CN109504858A - 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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- CN109504858A CN109504858A CN201811548751.1A CN201811548751A CN109504858A CN 109504858 A CN109504858 A CN 109504858A CN 201811548751 A CN201811548751 A CN 201811548751A CN 109504858 A CN109504858 A CN 109504858A
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- indium
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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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- 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 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 present invention relates to resource reclaim field more particularly to a kind of methods for preparing indium hydroxide using ITO waste material.
Background technique
Indium belongs to rare metal, is a kind of important electronic industrial material.ITO(tin indium oxide) target electronic information produce
Industry prepares thin film transistor (TFT), liquid crystal display, plasma display etc. and has a wide range of applications.ITO target is plated in sputtering
Utilization rate is very low in membrane process, and the waste materials such as the leftover pieces generated in process and chip are more, can be used as the original of recovery indium
Material, realizes recycling for resource.
Chinese patent CN101528988B discloses a kind of method that valuable metal is recycled from ITO waste material, utilizes electrolysis
Indium metal is recycled, technological deficiency is: needing to separate electrolytic cell using special amberplex, electrolytic process does not connect
Continuous, cumbersome, investment and production cost are higher, while anode scrap, fritter ITO waste material and useless powder are difficult to back by this method
It receives.
Chinese patent application CN104032133A discloses a kind of method of useless target recycling indium metal tin of ITO, and first ITO gives up
Target surface cleaning, using reducing substances activated carbon or graphite 1000 DEG C ~ 1600 DEG C of high temperature and non-oxidizing gas protection
Lower generation indium stannum alloy.Its technological deficiency is: this method needs high-temperature service, has to indium stannum alloy, does not divide further
From indium metal, tin.
Thus, it is necessary to design a kind of the method for indium hydroxide is prepared to solve the above technical problems using ITO waste material.
Summary of the invention
It is an object of the invention to propose it is a kind of can separate indium metal, tin and can finally obtain indium hydroxide utilize ITO
The method that waste material prepares indium hydroxide.
To realize foregoing purpose, the present invention adopts the following technical scheme: a kind of side for preparing indium hydroxide using ITO waste material
Method comprising following steps:
S1: broken ball milling: being crushed ITO waste material using crusher, ball mill, ball milling, crosses 230 meshes later, is sieved
Lower object；
S2: nitric acid leaches: above-mentioned screenings being added to the water with the first mixing speed according to the solid-to-liquid ratio 1:5-7 of screenings and water
It is stirred to form the first mixed liquor, the first mixed liquor is heated to 75-90 DEG C, then be added dropwise and be completely dissolved into the first mixed liquor
1.5-2 times of acid solution of required theoretical acid amount, the acid solution are the concentrated nitric acid that mass fraction is 65%-68%, and concentrated nitric acid is in 2-3h
It is added dropwise to form the second mixed liquor, the second mixed liquor is heated to 75-90 DEG C, insulation reaction 4-12h, is centrifuged to obtain the first filtrate
With the first filter residue, first filtrate is nitric acid solution of indium, and first filter residue is stannic oxide；
S3: adsorption-edulcoration: by above-mentioned resulting all or part of nitric acid solution of indium by plural serial stage chelating resin, with certain
Flow velocity carry out selective ion exchange, foreign ion is all adsorbed on chelating resin, and remainder is that pure indium nitrate is molten
Liquid；
S4: lye neutralizes: lye being added into above-mentioned pure nitric acid solution of indium and adjusts pH to 7.0-8.0 formation third mixing
Liquid, third mixed liquor are centrifuged to obtain the second filtrate and the second filter residue, and second filter residue is indium hydroxide.
As a further improvement of the present invention, the lye is concentrated ammonia liquor.
As a further improvement of the present invention, the mass fraction of the concentrated ammonia liquor is 25%-28%.
As a further improvement of the present invention, first mixing speed is 450-700r/min.
As a further improvement of the present invention, the chelating resin is 4 grades of series connection chelating resins.
As a further improvement of the present invention, the flow velocity of selective ion exchange is 2-6 BVH.
As a further improvement of the present invention, In accounts for the 74.44% of ITO waste material mass fraction, Sn and accounts for ITO waste material quality point
Several 7.88%.
The present invention makees raw material using ITO waste material, without the process of reducing metal simple substance, can separate metallic tin and indium, most
The indium hydroxide being prepared eventually can be used as the raw material for preparing indium oxide, and this method is with process is short, easy to operate, the rate of recovery is high
The advantages of.
Specific embodiment
Technical solution is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention proposes a kind of method for preparing indium hydroxide using ITO waste material comprising following steps.
S1: broken ball milling: being crushed ITO waste material using crusher, ball mill, ball milling, crosses 230 meshes later, obtains
To screenings.
S2: nitric acid leaches: above-mentioned screenings being added to the water with the first stirring according to the solid-to-liquid ratio 1:5-7 of screenings and water
Speed is stirred to form the first mixed liquor, and the first mixed liquor is heated to 75-90 DEG C, then is added dropwise completely into the first mixed liquor
1.5-2 times of acid solution of theoretical acid amount needed for dissolving, the acid solution is the concentrated nitric acid that mass fraction is 65%, and concentrated nitric acid is in 2-3h
It is added dropwise to form the second mixed liquor, the second mixed liquor is heated to 75-90 DEG C, insulation reaction 4-12h, is centrifuged to obtain the first filtrate
With the first filter residue, first filtrate is nitric acid solution of indium, and first filter residue is stannic oxide.
S3: adsorption-edulcoration: passing through plural serial stage chelating resin for above-mentioned resulting all or part of nitric acid solution of indium, with
Certain flow velocity carries out selective ion exchange, and foreign ion is all adsorbed on chelating resin, and remainder is pure nitric acid
Solution of indium.
S4: lye neutralizes: it is mixed that lye adjusting pH to 7.0-8.0 formation third being added into above-mentioned pure nitric acid solution of indium
Liquid is closed, third mixed liquor is centrifuged to obtain the second filtrate and the second filter residue, and second filter residue is indium hydroxide.
In certain embodiments of the present invention, the lye is concentrated ammonia liquor.
In certain embodiments of the present invention, the mass fraction of the concentrated ammonia liquor is 25%-28%.
In certain embodiments of the present invention, first mixing speed is 450-700r/min.
In certain embodiments of the present invention, the chelating resin is 4 grades of series connection chelating resins.
In certain embodiments of the present invention, the flow velocity of selective ion exchange is 2-6 BVH.
ITO waste material used by following embodiment is indium tin oxide, and In accounts for the 74.44% of ITO waste material mass fraction, Sn
7.88%, the ITO waste material of ITO waste material mass fraction is accounted for containing only micro impurity element.
This method has separated indium metal, tin first, and stannic oxide and indium hydroxide, the recycling of tin are then prepared respectively
Rate is more than 99%, and the rate of recovery of indium is more than 94%.
Embodiment 1.
A method of indium hydroxide is prepared using ITO waste material comprising following steps.
ITO waste material is crushed using crusher, ball mill, ball milling, crosses 230 meshes, screenings is less than 63 microns
Particle, can not pass through 230 meshes more than or equal to 63 microns particle return ball mill ball milling.
Weigh above-mentioned screenings 100g, by 100g screenings be added 500mL water in and with the mixing speed of 450r/min into
Row stirring forms the first mixed liquor, the first mixed liquor is heated to 80 DEG C, then slowly drop evenly 202mL into the first mixed liquor
The concentrated nitric acid that mass fraction is 65%, concentrated nitric acid are added dropwise to form the second mixed liquor in 2.5h, and insulation reaction 6h is mixed second
It closes liquid and is centrifuged to obtain the first filtrate and the first filter residue, the first filtrate amount to 720mL, and the first filter residue is stannic oxide, and the two of drying
Tin oxide weight 8.1g, samples inspection for the stannic oxide of drying, using ICP-MS detect indium in the first filtrate, tin, iron, copper, zinc,
The content of the impurity such as calcium, lead.Indium content is 102.87g/L in first filtrate, and other impurities metal element content is both less than 10mg/
L, through analyzing, indium leaching rate is 99.5%, and stannic oxide purity is 97.3%, and the rate of recovery of tin is 99.9%.
Above-mentioned resulting nitric acid solution of indium 600mL is passed through into four concatenated each chromatographies that 100mL chelating resin is housed
Column obtains pure nitric acid solution of indium after coutroi velocity 2BVH, 3h absorption, pure indium nitrate solution sampling is sent
Inspection, ICP-MS testing result are shown: indium content is 98.76 g/L, and other impurities metal element content is respectively less than 1mg/L.
Above-mentioned pure nitric acid solution of indium 500mL is taken, is stirred with the mixing speed of 300r/min, it is molten to pure indium nitrate
Liquid is added the concentrated ammonia liquor that mass fraction is 25% and adjusts the formation third mixed liquor of pH to 7.5, and third mixed liquor is centrifuged to obtain the second filter
Liquid and the second filter residue dry the second filter residue to obtain indium hydroxide 71.2g, and through analyzing, the purity of indium hydroxide reaches 99.96%,
The overall recovery of indium is 95.5%.
Embodiment 2.
A method of indium hydroxide is prepared using ITO waste material comprising following steps.
ITO waste material is crushed using crusher, ball mill, ball milling, crosses 230 meshes, screenings is less than 63 microns
Particle, can not pass through 230 meshes more than or equal to 63 microns particle return ball mill ball milling.
Weigh above-mentioned screenings 100g, by 100g screenings be added 600mL water in and with the mixing speed of 600r/min into
Row stirring forms the first mixed liquor, the first mixed liquor is heated to 85 DEG C, then slowly drop evenly 270mL into the first mixed liquor
The concentrated nitric acid that mass fraction is 65%, concentrated nitric acid are added dropwise to form the second mixed liquor in 3h, insulation reaction 10h, by the second mixing
Liquid is centrifuged to obtain the first filtrate and the first filter residue, and the first filtrate amounts to 870mL, and the first filter residue is stannic oxide, the dioxy of drying
Change tin weight 7.93g, the stannic oxide of drying sampled into inspection, using ICP-MS detect indium in the first filtrate, tin, iron, copper, zinc,
The content of the impurity such as calcium, lead.Indium content is 85.22g/L in first filtrate, and other impurities metal element content is both less than 10mg/
L, through analyzing, indium leaching rate is 99.6%, and stannic oxide purity is 99.4%, and the rate of recovery of tin is 99.9%.
Above-mentioned resulting nitric acid solution of indium 600mL is passed through into four concatenated each chromatographies that 100mL chelating resin is housed
Column obtains pure nitric acid solution of indium after coutroi velocity 4BVH, 1.5h absorption, pure indium nitrate solution sampling is sent
Inspection, ICP-MS testing result are shown: indium content 81.98g/L, other impurities metal element content are respectively less than 1mg/L.
Above-mentioned pure nitric acid solution of indium 500mL is taken, is stirred with the mixing speed of 400r/min, it is molten to pure indium nitrate
Liquid is added the concentrated ammonia liquor that mass fraction is 27% and adjusts the formation third mixed liquor of pH to 7.0, and third mixed liquor is centrifuged to obtain the second filter
Liquid and the second filter residue dry the second filter residue to obtain indium hydroxide 59.2g, and through analyzing, the purity of indium hydroxide reaches 99.97%,
The overall recovery of indium is 95.8%.
Embodiment 3.
A method of indium hydroxide is prepared using ITO waste material comprising following steps.
ITO waste material is crushed using crusher, ball mill, ball milling, crosses 230 meshes, screenings is less than 63 microns
Particle, can not pass through 230 meshes more than or equal to 63 microns particle return ball mill ball milling.
Weigh above-mentioned screenings 100g, by 100g screenings be added 700mL water in and with the mixing speed of 700r/min into
Row stirring forms the first mixed liquor, the first mixed liquor is heated to 75 DEG C, then slowly drop evenly 202mL into the first mixed liquor
The concentrated nitric acid that mass fraction is 68%, concentrated nitric acid are added dropwise to form the second mixed liquor in 2h, insulation reaction 8h, by the second mixing
Liquid is centrifuged to obtain the first filtrate and the first filter residue, and the first filtrate amounts to 910mL, and the first filter residue is stannic oxide, the dioxy of drying
Change tin weight 7.97g, the stannic oxide of drying sampled into inspection, using ICP-MS detect indium in the first filtrate, tin, iron, copper, zinc,
The content of the impurity such as calcium, lead.Indium content is 81.23g/L in first filtrate, and other impurities metal element content is both less than 10mg/
L, through analyzing, indium leaching rate is 99.3%, and stannic oxide purity is 98.9%, and the rate of recovery of tin is 99.9%.
Above-mentioned resulting nitric acid solution of indium 600mL is passed through into four concatenated each chromatographies that 100mL chelating resin is housed
Column obtains pure nitric acid solution of indium after coutroi velocity 6BVH, 1h absorption, pure indium nitrate solution sampling is sent
Inspection, ICP-MS testing result are shown: indium content 77.57g/L, other impurities metal element content are respectively less than 1mg/L.
Above-mentioned pure nitric acid solution of indium 500mL is taken, is stirred with the mixing speed of 500r/min, it is molten to pure indium nitrate
Liquid is added the concentrated ammonia liquor that mass fraction is 26% and adjusts the formation third mixed liquor of pH to 7.8, and third mixed liquor is centrifuged to obtain the second filter
Liquid and the second filter residue dry the second filter residue to obtain indium hydroxide 56.0g, and through analyzing, the purity of indium hydroxide reaches 99.95%,
The overall recovery of indium is 94.8%.
Embodiment 4.
A method of indium hydroxide is prepared using ITO waste material comprising following steps.
ITO waste material is crushed using crusher, ball mill, ball milling, crosses 230 meshes, screenings is less than 63 microns
Particle, can not pass through 230 meshes more than or equal to 63 microns particle return ball mill ball milling.
Weigh above-mentioned screenings 100g, by 100g screenings be added 600mL water in and with the mixing speed of 550r/min into
Row stirring forms the first mixed liquor, the first mixed liquor is heated to 90 DEG C, then slowly drop evenly 270mL into the first mixed liquor
The concentrated nitric acid that mass fraction is 66%, concentrated nitric acid are added dropwise to form the second mixed liquor in 3h, insulation reaction 6h, by the second mixing
Liquid is centrifuged to obtain the first filtrate and the first filter residue, and the first filtrate amounts to 855mL, and the first filter residue is stannic oxide, the dioxy of drying
Change tin weight 7.90g, the stannic oxide of drying sampled into inspection, using ICP-MS detect indium in the first filtrate, tin, iron, copper, zinc,
The content of the impurity such as calcium, lead.Indium content is 86.8g/L in first filtrate, and other impurities metal element content is both less than 10mg/L,
Through analyzing, indium leaching rate is 99.7%, and stannic oxide purity is 99.8%, and the rate of recovery of tin is 99.9%.
Above-mentioned resulting nitric acid solution of indium 600mL is passed through into four concatenated each chromatographies that 100mL chelating resin is housed
Column, coutroi velocity are 5 BVH, and 1.2h obtains pure nitric acid solution of indium after adsorbing, by pure indium nitrate solution sampling
Inspection, ICP-MS testing result are shown: indium content 82.8g/L, other impurities metal element content are respectively less than 1mg/L.
Above-mentioned pure nitric acid solution of indium 500mL is taken, is stirred with the mixing speed of 300r/min, it is molten to pure indium nitrate
Liquid is added the concentrated ammonia liquor that mass fraction is 28% and adjusts the formation third mixed liquor of pH to 8.0, and third mixed liquor is centrifuged to obtain the second filter
Liquid and the second filter residue dry the second filter residue to obtain indium hydroxide 59.8g, and through analyzing, the purity of indium hydroxide reaches 99.9%,
The overall recovery of indium is 95.1%.
The present invention makees raw material using ITO waste material, without the process of reducing metal simple substance, can separate metallic tin and indium, most
The indium hydroxide being prepared eventually can be used as the raw material for preparing indium oxide, and this method is with process is short, easy to operate, the rate of recovery is high
The advantages of.
Although for illustrative purposes, the preferred embodiment of the present invention is had been disclosed, but the ordinary skill people of this field
Member will realize without departing from the scope and spirit of the invention as disclosed by the appended claims, various to change
Into, increase and replace be possible.
Claims (7)
1. a kind of method for preparing indium hydroxide using ITO waste material, it is characterised in that: it includes the following steps:
S1: broken ball milling: being crushed ITO waste material using crusher, ball mill, ball milling, crosses 230 meshes later, is sieved
Lower object；
S2: nitric acid leaches: above-mentioned screenings being added to the water with the first mixing speed according to the solid-to-liquid ratio 1:5-7 of screenings and water
It is stirred to form the first mixed liquor, the first mixed liquor is heated to 75-90 DEG C, then be added dropwise and be completely dissolved into the first mixed liquor
1.5-2 times of acid solution of required theoretical acid amount, the acid solution are the concentrated nitric acid that mass fraction is 65%-68%, and concentrated nitric acid is in 2-3h
It is added dropwise to form the second mixed liquor, the second mixed liquor is heated to 75-90 DEG C, insulation reaction 4-12h, is centrifuged to obtain the first filtrate
With the first filter residue, first filtrate is nitric acid solution of indium, and first filter residue is stannic oxide；
S3: adsorption-edulcoration: by above-mentioned resulting all or part of nitric acid solution of indium by plural serial stage chelating resin, with certain
Flow velocity carry out selective ion exchange, foreign ion is all adsorbed on chelating resin, and remainder is that pure indium nitrate is molten
Liquid；
S4: lye neutralizes: lye being added into above-mentioned pure nitric acid solution of indium and adjusts pH to 7.0-8.0 formation third mixing
Liquid, third mixed liquor are centrifuged to obtain the second filtrate and the second filter residue, and second filter residue is indium hydroxide.
2. the method for preparing indium hydroxide using ITO waste material according to claim 1, it is characterised in that: the lye is
Concentrated ammonia liquor.
3. the method for preparing indium hydroxide using ITO waste material according to claim 2, it is characterised in that: the concentrated ammonia liquor
Mass fraction be 25%-28%.
4. the method for preparing indium hydroxide using ITO waste material according to claim 1, it is characterised in that: described first stirs
Mixing speed is 450-700r/min.
5. the method for preparing indium hydroxide using ITO waste material according to claim 1, it is characterised in that: the chelating tree
Rouge is 4 grades of series connection chelating resins.
6. the method for preparing indium hydroxide using ITO waste material according to claim 1, it is characterised in that: selective ion
The flow velocity of exchange is 2-6 BVH.
7. the method for preparing indium hydroxide using ITO waste material according to claim 1, it is characterised in that: it is useless that In accounts for ITO
Expect that the 74.44% of mass fraction, Sn accounts for the 7.88% of ITO waste material mass fraction.
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| CN201811548751.1A CN109504858B (en) | 2018-12-18 | 2018-12-18 | Method for preparing indium hydroxide by using ITO waste material |
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| CN201811548751.1A CN109504858B (en) | 2018-12-18 | 2018-12-18 | Method for preparing indium hydroxide by using ITO waste material |
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| CN109504858B CN109504858B (en) | 2020-10-27 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112359243A (en) * | 2020-11-11 | 2021-02-12 | 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 |
| CN112708763A (en) * | 2020-12-15 | 2021-04-27 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092781A (en) * | 2010-12-10 | 2011-06-15 | 株洲冶炼集团股份有限公司 | Method for preparing battery grade indium hydroxide and indium oxide |
| 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 |
| CN104630486A (en) * | 2015-01-28 | 2015-05-20 | 江苏理工学院 | Method for recovering indium oxide and stannum from ITO coating film of conducting glass |
-
2018
- 2018-12-18 CN CN201811548751.1A patent/CN109504858B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092781A (en) * | 2010-12-10 | 2011-06-15 | 株洲冶炼集团股份有限公司 | Method for preparing battery grade indium hydroxide and indium oxide |
| 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 |
| CN104630486A (en) * | 2015-01-28 | 2015-05-20 | 江苏理工学院 | Method for recovering indium oxide and stannum from ITO coating film of conducting glass |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112359243A (en) * | 2020-11-11 | 2021-02-12 | 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 |
| 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 |
| CN112708763A (en) * | 2020-12-15 | 2021-04-27 | 先导薄膜材料（广东）有限公司 | Method for recovering valuable metal from ITO waste target |
| 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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| CN109504858B (en) | 2020-10-27 |
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