CN112708763B - Method for recovering valuable metal from ITO waste target - Google Patents

Method for recovering valuable metal from ITO waste target Download PDF

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CN112708763B
CN112708763B CN202011472228.2A CN202011472228A CN112708763B CN 112708763 B CN112708763 B CN 112708763B CN 202011472228 A CN202011472228 A CN 202011472228A CN 112708763 B CN112708763 B CN 112708763B
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indium
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zinc
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CN112708763A (en
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耿瑞丽
刘鸿飞
张文涛
肖红军
殷亮
朱刘
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Vital Thin Film Materials Guangdong Co Ltd
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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
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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
    • C22B25/00—Obtaining tin
    • C22B25/04—Obtaining tin by wet processes
    • 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
    • C22B25/00—Obtaining tin
    • C22B25/06—Obtaining tin from scrap, especially tin scrap
    • 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
    • C22B58/00—Obtaining gallium or indium
    • 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 recovering valuable metals from an ITO waste target, which comprises the following steps: dissolving an ITO waste target by using acid to obtain a first solution, adjusting the pH value of the first solution to 0.5-2.5, adding indium-zinc alloy powder into the first solution for reaction, filtering and separating to obtain tin slag and a second solution, adding zinc powder into the second solution for reaction, filtering and separating to obtain sponge indium and a third solution. According to the difference of metal activity of zinc, indium and tin, indium-zinc alloy powder is used for replacing a first solution to obtain tin slag and a second solution, the tin slag can be purified to obtain metal tin, the second solution is replaced by zinc powder to obtain sponge indium and a third solution, and the sponge indium is distilled by a vacuum distillation furnace to remove zinc to obtain refined indium, so that valuable metals are effectively recovered from the ITO waste target.

Description

Method for recovering valuable metal from ITO waste target
Technical Field
The invention relates to the technical field of resource recovery, in particular to a method for recovering valuable metals from an ITO (indium tin oxide) waste target.
Background
In recent years, indium-tin oxide (In) 2 O 3 -SnO 2 Generally referred to as ITO) sputtering targets are widely used in many electronic components such as transparent conductive thin films of liquid crystal display devices and gas sensors, and in the application of ITO, a thin film of conductive oxide is formed on a substrate by a sputtering method, which is called sputtering coating, in which a target material is not uniformly consumed but a part of the target material is severely consumed, called an etching portion, which continues a sputtering operation until a backing plate supporting the target is exposed, and the target material cannot be reused 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 abrasive powder and 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, in a method for recovering valuable metals from an ITO (indium tin oxide) waste target by adopting an electrolysis method, inorganic waste liquid is generated by mostly adopting inorganic acid as electrolyte, and when an anode tank and a cathode tank are 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 valuable metals from the ITO waste target.
Disclosure of Invention
An object of the present invention is to provide a method for recovering valuable metals from ITO-waste targets, in order to overcome the disadvantages of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a method for recovering valuable metals from an ITO waste target, which comprises the following steps: dissolving an ITO waste target by using acid to obtain a first solution, adjusting the pH value of the first solution to 0.5-2.5, adding indium-zinc alloy powder into the first solution for reaction, filtering and separating to obtain tin slag and a second solution, adding zinc powder into the second solution for reaction, filtering and separating to obtain sponge indium and a third solution.
As a further improvement of the invention, the indium-zinc alloy powder is prepared by the following method: firstly, the mass ratio is 1: 1-1: melting the indium ingots and the zinc ingots of 20 to prepare indium-zinc alloy, and preparing the indium-zinc alloy into indium-zinc alloy powder by using an ultrasonic atomization method.
As a further improvement of the invention, the particle size of the indium-zinc alloy powder is controlled to be between 10 and 100 um.
As a further improvement of the invention, the indium raw material is 4N indium ingot, and the zinc raw material is 4N zinc ingot.
As a further improvement of the present invention, the acid used for dissolving the ITO waste target is one of hydrochloric acid, sulfuric acid, or nitric acid.
As a further improvement of the present invention, after the step of adding zinc powder into the second solution to react and filtering and separating to obtain sponge indium and a third solution, the method further comprises: and casting the sponge indium briquettes into indium ingots, and then putting the indium ingots into a vacuum distillation furnace for removing zinc by distillation to obtain refined indium.
As a further improvement of the invention, in the process of adding the indium-zinc alloy powder into the first solution for reaction, the reaction time is controlled to be 30-120 min, the reaction temperature is controlled to be 30-60 ℃, and the stirring is continuously carried out.
As a further improvement of the method, in the process of adding the zinc powder into the second solution for reaction, the reaction time is controlled to be 30-240 min, and the stirring is continuously carried out.
As a further improvement of the invention, the reaction temperature is controlled to be between 40 and 60 ℃.
As a further improvement of the invention, the purity of the zinc powder is 4N.
According to the difference of metal activity of zinc, indium and tin, indium-zinc alloy powder is used for replacing a first solution to obtain tin slag and a second solution, the tin slag can be purified to obtain metal tin, the second solution is replaced by zinc powder to obtain sponge indium and a third solution, and the sponge indium is distilled by a vacuum distillation furnace to remove zinc to obtain refined indium, so that valuable metals are effectively recovered from the ITO waste target.
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 present invention provides a method for recovering valuable metals from an ITO scrap target, the preparation method comprising the following steps.
Dissolving the waste ITO target with acid to obtain a first solution, wherein the acid used for dissolving the waste ITO target is one of hydrochloric acid, sulfuric acid or nitric acid, the hydrochloric acid is used for dissolving the waste ITO target, and the first solution obtained after dissolving the waste ITO target is mainly indium chloride solution, and the main metal impurity of the first solution is Sn 4+ 、Ni 2+ 、Cd 2+ 、Cu 2+ 、Co 2+ 、Pb 2+ 。
After the first solution is obtained, the pH value of the first solution is adjusted to be 0.5-2.5, the pH value is preferably adjusted to be 0.5-1.5, when the pH value is too high, indium ions and tin ions in the solution are hydrolyzed to form hydroxide precipitates, when the pH value is too low, excessive hydrogen ions in the solution react with indium-zinc alloy powder, the consumption of the indium-zinc alloy powder in the replacement and impurity removal process is increased, acid or alkali can be adopted for adjusting the pH value, the adopted acid can be one of hydrochloric acid, sulfuric acid or nitric acid, and the alkali adopted for adjusting the pH value can be one of sodium hydroxide, potassium hydroxide, calcium hydroxide or ammonia water.
And adding indium-zinc alloy powder into the first solution for reaction, and filtering and separating to obtain tin slag and a second solution.
Because the metal activity of zinc is greater than that of indium and the metal activity of indium is greater than that of tin, the indium-zinc alloy powder can convert Sn in solution 4+ The first solution is replaced by simple substance, and the indium-zinc alloy powder also converts Ni in the first solution 2+ 、Cd 2+ 、Cu 2+ 、Co 2+ 、Pb 2+ And displacing the simple substance to form tin slag mainly containing nickel, cadmium, copper, cobalt and lead after the displacement reaction, purifying the tin slag to obtain metal tin, and using indium chloride and zinc chloride solutions as the second solution.
In the process of recovering tin and indium from the ITO waste target, the indium-zinc alloy powder is prepared by the following method: mixing the components in a mass ratio of 1: 1-1: melting the 4N indium ingots and the 4N zinc ingots of 20 to prepare indium-zinc alloy, and then preparing the indium-zinc alloy into indium-zinc alloy powder by an ultrasonic atomization method, wherein the granularity of the obtained indium-zinc alloy powder is controlled to be 10-100 um, the granularity of the indium-zinc alloy powder is preferably controlled to be 10-50 um, and the zinc-indium alloy powder has a large specific surface area, so that impurity metals in the solution can be quickly replaced, and the replacement and impurity removal effects are improved.
In the process of adding the indium-zinc alloy powder into the first solution for reaction, the reaction time is controlled to be 30-120 min, the reaction temperature is controlled to be 30-60 ℃, and the mixture is continuously stirred; and in the process of adding the zinc powder into the second solution for reaction, the reaction time is controlled to be 30-240 min, the reaction temperature is controlled to be 40-60 ℃, and the stirring is continuously carried out.
In the process of adding the indium-zinc alloy powder into the first solution for reaction, the reaction time is preferably controlled to be 40-60 min, and the reaction temperature is preferably controlled to be 30-45 ℃; in the process of adding the zinc powder into the second solution for reaction, the reaction time is preferably controlled to be 40-60 min, and the reaction temperature is preferably controlled to be 30-45 ℃.
The zinc element in the indium-zinc alloy powder can be replaced by at least one element of zinc, magnesium, aluminum or iron, preferably a single zinc element, one or more metals which are more active than tin metal are adopted to form an alloy with indium metal for replacement reaction, and not only can Sn in solution be replaced 4+ Can also effectively remove impurity Ni after replacement 2+ 、Cd 2+ 、Cu 2+ 、Co 2+ 、Pb 2+ Therefore, the first solution with lower impurity content is obtained, the consumption of the zinc powder can be saved by adopting the alloy powder, the cost is saved, and the technical problem of lower impurity removal efficiency caused by only using the zinc powder is solved.
After obtaining the tin slag and the second solution, adding zinc powder with the purity of 4N into the second solution for reaction, filtering and separating to obtain sponge and a third solution, wherein the sponge contains zinc as a main impurity and also contains a small amount of inevitable impurities of tin, nickel, copper, cadmium, cobalt and lead, melting indium into indium ingots, and then placing the indium ingots into a vacuum distillation furnace for distillation, wherein the melting point of indium is 156.51 ℃, the boiling point of zinc is 2060 ℃, the melting point of zinc is 419.53 ℃, the boiling point of zinc is 907 ℃, and zinc is evaporated after vacuum distillation, so that 4.5N refined indium and zinc alloy are obtained.
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 carried out according to 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.
Weighing 100g of indium ingot and 100g of zinc ingot, mixing and melting to obtain indium-zinc alloy, and carrying out ultrasonic atomization on the indium-zinc alloy to obtain indium-zinc alloy powder with the granularity of 80-100 um.
Dissolving the ITO waste target by using hydrochloric acid to obtain a first solution, adjusting the pH of the first solution to be 1.5, and taking the first solution for component detection, wherein the components of the first solution are shown in Table 1.
TABLE 1 first solution composition (g/L).
Name (R) In Sn Cd Ni Co Pb
Content (wt.) 147 2.5 0.073 0.017 0.003 0.004
The process conditions are as follows: stirring at 120 rpm, pH 1.5 and temperature 40 deg.C, taking 1000ml of the first solution, adding 5.0g of common zinc powder into No. 1, adding 3.5g of indium-zinc alloy zinc powder into No. 2, performing 3 parallel tests on each group, reacting for 60min to obtain tin slag and a second solution, vacuum filtering, and testing the impurity content in the second solution, wherein the test results are shown in Table 2.
TABLE 2 impurity content (g/L) in the second solution.
Figure 713421DEST_PATH_IMAGE002
As seen from the above table: the purification effect of the indium-zinc alloy zinc powder with the dosage of 3.0g/L is better than that of the common zinc powder with the dosage of 5.0 g/L.
According to the tests, the impurity content of the second solution treated by the indium-zinc alloy powder is very low, the sponge indium is obtained by adding 4N zinc powder into the second solution for reaction, filtering and separating, then the sponge indium is pressed and cast into indium ingots, and then the indium ingots are placed in a vacuum distillation furnace for distillation, so that 4.5N refined indium is obtained.
Example 2.
Weighing 10g of indium ingot and 200g of zinc ingot, mixing and melting to obtain indium-zinc alloy, and carrying out ultrasonic atomization on the indium-zinc alloy to obtain indium-zinc alloy powder with the granularity of 10-30 um.
Dissolving the ITO waste target by using hydrochloric acid to obtain a first solution, adjusting the pH of the first solution to be 2.5, and taking the first solution for component detection, wherein the components of the first solution are shown in Table 3.
TABLE 3 first solution composition (g/L).
Composition (I) In Sn Cd Ni Co Pb
Content (wt.) 132 2.1 0.042 0.014 0.03 0.02
The process conditions are as follows: stirring at 120 rpm, pH 2.5 and 30 deg.C, taking 1000ml of the first solution, adding 5.0g of common zinc powder into No. 1, adding 3.0g of indium-zinc alloy zinc powder into No. 2, performing 3 parallel tests on each group, reacting for 120min to obtain tin slag and a second solution, vacuum filtering, and testing the impurity content in the second solution, wherein the test results are shown in Table 4.
TABLE 4 impurity level (g/L) in the second solution.
Figure 99403DEST_PATH_IMAGE004
From the above table: the purification effect of the indium-zinc alloy zinc powder with the dosage of 3.5g/L is better than that of the common zinc powder with the dosage of 5.0 g/L.
According to the tests, the impurity content of the second solution treated by the indium-zinc alloy powder is very low, the second solution is mainly indium chloride, 4N zinc powder is added into the second solution for reaction, filtering and separation are carried out, metal sponge indium is obtained, the metal sponge indium is melted, pressed into balls and cast into indium ingots, and then the indium ingots are placed in a vacuum distillation furnace for distillation, so that 4.5N refined indium is obtained.
Example 3.
Weighing 40g of indium ingot and 200g of zinc ingot, mixing and melting to obtain indium-zinc alloy, and carrying out ultrasonic atomization on the indium-zinc alloy to obtain indium-zinc alloy powder with the granularity of 40-60 um.
Dissolving the ITO waste target by using hydrochloric acid to obtain a first solution, adjusting the pH of the first solution to be 1.0, and taking the first solution for component detection, wherein the components of the first solution are shown in Table 5.
TABLE 5 first solution composition (g/L).
Name (R) In Sn Cd Ni Co Pb
Content (wt.) 183 3.4 0.072 0.016 0.04 0.01
The process conditions are as follows: stirring at 120 rpm, pH 1.0 and temperature 60 deg.C, taking 1000ml of the first solution, adding 5.0g of common zinc powder into No. 1, adding 3.8g of indium-zinc alloy zinc powder into No. 2, performing 3 parallel tests on each group, reacting for 30min to obtain tin slag and a second solution after reaction, vacuum filtering, and testing the impurity content in the second solution, wherein the test results are shown in Table 6.
TABLE 6 impurity level (g/L) in the second solution.
Figure 347982DEST_PATH_IMAGE006
As seen from the above table: the purification effect of the indium-zinc alloy zinc powder with the dosage of 3.8g/L is better than that of the common zinc powder with the dosage of 5.0 g/L.
According to the tests, the impurity content of the second solution treated by the indium-zinc alloy powder is very low, the second solution is mainly indium chloride, 4N zinc powder is added into the second solution for reaction, filtering and separation are carried out, metal sponge indium is obtained, the metal sponge indium is melted, pressed into balls and cast into indium ingots, and then the indium ingots are placed in a vacuum distillation furnace for distillation, so that 4.5N refined indium is obtained.
Example 4.
Weighing 20g of indium ingot and 200g of zinc ingot, mixing and melting to obtain indium-zinc alloy, and carrying out ultrasonic atomization on the indium-zinc alloy to obtain indium-zinc alloy powder with the granularity of 20-60 um.
Dissolving the ITO waste target by using hydrochloric acid to obtain a first solution, adjusting the pH of the first solution to be 0.5, and taking the first solution for component detection, wherein the components of the first solution are shown in Table 7.
TABLE 7 first solution composition (g/L).
Name (R) In Sn Cd Ni Co Pb
Content (c) of 152 2.8 0.025 0.01 0.03 0.02
The process conditions are as follows: stirring at 120 rpm, pH 1.0 and 50 deg.C, taking 1000ml of the first solution, adding 5.0g of common zinc powder into No. 1, adding 4.0g of indium-zinc alloy zinc powder into No. 2, performing 3 parallel tests on each group, reacting for 40min to obtain tin slag and a second solution, vacuum filtering, and testing the impurity content in the second solution, wherein the test results are shown in Table 8.
TABLE 8 impurity content (g/L) in the second solution.
Figure 8770DEST_PATH_IMAGE008
From the above table: the purification effect of the indium-zinc alloy zinc powder with the concentration of 4.0g/L is better than that of the common zinc powder with the concentration of 5.0 g/L.
According to the tests, the impurity content in the second solution is very low, the second solution is mainly indium chloride, 4N zinc powder is added into the second solution for reaction, filtering and separation are carried out, sponge indium is obtained, the sponge is pressed and cast into indium ingots, and then the indium ingots are placed in a vacuum distillation furnace for distillation, so that 4.5N refined indium is obtained.
According to the difference of metal activity of zinc, indium and tin, indium-zinc alloy powder is used for replacing a first solution to obtain tin slag and a second solution, the tin slag can be purified to obtain metal tin, the second solution is replaced by zinc powder to obtain sponge indium and a third solution, and the sponge indium is distilled by a vacuum distillation furnace to remove zinc to obtain refined indium, so that the valuable metal is effectively recovered from the ITO waste target.
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 (4)

1. A method for recovering valuable metals from an ITO scrap target, comprising the steps of:
dissolving an ITO waste target by using acid to obtain a first solution, adjusting the pH value of the first solution to 0.5-2.5, adding indium-zinc alloy powder into the first solution for reaction, filtering and separating to obtain tin slag and a second solution, adding zinc powder into the second solution for reaction, filtering and separating to obtain sponge indium and a third solution;
the acid used for dissolving the ITO waste target is hydrochloric acid;
first solution-indium chloride solution, which includes metallic impurity Sn 4+ 、Ni 2+ 、Cd 2+ 、Cu 2+ 、Co 2+ 、Pb 2+ ；
The indium-zinc alloy powder is prepared by the following method: firstly, the mass ratio is 1: 1-1: 20 melting the indium raw material and the zinc raw material to prepare indium-zinc alloy, and preparing the indium-zinc alloy into indium-zinc alloy powder by using an ultrasonic atomization method;
the granularity of the indium-zinc alloy powder is controlled to be between 10 and 100 um;
the indium raw material is 4N indium ingots, and the zinc raw material is 4N zinc ingots;
in the process of adding the indium-zinc alloy powder into the first solution for reaction, the reaction time is controlled to be 30-120 min, the reaction temperature is controlled to be 30-60 ℃, and the mixture is continuously stirred;
after the step of adding zinc powder into the second solution for reaction and filtering and separating to obtain sponge indium and a third solution, the method further comprises the following steps: and casting the sponge indium briquettes into indium ingots, and then putting the indium ingots into a vacuum distillation furnace for removing zinc by distillation to obtain refined indium.
2. The method for recovering valuable metals from an ITO waste target according to claim 1, wherein the reaction time is controlled to be 30-240 min and the stirring is continuously performed during the reaction of adding the zinc powder into the second solution.
3. The method for recovering valuable metals from an ITO waste target according to claim 2, wherein the reaction temperature is controlled to be 40-60 ℃.
4. The method for recovering valuable metals from an ITO waste target according to claim 1, wherein the purity of the zinc powder is 4N.
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