CN104630486B - Method for recovering indium oxide and metal tin from ITO (indium tin oxide) coating film of conductive glass - Google Patents
Method for recovering indium oxide and metal tin from ITO (indium tin oxide) coating film of conductive glass Download PDFInfo
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- CN104630486B CN104630486B CN201510044282.XA CN201510044282A CN104630486B CN 104630486 B CN104630486 B CN 104630486B CN 201510044282 A CN201510044282 A CN 201510044282A CN 104630486 B CN104630486 B CN 104630486B
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- indium
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000011521 glass Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 12
- 239000002184 metal Substances 0.000 title claims abstract description 12
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 title abstract description 3
- 229910003437 indium oxide Inorganic materials 0.000 title abstract 4
- 239000011248 coating agent Substances 0.000 title abstract 3
- 238000000576 coating method Methods 0.000 title abstract 3
- 229910052738 indium Inorganic materials 0.000 claims abstract description 46
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000002386 leaching Methods 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 17
- 238000006073 displacement reaction Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000002203 pretreatment Methods 0.000 claims description 7
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 5
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 14
- 239000004973 liquid crystal related substance Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of alloy waste recycling, in particular to an industrialized method for recycling indium oxide and metallic tin from an ITO (indium tin oxide) coating film of conductive glass, which comprises the following steps: the method comprises the steps of raw material pretreatment, acid leaching, filtering and washing, circulating leaching, extraction and back extraction, tin displacement, indium precipitation and normal-temperature drying. By adopting the technical scheme of the invention, higher indium leaching rate can be obtained, the purity of the recovered indium oxide and metal tin is higher, the energy consumption is low, the acid consumption is less, the operation is simple and easy to implement, and the method is suitable for large-scale industrial application of enterprises. The method of the invention strictly controls the steps, the recovery rate of indium can reach more than 90%, the purity of indium oxide can reach 95%, and the purity of metal tin can reach 80%. The technical scheme of the invention can realize resource utilization of the ITO coating film of the conductive glass to the maximum extent, and has more obvious economic benefit and social benefit.
Description
Technical field
The present invention relates to alloyed scrap utilization technology field, particularly a kind of recovery from electro-conductive glass ITO plated film
Indium sesquioxide. and metallic tin can industrialized mode.
Background technology
ITO full name indium tin oxide, Indium sesquioxide., stannum oxide is mixed to get according to a certain percentage, this is mixed
Thing is processed into suitable shape and just obtains ITO target, plates the very thin ITO of last layer by plane magnetic control mode thin on glass
Film, has just obtained electro-conductive glass, and ito thin film electrical conductivity is high, visible light permeability is good, is produce LCDs important zero
Part.
The very big popularization of the fast development of electronics industry and electronic product makes liquid crystal display as most of electronic product
Requisite part, is widely used in computer monitor, LCD TV, smart mobile phone etc., and its yield also expands continuous
Greatly.Only 2013, more than 100,000,000, more than 200,000,000, smart mobile phone produced computer liquid-crystal display yield Chinese LCD TV yield
Amount is more than 1,200,000,000.After these electronic products reach service life and scrap, substantial amounts of electron wastes will be produced, wherein have
Quite a few is LCDs, containing multiple rare precious metals, heavy metal, and a large amount of nonmetallic materials, simple process meeting
Cause the wasting of resources and serious environmental pollution, most important of which rare metal is exactly indium, and indium reserves are few, consumption is big, waste liquid
Crystal display screen is increasingly subject to people's attention as important secondary resource containing indium, in useless electro-conductive glass, waste liquid crystal display screen
Though the content of indium is few, learies are big, take care of the pence, and from resources circulation angle, reclaim indium therein significant.
From waste, the patent of recovery indium is existing some, in the patent leaching indium using acidleach method, all using sulphuric acid
Or hydrochloric acid, all rare report of content to foreign metal ion in leachate.Recovery patent for indium in liquid crystal display is big
Need to crush, leaching process needs stirring or ultrasonic vibration, this increases energy consumption to a certain extent, increased operation more
Complexity.
In sum, study and a kind of suitable leach acid so that impurity metal content in electro-conductive glass ITO plated film leachate
Less and simple and easy to do, simple to operate reclaim from electro-conductive glass ITO plated film Indium sesquioxide. and metallic tin mode are currently will to grind
The problem studied carefully.
Content of the invention
The technical problem to be solved in the present invention is：For in prior art from waste recovery indium technology exist ask
Topic, provides a kind of method reclaiming Indium sesquioxide. and metallic tin ITO plated film from electro-conductive glass.
The technical solution adopted for the present invention to solve the technical problems is：A kind of recovery oxygen from electro-conductive glass ITO plated film
The method changing indium and metallic tin, is characterized in that：The method comprises the steps：
A. raw material pre-treatment raw material is not required to pulverize, or suitably broken according to reaction vessel size, to later stage leaching effect
Do not affect；Raw material be in the electro-conductive glass production process containing ITO plated film produce waste product and through pre-treatment, eliminate
The LCDs face glass of liquid crystal and light polarizing film；
B. acidleach controls leaching condition, using acid solution, electro-conductive glass is soaked；Described acid is nitric acid, nitric acid
Solution concentration is 8-10mol/L, and salpeter solution volume is 0.8-2.0 with the ratio (i.e. liquid-solid ratio) of electro-conductive glass quality, reaction
Temperature is 85-90 DEG C, and the response time is 3-5h；
C. filtration washing reaction is filtered after terminating, and washing sample can contain solution of indium；
D. circulating leaching contains solution of indium again as the raw material that leachate process is new, and this contains solution of indium and repeats using secondary
Number is 5-12 time；
E. extraction and back extraction are 0.5-2.0 by repeatedly leach the solution obtaining in step d adjusting pH value, with extraction with instead
The mode of extraction obtains the solution containing indium stannum；Described extractant is the P of 50% volume ratio204With the sulfonated kerosene of 50% volume ratio,
Strippant is the hydrochloric acid solution of 3-6mol/L；
F. displacement stannum is 1.0-2.5 by obtain solution of tin containing indium in step e adjusting pH value, adds appropriate active metal
And heat to replace stannum, it is filtrated to get metallic tin and filtrate；The described active metal for replacing metallic tin is indium, and displacement is anti-
Temperature is answered to be 50-60 DEG C of heating in water bath, time swap is 3-5h；
G. precipitation of indium will add excessive ammonia in the filtrate obtaining in step f, is filtrated to get white precipitate；
H. normal temperature drying, by the white precipitate obtaining in step g normal temperature drying, obtains Indium sesquioxide.；Described baking temperature
For 15-30 DEG C, drying time is 8-12h.
Compared with leachate of the prior art, used in technical scheme, salpeter solution leachate can obtain
Higher leaching rate, in leachate, the content of foreign metal is less, all less than the 1% of indium content simultaneously；Sample need not be pulverized,
Extraction temperature be room temperature, leaching process without stirring for or concussion, no additional energy source consumption；Leachate can repeated multiple times use, and subtracts
Lack sour consumption and improve the concentration of indium in leachate；Extraction and back extraction can effectively remove foreign metal ion；Using gold
Belong to indium displacement stannum, do not introduce new metal ion, ensure that the concentration of indium ion simultaneously.
Higher indium leaching rate can be obtained using technical scheme, the Indium sesquioxide. of recovery and metallic tin purity are relatively
Height, and energy consumption is low, sour consumption is few, and operation is simple, is suitable to the extensive commercial application of enterprise.The inventive method is to each step
Strict control, up to more than 90%, up to 95%, metallic tin purity is up to 80% for Indium sesquioxide. purity for the response rate of indium.The present invention
Technical scheme can farthest realize the recycling of electro-conductive glass ITO plated film, there is more significant economic benefit
And social benefit.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment one
A kind of method reclaiming Indium sesquioxide. and metallic tin ITO plated film from electro-conductive glass, is characterized in that：The method include as
Lower step：
A. raw material pre-treatment East China man resource regeneration enterprise carries out pre-treatment to waste liquid crystal display screen, eliminates liquid crystal
And light polarizing film, face glass and useless electro-conductive glass are mixed to get raw material, the raw material taking quality to be 50kg, putting into volume is 80L
Acid-leaching reaction container in；
B. acidleach, at 20 DEG C, is soaked with the salpeter solution that 40L concentration is 8mol/L, reaction temperature is 85-90 DEG C, instead
It is 3-5h between seasonable；
C. filtration washing takes out raw material and with a small amount of water washing from solution, can contain solution of indium；
D. circulating leaching contains solution of indium again as the raw material 50kg that leachate process is new, is leached with identical condition,
Repeatable operation 10 times；
E. extract and back extraction is 1.0 by repeatedly leach the solution obtaining in step d adjusting pH value, to extract and back extraction
Mode obtains the solution containing indium stannum；Described extractant is the P of 50% volume ratio204With the sulfonated kerosene of 50% volume ratio, back extraction
Take the hydrochloric acid solution that agent is 3mol/L；
F. displacement stannum is 2.0 by obtain solution of tin containing indium in step e adjusting pH value, adds appropriate active metal sponge
Indium is simultaneously heated to 60 DEG C to replace stannum, is filtrated to get metallic tin and filtrate；Displacement reaction temperature is 60 DEG C of heating in water bath, during displacement
Between be 5h；
G. precipitation of indium will add excessive ammonia in the filtrate obtaining in step f, is filtrated to get white precipitate；
H. normal temperature drying, by the white precipitate obtaining in step g normal temperature drying, obtains Indium sesquioxide.；The leaching rate of indium is
95.59%, obtaining Indium sesquioxide. purity is 96.32%, and metallic tin purity is 85.72%.
Embodiment two
A kind of method reclaiming Indium sesquioxide. and metallic tin ITO plated film from electro-conductive glass, is characterized in that：The method include as
Lower step：
A. raw material pre-treatment East China man resource regeneration enterprise carries out pre-treatment to waste liquid crystal display screen, eliminates liquid crystal
And light polarizing film, face glass and useless electro-conductive glass are mixed to get raw material, the raw material taking quality to be 500kg, putting into volume is
In the acid-leaching reaction container of 800L；
B. acidleach, at 20 DEG C, is soaked with the salpeter solution that 400L concentration is 8mol/L, reaction temperature is 85-90 DEG C,
Response time is 3-5h；
C. filtration washing takes out raw material and with a small amount of water washing from solution, can contain solution of indium；
D. circulating leaching contains solution of indium again as the raw material 500kg that leachate process is new, is leached with identical condition,
Repeatable operation 10 times；
E. extract and back extraction is 1.0 by repeatedly leach the solution obtaining in step d adjusting pH value, to extract and back extraction
Mode obtains the solution containing indium stannum；Described extractant is the P of 50% volume ratio204With the sulfonated kerosene of 50% volume ratio, back extraction
Take the hydrochloric acid solution that agent is 3mol/L；
F. displacement stannum is 2.0 by obtain solution of tin containing indium in step e adjusting pH value, adds appropriate active metal sponge
Indium is simultaneously heated to 60 DEG C to replace stannum, is filtrated to get metallic tin and filtrate；Displacement reaction temperature is 60 DEG C of heating in water bath, during displacement
Between be 5h；
G. precipitation of indium will add excessive ammonia in the filtrate obtaining in step f, is filtrated to get white precipitate；
H. normal temperature drying, by the white precipitate obtaining in step g normal temperature drying, obtains Indium sesquioxide., and the leaching rate of indium is
95.14%, obtaining Indium sesquioxide. purity is 95.47%, and metallic tin purity is 88.34%.
Claims (3)
1. a kind of method reclaiming Indium sesquioxide. and metallic tin ITO plated film from electro-conductive glass, is characterized in that：The method includes as follows
Step：
A. raw material pre-treatment is suitably broken by raw material according to reaction vessel size；
B. acidleach is soaked to electro-conductive glass raw material using acid solution；
C. filtration washing reaction is filtered after terminating, and washing sample can contain solution of indium；
D. circulating leaching contains solution of indium again as the raw material that leachate process is new, and this contains, and solution of indium is repeatable using number of times to be
5-12 time；
E. extract and back extraction is 0.5-2.0 by repeatedly leach the solution obtaining in step d adjusting pH value, to extract and back extraction
Mode obtains the solution containing indium stannum；
F. displacement stannum is 1.0-2.5 by obtain solution of tin containing indium in step e adjusting pH value, adds appropriate active metal and adds
Heat, to replace stannum, is filtrated to get metallic tin and filtrate；
G. precipitation of indium will add excessive ammonia in the filtrate obtaining in step f, is filtrated to get white precipitate；
H. normal temperature drying, by the white precipitate obtaining in step g normal temperature drying, obtains Indium sesquioxide.；
Acid described in described step b is nitric acid, and salpeter solution volume is 0.8-2.0 with the ratio of electro-conductive glass quality, reaction
Temperature is 85-90 DEG C, and the response time is 3-5h, and salpeter solution concentration is 8-10mol/L；Extractant described in described step e
P for 50% volume ratio204With the sulfonated kerosene of 50% volume ratio, strippant is the hydrochloric acid solution of 3-6mol/L.
2. the method reclaiming Indium sesquioxide. and metallic tin a kind of ITO plated film from electro-conductive glass according to claim 1, it is special
Levying is：The active metal for replacing metallic tin described in described step f is indium, and displacement reaction temperature is 50-60 DEG C of water-bath
Heating, time swap is 3-5h.
3. the method reclaiming Indium sesquioxide. and metallic tin a kind of ITO plated film from electro-conductive glass according to claim 1, it is special
Levying is：Baking temperature described in described step h is 15-30 DEG C, and drying time is 8-12h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510044282.XA CN104630486B (en) | 2015-01-28 | 2015-01-28 | Method for recovering indium oxide and metal tin from ITO (indium tin oxide) coating film of conductive glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510044282.XA CN104630486B (en) | 2015-01-28 | 2015-01-28 | Method for recovering indium oxide and metal tin from ITO (indium tin oxide) coating film of conductive glass |
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| Publication Number | Publication Date |
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| CN104630486A CN104630486A (en) | 2015-05-20 |
| CN104630486B true CN104630486B (en) | 2017-02-22 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722563B (en) * | 2015-03-18 | 2017-05-03 | 合肥鑫晟光电科技有限公司 | Method for recycling indium on panel |
| CN104975186B (en) * | 2015-07-30 | 2017-03-22 | 赤峰海镧金属材料科技有限公司 | Comprehensive recycling method for ITO film sensor |
| CN105420502B (en) * | 2015-11-27 | 2018-08-14 | 四川长虹格润环保科技股份有限公司 | The method of recovery indium from waste LCD panel |
| CN106834698B (en) * | 2017-01-19 | 2019-02-19 | 昆明理工大学 | A method of the enriching and reclaiming indium from acid solution of the low concentration containing indium |
| CN106868323A (en) * | 2017-02-23 | 2017-06-20 | 同济大学 | A kind of method that indium is extracted from discarded liquid crystal display panel |
| CN106868324B (en) * | 2017-03-07 | 2018-08-21 | 北京工业大学 | A method of using salting out from the pickle liquor enriching and purifying indium of waste material containing ITO |
| CN107513619B (en) * | 2017-08-14 | 2019-03-05 | 中南大学 | A method of recovery indium and tin from ito glass waste material |
| CN109504858B (en) * | 2018-12-18 | 2020-10-27 | 广东先导稀材股份有限公司 | Method for preparing indium hydroxide by using ITO waste material |
| CN112646985B (en) * | 2020-11-24 | 2022-02-18 | 厦门大学 | Method for enriching and purifying metal indium in ITO film etching waste liquid |
| CN115418501A (en) * | 2022-09-02 | 2022-12-02 | 合肥工业大学 | Method for recovering metal indium from waste ITO glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000128531A (en) * | 1998-10-23 | 2000-05-09 | Asahi Puritekku Kk | Separation of indium |
| KR20090055649A (en) * | 2006-10-24 | 2009-06-02 | 닛코 킨조쿠 가부시키가이샤 | Method for collection of valuable metal from ito scrap |
| JP5043027B2 (en) * | 2006-10-24 | 2012-10-10 | Ｊｘ日鉱日石金属株式会社 | Recovery method of valuable metals from ITO scrap |
| CN103103356B (en) * | 2012-11-09 | 2014-12-10 | 柳州百韧特先进材料有限公司 | Process for recovering crude indium and tin from ITO (indium tin oxide) waste target |
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Denomination of invention: A method for recovering indium oxide and tin from ITO coating on conductive glass Effective date of registration: 20210525 Granted publication date: 20170222 Pledgee: Bank of China Limited Suichang County Branch Pledgor: ZHEJIANG SUICHANG HUIJIN NON-FERROUS METAL Co.,Ltd. Registration number: Y2021330000442 |
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Date of cancellation: 20230920 Granted publication date: 20170222 Pledgee: Bank of China Limited Suichang County Branch Pledgor: ZHEJIANG SUICHANG HUIJIN NON-FERROUS METAL CO.,LTD. Registration number: Y2021330000442 |
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