CN105483389A - Leaching method for indium in waste liquid crystal panel and leaching agent - Google Patents

Leaching method for indium in waste liquid crystal panel and leaching agent Download PDF

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Publication number
CN105483389A
CN105483389A CN201610019764.4A CN201610019764A CN105483389A CN 105483389 A CN105483389 A CN 105483389A CN 201610019764 A CN201610019764 A CN 201610019764A CN 105483389 A CN105483389 A CN 105483389A
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China
Prior art keywords
indium
leaching
liquid crystal
waste
crystal panel
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CN201610019764.4A
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Chinese (zh)
Inventor
黄强
寸唐湘
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Yunnan University YNU
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Yunnan University YNU
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Priority to CN201610019764.4A priority Critical patent/CN105483389A/en
Publication of CN105483389A publication Critical patent/CN105483389A/en
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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
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/16Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
    • 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

Abstract

The invention relates to a leaching method for indium in a waste liquid crystal panel and a corresponding leaching agent, and belongs to the technical field of solid waste recycling. Eutecticevaporate ionic liquid formed through choline chloride and diacid substances serves as the leaching agent, after a liquid crystal panel glass substrate is crushed into powder with the granularity of 50-200 meshes, the powder is immersed through the eutecticevaporate ionic liquid, the immersing temperature is 50-90 DEG C, the immersing time is 12-48 h, the solid and liquid mass ratio of the glass powder to the eutecticevaporate ionic liquid is 1:0.5-1:2, and the indium leaching rate is higher than 95%. The leaching method has the advantages that the leaching agent preparing method is simple, the leaching agent is environment-friendly and capable of being circularly used, the leaching method operation technology is simple, the indium leaching rate is high, and selectivity is high, and an effective method for recycling indium from the waste liquid crystal panel is provided.

Description

The leaching method of indium and leaching agent in a kind of waste and old liquid crystal panel
Technical field
The present invention relates to the leaching method of indium in a kind of waste and old liquid crystal panel and corresponding leaching agent, belong to solid waste recovery technology field.
Background technology
Liquid crystal display (LCD) is the key part of various information equipment indicating meter, is widely used in hyundai electronics, the engineering goods such as the operating panel of notebook computer, computer, TV, mobile phone and various mechanical means.Along with the quick growth of LCD product and model change, eliminate, LCD waste and old in a large number becomes the important composition of waste electronic thing gradually, and the resource utilization of consequent ecological environment problem and waste and old LCD attracts wide attention.China disclosed in 2009 " waste electric products recycling management rules ", and came into effect in 1 day January in 2011.Waste and old LCD TV and computer monitor include the management of these regulations in as first catalogue.Therefore, the recycling technology of waste and old LCD receives increasing concern.
At present, indium tin oxide (ITO) film is the requisite critical material of LCD produced, and wherein required indium metal (In) is a kind of important dissipated metal, and in earth mineral deposit, content is few, and seldom has independent deposit to exist.Due to scarcity and the preciousness of indium resource, from waste and old LCD, recovery indium is the emphasis in LCD recycling technology always.Meanwhile, the generation of a large amount of waste and old LCD is also a kind of important indium metal secondary resource.Such as the indium metal of Japan more than 80% derives from the recycling to indium secondary resource.China well below the developed country such as Japanese, American-European, causes the significant wastage of indium resource to the recovery utilization rate of indium secondary resource.From the patent documentation reported at present and non-patent literature, from waste and old LCD, the method for recovery indium mainly contains physicomechanical processes, high temperature reduction method and method of chemical treatment etc.First two method, owing to needing special main equipment, is invested huge and organic efficiency is not high, and therefore method of chemical treatment is the main method that current indium secondary resource reclaims.The ultimate principle of method of chemical treatment recovery indium adopts chemical soaker process and makes indium be that ionic state is dissolved in liquid phase from oxidation state, and then the enrichment being realized indium by methods such as extraction, displacements be separated, the preparation of soaker with select to be committed step wherein.Such as, application number be 201010295590.7 patent of invention disclose a kind of method of refining indium from waste and old LCD being soaker with the mixed solution of sulfuric acid and Manganse Dioxide; Application number be 201310544686.6 patent of invention adopt sulfuric acid dipping in conjunction with the method for sonic oscillation; Application number be 201010513266.8 patent of invention then adopt sodium hydroxide or potassium hydroxide alkali lye as steeping fluid.These methods all adopt strong acid and strong base liquid as soaker.The use of strong acid and strong base liquid is very strong to the corrodibility of equipment, and consequent acid, alkali wasteliquid also can produce serious pollution to environment, causes that the most cost of current China's indium recovery technology route is higher and environmental economy is not good enough.Therefore, exploitation is efficient, simple, the soaker of recovery indium from waste and old LCD of environmental protection and corresponding indium recovery technology, has well society and economic worth.
Eutectic ionic liquid is the ionic solvent of a kind of polycomponent that development in recent years is got up, and having the advantages such as raw material sources are extensive, cheap, preparation method is simple, volatility is little, physicochemical property are stable, is a class new green environment protection solvent.Eutectic ionic liquid realizes low melting point congruent melting by accepting or give electronics or proton and forming hydrogen bond, has selective dissolution ability to some metal oxides.This character of eutectic ionic liquid imparts in its selective separation at metal, recovery and purification etc. has potential using value.
Summary of the invention
The object of the present invention is to provide leaching agent and the leaching method of indium in a kind of waste and old liquid crystal display, leaching agent has that compound method is simple, environmental protection, the advantage that can be recycled, leaching method operating procedure is simple, and indium leaching yield is high, selectivity good, is conducive to use of large-scale production.
Solving the leaching agent that technical problem of the present invention adopts is: the eutectic ionic liquid that choline chloride 60 and two acids are formed, and the mol ratio of choline chloride 60 and diacid is 1:(0.5 ~ 2).
Wherein the molecular structure of diacid is: HOOC (CH 2) ncOOH, in formula, n value is 0 ~ 4.
The compound method of the eutectic ionic liquid that the present invention is used is:
The diacid of choline chloride 60 with corresponding molar weight is mixed, stir be placed on 80 ~ 100 DEG C environment in, until the limpid liquid of homogeneous transparent is formed.
In the waste and old liquid crystal display that the present invention adopts, the leaching method of indium is:
(1) glass substrate is separated from waste and old liquid crystal panel;
(2) glass substrate pulverizing is obtained glass powder;
(3) glass powder is soaked the organic compositions such as removing liquid crystal with acetone, after filtration, washing, drying, obtain cleaning glass powder;
(4), after the glass powder after clean being soaked the regular hour with the eutectic ionic liquid prepared as stated above, filter, washing solid, collects filtrate;
(5) by diacid, choline chloride 60 extracted with diethyl ether from aqueous phase separation, the filtrate after concentrated with after zinc metal sheet displacement thick indium.
Wherein, in the step (2) described in aforesaid method, the particle size range of described glass powder is 50 ~ 200 orders, and preferred particle size range is 50 ~ 100 orders.
Wherein, in the step (3) described in aforesaid method, described acetone soaks and usually at room temperature carries out, and soak time is 1 ~ 6 hour, and preferred soak time is 2 ~ 3 hours.
Wherein, in the step (4) described in aforesaid method, described eutectic ionic liquid soaking temperature is 50 ~ 90 DEG C, and preferred soaking temperature is 60 ~ 80 temperature; Described soak time is 12 ~ 48 hours, and preferred soak time is 16 ~ 30 hours; The solid-liquid mass ratio of described glass powder and eutectic ionic liquid is 1:0.5 ~ 1:2, and preferred solid-liquid mass ratio is 1:0.8 ~ 1:1.2.
The oxide compound of the Promethean employing eutectic ionic liquid of the present invention to indium has the characteristic of selective dissolution, by soak waste and old liquid crystal display powder leach indium method, do not need high temperature, pressure exerting device, technological process is simple, easy control of process conditions, realizing indium contained in waste and old liquid crystal display transfers to liquid phase from solid-state, and the leaching yield of indium higher than 95%, and eliminates effectively containing the interference of other metallic elements in solution of indium to the step such as enrichment, displacement of indium.In addition, the making of leaching agent is simple, and associated materials used can be recycled, and reduces production cost, does not produce noxious pollutant.
Embodiment:
Below in conjunction with example, the application of this leaching agent is described in detail, after specific embodiment is described in.
Embodiment 1
The concrete steps of the present embodiment are as follows:
(1) take choline chloride 60 70.0g and propanedioic acid 52.2g respectively, be uniformly mixed in the baking oven being placed on 80 DEG C and leave standstill, until form transparent, even, limpid eutectic ionic liquid, taking-up cooling is stand-by;
(2) take waste and old liquid crystal display powder 100g, add 200mL acetone, soak 2 hours under room temperature, filter, wash powder twice by proper amount of acetone, underpressure distillation filtrate reclaims acetone, and pressed powder is dried stand-by;
(3) joined by the eutectic ionic liquid that step (1) prepares in the pressed powder that step (2) handles well, agitation leach 24 hours at 80 DEG C, the leaching yield of indium is 100%.
Embodiment 2
The concrete steps of the present embodiment are as follows:
(1) take choline chloride 60 70.0g and oxalic acid dihydrate 63.2g respectively, be uniformly mixed in the baking oven being placed on 80 DEG C and leave standstill, until form transparent, even, limpid eutectic ionic liquid, taking-up cooling is stand-by;
(2) take waste and old liquid crystal display powder 100g, add 200mL acetone, soak 2 hours under room temperature, filter, wash powder twice by proper amount of acetone, underpressure distillation filtrate reclaims acetone, and pressed powder is dried stand-by;
(3) joined by the eutectic ionic liquid that step (1) prepares in the pressed powder that step (2) handles well, agitation leach 24 hours at 80 DEG C, the leaching yield of indium is 98%.
Embodiment 3
The concrete steps of the present embodiment are as follows:
(1) take choline chloride 60 70.0g and succinic acid 59.2g respectively, be uniformly mixed in the baking oven being placed on 80 DEG C and leave standstill, until form transparent, even, limpid eutectic ionic liquid, taking-up cooling is stand-by;
(2) take waste and old liquid crystal display powder 100g, add 200mL acetone, soak 2 hours under room temperature, filter, wash powder twice by proper amount of acetone, underpressure distillation filtrate reclaims acetone, and pressed powder is dried stand-by;
(3) joined by the eutectic ionic liquid that step (1) prepares in the pressed powder that step (2) handles well, agitation leach 24 hours at 80 DEG C, the leaching yield of indium is 97%.

Claims (4)

1. the leaching agent of indium in waste and old liquid crystal panel, it is characterized in that: leaching agent is the eutectic ionic liquid that choline chloride 60 and two acids are formed, the mol ratio of choline chloride 60 and diacid is 1:(0.5 ~ 2).
2. the leaching agent of indium in waste and old liquid crystal panel as claimed in claim 1, its compound method is: mixed by the diacid of choline chloride 60 with corresponding molar weight, stir be placed on 80 ~ 100 DEG C environment in, until the limpid liquid of homogeneous transparent is formed.
3. the leaching method of the leaching agent of indium in waste and old liquid crystal panel as claimed in claim 1, is characterized in that the method comprises the following steps:
(1) glass substrate is separated from waste and old liquid crystal panel;
(2) glass substrate pulverizing is obtained glass powder, the particle size range of glass powder controls at 50 ~ 200 orders;
(3) glass powder is soaked the organic compositions such as removing liquid crystal with acetone, after filtration, washing, drying, obtain cleaning glass powder;
(4), after the glass powder after clean being soaked the regular hour with the eutectic ionic liquid prepared as stated above, filter, washing solid, collects filtrate.
4. the leaching method of the leaching agent of indium in waste and old liquid crystal panel as claimed in claim 3, it is characterized in that: soaking temperature controls at 50 ~ 90 DEG C, soak time controls at 12 ~ 48 hours, and the solid-liquid mass ratio of glass powder and eutectic ionic liquid controls at 1:0.5 ~ 1:2.
CN201610019764.4A 2016-01-13 2016-01-13 Leaching method for indium in waste liquid crystal panel and leaching agent Pending CN105483389A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106011481A (en) * 2016-06-30 2016-10-12 华南理工大学 Method for recovering indium (In) from waste liquid crystal displays
CN106702167A (en) * 2017-03-07 2017-05-24 北京工业大学 Method for efficiently removing impurities from pickle liquor of abandoned liquid crystal display
CN106734107A (en) * 2017-01-04 2017-05-31 长沙汇聚环境技术有限公司 A kind of its recovery method as resource of waste liquid crystal display screen panel glass
CN110055422A (en) * 2019-05-21 2019-07-26 华南理工大学 A kind of method of indium in recycling waste liquid crystal displays

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106011481A (en) * 2016-06-30 2016-10-12 华南理工大学 Method for recovering indium (In) from waste liquid crystal displays
CN106734107A (en) * 2017-01-04 2017-05-31 长沙汇聚环境技术有限公司 A kind of its recovery method as resource of waste liquid crystal display screen panel glass
CN106734107B (en) * 2017-01-04 2019-05-21 河源市龙鑫光学科技有限公司 A kind of recovery method as resource of waste liquid crystal display screen panel glass
CN106702167A (en) * 2017-03-07 2017-05-24 北京工业大学 Method for efficiently removing impurities from pickle liquor of abandoned liquid crystal display
CN110055422A (en) * 2019-05-21 2019-07-26 华南理工大学 A kind of method of indium in recycling waste liquid crystal displays

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Application publication date: 20160413