CN104032133A - Method for recovering metal indium and tin from ITO waste target - Google Patents
Method for recovering metal indium and tin from ITO waste target Download PDFInfo
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- CN104032133A CN104032133A CN201410201193.7A CN201410201193A CN104032133A CN 104032133 A CN104032133 A CN 104032133A CN 201410201193 A CN201410201193 A CN 201410201193A CN 104032133 A CN104032133 A CN 104032133A
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- ito
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- indium
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- tin
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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
Abstract
A method for recovering metal indium and tin from ITO waste target comprises the steps: (1) cleaning the surface of ITO waste target, namely removing foreign materials on the surface layer of the waste target, then performing ultrasonic cleaning by using an organic solvent, taking out and wiping to dry, then performing ultrasonic cleaning by using purified water, and drying for usage; and (2) using a high-temperature reducing method to recover ITO waste target. According to the method for recovering metal indium and tin from ITO waste target, the recovery rate of indium and tin is 99%, the purity of the prepared indium tin alloy is 99.99% or more, and the total content of impurities is 100 ppm. High-purity indium-tin alloy billets are directly prepared from the ITO waste target by using the one-step reducing method, is directly used to manufacture ITO powder and used to prepare ITO target materials, so that the reutilization period of waste targets is substantially shortened. Compared with a conventional wet method, the method is substantially shortened in operations and substantially improved in efficiency, and also environment pollution is reduced.
Description
Technical field
The present invention relates to the recycle utilization field of a kind photoelectric material, especially relate to the method for the useless target recovery of a kind of ITO indium metal tin.
Background technology
Known, the useless target recovery technology of ITO of having announced is at present mainly hydrometallurgic recovery, dissolves then electrolysis, hydrolytic precipitation, alkaline process separation, displacement etc. by the useless target of ITO with strong acid.
Open application number CN1487102A proposes a kind of method that reclaims indium from the useless target of indium tin oxide: useless ITO target cracker is milled to after granularity <149 μ m, adopt the full wet process of leaching, removal of impurities, displacement, electrolysis to reclaim indium from the useless target of ITO, obtain reaching 99.99% high purity indium containing indium.
What Granted publication CN101701292A adopted is the method that oxidation style reclaims indium tin from the useless target of ITO: ITO is given up to target after fragmentation, ball milling, enriching dissolving with hydrochloric acid leaches, by adding NaOH Oxidation Leaching liquid and adjusting pH value to obtain leached mud, after washing, roasting, oxidation, realizing tin separates again, obtain thick indium, after once electrolytic, obtain 4N indium, the rate of recovery of indium can be stabilized in more than 97%
What Granted publication CN101701291B adopted is the method that distillation method reclaims indium tin from the useless target of ITO, and ITO is given up to target after fragmentation, ball milling, by Leaching in Hydrochloric Acid, add appropriate oxygenant, make distillation stoste, by certain distil process separating indium, tin, reach the object that useless target reclaims.
Aforesaid method all exists that flow process is loaded down with trivial details, inefficiency, the high deficiency of cost recovery, and traditional method need add strong acid and reacts simultaneously, can produce a large amount of acid waste liquids, serious environment pollution.
Summary of the invention
in order to overcome the deficiency in background technology, the invention discloses the method for the useless target recovery of a kind of ITO indium metal tin, for the deficiency of the useless target recovery technology of conventional I TO, realize the objects such as technical process is simple, organic efficiency is high, cost recovery is low, energy-conserving and environment-protective.
In order to realize described goal of the invention, the present invention adopts following technical scheme:
The useless target of ITO reclaims a method for indium metal tin, the steps include: (1) ITO target surface cleaning that give up: will give up after the foreign material removal of target top layer, and carry out ultrasonic cleaning with organic solvent, taking-up is dried, then uses pure water ultrasonic cleaning, dried for standby;
(2) high temperature reduction method reclaims the useless target of ITO: in the crucible that useless dried ITO target and reducing substances activated carbon or graphite are placed in, be warming up to 1000 ° of C ~ 1600 ° C in atmosphere heat treatment stove time, be filled with any one or more mixed gass of non-oxidizing gas argon gas, helium, nitrogen, methane, carbonic acid gas as shielding gas, be incubated 1 ~ 10 hour; Under high temperature nonoxidizing atmosphere, the useless target of ITO reacts with reducing substances activated carbon or graphite, and Indium sesquioxide and stannic oxide are reduced, and generate indium metal tin alloy.
The described organic solvent of step of the present invention (1) is any material of ethanol, ether, acetone, benzene, toluene, gasoline.
The material of crucible of the present invention be zirconium white, the stable calcium oxide of corundum, stabilized with yttrium oxide zirconium white, corundum-mullite, silicon carbide wherein any one.
Owing to having adopted technique scheme, the present invention has following beneficial effect:
The useless target of ITO of the present invention reclaims the method for indium metal tin, and the rate of recovery that can realize indium tin reaches 99%, purity >=99.99% of prepared indium stannum alloy, foreign matter content summation ￡ 100ppm.
The present invention can directly be prepared into high purity indium tin alloy ingot by useless ITO target by a stage reduction method, is directly used in manufacture ito powder, and for the preparation of ITO target, has greatly shortened the recycling cycle of useless target.Compared with current wet method, operation significantly shortens, and efficiency significantly improves, and has reduced environmental pollution simultaneously.
Embodiment
Explanation the present invention that can be detailed by the following examples, discloses object of the present invention and is intended to protect all technological improvements in the scope of the invention.
Embodiment 1:
After the obvious foreign material in the useless target of 500gITO top layer are removed, with ethanol ultrasonic cleaning 15min, taking-up is dried; use again pure water ultrasonic cleaning 20min; take out and be dried, afterwards useless ITO target and 33g high purity graphite are placed in zirconium white crucible, in atmosphere heat treatment stove; use argon gas as protective atmosphere; be warming up to 1400 ° of C, and be incubated 2h, at high temperature the useless target of ITO reacts with graphite; Indium sesquioxide and stannic oxide are reduced, and generate indium metal tin alloy.Concrete reaction formula is:
Reclaim altogether 408g indium stannum alloy, the indium stannum alloy rate of recovery reaches 99%.Reclaimed indium stannum alloy is carried out to composition analysis, and result shows the foreign matter content ￡ 100ppm of alloy.
Embodiment 2:
After the obvious foreign material in the useless target of 300gITO top layer are removed, with acetone ultrasonic cleaning 15min, taking-up is dried; use again pure water ultrasonic cleaning 20min, take out and be dried, afterwards useless ITO target and 20g gac are placed in zirconium white crucible; in atmosphere heat treatment stove; use argon gas as protective atmosphere, be warming up to 1350 ° of C, and be incubated 3h; at high temperature the useless target of ITO reacts with highly pure active charcoal; Indium sesquioxide and stannic oxide are reduced, and generate indium metal tin alloy, and concrete reaction formula is:
Reclaim altogether 245g indium stannum alloy, the rate of recovery reaches 99%.Reclaimed indium stannum alloy is carried out to composition analysis, and result shows the foreign matter content ￡ 100ppm of alloy.
Part not in the detailed description of the invention is prior art.
Claims (3)
1. the useless target of ITO reclaims a method for indium metal tin, it is characterized in that: the steps include: (1) ITO target surface cleaning that give up: will give up after the foreign material removal of target top layer, and carry out ultrasonic cleaning with organic solvent, taking-up is dried, then uses pure water ultrasonic cleaning, dried for standby;
(2) high temperature reduction method reclaims the useless target of ITO: in the crucible that useless dried ITO target and reducing substances activated carbon or graphite are placed in, be warming up to 1000 ° of C ~ 1600 ° C in atmosphere heat treatment stove time, be filled with any one or more mixed gass of non-oxidizing gas argon gas, helium, nitrogen, methane, carbonic acid gas as shielding gas, be incubated 1 ~ 10 hour; Under high temperature nonoxidizing atmosphere, the useless target of ITO reacts with reducing substances activated carbon or graphite, and Indium sesquioxide and stannic oxide are reduced, and generate indium metal tin alloy.
2. the useless target of ITO as claimed in claim 1 reclaims the method for indium metal tin, it is characterized in that: the described organic solvent of step (1) is any material of ethanol, ether, acetone, benzene, toluene, gasoline.
3. the useless target of ITO as claimed in claim 1 reclaims the method for indium metal tin, it is characterized in that: the material of described crucible be zirconium white, the stable calcium oxide of corundum, stabilized with yttrium oxide zirconium white, corundum-mullite, silicon carbide wherein any one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410201193.7A CN104032133A (en) | 2014-05-14 | 2014-05-14 | Method for recovering metal indium and tin from ITO waste target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410201193.7A CN104032133A (en) | 2014-05-14 | 2014-05-14 | Method for recovering metal indium and tin from ITO waste target |
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| CN104032133A true CN104032133A (en) | 2014-09-10 |
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| CN201410201193.7A Pending CN104032133A (en) | 2014-05-14 | 2014-05-14 | Method for recovering metal indium and tin from ITO waste target |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104711426A (en) * | 2014-11-21 | 2015-06-17 | 株洲冶炼集团股份有限公司 | Method for extracting indium and tin from waste ITO targets through reduction and electrolysis |
| CN104818388A (en) * | 2015-05-06 | 2015-08-05 | 昆明鼎邦科技有限公司 | Method of vacuum-reducing separating indium from tin from an In/Sn oxide |
| CN104843771A (en) * | 2015-04-24 | 2015-08-19 | 柳州百韧特先进材料有限公司 | Method for recovering and preparing nanometer TIO powder from ITO target wastes |
| CN105366709B (en) * | 2015-10-15 | 2017-03-22 | 中国船舶重工集团公司第七二五研究所 | Method for effectively recycling indium and tin oxide (ITO) waste targets |
| CN109023526A (en) * | 2018-08-17 | 2018-12-18 | 上海交通大学 | A method of preparing calcium analysis YBCO HTS single crystals body |
| CN109457125A (en) * | 2018-10-08 | 2019-03-12 | 上海交通大学 | The method for controlling liquid crystal and enriching and reclaiming indium that carbon pyrolysis-vacuum autoreduction separates in discarded liquid crystal display panel |
| CN109762993A (en) * | 2019-03-04 | 2019-05-17 | 河北恒博新材料科技股份有限公司 | A method of it gives up from ITO and recycles indium metal in target |
| CN111606353A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO target grinding waste liquid |
| CN111620367A (en) * | 2020-06-08 | 2020-09-04 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
| 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 |
| CN114752770A (en) * | 2022-04-18 | 2022-07-15 | 株洲火炬安泰新材料有限公司 | High-recovery-rate reduction method and equipment for ITO (indium tin oxide) waste target powder |
| CN114956162A (en) * | 2022-07-04 | 2022-08-30 | 广东先导稀材股份有限公司 | Method for recovering indium oxide waste |
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| WO2006080742A1 (en) * | 2004-10-26 | 2006-08-03 | 9Digit Company Limited | Method for recovering high purity indium |
| CN102367519A (en) * | 2011-09-16 | 2012-03-07 | 中国船舶重工集团公司第七二五研究所 | Efficient recovering method for waste indium tin oxide (ITO) targets |
| CN103590072A (en) * | 2013-10-17 | 2014-02-19 | 清远先导材料有限公司 | Preparation method of high-purity indium |
-
2014
- 2014-05-14 CN CN201410201193.7A patent/CN104032133A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006080742A1 (en) * | 2004-10-26 | 2006-08-03 | 9Digit Company Limited | Method for recovering high purity indium |
| CN102367519A (en) * | 2011-09-16 | 2012-03-07 | 中国船舶重工集团公司第七二五研究所 | Efficient recovering method for waste indium tin oxide (ITO) targets |
| CN103590072A (en) * | 2013-10-17 | 2014-02-19 | 清远先导材料有限公司 | Preparation method of high-purity indium |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104711426A (en) * | 2014-11-21 | 2015-06-17 | 株洲冶炼集团股份有限公司 | Method for extracting indium and tin from waste ITO targets through reduction and electrolysis |
| CN104843771A (en) * | 2015-04-24 | 2015-08-19 | 柳州百韧特先进材料有限公司 | Method for recovering and preparing nanometer TIO powder from ITO target wastes |
| CN104818388A (en) * | 2015-05-06 | 2015-08-05 | 昆明鼎邦科技有限公司 | Method of vacuum-reducing separating indium from tin from an In/Sn oxide |
| CN104818388B (en) * | 2015-05-06 | 2017-03-01 | 昆明鼎邦科技股份有限公司 | A kind of indium tin oxide vacuum reduction separating indium and the method for stannum |
| CN105366709B (en) * | 2015-10-15 | 2017-03-22 | 中国船舶重工集团公司第七二五研究所 | Method for effectively recycling indium and tin oxide (ITO) waste targets |
| CN109023526B (en) * | 2018-08-17 | 2020-11-27 | 上海交通大学 | Method for preparing calcium-doped YBCO high-temperature superconducting monocrystal |
| CN109023526A (en) * | 2018-08-17 | 2018-12-18 | 上海交通大学 | A method of preparing calcium analysis YBCO HTS single crystals body |
| CN109457125A (en) * | 2018-10-08 | 2019-03-12 | 上海交通大学 | The method for controlling liquid crystal and enriching and reclaiming indium that carbon pyrolysis-vacuum autoreduction separates in discarded liquid crystal display panel |
| CN109762993A (en) * | 2019-03-04 | 2019-05-17 | 河北恒博新材料科技股份有限公司 | A method of it gives up from ITO and recycles indium metal in target |
| CN111606353A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO target grinding waste liquid |
| CN111606353B (en) * | 2020-06-03 | 2022-04-26 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO target grinding waste liquid |
| CN111620367A (en) * | 2020-06-08 | 2020-09-04 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
| CN111620367B (en) * | 2020-06-08 | 2022-06-28 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
| 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 |
| CN114752770A (en) * | 2022-04-18 | 2022-07-15 | 株洲火炬安泰新材料有限公司 | High-recovery-rate reduction method and equipment for ITO (indium tin oxide) waste target powder |
| CN114956162A (en) * | 2022-07-04 | 2022-08-30 | 广东先导稀材股份有限公司 | Method for recovering indium oxide waste |
| CN114956162B (en) * | 2022-07-04 | 2023-10-13 | 广东先导稀贵金属材料有限公司 | Recovery method of indium oxide waste |
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Application publication date: 20140910 |
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