CN107130112A - A kind of method of recovery indium in crystal display screen from waste liquid - Google Patents

A kind of method of recovery indium in crystal display screen from waste liquid Download PDF

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Publication number
CN107130112A
CN107130112A CN201710359917.4A CN201710359917A CN107130112A CN 107130112 A CN107130112 A CN 107130112A CN 201710359917 A CN201710359917 A CN 201710359917A CN 107130112 A CN107130112 A CN 107130112A
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China
Prior art keywords
liquid crystal
indium
crystal display
display screen
waste liquid
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Pending
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CN201710359917.4A
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Chinese (zh)
Inventor
白航空
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Hefei Huike Precision Mould Co Ltd
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Hefei Huike Precision Mould Co Ltd
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Publication date
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Priority to CN201710359917.4A priority Critical patent/CN107130112A/en
Publication of CN107130112A publication Critical patent/CN107130112A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B58/00Obtaining gallium or indium
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of method of recovery indium in crystal display screen from waste liquid, comprise the following steps:Waste liquid crystal display screen is cleaned with water, dried, clean waste liquid crystal display screen is obtained;The ultimate range that two outside faceplate panels of LCDs are shredded between any two points is 4 30 centimetres of fragment, obtains the glass sheet of exposed liquid crystal surface;Glass sheet after scraping is ground with high pressure water washing, the mixture being made up of liquid crystal, indium concentrate and water is obtained, the mixture dissolved with liquid crystal is entered closed separator by reducing pressure, allows liquid crystal to be converted to liquid;After liquid liquid crystal filtering, obtained indium concentrate sulfuric acid solution immersion obtains leachate, and leachate is handled with the technological operation for extracting and being stripped, and obtains containing solution of indium;To its pH is adjusted to 36 containing adding alkali lye in solution of indium, solid is filtered out, the solid is scrubbed, after drying, obtains thick indium.

Description

A kind of method of recovery indium in crystal display screen from waste liquid
Technical field
The present invention relates to LCDs technical field, and in particular to the side of recovery indium in a kind of crystal display screen from waste liquid Method.
Background technology
Liquid crystal display is developed rapidly since 1990s, and is progressively moved to maturity, because it has definition It is height, good, environmentally friendly image color, power saving, frivolous and the advantages of be easy to carry, it has been widely used in household electrical appliance, computer and logical Believe in product.In recent years, the yield of China's LCD product increases substantially.The LCD TV annual production of China in 2004 is not enough 1000000;Between 2004~2007 years, the yield of the annual computer liquid-crystal display of China is all more than 60,000,000;Domestic flat board Liquid crystal panel production capacity, less than the share in the whole world 1%, global 21% share in 2012 is developed into from 2008 from originally.With one The operation of a little large scale liquid crystal panel production lines, inland of China panel production capacity will exceed China Taiwan in 2016, leap to the world Second.One of a large amount of main sources for becoming current and electron wastes in future of LCD product.
Current LCDs is to be sealed the glass substrate that two panels is carved with indium electrode using epoxy resin mostly, injection Liquid crystal, then overlays polaroid on the outside of two pieces of glass substrates, so as to constitute a complete liquid crystal display device.Therefore reclaim The key shielded with the crystalline substance that disposes waste liquid is how to have by polaroid, glass substrate and for the ito film three for scribing indium electrode The separation of effect ground.
Indium is a kind of rare precious metal, softer than lead, with good plasticity and ductility, almost can arbitrarily be become Shape, is widely used in the fields such as high-performance enginer bearing, acolite, semi-conducting material and command bundle rods for nuclear reactors.Mesh Preceding indium product is mainly used in LCDs manufacturing industry, and the indium more than 60% is used to manufacture ITO target.With liquid crystal display skill Art is flourished, and liquid crystal display device manufacture is continuously increased, and waste liquid crystal display part is consequently increased, waste liquid crystal display Indium resource total amount in part is considerable.And the reserves of indium are only the 1/6 of gold reserve, can constantly it be reduced with indium resource, from useless Recovery indium is imperative in old liquid crystal display device.How efficiently, the research of indium economically reclaimed in liquid crystal display device is The focus of current recycle business research.
The content of the invention
The present invention is intended to provide in a kind of crystal display screen from waste liquid recovery indium method.
The present invention provides following technical scheme:
The method of recovery indium, comprises the following steps in a kind of crystal display screen from waste liquid:
(1) waste liquid crystal display screen is cleaned with water, dried, obtain clean waste liquid crystal display screen;
(2) clean waste liquid crystal display screen is disassembled, isolates liquid crystal cell, excision liquid crystal cell surrounding is stained with sealant Side glass, the outside of LCDs two faceplate panels are shredded into the ultimate range between any two points broken for 4-30 centimetres Piece, obtains the glass sheet of exposed liquid crystal surface;
(3) glass sheet after scraping is ground with high pressure water washing, obtains the mixture being made up of liquid crystal, indium concentrate and water, led to Crossing reduction pressure makes the mixture dissolved with liquid crystal enter closed separator, allows liquid crystal to be converted to liquid;
(4) the indium concentrate sulfuric acid solution after liquid liquid crystal filtering, obtained immersion is obtained into leachate, to extract and be stripped Technological operation processing leachate, obtain contain solution of indium;
(5) to its pH is adjusted to 3-6 containing adding alkali lye in solution of indium, solid is filtered out, the solid is scrubbed, after drying, Obtain thick indium.
It is that water rinses glass sheet with 1.8~3kg/cm2 spray pressure that step (3) the mesohigh water, which is rinsed, is rinsed The moisture on glass sheet is absorbed afterwards, then is placed in drying in 70-80 DEG C of environment.
The dilute sulfuric acid leached in the step (4) is the aqueous sulfuric acid of mass percent≤20%.
Ethanol, methyl ether or ethyl acetate extraction and back extraction operation are utilized in the step (4).
Alkali lye is the saturated solution of soluble highly basic in the step (5), and described soluble highly basic is NaOH or KOH.
Compared with prior art, the beneficial effects of the invention are as follows:Present invention recycling sulfuric acid solution reduces medicament and disappeared Consumption, significantly reduces production cost;Rinse water improves indium recovery for complex acid;The present invention to each step Fine design and Strict control, makes the rate of recovery of indium can reach more than 95%;Present invention leaching gained sulfuric acid solution does not adjust pH and directly extracted Take, organic phase is removed after extraction and returns again to leading portion leaching, soda acid usage amount is greatly reduced, therefore the present invention has operability By force, the low advantage of operating cost, suitable for the extensive commercial application of enterprise.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all Belong to the scope of protection of the invention.
The method of recovery indium, comprises the following steps in a kind of crystal display screen from waste liquid of embodiment:
(1) waste liquid crystal display screen is cleaned with water, dried, obtain clean waste liquid crystal display screen;
(2) clean waste liquid crystal display screen is disassembled, isolates liquid crystal cell, excision liquid crystal cell surrounding is stained with sealant Side glass, the outside of LCDs two faceplate panels are shredded into the ultimate range between any two points broken for 4-30 centimetres Piece, obtains the glass sheet of exposed liquid crystal surface;
(3) glass sheet after scraping is ground with high pressure water washing, obtains the mixture being made up of liquid crystal, indium concentrate and water, led to Crossing reduction pressure makes the mixture dissolved with liquid crystal enter closed separator, allows liquid crystal to be converted to liquid;
(4) the indium concentrate sulfuric acid solution after liquid liquid crystal filtering, obtained immersion is obtained into leachate, to extract and be stripped Technological operation processing leachate, obtain contain solution of indium;
(5) to its pH is adjusted to 3-6 containing adding alkali lye in solution of indium, solid is filtered out, the solid is scrubbed, after drying, Obtain thick indium.
It is that water rinses glass sheet with 1.8~3kg/cm2 spray pressure that step (3) the mesohigh water, which is rinsed, is rinsed The moisture on glass sheet is absorbed afterwards, then is placed in drying in 70-80 DEG C of environment.
The dilute sulfuric acid leached in the step (4) is the aqueous sulfuric acid of mass percent≤20%.
Ethanol, methyl ether or ethyl acetate extraction and back extraction operation are utilized in the step (4).
Alkali lye is the saturated solution of soluble highly basic in the step (5), and described soluble highly basic is NaOH or KOH.
It is obvious to a person skilled in the art that the invention is not restricted to the details of the one exemplary embodiment, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit is required rather than the explanation is limited, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.Although not each moreover, it will be appreciated that the present specification is described in terms of embodiments Embodiment is only comprising an independent technical scheme, and this narrating mode of specification is only this area for clarity Technical staff should be using specification as an entirety, and the technical solutions in the various embodiments may also be suitably combined, forms this Art personnel may be appreciated other embodiment.

Claims (5)

1. a kind of method of recovery indium in crystal display screen from waste liquid, it is characterised in that comprise the following steps:
(1) waste liquid crystal display screen is cleaned with water, dried, obtain clean waste liquid crystal display screen;
(2) clean waste liquid crystal display screen is disassembled, isolates liquid crystal cell, excision liquid crystal cell surrounding is stained with the side of sealant Glass, the ultimate range that two outside faceplate panels of LCDs are shredded between any two points is 4-30 centimetres of fragment, Obtain the glass sheet of exposed liquid crystal surface;
(3) glass sheet after scraping is ground with high pressure water washing, obtains the mixture being made up of liquid crystal, indium concentrate and water, pass through drop Low-pressure makes the mixture dissolved with liquid crystal enter closed separator, allows liquid crystal to be converted to liquid;
(4) the indium concentrate sulfuric acid solution after liquid liquid crystal filtering, obtained immersion is obtained into leachate, with the work for extracting and being stripped Skill operation processing leachate, obtains containing solution of indium;
(5) to its pH is adjusted to 3-6 containing adding alkali lye in solution of indium, solid is filtered out, the solid is scrubbed, after drying, obtains Thick indium.
2. the method for recovery indium in a kind of crystal display screen from waste liquid according to claim 1, it is characterised in that:The step (3) it is that water rinses glass sheet with 1.8~3kg/cm 2 spray pressure that mesohigh water, which is rinsed, is absorbed after flushing on glass sheet Moisture, then be placed in 70-80 DEG C of environment dry.
3. the method for recovery indium in a kind of crystal display screen from waste liquid according to claim 1, it is characterised in that:The step (4) dilute sulfuric acid leached in is the aqueous sulfuric acid of mass percent≤20%.
4. the method for recovery indium in a kind of crystal display screen from waste liquid according to claim 1, it is characterised in that:The step (4) ethanol, methyl ether or ethyl acetate extraction and back extraction operation are utilized in.
5. the method for recovery indium in a kind of crystal display screen from waste liquid according to claim 1, it is characterised in that:The step (5) alkali lye is the saturated solution of soluble highly basic in, and described soluble highly basic is NaOH or KOH.
CN201710359917.4A 2017-05-20 2017-05-20 A kind of method of recovery indium in crystal display screen from waste liquid Pending CN107130112A (en)

Priority Applications (1)

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CN201710359917.4A CN107130112A (en) 2017-05-20 2017-05-20 A kind of method of recovery indium in crystal display screen from waste liquid

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002591A (en) * 2010-09-28 2011-04-06 苏州群瑞环保科技有限公司 Process for extracting indium from waste liquid crystal display screen
CN102500128A (en) * 2011-10-14 2012-06-20 合肥工业大学 Method and system for recovering crystal liquid in abandoned liquid crystal display
CN103602815A (en) * 2013-11-06 2014-02-26 四川长虹电器股份有限公司 Method for recycling indium from waste liquid crystal displays
CN105063364A (en) * 2015-09-02 2015-11-18 扬州宁达贵金属有限公司 Method for recycling indium from waste liquid crystal display
CN105420502A (en) * 2015-11-27 2016-03-23 四川长虹格润再生资源有限责任公司 Method for recovering indium from waste liquid crystal display screen panel

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002591A (en) * 2010-09-28 2011-04-06 苏州群瑞环保科技有限公司 Process for extracting indium from waste liquid crystal display screen
CN102500128A (en) * 2011-10-14 2012-06-20 合肥工业大学 Method and system for recovering crystal liquid in abandoned liquid crystal display
CN103602815A (en) * 2013-11-06 2014-02-26 四川长虹电器股份有限公司 Method for recycling indium from waste liquid crystal displays
CN105063364A (en) * 2015-09-02 2015-11-18 扬州宁达贵金属有限公司 Method for recycling indium from waste liquid crystal display
CN105420502A (en) * 2015-11-27 2016-03-23 四川长虹格润再生资源有限责任公司 Method for recovering indium from waste liquid crystal display screen panel

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Application publication date: 20170905