium hydroxide precipitate in a potassium stannate solution, and adding a hydrogen chloride solid into the potassium stannate solution to react to obtain a potassium chloride solution and a tin hydroxide precipitate.
As a further improvement of the invention, after the indium hydroxide is precipitated in the potassium stannate solution, the method further comprises the following steps: and filtering, cleaning, drying and sintering the indium hydroxide precipitate to obtain the indium oxide.
As a further improvement of the invention, after the steps of adding hydrogen chloride solid into the potassium stannate solution to react to obtain the potassium chloride solution and precipitating the tin hydroxide, the method also comprises the following steps: and filtering, cleaning, drying and sintering the tin hydroxide precipitate to obtain the tin oxide.
As a further improvement of the invention, the pH value of the reaction environment of the anode tank is more than 13 in the electrolysis process.
As a further improvement of the invention, the pH value of the reaction environment of the cathode cell during the electrolysis process is less than 14.
As a further improvement of the invention, the salt bridge is a U-shaped round or square pipeline which is composed of agar and saturated potassium chloride solution.
As a further improvement of the invention, during the electrolysis process, ultrasonic waves are introduced into the anode tank by using an ultrasonic generator.
As a further improvement of the invention, the temperature of the cathode tank and the anode tank is kept between 20 and 50 ℃ in the electrolysis process.
As a further improvement of the invention, in the electrolysis process, the electrolysis voltage is 2-20V.
The invention provides a method for recycling an ITO waste target, wherein a cathode is the ITO waste target, an anode is a reduction waste target obtained after the electrolysis of the cathode ITO waste target, an anode tank and a cathode tank are connected through a salt bridge to form an electrolysis loop for coupled electrolysis, indium oxide is prepared after indium hydroxide generated by the anode tank is roasted, tin oxide is prepared after tin hydroxide obtained by the reaction of potassium stannate solution and hydrogen chloride in the anode tank is roasted, the salt bridge can be prepared from the residual potassium chloride solution, so that inorganic waste liquid is not generated in the whole electrolysis process, the maximum utilization of reactants is realized in the whole process, the cathode and anode tanks are not required to be separated by ion diaphragms, the separation effect of indium and tin ions is good, and the ITO waste target is recycled at the lowest electrolysis cost.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for recycling an ITO waste target, which comprises the following steps:
the method comprises the steps of taking an ITO waste target as a cathode and deionized water as a cathode tank electrolyte, generating a reduction waste target after electrolysis in a cathode area, taking the reduction waste target as an anode and a potassium hydroxide solution as an anode tank electrolyte, connecting the anode tank and the cathode tank through a salt bridge to form an electrolysis loop for coupling electrolysis, obtaining a potassium stannate solution and an indium hydroxide precipitate after electrolysis in the anode area, and filtering, cleaning, drying and sintering the indium hydroxide precipitate to obtain indium oxide, wherein the reduction waste target is a U-shaped circular or square pipeline which is composed of agar and a saturated potassium chloride solution, and the reduction waste target is simple substance indium, simple substance tin, partial low-valence indium oxide and tin oxide.
The electrolytic reaction generated by the method for recovering the ITO waste target of the invention is as follows:
a cathode region:
3H2O+In2O3+6e-→2In+6OH-；
2H2O+SnO2+4e-→Sn+4OH-；
H2O+In2O3+2e-→2InO+2OH-；
H2O+SnO2+2e-→SnO+2OH-；
2H2O-2e-→H2+2OH-；
an anode region:
In-3e-→In3+；
In+-2e-→In3+；
Sn-4e-→Sn4+；
Sn-2e-→Sn2+；
In3++3OH-→In(OH)3；
Sn4++6OH-→SnO3 2-+3H2O；
Sn2++4OH-→SnO2 2-+2H2O；
as can be seen from the electrolytic reaction, a potassium stannate solution and an indium hydroxide precipitate are obtained after electrolysis in the anode region, the indium hydroxide precipitate is separated out in the potassium stannate solution, the indium hydroxide precipitate is filtered, cleaned, dried and sintered to obtain indium oxide, hydrogen chloride is added into the potassium stannate solution to carry out solid reaction to obtain a potassium chloride solution and a tin hydroxide precipitate, and the tin hydroxide precipitate is filtered, cleaned, dried and sintered to obtain tin oxide.
In the electrolysis process, the pH value of the reaction environment of the anode tank needs to be ensured to be more than 13, because no chloride ions exist In the solution at the beginning of electrolysis, the content of the chloride ions In the anode tank can be slowly increased along with the prolonging of the electrolysis time, when the content of the chloride ions In the anode tank is increased to a certain concentration, the concentration of the hydroxyl ions can be reduced along with the increase of the chloride ions, and alkali salt containing indium hydroxyl, such as In, can be generated5(OH)14Cl, so that the alkaline reaction conditions of the anode tank need to be ensuredThe pH value of the reaction environment of the anode tank is more than 13.
Meanwhile, if the pH value of the reaction environment of the anode tank is less than 13, tin hydroxide precipitation is started to separate out, the electrolysis is stopped at the moment, the tin hydroxide and the indium hydroxide are prevented from being mixed, after the electrolysis is stopped, a potassium stannate solution and an indium hydroxide precipitate obtained by the reaction in the anode tank are taken out, a new potassium hydroxide solution is replaced to be used as an anode tank electrolyte for continuous electrolysis, wherein a potassium hydroxide solution generated by the reaction of a cathode tank electrolyte and potassium ions in a salt bridge can be used as a potassium hydroxide solution required by the anode tank electrolyte, and therefore the maximum utilization of reactants is achieved.
After the electrolysis is stopped, adding hydrogen chloride solid into the potassium stannate solution obtained by the anode tank reaction to react to obtain potassium chloride solution and tin hydroxide precipitate, wherein the reaction comprises the following steps: h2O+SnO3 2-+2H+→Sn(OH)4The pH value of the solution is slowly reduced along with the increase of the added hydrogen chloride solid, when the pH value of the solution is reduced to 1, the tin hydroxide precipitate is completely separated out, the tin hydroxide precipitate is filtered, and is filtered, cleaned, dried and sintered to obtain tin oxide, and the residual potassium chloride solution can be recycled for preparing a salt bridge, so that the maximum utilization of reactants is realized.
In the electrolytic process, the pH value of the reaction environment of the cathode slot needs to be ensured to be less than 14, if the pH value of the reaction environment of the cathode slot is greater than 14, the cathode electrolytic voltage is higher due to the overhigh pH value of the electrolyte of the cathode slot, the energy consumption is increased, and a small amount of hydrogen escapes to increase the risk.
In the electrolysis process, the electrolytic voltage is 2~20V, and when voltage was less than 2V, the deposit was appeared slowly, and electrolysis is inefficient, and when voltage was greater than 20V, because the voltage increase leads to the energy consumption to increase, and the deposit is appeared at a rate too fast in the anode tank in addition, and it is unstable to appear, can lead to the indium hydroxide granule that generates inhomogeneous, the granularity broad.
In the electrolytic process, indium hydroxide generated in the anode is prevented from being attached to the anode plate, so that the electrolysis of the reduced waste target is hindered, ultrasonic waves are introduced to the anode plate, the reaction process is stably carried out, and the uniformity of generated indium hydroxide particles is ensured.
In the electrolysis process, the temperature of the cathode tank and the anode tank is kept at 20-50 ℃, the conductivity of the deionized water is more than 10 mu s/cm, and when the conductivity of the deionized water is less than 10 mu s/cm, the electrolysis voltage is increased, and the energy consumption is increased.
For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1.
One embodiment of the present invention is a method of recycling an ITO scrap target. The method adopts an anode tank and a cathode tank with the size of 230 x 400mm and the capacity of 2.1L, wherein an anode and a cathode are respectively arranged in the anode tank and the cathode tank, and the anode tank and the cathode tank are connected through a salt bridge; using ITO waste target with the size of 20 x 100 x 6mm as a cathode to be installed in a cathode tank, using deionized water as cathode tank electrolyte, using reduction waste target as an anode to be installed in an anode tank, using potassium hydroxide solution as anode tank electrolyte, heating the anode tank and the cathode tank to 20 ℃, switching on a power supply, setting the voltage to be 2V, continuously carrying out electrolysis, monitoring the pH values of the anode tank and the cathode tank in real time in the electrolysis process, stopping electrolysis when the pH value of the reaction environment of the cathode tank is monitored to be more than 14, taking out the reduction waste target generated by the electrolysis reaction in the cathode tank as the anode to be installed in the anode tank, taking out the potassium hydroxide solution generated by the electrolysis reaction in the cathode tank as the anode tank electrolyte, continuously carrying out electrolysis, stopping the electrolysis when the pH value of the reaction environment of the anode tank is monitored to be less than 13, precipitating and filtering indium hydroxide generated by the electrolysis reaction in the anode tank, Washing, drying and sintering to obtain indium oxide, taking out a potassium stannate solution generated by an anode tank electrolysis reaction, adding hydrogen chloride to react to obtain a potassium chloride solution and a tin hydroxide precipitate, wherein the potassium chloride solution is used for recovering and preparing a salt bridge, and the tin hydroxide precipitate is filtered, washed, dried and sintered to obtain tin oxide.
Example 2.
One embodiment of the present invention is a method of recycling an ITO scrap target. The method adopts an anode tank and a cathode tank with the size of 230 x 400mm and the capacity of 2.1L, wherein an anode and a cathode are respectively arranged in the anode tank and the cathode tank, and the anode tank and the cathode tank are connected through a salt bridge; using ITO waste target with the size of 20 x 100 x 6mm as a cathode to be installed in a cathode tank, using deionized water as cathode tank electrolyte, using reduction waste target as an anode to be installed in an anode tank, using potassium hydroxide solution as anode tank electrolyte, heating the anode tank and the cathode tank to 50 ℃, switching on a power supply, setting the voltage to be 20V, continuously carrying out electrolysis, monitoring the pH values of the anode tank and the cathode tank in real time in the electrolysis process, stopping electrolysis when the pH value of the reaction environment of the cathode tank is monitored to be more than 14, taking out the reduction waste target generated by the electrolysis reaction in the cathode tank as the anode to be installed in the anode tank, taking out the potassium hydroxide solution generated by the electrolysis reaction in the cathode tank as the anode tank electrolyte, continuously carrying out electrolysis, stopping the electrolysis when the pH value of the reaction environment of the anode tank is monitored to be less than 13, precipitating and filtering indium hydroxide generated by the electrolysis reaction in the anode tank, Washing, drying and sintering to obtain indium oxide, taking out a potassium stannate solution generated by an anode tank electrolysis reaction, adding hydrogen chloride to react to obtain a potassium chloride solution and a tin hydroxide precipitate, wherein the potassium chloride solution is used for recovering and preparing a salt bridge, and the tin hydroxide precipitate is filtered, washed, dried and sintered to obtain tin oxide.
Example 3.
One embodiment of the present invention is a method of recycling an ITO scrap target. The method adopts an anode tank and a cathode tank with the size of 230 x 400mm and the capacity of 2.1L, wherein an anode and a cathode are respectively arranged in the anode tank and the cathode tank, and the anode tank and the cathode tank are connected through a salt bridge; using ITO waste target with the size of 20 x 100 x 6mm as a cathode to be installed in a cathode tank, using deionized water as cathode tank electrolyte, using reduction waste target as an anode to be installed in an anode tank, using potassium hydroxide solution as anode tank electrolyte, heating the anode tank and the cathode tank to 35 ℃, switching on a power supply, setting the voltage to be 11V, continuously carrying out electrolysis, monitoring the pH values of the anode tank and the cathode tank in real time in the electrolysis process, stopping electrolysis when the pH value of the reaction environment of the cathode tank is monitored to be more than 14, taking out the reduction waste target generated by the electrolysis reaction in the cathode tank as the anode to be installed in the anode tank, taking out the potassium hydroxide solution generated by the electrolysis reaction in the cathode tank as the anode tank electrolyte, continuously carrying out electrolysis, stopping the electrolysis when the pH value of the reaction environment of the anode tank is monitored to be less than 13, precipitating and filtering indium hydroxide generated by the electrolysis reaction in the anode tank, Washing, drying and sintering to obtain indium oxide, taking out a potassium stannate solution generated by an anode tank electrolysis reaction, adding hydrogen chloride to react to obtain a potassium chloride solution and a tin hydroxide precipitate, wherein the potassium chloride solution is used for recovering and preparing a salt bridge, and the tin hydroxide precipitate is filtered, washed, dried and sintered to obtain tin oxide.
The invention provides a method for recycling an ITO waste target, wherein a cathode is the ITO waste target, an anode is a reduction waste target obtained after the electrolysis of the cathode ITO waste target, an anode tank and a cathode tank are connected through a salt bridge to form an electrolysis loop for coupled electrolysis, indium oxide is prepared after indium hydroxide generated by the anode tank is roasted, tin oxide is prepared after tin hydroxide obtained by the reaction of potassium stannate solution and hydrogen chloride in the anode tank is roasted, the salt bridge can be prepared from the residual potassium chloride solution, so that inorganic waste liquid is not generated in the whole electrolysis process, the maximum utilization of reactants is realized in the whole process, the cathode and anode tanks are not required to be separated by ion diaphragms, the separation effect of indium and tin ions is good, and the ITO waste target is recycled at the lowest electrolysis cost.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (10)
1. A method for recycling an ITO waste target is characterized by comprising the following steps: the method comprises the steps of taking an ITO waste target as a cathode and deionized water as cathode tank electrolyte, generating a reduction waste target after electrolysis in a cathode area, taking the reduction waste target as an anode and a potassium hydroxide solution as anode tank electrolyte, connecting the anode tank and the cathode tank through a salt bridge to form an electrolysis loop for coupling electrolysis, and obtaining a potassium stannate solution and an indium hydroxide precipitate after electrolysis in the anode area.
2. The method for recycling the ITO waste target according to claim 1, wherein the step of obtaining a potassium stannate solution and an indium hydroxide precipitate after the anode region electrolysis further comprises the following steps: and (3) precipitating the indium hydroxide precipitate in a potassium stannate solution, and adding a hydrogen chloride solid into the potassium stannate solution to react to obtain a potassium chloride solution and a tin hydroxide precipitate.
3. The method for recycling the ITO waste target according to claim 2, wherein the method further comprises the following steps after the indium hydroxide is precipitated in the potassium stannate solution: and filtering, cleaning, drying and sintering the indium hydroxide precipitate to obtain the indium oxide.
4. The method for recycling the ITO waste target according to claim 2, further comprising the steps of, after the step of adding hydrogen chloride solid into the potassium stannate solution to react to obtain a potassium chloride solution and a tin hydroxide precipitate: and filtering, cleaning, drying and sintering the tin hydroxide precipitate to obtain the tin oxide.
5. The method for recycling an ITO waste target according to claim 1, wherein the pH of the reaction environment of the anode bath during the electrolysis is greater than 13.
6. The method for recycling an ITO waste target according to claim 1, wherein the pH of the reaction environment of the cathode bath during the electrolysis is less than 14.
7. The method for recycling an ITO waste target according to claim 1, wherein the salt bridge is a U-shaped circular or square pipeline composed of agar and a saturated potassium chloride solution.
8. The method for recycling an ITO waste target according to claim 1, wherein ultrasonic waves are introduced into the anode tank using an ultrasonic generator during the electrolysis.
9. The method for recycling an ITO waste target according to claim 1, wherein the temperature of the cathode bath and the anode bath is maintained at 20 to 50 ℃ during the electrolysis.
10. The method for recycling the ITO waste target according to claim 1, wherein the voltage of electrolysis is 2 to 20V during the electrolysis.
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Application publication date: 20201023 |