CN106011481A - Method for recovering indium (In) from waste liquid crystal displays - Google Patents
Method for recovering indium (In) from waste liquid crystal displays Download PDFInfo
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- CN106011481A CN106011481A CN201610501280.3A CN201610501280A CN106011481A CN 106011481 A CN106011481 A CN 106011481A CN 201610501280 A CN201610501280 A CN 201610501280A CN 106011481 A CN106011481 A CN 106011481A
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- indium
- liquid crystal
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- waste liquid
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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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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for recovering indium (In) from waste liquid crystal displays. The method which comprises the following steps: (1) disassembling the waste liquid crystal displays to obtain glass panels; (2) completely dissolving liquid crystal of the glass panels in acetone, scraping pressure-sensitive adhesive and inner wall black matrixes, cleaning the treated glass panels, and airing the cleaned glass panels to obtain dry glass panels; (3) crushing the dry glass panels, decompounding the crushed glass panels with sulfuric acid, and carrying out filtering and dilution to obtain indium leachate; (4) adding Fe powder into the obtained indium leachate, carrying out sealed reduction, and extracting with an extracting solution P204 to obtain an indium extract; (5) adding hydrochloric acid into the indium extract for stripping to obtain an indium stripped solution; and (6) finally, adjusting the pH value of the indium stripped solution with NaOH, and carrying out reduction with zinc sheets to obtain sponge indium. The method has the advantages of high efficiency, environmental protection, high extraction recovery rate, low raw material price, and the like, and can solve the problems in recovery of indium in the waste liquid crystal displays, promote the development of the indium recovering enterprises, and create economic and social benefits.
Description
Technical field
The invention belongs to secondary resource technical field of comprehensive utilization, be specifically related to a kind of method of recovery indium (In) from waste liquid crystal display.
Background technology
Along with the development of industrial technology, the fields such as electronics manufacturing, aerospace instrument and equipment, semi-conducting material, being widely used of indium.That the usage amount of indium is most is the ITO of liquid crystal display, consumes the indium of about 75%.Indium is a kind of dissipated metal, and the abundance in the earth's crust is only 1 × 10-5.Owing to indium is dispersed in other mineral reserve, content is the lowest, causes exploitation and refines difficulty greatly, and cost is high, so, the yield of indium is relatively low.The distribution of indium is the most uneven, and its mineral reserve are mainly distributed on China, Peru, Canada, the U.S..China is with the obvious advantage on the reserves of indium, accounts for the 62% of whole world indium recoverable amount.The yield of primary indium occupies leading position the most in the market close to the limit, regeneration indium.During indium is carried out recycling, in liquid crystal display, other poisonous material is also processed.Glass of liquid crystal display panel contains the indium of 0.06%, if directly taking the means burned or fill to process, it will bring huge harm to air, soil, subsoil water, will also result in the waste of indium.At present, indium recovery technology immature, the problems such as leaching rate is the highest, process energy consumption is big, plus stock dispersion, can not process disposal on a large scale causes cost to increase so that from waste liquid crystal display, recovery indium is the most difficult, seeks a kind of technique method simple, high efficiente callback indium particularly important.
Summary of the invention
It is an object of the invention to provide a kind of method of recovery indium from waste liquid crystal display, solve the difficult problem that in waste liquid crystal display, indium reclaims, it is achieved to efficient, cheap, the recovery of of low pollution of indium in waste liquid crystal display.
For realizing described goal of the invention, present invention employs following technical scheme:
A kind of method of recovery indium (In) from waste liquid crystal display, the method for this recovery indium is divided into pretreatment, extraction back extraction system, displacement refine recovery indium three part, comprises the steps:
(1) disassemble frame before and after waste liquid crystal display, metal cap and can, tear the data wire gummed paper on face glass off, obtain face glass；
(2) the face glass blade obtained in step (1) is torn polaroid, add acetone and do not had face glass, make liquid crystal be completely dissolved in acetone, take out panel, scrape pressure sensitive adhesive and inwall black matrix", clean and dry, obtain glass substrate；
(3) glass substrate of gained in step (2) is crushed to about 1mm, uses Sulfuric-Acid Digestion, filter, dilute, it is thus achieved that indium leachate；
(4) the indium leachate of gained adds in step (3) Fe powder, after sealing reduction, use P
204 extract extractions, it is thus achieved that indium extract；
(5) the indium extract obtained in step (4) adds hydrochloric acid back extraction, it is thus achieved that indium strip liquor；
(6) finally the indium strip liquor NaOH in step (5) is regulated pH value, use zinc metal sheet reduction, it is thus achieved that sponge indium.
Further, in described step (1), Phillips screwdriver, flat mouth screwdriver is used to take out face glass.
Further, in described step (2), use glass blade to scratch face glass, tiger's jaw pincers break down the glass scratched, acetone soak 3h, make liquid crystal be completely dissolved in acetone.
Further, in described step (3), using omnipotent high speed disintegrator that glass substrate is crushed to about 1mm, by solid-to-liquid ratio 1:1 Sulfuric-Acid Digestion 1h at 160 DEG C, after cooling, acid solution sucking filtration, indium leachate is diluted to 0.5mol/L.
Further, in described step (4), add the iron powder of theoretical amount 1.5 times, seal, constant temperature 60 DEG C stirring 4h, cooling.Use 1mol/LP
204 (normal hexane dilutions) are as extractant, and oil-water ratio is 1:9, and concussion frequency is 200r/min, and extraction time is to carry out under 5min, room temperature.
Further, in described step (5), indium extract uses 4mol/L hydrochloric acid back extraction, and oil-water ratio is 4:1, and concussion frequency is 200r/min, and Stripping times is 20min.
Further, in described step (6), use NaOH regulation strip liquor pH value to 1.4, add zinc metal sheet, temperature constant magnetic stirring 36h at 60 DEG C, obtain the sponge indium being attached on zinc metal sheet.
Advantages of the present invention and good effect:
(1) method from waste liquid crystal display recovery indium that the present invention provides, uses Physical to peel off polaroid, and flow process is simple, decreases the use of acetone, has certain economical and environmentally friendly benefit.
(2) the used normal hexane of the present invention is as the diluent of di-(2-ethylhexyl)phosphoric acid ester (P 204) extractant, with existing sulfonated kerosene as compared with diluent, cheap, environmental protection, good stability, the more high advantage of extraction yield, its extraction yield is up to 99.4%.
(3) method of recovery indium that the present invention provides, by disassembling, crush, soak, extract, back extraction, the process such as reduction, silver-colored extraction yield is 99.4%, and back extraction ratio is 90.9%, and percent reduction is 90.8%, and its comprehensive recovery is about 82.4%.
Accompanying drawing explanation
Fig. 1 is present invention process system flow chart.
Detailed description of the invention
It is intended to further illustrate the present invention below in conjunction with embodiment, and the unrestricted present invention.
Embodiment
As it is shown in figure 1, one method of recovery indium (In) from waste liquid crystal display, the method for this recovery indium is divided into pretreatment, extraction back extraction system, displacement refine recovery indium three part, comprises the steps:
1. the liquid crystal display back side is placed towards sky, screws out all screws in the back side with Phillips screwdriver.Utilize flat mouth screwdriver to pry open along the commissure of the front and back of plastic frame, cut off button and the line of wiring board that front frame is carried secretly, take off front frame.After removing front frame, screw out metal cap and the screw of after-frame, take out metal cap.Before and after can, frame uses wedge shape occlusion, flat mouth screwdriver can only be used to pry open along frame gap strength, to open can, tear the data wire gummed paper connected on face glass, and the wiring board connected of tearing obtains face glass.
2., with blade at the corner teasing of polaroid, tear polaroid along opening.Diamant is used to scratch face glass, the repetitive operation of corresponding region, the back side along face glass surrounding.The glass separation of glasses substrate scratched is broken down with tiger's jaw pincers；Add acetone and do not had glass substrate, soak 3 hours, make liquid crystal be completely dissolved in acetone；Take out glass substrate, scrape the black matrix" of pressure sensitive adhesive and inwall, clean, dry.
3. (unit are is less than 1cm to preliminary broken glass substrate2) pour omnipotent high speed disintegrator into, screw upper cover；Open the switch of omnipotent high speed disintegrator, work 1 minute；The particle diameter of the glass substrate through pulverizing is less than 1mm；The glass substrate powder weighing 40g adds in beaker, adds 40mL sulphuric acid by liquid-solid ratio 1:1, and cap upper surface ware is placed on electric hot plate 160 DEG C of heated at constant temperature 1 hour, takes off beaker cooling；Simple filtration acid extract, solid-liquid separation, acid solution sucking filtration (< 0.45 μm), stand, the acid extract of measured amounts, add deionized water, be diluted to 0.5mol/L.
4. take the feed liquid of a certain amount of 0.5mol/L, add reduced iron powder by the 1.5 of theoretical amount times；Sealing or under protection of reducing atmosphere, be placed on magnetic stirring apparatus, constant temperature 60 DEG C heats 4 hours.Take off quickly cooling.The P 204(normal hexane dilution of 1mol/L is added toward reducing solution), oil-water ratio is 1:9, and frequency of oscillation is 200r/min, and vibrate 5min.Using separatory funnel to discharge lower floor's aqueous phase, oil phase is standby, and the extraction yield of indium is 99.4%.
5. taking a certain amount of indium extract, 4mol/L hydrochloric acid makees back washing agent, and oil-water ratio is 4:1, and frequency of oscillation is 200r/min, and Stripping times is 20min, stands, separatory funnel separation aqueous phase, obtains indium strip liquor, and the back extraction ratio of indium is 90.9%.
6. with the pH value of the hydrochloric acid strip liquor of NaOH solution regulation 4mol/L to 1.4.Beaker loads the hydrochloric acid strip liquor that a certain amount of pH value is 1.4, adds zinc metal sheet, is placed in constant temperature blender with magnetic force, 60 DEG C of heated at constant temperature, takes off beaker after 36h, and cooling obtains sponge indium.
The percent reduction of the present embodiment indium is 90.8%, then the overall recovery of indium is 82.4%.
Described above and shown embodiment, can not resolve is limited determines the design philosophy of the present invention.Technical field in the present invention holds identical skill can be by the technical thought of the present invention with various form improvement change; as being not limited to above-mentioned embodiment; the kind of raw material and the difference of silver content is combined in this area; can suitably select this process system to select on the basis of native system core process, such improvement and change be interpreted as belonging to protection scope of the present invention.
Claims (7)
1. the method for a recovery indium from waste liquid crystal display (In), it is characterised in that the method for this recovery indium is divided into pretreatment, extraction back extraction system, displacement refine recovery indium three part, comprises the steps:
(1) disassemble frame before and after waste liquid crystal display, metal cap and can, tear the data wire gummed paper on face glass off, obtain face glass；
(2) the face glass blade obtained in step (1) is torn polaroid, add acetone and do not had face glass, make liquid crystal be completely dissolved in acetone, take out panel, scrape pressure sensitive adhesive and inwall black matrix", clean and dry, obtain glass substrate；
(3) glass substrate of gained in step (2) is crushed to about 1mm, uses Sulfuric-Acid Digestion, filter, dilute, it is thus achieved that indium leachate；
(4) the indium leachate of gained adds in step (3) Fe powder, after sealing reduction, use the extraction of P204 extract, it is thus achieved that indium extract；
(5) the indium extract obtained in step (4) adds hydrochloric acid back extraction, it is thus achieved that indium strip liquor；
(6) finally the indium strip liquor NaOH in step (5) is regulated pH value, use zinc metal sheet reduction, it is thus achieved that sponge indium.
2. the method for recovery indium (In) as claimed in claim 1, it is characterised in that: in described step (1), use Phillips screwdriver, flat mouth screwdriver to take out face glass.
3. the method for recovery indium (In) as claimed in claim 1, it is characterised in that: in described step (2), use glass blade to scratch face glass, tiger's jaw pincers break down the glass scratched, acetone soak 3h, make liquid crystal be completely dissolved in acetone.
4. the method for recovery indium (In) as claimed in claim 1, it is characterized in that: in described step (3), use omnipotent high speed disintegrator that glass substrate is crushed to about 1mm, by solid-to-liquid ratio 1:1 Sulfuric-Acid Digestion 1h at 160 DEG C, after cooling, acid solution sucking filtration, indium leachate is diluted to 0.5mol/L.
5. the method for recovery indium (In) as claimed in claim 1, it is characterised in that: in described step (4), add the iron powder of theoretical amount 1.5 times, seal, constant temperature 60 DEG C stirring 4h, cooling；Use 1mol/LP
204 (normal hexane dilutions) are as extractant, and oil-water ratio is 1:9, and concussion frequency is 200r/min, and extraction time is to carry out under 5min, room temperature.
6. the method for recovery indium (In) as claimed in claim 1, it is characterised in that: in described step (5), indium extract uses 4mol/L hydrochloric acid back extraction, and oil-water ratio is 4:1, and concussion frequency is 200r/min, and Stripping times is 20min.
7. the method for recovery indium (In) as claimed in claim 1, it is characterised in that: in described step (6), use NaOH regulation strip liquor pH value to 1.4, add zinc metal sheet, temperature constant magnetic stirring 36h at 60 DEG C, obtain the sponge indium being attached on zinc metal sheet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610501280.3A CN106011481A (en) | 2016-06-30 | 2016-06-30 | Method for recovering indium (In) from waste liquid crystal displays |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610501280.3A CN106011481A (en) | 2016-06-30 | 2016-06-30 | Method for recovering indium (In) from waste liquid crystal displays |
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| CN106011481A true CN106011481A (en) | 2016-10-12 |
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| CN201610501280.3A Pending CN106011481A (en) | 2016-06-30 | 2016-06-30 | Method for recovering indium (In) from waste liquid crystal displays |
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Cited By (3)
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| CN106868324A (en) * | 2017-03-07 | 2017-06-20 | 北京工业大学 | A kind of method of utilization salting out from the pickle liquor enriching and purifying indium of waste material containing ITO |
| CN110016566A (en) * | 2019-05-17 | 2019-07-16 | 河海大学常州校区 | A method of recycling indium in discarded photovoltaic module |
| CN110541076A (en) * | 2019-09-26 | 2019-12-06 | 华南理工大学 | reactor for leaching metals in solid waste and leaching method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110016566A (en) * | 2019-05-17 | 2019-07-16 | 河海大学常州校区 | A method of recycling indium in discarded photovoltaic module |
| CN110541076A (en) * | 2019-09-26 | 2019-12-06 | 华南理工大学 | reactor for leaching metals in solid waste and leaching method |
| CN110541076B (en) * | 2019-09-26 | 2021-05-14 | 华南理工大学 | Reactor for leaching metals in solid waste and leaching method |
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Application publication date: 20161012 |