CN109504858B - Method for preparing indium hydroxide by using ITO waste material - Google Patents
Method for preparing indium hydroxide by using ITO waste material Download PDFInfo
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- CN109504858B CN109504858B CN201811548751.1A CN201811548751A CN109504858B CN 109504858 B CN109504858 B CN 109504858B CN 201811548751 A CN201811548751 A CN 201811548751A CN 109504858 B CN109504858 B CN 109504858B
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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
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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
- C22B58/00—Obtaining gallium or indium
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Abstract
The invention relates to a method for preparing indium hydroxide by using ITO waste materials, which comprises the following steps: s1: crushing and ball-milling; s2: leaching with nitric acid; s3: adsorbing and removing impurities; s4: neutralizing with alkali liquor. The method utilizes the ITO waste as the raw material, does not need the process of reducing the metal simple substance, can separate the metal tin and the indium, and finally prepares the indium hydroxide which can be used as the raw material for preparing the indium oxide.
Description
Technical Field
The invention relates to the field of resource recovery, in particular to a method for preparing indium hydroxide by using ITO waste materials.
Background
Indium belongs to rare metals and is an important material for electronic industry. ITO (indium tin oxide) target material is widely used in the electronic information industry for manufacturing thin film transistors, liquid crystal displays, plasma displays, and the like. The utilization rate of the ITO target material in the sputtering coating process is low, and the scrap materials such as leftover materials, cutting scraps and the like generated in the processing process are more, so that the ITO target material can be used as a raw material for recycling indium, and the recycling of resources is realized.
Chinese patent CN101528988B discloses a method for recovering valuable metals from ITO scrap by electrolysis, which has the technical defects: the electrolysis bath is separated by using a special ion exchange membrane, the electrolysis process is discontinuous, the operation is complicated, the investment and the production cost are high, and the residual anode, small ITO waste materials and waste powder are difficult to recover by the method.
Chinese patent application CN104032133A discloses a method for recovering metal indium and tin from an ITO waste target, which comprises the steps of cleaning the surface of the ITO waste target, and generating indium-tin alloy by using reducing substance activated carbon or graphite at the high temperature of 1000-1600 ℃ under the protection of non-oxidizing gas. The technical defects are as follows: the method only needs high-temperature equipment to obtain the indium-tin alloy without further separating the metal indium and tin.
Therefore, it is necessary to design a method for preparing indium hydroxide using ITO scrap to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a method for preparing indium hydroxide by using an ITO scrap, which can separate metal indium and tin and finally obtain indium hydroxide.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for preparing indium hydroxide by using ITO scrap comprises the following steps:
s1: crushing and ball-milling: crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, and then sieving the ITO waste material by a 230-mesh sieve to obtain undersize materials;
s2: leaching with nitric acid: according to the solid-liquid ratio of undersize materials to water of 1: 5-7, adding the undersize into water, stirring at a first stirring speed to form a first mixed solution, heating the first mixed solution to 75-90 ℃, dropwise adding acid liquor which is 1.5-2 times of the theoretical acid amount required by complete dissolution into the first mixed solution, wherein the acid liquor is 65-68% by mass of concentrated nitric acid, dropwise adding the concentrated nitric acid for 2-3 hours to form a second mixed solution, heating the second mixed solution to 75-90 ℃, carrying out heat preservation reaction for 4-12 hours, and centrifuging to obtain a first filtrate and a first filter residue, wherein the first filtrate is an indium nitrate solution, and the first filter residue is tin dioxide;
s3: adsorbing and removing impurities: enabling all or part of the obtained indium nitrate solution to pass through multistage series chelating resin, and carrying out selective ion exchange at a certain flow rate, wherein impurity ions are all adsorbed on the chelating resin, and the balance is pure indium nitrate solution;
s4: alkali liquor neutralization: and adding alkali liquor into the pure indium nitrate solution to adjust the pH value to 7.0-8.0 to form a third mixed solution, and centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, wherein the second filter residue is indium hydroxide.
As a further improvement of the invention, the alkali liquor is concentrated ammonia water.
As a further improvement of the invention, the mass fraction of the strong ammonia water is 25-28%.
As a further improvement of the invention, the first stirring speed is 450-700 r/min.
As a further improvement of the invention, the chelating resin is a 4-stage series chelating resin.
As a further improvement of the invention, the flow rate of the selective ion exchange is 2-6 BVH.
As a further improvement of the present invention, In accounts for 74.44% of the mass fraction of the ITO scrap, and Sn accounts for 7.88% of the mass fraction of the ITO scrap.
The method utilizes the ITO waste as the raw material, does not need the process of reducing the metal simple substance, can separate the metal tin and the indium, and finally prepares the indium hydroxide which can be used as the raw material for preparing the indium oxide.
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 preparing indium hydroxide by using an ITO waste material, which comprises the following steps.
S1: crushing and ball-milling: and crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, and then sieving the ITO waste material by using a 230-mesh sieve to obtain undersize materials.
S2: leaching with nitric acid: according to the solid-liquid ratio of undersize materials to water of 1: 5-7, adding the undersize into water, stirring at a first stirring speed to form a first mixed solution, heating the first mixed solution to 75-90 ℃, dropwise adding acid liquor which is 1.5-2 times of the theoretical acid amount required for complete dissolution into the first mixed solution, wherein the acid liquor is 65% concentrated nitric acid in mass fraction, dropwise adding the concentrated nitric acid for 2-3h to form a second mixed solution, heating the second mixed solution to 75-90 ℃, carrying out heat preservation reaction for 4-12h, and centrifuging to obtain a first filtrate and a first filter residue, wherein the first filtrate is an indium nitrate solution, and the first filter residue is tin dioxide.
S3: adsorbing and removing impurities: and (3) passing all or part of the obtained indium nitrate solution through multistage series chelating resin, carrying out selective ion exchange at a certain flow rate, adsorbing all impurity ions on the chelating resin, and leaving pure indium nitrate solution.
S4: alkali liquor neutralization: and adding alkali liquor into the pure indium nitrate solution to adjust the pH value to 7.0-8.0 to form a third mixed solution, and centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, wherein the second filter residue is indium hydroxide.
In certain embodiments of the invention, the base solution is concentrated ammonia.
In certain embodiments of the present invention, the mass fraction of the concentrated aqueous ammonia is 25% to 28%.
In some embodiments of the present invention, the first stirring speed is 450-.
In certain embodiments of the invention, the chelating resin is a 4-stage tandem chelating resin.
In certain embodiments of the invention, the flow rate of the selective ion exchange is 2 to 6 BVH.
The ITO scrap used In the following examples was indium tin oxide, In was 74.44% by mass of the ITO scrap, and Sn was 7.88% by mass of the ITO scrap, and the ITO scrap contained only trace amounts of impurity elements.
The method firstly separates metal indium and tin, then prepares tin dioxide and indium hydroxide respectively, the recovery rate of tin is over 99 percent, and the recovery rate of indium is over 94 percent.
Example 1.
A method for preparing indium hydroxide from an ITO scrap includes the following steps.
Crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, sieving with a 230-mesh sieve to obtain sieved substances, wherein the sieved substances are particles smaller than 63 micrometers, and the particles larger than or equal to 63 micrometers, which cannot pass through the 230-mesh sieve, return to the ball mill for ball milling.
Weighing 100g of the undersize, adding 100g of the undersize into 500mL of water, stirring at a stirring speed of 450r/min to form a first mixed solution, heating the first mixed solution to 80 ℃, slowly and uniformly dropwise adding 202mL of concentrated nitric acid with a mass fraction of 65% into the first mixed solution, dropwise adding the concentrated nitric acid for 2.5 hours to form a second mixed solution, carrying out heat preservation reaction for 6 hours, centrifuging the second mixed solution to obtain a first filtrate and a first filter residue, wherein the first filtrate accounts for 720mL, the first filter residue is tin dioxide, the dried tin dioxide weighs 8.1g, sampling and inspecting the dried tin dioxide, and detecting the contents of impurities such as indium, tin, iron, copper, zinc, calcium, lead and the like in the first filtrate by adopting ICP-MS. The indium content in the first filtrate is 102.87g/L, the contents of other impurity metal elements are less than 10mg/L, and analysis shows that the leaching rate of indium is 99.5%, the purity of tin dioxide is 97.3%, and the recovery rate of tin is 99.9%.
Enabling 600mL of the obtained indium nitrate solution to pass through four serially-connected chromatographic columns each containing 100mL of chelate resin, controlling the flow rate to be 2BVH, obtaining a pure indium nitrate solution after 3h of adsorption, sampling and inspecting the pure indium nitrate solution, and displaying an ICP-MS detection result: the content of indium is 98.76 g/L, and the content of other impurity metal elements is less than 1 mg/L.
And (3) taking 500mL of the pure indium nitrate solution, stirring at a stirring speed of 300r/min, adding 25% by mass of concentrated ammonia water into the pure indium nitrate solution to adjust the pH value to 7.5 to form a third mixed solution, centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, and drying the second filter residue to obtain 71.2g of indium hydroxide, wherein the purity of the indium hydroxide reaches 99.96% through analysis, and the total recovery rate of the indium is 95.5%.
Example 2.
A method for preparing indium hydroxide from an ITO scrap includes the following steps.
Crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, sieving with a 230-mesh sieve to obtain sieved substances, wherein the sieved substances are particles smaller than 63 micrometers, and the particles larger than or equal to 63 micrometers, which cannot pass through the 230-mesh sieve, return to the ball mill for ball milling.
Weighing 100g of the undersize, adding 100g of the undersize into 600mL of water, stirring at a stirring speed of 600r/min to form a first mixed solution, heating the first mixed solution to 85 ℃, slowly and uniformly dropwise adding 270mL of concentrated nitric acid with a mass fraction of 65% into the first mixed solution, after dropwise adding the concentrated nitric acid for 3 hours, forming a second mixed solution, carrying out heat preservation reaction for 10 hours, centrifuging the second mixed solution to obtain a first filtrate and a first filter residue, wherein the first filtrate accounts for 870mL in total, the first filter residue is tin dioxide, the dried tin dioxide weighs 7.93g, sampling and inspecting the dried tin dioxide, and detecting the contents of impurities such as indium, tin, iron, copper, zinc, calcium, lead and the like in the first filtrate by adopting ICP-MS. The indium content in the first filtrate is 85.22g/L, the contents of other impurity metal elements are less than 10mg/L, and analysis shows that the leaching rate of indium is 99.6%, the purity of tin dioxide is 99.4%, and the recovery rate of tin is 99.9%.
Enabling 600mL of the obtained indium nitrate solution to pass through four serially-connected chromatographic columns each containing 100mL of chelate resin, controlling the flow rate to be 4BVH, obtaining a pure indium nitrate solution after 1.5h of adsorption, sampling and inspecting the pure indium nitrate solution, and displaying the detection result of ICP-MS: the content of indium is 81.98g/L, and the content of other impurity metal elements is less than 1 mg/L.
Taking 500mL of the pure indium nitrate solution, stirring at a stirring speed of 400r/min, adding 27% by mass of concentrated ammonia water into the pure indium nitrate solution to adjust the pH value to 7.0 to form a third mixed solution, centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, drying the second filter residue to obtain 59.2g of indium hydroxide, and analyzing to obtain the indium hydroxide with the purity of 99.97% and the total recovery rate of 95.8%.
Example 3.
A method for preparing indium hydroxide from an ITO scrap includes the following steps.
Crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, sieving with a 230-mesh sieve to obtain sieved substances, wherein the sieved substances are particles smaller than 63 micrometers, and the particles larger than or equal to 63 micrometers, which cannot pass through the 230-mesh sieve, return to the ball mill for ball milling.
Weighing 100g of the undersize, adding 100g of the undersize into 700mL of water, stirring at a stirring speed of 700r/min to form a first mixed solution, heating the first mixed solution to 75 ℃, slowly and uniformly dropwise adding 202mL of concentrated nitric acid with a mass fraction of 68% into the first mixed solution, after dropwise adding the concentrated nitric acid for 2 hours, forming a second mixed solution, carrying out heat preservation reaction for 8 hours, centrifuging the second mixed solution to obtain a first filtrate and a first filter residue, wherein the first filtrate accounts for 910mL in total, the first filter residue is tin dioxide, the dried tin dioxide weighs 7.97g, sampling and inspecting the dried tin dioxide, and detecting the contents of impurities such as indium, tin, iron, copper, zinc, calcium, lead and the like in the first filtrate by adopting ICP-MS. The indium content in the first filtrate is 81.23g/L, the contents of other impurity metal elements are less than 10mg/L, and analysis shows that the leaching rate of indium is 99.3%, the purity of tin dioxide is 98.9%, and the recovery rate of tin is 99.9%.
Enabling 600mL of the obtained indium nitrate solution to pass through four serially-connected chromatographic columns each containing 100mL of chelate resin, controlling the flow rate to be 6BVH, obtaining a pure indium nitrate solution after 1h of adsorption, sampling and inspecting the pure indium nitrate solution, and displaying an ICP-MS detection result: the content of indium is 77.57g/L, and the content of other impurity metal elements is less than 1 mg/L.
And (3) taking 500mL of the pure indium nitrate solution, stirring at a stirring speed of 500r/min, adding 26% by mass of concentrated ammonia water into the pure indium nitrate solution to adjust the pH value to 7.8 to form a third mixed solution, centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, and drying the second filter residue to obtain 56.0g of indium hydroxide, wherein the purity of the indium hydroxide reaches 99.95% and the total recovery rate of the indium is 94.8% through analysis.
Example 4.
A method for preparing indium hydroxide from an ITO scrap includes the following steps.
Crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, sieving with a 230-mesh sieve to obtain sieved substances, wherein the sieved substances are particles smaller than 63 micrometers, and the particles larger than or equal to 63 micrometers, which cannot pass through the 230-mesh sieve, return to the ball mill for ball milling.
Weighing 100g of the undersize, adding 100g of the undersize into 600mL of water, stirring at a stirring speed of 550r/min to form a first mixed solution, heating the first mixed solution to 90 ℃, slowly and uniformly dropwise adding 270mL of concentrated nitric acid with a mass fraction of 66% into the first mixed solution, after dropwise adding the concentrated nitric acid for 3 hours, forming a second mixed solution, carrying out heat preservation reaction for 6 hours, centrifuging the second mixed solution to obtain a first filtrate and a first filter residue, wherein the first filtrate totally 855mL, the first filter residue is tin dioxide, the dried tin dioxide weighs 7.90g, sampling and inspecting the dried tin dioxide, and detecting the contents of impurities such as indium, tin, iron, copper, zinc, calcium, lead and the like in the first filtrate by adopting ICP-MS. The indium content in the first filtrate is 86.8g/L, the contents of other impurity metal elements are less than 10mg/L, and analysis shows that the indium leaching rate is 99.7%, the purity of the tin dioxide is 99.8%, and the recovery rate of the tin is 99.9%.
Enabling 600mL of the obtained indium nitrate solution to pass through four serially-connected chromatographic columns each containing 100mL of chelate resin, controlling the flow rate to be 5 BVH, obtaining a pure indium nitrate solution after 1.2h of adsorption, sampling and inspecting the pure indium nitrate solution, and displaying the detection result of ICP-MS: the content of indium is 82.8g/L, and the content of other impurity metal elements is less than 1 mg/L.
And (3) taking 500mL of the pure indium nitrate solution, stirring at a stirring speed of 300r/min, adding 28% by mass of concentrated ammonia water into the pure indium nitrate solution to adjust the pH value to 8.0 to form a third mixed solution, centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, and drying the second filter residue to obtain 59.8g of indium hydroxide, wherein the purity of the indium hydroxide reaches 99.9% through analysis, and the total recovery rate of the indium is 95.1%.
The method utilizes the ITO waste as the raw material, does not need the process of reducing the metal simple substance, can separate the metal tin and the indium, and finally prepares the indium hydroxide which can be used as the raw material for preparing the indium oxide.
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 (7)
1. A method for preparing indium hydroxide by using ITO waste materials is characterized by comprising the following steps: which comprises the following steps:
s1: crushing and ball-milling: crushing and ball-milling the ITO waste material by adopting a crusher and a ball mill, and then sieving the ITO waste material by a 230-mesh sieve to obtain undersize materials;
s2: leaching with nitric acid: according to the solid-liquid ratio of undersize materials to water of 1: 5-7, adding the undersize into water, stirring at a first stirring speed to form a first mixed solution, heating the first mixed solution to 75-90 ℃, dropwise adding acid liquor which is 1.5-2 times of the theoretical acid amount required by complete dissolution into the first mixed solution, wherein the acid liquor is 65-68% by mass of concentrated nitric acid, dropwise adding the concentrated nitric acid for 2-3 hours to form a second mixed solution, heating the second mixed solution to 75-90 ℃, carrying out heat preservation reaction for 4-12 hours, and centrifuging to obtain a first filtrate and a first filter residue, wherein the first filtrate is an indium nitrate solution, and the first filter residue is tin dioxide;
s3: adsorbing and removing impurities: enabling all or part of the obtained indium nitrate solution to pass through multistage series chelating resin, and carrying out selective ion exchange at a certain flow rate, wherein impurity ions are all adsorbed on the chelating resin, and the balance is pure indium nitrate solution;
s4: alkali liquor neutralization: and adding alkali liquor into the pure indium nitrate solution to adjust the pH value to 7.0-8.0 to form a third mixed solution, and centrifuging the third mixed solution to obtain a second filtrate and a second filter residue, wherein the second filter residue is indium hydroxide.
2. The method for preparing indium hydroxide using an ITO scrap according to claim 1, wherein: the alkali liquor is strong ammonia water.
3. The method for preparing indium hydroxide using an ITO scrap according to claim 2, wherein: the mass fraction of the strong ammonia water is 25-28%.
4. The method for preparing indium hydroxide using an ITO scrap according to claim 1, wherein: the first stirring speed is 450-700 r/min.
5. The method for preparing indium hydroxide using an ITO scrap according to claim 1, wherein: the chelating resin is a 4-grade series chelating resin.
6. The method for preparing indium hydroxide using an ITO scrap according to claim 1, wherein: the flow rate of the selective ion exchange was 2-6 BVH.
7. The method for preparing indium hydroxide using an ITO scrap according to claim 1, wherein: in was 74.44% by mass of the ITO scrap and Sn was 7.88% by mass of the ITO scrap.
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| CN112359243B (en) * | 2020-11-11 | 2022-06-17 | 广东先导稀材股份有限公司 | Method for preparing indium tin alloy by reducing ITO waste target by starch |
| CN112708763B (en) * | 2020-12-15 | 2022-09-06 | 先导薄膜材料（广东）有限公司 | Method for recovering valuable metal from ITO waste target |
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| CN102828054A (en) * | 2012-09-03 | 2012-12-19 | 四川长虹电器股份有限公司 | Method for recovering indium from waste liquid crystal panels through acid leaching-cation exchange resin adsorption technology |
| CN104630486B (en) * | 2015-01-28 | 2017-02-22 | 江苏理工学院 | Method for recovering indium oxide and stannum from ITO coating film of conducting glass |
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