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WO2007015392A1 - Procédé et appareil de récupération d’indium d’un affichage à cristaux liquides mis au rebut - Google Patents

Procédé et appareil de récupération d’indium d’un affichage à cristaux liquides mis au rebut Download PDF

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Publication number
WO2007015392A1
WO2007015392A1 PCT/JP2006/314626 JP2006314626W WO2007015392A1 WO 2007015392 A1 WO2007015392 A1 WO 2007015392A1 JP 2006314626 W JP2006314626 W JP 2006314626W WO 2007015392 A1 WO2007015392 A1 WO 2007015392A1
Authority
WO
WIPO (PCT)
Prior art keywords
indium
metal
metal particles
liquid crystal
crystal display
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2006/314626
Other languages
English (en)
Japanese (ja)
Inventor
Toshiaki Muratani
Takamichi Honma
Tomoharu Maeseto
Mitsushige Shimada
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shinko Pantec Co Ltd
Sharp Corp
Original Assignee
Sharp Corp
Kobelco Eco Solutions Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sharp Corp, Kobelco Eco Solutions Co Ltd filed Critical Sharp Corp
Priority to JP2007529217A priority Critical patent/JPWO2007015392A1/ja
Priority to US11/997,884 priority patent/US20100101367A1/en
Publication of WO2007015392A1 publication Critical patent/WO2007015392A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • 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
    • C22B25/00—Obtaining tin
    • C22B25/06—Obtaining tin from scrap, especially tin scrap
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
    • 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
    • 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
    • C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • 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

Definitions

  • the present invention relates to a method and apparatus for recovering indium from a discarded liquid crystal display, and more specifically, a discarded liquid crystal television, a mobile phone, a portable game machine, etc., or a liquid crystal discharged as a defective product in a production process.
  • the present invention relates to a method and apparatus for recovering valuable indium (In) from a display (hereinafter also referred to as “waste LCD”) as an alloy or a single metal.
  • ITO film An indium tin oxide (ITO) film is used as a transparent electrode in a liquid crystal display (hereinafter also referred to as LCD!).
  • the ITO film is mainly formed by sputtering, but In is used as the target.
  • In is a rare metal obtained during the zinc refining process, and its death has been feared in recent years.
  • Waste LCD contains about 300mgZL of In, and with the Withering of In, it is required to collect In during the recycling process.
  • Non-Patent Document 1 relates to a fluidized bed LCD processing system, and the fluidized bed LCD processing system comprises a fluidized bed processing section, a cyclone, a cooler, a high temperature bag filter, a catalyst fluidized bed, and a water washing tower.
  • the fluidized bed LCD processing system comprises a fluidized bed processing section, a cyclone, a cooler, a high temperature bag filter, a catalyst fluidized bed, and a water washing tower.
  • the silicon sand of the fluid medium in the processing section is accumulated in the fluid medium.
  • about 60% of the waste LCD accumulates in the fluid medium and the rest is collected by the bag filter, so the indium recovery rate is about 60% overall, and the recovery is The rate was as low as about 60%.
  • Non-Patent Document 1 Monthly Display April 2002 P36-46
  • Patent Document 1 is a method in which ITO is dissolved in an acid such as nitric acid or hydrochloric acid, impurities such as Sn are precipitated and removed, neutralized by adding ammonia, and recovered as indium hydroxide. .
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2000-128531
  • the filterability of indium hydroxide obtained by the treatment is poor, the operation takes a long time, and the indium hydroxide obtained by neutralization or the like is used. There is a problem that the nature of the system changes.
  • the present invention has been made to solve such a problem, and it is possible to recover In as a valuable metal, which does not need to be recovered in the state of hydroxide hydroxide as in the prior art.
  • the present invention has been made to solve such a problem, and the invention according to claim 1 relating to a method for recovering In from waste LCD includes a waste liquid crystal display containing indium tin oxide.
  • the crushed waste liquid crystal display also uses acid to dissolve indium tin oxide to obtain an indium compound-containing solution, which flows into the recovery reactor and has an ionic value higher than that of indium in the recovery reactor.
  • Metal particles that also have a strong metal force are added, the metal particles are flowed, and indium or an indium alloy contained in the indium compound-containing solution is deposited on the surface of the metal particles, and then the metal is separated by a peeling means. Particle force The deposited indium or indium alloy is peeled off, and the peeled solid indium or indium alloy is liquidized. It is characterized by separating the components and collecting them.
  • the invention according to claim 2 is the method for recovering indium from the waste liquid crystal display according to claim 1, wherein the metal particles having a metal force having a larger ionic tendency than indium are zinc particles or aluminum particles. It is characterized by being.
  • the invention of claim 3 is the method for recovering indium from the waste liquid crystal display according to claim 1 or 2, wherein the means for peeling off the indium or indium alloy deposited on the metal particles by the metal particle force, It is a means for vibrating metal particles by ultrasonic waves, or a means for stirring metal particles by an electromagnet and causing them to collide with each other.
  • the invention of claim 4 is an indium in which indium tin oxide is dissolved from the waste liquid crystal display by using the method for recovering indium from the waste liquid crystal display according to any of claims 1 to 3.
  • the indium compound-containing solution Before flowing the compound-containing solution into the recovery reactor, the indium compound-containing solution is allowed to flow into the impurity removal reactor, and the ionic valence tendency is larger than that of impurity metals other than indium in the indium compound-containing solution!
  • metal particles made of metal are added into the impurity removal reactor to cause the metal particles to flow, and the impurity metal is deposited on the surface of the metal particles, and then the metal particle force is separated by a peeling means. Peeling and removing the deposited impurity metal
  • the invention according to claim 5 is the method for recovering indium of waste liquid crystal display power according to claim 4, wherein the means for separating the impurity metal deposited on the metal particles from the metal particles by ultrasonic waves It is a means for vibrating particles, or a means for stirring metal particles with an electromagnet and causing them to collide with each other. Furthermore, the invention described in claim 6 is characterized in that in the method for recovering indium from the waste liquid crystal display according to claim 4 or 5, the impurity metal is tin.
  • the metal particles made of a metal having a higher ionic tendency than an impurity metal are iron particles. It is a feature.
  • the invention according to claim 8 is the method for recovering indium from the waste liquid crystal display according to claim 7, wherein an alkali is added to the solution containing the indium compound after removing the impurity metal, and iron is used as a hydroxide. It is characterized by removing the precipitate.
  • the invention according to claim 9 is a method in which an indium compound-containing solution is obtained by dissolving indium tin oxide using an acid from the waste liquid crystal display in a state where the waste liquid crystal display is contained in a bag.
  • the waste liquid crystal display contained in the bag is washed and neutralized, and then dried.
  • the invention according to claim 10 further relates to an apparatus for recovering indium from a waste liquid crystal display, wherein a crusher for crushing a waste liquid crystal display containing indium tin oxide and an acid for the crushed waste liquid crystal display are used. And an indium dissolution apparatus for obtaining an indium compound-containing solution by dissolving indium tin oxide, and an indium dissolution apparatus obtained by the indium dissolution apparatus. An indium compound-containing solution is introduced, and the ionic valence tendency is larger than that of the indium.
  • the metal precipitation reaction is performed by adding metal particles having metal power to deposit indium or an indium alloy on the surface of the metal particles.
  • a separation reactor for separating the separated solid indium or indium alloy from the liquid component a separation reactor for separating the deposited indium or indium alloy from the liquid, and a separating means for separating the separated indium or indium alloy from the liquid component. It is characterized by comprising.
  • the invention according to claim 11 is the apparatus for recovering indium from the waste liquid crystal display according to claim 10, wherein the metal particles having a metal force having a larger ionic tendency than indium are zinc particles or aluminum particles. It is characterized by being.
  • the invention described in claim 12 is the indium recovery device for waste liquid crystal display power according to claim 10 or 11, wherein the means for peeling off the indium or indium alloy deposited on the metal particles includes: It is a means for vibrating metal particles by ultrasonic waves, or a means for stirring metal particles with an electromagnet and causing them to collide with each other.
  • the invention according to claim 13 is an indium compound-containing solution obtained by an indium dissolution apparatus in addition to the indium recovery apparatus from the waste liquid crystal display according to any one of claims 10 to 12. And flowing metal particles having a higher ionic valence than the impurity metals other than indium in the indium compound-containing solution to cause the metal particles to flow, and allowing the impurity metals to flow on the surface of the metal particles.
  • An impurity removing reactor having means for separating and removing the precipitated impurity metal by peeling off the metal particle force is provided on the upstream side of the recovery reactor.
  • the means for separating the impurity metal deposited on the metal particles from the metal particles by ultrasonic waves It is a means for vibrating particles, or a means for stirring metal particles with an electromagnet and causing them to collide with each other.
  • the invention described in claim 15 is characterized in that in the indium recovery apparatus having the power for waste liquid crystal display according to claim 13 or 14, the impurity metal is tin.
  • the apparatus for recovering indium from the waste liquid crystal display described in claims 13 to 15 has a higher ionic tendency than the impurity metal!
  • the metal particles are iron particles.
  • the invention described in claim 17 is the apparatus for recovering indium from the waste liquid crystal display according to claim 16, wherein the alkali is added to the indium-containing solution after removing the impurity metal, and iron is precipitated as a hydroxide. It is characterized by having a precipitation removing device for removing.
  • the present invention provides a solution containing an indium compound by crushing a waste liquid crystal display (waste LCD) containing indium tin oxide, and dissolving the crushed waste LCD force using an acid to dissolve indium tin oxide. And flowing into the recovery reactor, adding metal particles having a metal force having a larger ionic valence than indium (In) into the recovery reactor, causing the metal particles to flow, and In or In alloy contained in the contained solution is deposited on the surface of the metal particles, and then the deposited In or In alloy is also peeled off by the peeling means, and the peeled solid In or In alloy is peeled off.
  • waste LCD waste liquid crystal display
  • the waste LCD force can dissolve ITO easily and efficiently, and the ionization tendency is used to recover In from the solution in which In is dissolved.
  • the combination of the cementation reaction and the stripping technology that is, the use of metal particles increases the total surface area of the metal for the metal deposition reaction, improves the deposition reaction rate, and increases the growth of the deposited metal to some extent. Peeling with a peeling means always exposes a new metal surface and maintains the reaction rate, so the recovery rate of In from waste LCD is significantly higher than conventional dry and wet methods. If it can be improved, it has a positive effect.
  • an indium compound in which waste LCD power indium oxide is dissolved Metals other than In contained in the containing solution such as tin A metal having a higher ionic tendency than the impurity metal such as (Sn), for example, metal particles such as iron (Fe) is added and fluidized, and the impurity metal such as Sn contained in the waste liquid is added to the iron or the like.
  • the waste liquid can be supplied to the recovery reactor in a state where impurity metals other than In such as Sn are removed in advance, the purity of In recovered in the recovery reactor is further improved. There is an effect of doing.
  • the waste LCD is stored in the bag and subjected to In elution with acid, neutralization with washing, and drying, the fine waste LCD crushed in the waste LCD crushing process is knocked out. It is possible to perform consistent processing while it is housed inside, and to simplify processing as a whole. In addition, since it is not necessary to handle fine waste LCD pieces that accept the waste LCD crushing process power as powder, there is an effect that it will not be difficult to handle.
  • FIG. 1 is a schematic block diagram of an In recovery device for waste LCD power as one embodiment.
  • FIG. 2 is a schematic front view of an impurity removal reactor or a recovery reactor in the In recovery apparatus.
  • FIG. 3 is a schematic front view of an impurity removal reactor or a recovery reactor according to another embodiment.
  • FIG. 4 is a schematic front view of an impurity removal reactor or a recovery reactor according to another embodiment.
  • FIG. 5 is a schematic plan view of a slide board provided with an electromagnet used in the embodiment of FIG.
  • FIG. 6 is a schematic block diagram showing an In recovery apparatus according to another embodiment.
  • FIG. 7 is a schematic sectional view of an elution treatment apparatus in the same apparatus.
  • FIG. 8 is a schematic explanatory diagram of an apparatus used in the examples.
  • the waste LCD force indium recovery device of this embodiment is composed of an indium dissolution device (hereinafter also referred to as an In dissolution device) 1 that dissolves ITO using hydrochloric acid as well as the waste LCD force.
  • Impurity removing reactor 2 for adding iron particles (Fe particles) to the indium compound-containing solution dissolved in dissolving apparatus 1 to remove impurity metals other than In, and for removing the impurities
  • Precipitation removal device 3 that precipitates and removes the Fe particles in the waste liquid from which impurity metals have been removed in reactor 2 as iron (Fe) hydroxide
  • precipitation removal device 3 removes the precipitate of Fe hydroxide.
  • a recovery reactor 4 for recovering the generated waste liquid power In.
  • the In dissolution apparatus 1 is for obtaining an indium compound-containing solution by dissolving In with crushed waste LCD and hydrochloric acid (hydrochloric acid aqueous solution).
  • the indium compound-containing solution is prepared so that the In content is 100 to 300 mgZL.
  • This indium compound-containing solution is prepared so that the concentration of hydrochloric acid is 20% and the pH of hydrochloric acid is 1.5.
  • the impurity removal reactor 2 is for removing Sn, which is an impurity, from the indium compound-containing solution, and includes a vertically long reactor body 5 as shown in FIG.
  • the reactor main body 5 includes a reactor upper part 6, a reactor intermediate part 7, and a reactor lower part 8, which are connected via connecting parts 9 and 10, respectively.
  • Reactor upper part 6, reactor intermediate part 7, and reactor lower part 8 are each formed to have the same width, but the cross-sectional area of reactor upper part 6 is formed to be larger than the cross-sectional area of reactor intermediate part 7.
  • the cross-sectional area is larger than the cross-sectional area of the lower reactor 8.
  • the connecting portions 9 and 10 are formed in a tapered shape that is wide upward.
  • a substantially conical inflow chamber 11 for inflow of an indium compound-containing solution to be processed is provided below the reactor lower part 8, and an inflow pipe 12 is provided at the lower part thereof. Yes.
  • the inflow pipe 12 is provided with a check valve.
  • an upper chamber 13 is provided on the upper side of the upper part 6 of the reactor, and a discharge pipe 14 is provided on the side to deposit Sn, which is an impurity metal, on metal particles (Fe particles) and discharge it. It is.
  • the upper chamber 13 is a part for discharging Sn together with Fe particles by such an exhaust pipe 14, and based on the difference in ionization tendency with Sn to be removed as impurities, it is a so-called cementation. It is also the part where Fe particles are added to cause the reaction (metal precipitation reaction). Actually, the cementation reaction between Fe and Sn occurs in the entire reactor body 1.
  • Fe particles are used as the metal particles to be input as described above.
  • the average particle diameter of Fe particles is preferably 0.1 to 8 mm, but in this embodiment, an average particle diameter of about 3 mm is used.
  • the average particle diameter is measured by an image analysis method or a WIS Z 8801 screening test method.
  • the precipitation removing apparatus 3 is for removing the Fe particles as a hydroxide by precipitation. Hydroxide precipitation is removed by adding an alkali (alkaline solution) such as sodium hydroxide. The pH of the waste liquid in the sediment removal device 3 is adjusted to 8-9.
  • the recovery reactor 4 is for recovering the indium compound-containing solution force In after removing Sn, which is an impurity, and precipitating and removing Fe as a hydroxide, as described above. It has the same construction power as the reactor 2 for removal. That is, as shown in FIG. 2, the reactor main body 5 is configured such that the reactor upper part 6, the reactor intermediate part 7, and the reactor lower part 8 are connected through the connection parts 9 and 10. In the recovery reactor 4, the pH is adjusted to 1.5 or lower.
  • the inflow chamber 11, the inflow pipe 12, the upper chamber 13, the discharge pipe 14, and the ultrasonic oscillators 15a, 15b, 15c are the reactor upper part 6, the reactor intermediate part 7, and The point provided at the lower part 8 of the reactor is the same as the reactor 2 for removing impurities.
  • this indium compound-containing solution is supplied to the impurity removing reactor 2.
  • the indium compound-containing solution supplied to the impurity removing reactor 2 flows into the reactor body 5 from the inflow pipe 12 of the impurity removing reactor 2 through the inflow chamber 11.
  • the gold used to cause a cementation reaction from the upper chamber 13. Add metal particles (Fe particles).
  • the indium compound-containing solution that has flowed in rises in the vertical direction, while the indium compound-containing solution and the Fe particles introduced from the upper chamber 13 flow so as to form a fluidized bed. State.
  • the standard electrode potential of Fe 2+ is smaller than that of Sn 2+ .
  • the ionization tendency of Fe is larger than Sn.
  • Fe having a high ionization tendency becomes Fe 2+ (reaction opposite to the above equation (1)) and is eluted in the indium compound-containing solution, together with the indium compound.
  • Sn 2+ becomes Sn and precipitates on the surface of Fe particles.
  • the ultrasonic oscillators 15a, 15b, 15c are operated.
  • the ultrasonic waves oscillated from the ultrasonic oscillators 15a, 15b, and 15c generate vibration force and stirring force on the Fe particles on which the Sn is deposited.
  • Sn that has been deposited is forcibly separated from the Fe particles.
  • the Sn thus peeled is discharged from the upper chamber 13 through the discharge pipe 14 to the outside of the reactor body 5, and as a result, removed from the indium compound-containing solution.
  • the metal (Fe) used for removing the impurity metal is in the form of particles, for example, compared with a case where an iron lump or the like is input,
  • the surface area of the metal (Fe) for causing the cementation reaction is increased, and the speed of the Sn precipitation reaction is improved.
  • the forced separation by ultrasonic vibration as described above always exposes a new metal surface (the surface of Fe particles) and maintains the reaction rate.
  • the cross-sectional area of the reactor body 5 is formed so as to increase discontinuously with upward force in the present embodiment.
  • the counter-flow velocity gradually decreases, so that the metal particles whose particle size has decreased due to the cementation reaction as described above will inadvertently overflow at the top of the reactor body 5 where the cross-sectional area increases. The possibility of being held in the reactor body 5 without increasing becomes high.
  • the indium compound-containing solution flows into the lower side force of the reactor main body 5 and passes through the reactor main body 5, a target metal such as Sn is deposited on the metal particles made of Fe by a cementation reaction. Therefore, the concentration of the impurity metal in the indium compound-containing solution decreases as the force toward the top of the reactor body 5 increases.
  • finer metal particles exist in the upper part of the reactor body 5 and the upward flow velocity of the indium compound-containing solution gradually decreases, so that the number of metal particles is increased. It is recognized that the total surface area of the metal particles increases toward the top of the reactor body 5. As a result, the reaction rate of the cementation reaction (impurity metal impurity extraction efficiency) is improved, so that the impurity metals Ni and Sn are also added to the upper part of the reactor body 5 where the impurity metal concentration is lower. It is possible to remove the waste liquid efficiently.
  • the indium compound-containing solution from which Sn has been removed is supplied to the precipitation removing device 3.
  • An alkali (alkaline solution) such as sodium hydroxide is added to the precipitation removing device 3.
  • the indium compound-containing solution after precipitation and removal of Fe hydroxide is adjusted to pHl. 5 or lower and indium hydroxide is redissolved, and then supplied to the recovery reactor 4.
  • the indium compound-containing solution supplied to the recovery reactor 4 flows into the reactor body 5 from the inflow pipe 12 through the inflow chamber 11 as in the case of the impurity removal reactor 2.
  • metal particles Zn particles or A1 particles
  • for causing a cementation reaction are introduced from the upper chamber 13.
  • the indium compound-containing solution that has flowed in rises and the metal particles introduced from the upper chamber 13 become a fluid state.
  • the standard electrode potential force S of Zn 2+ or Al 3+ is smaller than that of In 3+ .
  • the ionization tendency of Zn or A1 is larger than that of In. Therefore, Zn or A1 with a large ionization tendency becomes Zn 2+ or Al 3+ (reaction opposite to the above formulas (4) and (5)) in the fluidized state as described above.
  • solution In 3+ is dissolved in and contained in the indium compound-containing solution, and In 3+ becomes In and precipitates on the surface of Zn or A1 particles.
  • the ultrasonic oscillators 15a, 15b, and 15c are operated.
  • the ultrasonic waves oscillated from the ultrasonic oscillators 15a, 15b, and 15c are vibrated and stirred on the Zn or A1 particles on which the In is precipitated.
  • a force is applied, so that the precipitated In is forcibly separated from the Zn or A1 particles.
  • the In peeled in this way is discharged from the upper chamber 13 through the discharge pipe 14 to the outside of the reactor main body 5, whereby In is recovered as a valuable metal.
  • the particulate Zn is used as Zn or A1 in the same manner as in the case of iron in the impurity removal reactor 2, a metal for causing a cementation reaction is used.
  • the surface area increases and the rate of In precipitation reaction increases.
  • the surface of new Zn or A1 particles can always be exposed and the reaction rate can be maintained by forced peeling by ultrasonic vibration as described above. .
  • the particle size of Zn or A1 introduced into the upper chamber 13 is as follows. It will inevitably decrease over time. As a result, the indium compound-containing solution normally moves up in the reactor main body 5 at almost the same upward flow rate, so that the particle size decreases and becomes smaller toward the upper part. Particles may inadvertently overflow from the reactor body 5.
  • the indium compound is contained in the reactor body 5.
  • the upward flow velocity of the solution gradually decreases. Therefore, the metal particles whose particle size has been reduced by the cementation reaction or the like as described above are not suitable for the upper part of the reactor body 5 where the cross-sectional area increases. The possibility of being held in the reactor body 5 without overflowing is increased.
  • the indium compound-containing solution also flows in the lower side force of the reactor main body 5, and when passing through the reactor main body 5, the target In is deposited on Zn or A1 particles by a cementation reaction. Therefore, the concentration of In in the indium compound-containing solution decreases as the force toward the top of the reactor body 5 increases.
  • finer Zn or A1 particles are present in the upper part of the reactor body 5 and the upward flow rate of the indium compound-containing solution gradually decreases.
  • the total surface area of Zn or A1 particles increases toward the top of the reactor body 5.
  • the reaction speed of the cementation reaction In precipitation efficiency
  • the recovery target In is contained in the indium compound even in the upper part of the reactor body 5 where the In concentration is lower. This makes it possible to efficiently recover from the solution.
  • the present embodiment is different from the first embodiment in the structure of the reactor main body 5 of the impurity removing reactor 2 and the recovery reactor 4. That is, in the present embodiment, as shown in FIG. 3, the entire peripheral surface of the reactor body 5 is formed to be tapered upward, so that the cross-sectional area of the reactor body 5 continuously increases upward. It is configured. This is different from the case of the first embodiment in which the cross-sectional area of the reactor body 5 discontinuously increases upward.
  • the ultrasonic oscillators 15a, 15b, 15c are provided in three places from the upper part to the lower part of the reactor main body 5 in common with the first embodiment. Therefore, in the present embodiment, as in the first embodiment, Sn which is an impurity metal to be removed, which is deposited on the metal particles by the ultrasonic waves oscillated from the ultrasonic oscillators 15a, 15b, 15c. Alternatively, it is possible to forcibly peel In, which is the metal to be collected.
  • the cross-sectional area is configured to increase upward, and in common with Embodiment 1, So this implementation Even in the form, a fine metal particle having a reduced particle size is retained at the upper part of the reactor body 5 to prevent inadvertent overflow and a reactor with a low concentration of the target metal. The effect is that the target metal can be efficiently removed or recovered at the upper part of the main body 5.
  • the slide board 17 having the electromagnet 16 as shown in FIG. 5 is connected to the guide rail 18 provided on the side of the reactor body 5 having a rectangular horizontal section as shown in FIG. It can be moved up and down. As shown in FIG. 5, the slide board 17 has a space portion 19 in the center, and is disposed so as to surround the reactor body 5 by inserting the reactor body 5 into the space portion 19.
  • the metal particles used in the present embodiment are iron or the like that is a magnetic material.
  • the metal particles in the reactor main body 5 are stirred, and a large number of metal particles collide with each other.
  • Metal particle force The deposited metal is forcibly separated.
  • Metal Particle Force Precipitation Although the means for separating the metal is different, in this embodiment as well, the deposited metal is preferably peeled from the metal particle to suitably remove the impurity metal or recover In which is a valuable metal. it can.
  • the apparatus for recovering indium from the waste LCD of this embodiment includes an elution treatment device 25, a washing neutralization treatment device 26, and a drying treatment 27.
  • the elution treatment apparatus 25 includes an elution treatment container 22 such as an FRP tank.
  • the elution processing container 22 is formed to have a size capable of storing a waste LCD accommodated in a bag 21 made of a resin or cloth such as a flexible container bag.
  • a perforated plate 23 and a perforated plate support 24 are provided below the elution processing container 22.
  • the bag 21 is made of the perforated plate 2 Configured to be held on 3!
  • the waste LCD crushed by a crusher or the like is circulated through the hydrochloric acid solution for In dissolution extraction while being contained in the bag 21, and the waste LCD force is also reduced when the hydrochloric acid solution passes through the waste LCD layer 28. In is dissolved and extracted. In other words, the waste LCD force is also dissolved in indium tin oxide using hydrochloric acid to obtain an indium compound-containing solution.
  • the waste LCD after the dissolution and extraction treatment is moved to the next cleaning neutralization treatment device 26 while being accommodated in the bag 21 as it is, and is accommodated in the cleaning neutralization treatment device 26.
  • Wash neutralization treatment The movement from the elution treatment device 25 to the washing neutralization treatment device 26 is performed using a hoist or the like.
  • the circulation process may be performed in a downward flow or an upward flow.
  • the waste LCD that has been washed and neutralized is moved to the drying device 27 while being stored and held in the bag.
  • the drying processing device 27 can perform the drying processing by a drying method such as sun drying without using such a drying processing device 27.
  • the waste LCD after the drying process is held in the bag 21 as it is, and transported to the tile factory, glass factory, etc. as recycled raw materials.
  • the processing can be simplified by performing the consistent processing while the fine waste LCD crushed in the waste LCD crushing step is stored in the bag 21 as described above.
  • the processing since it is not necessary to handle the fine waste LCD pieces that have been accepted as waste LCD crushing process as powder, handling does not become difficult.
  • the bag 21 only needs to have a mesh (porosity) that does not allow the waste LCD to fall off, and a cloth is sufficient.
  • the entire noggle is porous enough to allow the hydrochloric acid solution to pass through! /, Or the bottom of the nod 21 may be formed to be porous.
  • the present invention is not limited to In being a simple metal, but an alloy of In and other metals, that is, The present invention can also be applied to the case where an In alloy is deposited on metal particles and the deposited In alloy is separated from the metal particles.
  • hydrochloric acid is used as the acid for dissolving ITO as the waste LCD force.
  • the type of this acid is not limited to hydrochloric acid.
  • sulfuric acid, nitric acid or the like may be used. It is also possible to use a mixed acid or the like.
  • the force that provides the above-described preferable effect by providing the impurity removal reactor 2 as described above is provided in the present invention.
  • the metal particles added to the force recovery reactor described in the case of collecting In by adding Zn or A1 particles are not limited to the Zn or A1 particles of the embodiment. In short, the ionization tendency is larger than In, metal is used!
  • the particle size of the metal particles is about 3 mm, but the particle size of the metal particles is not limited to the embodiment, and is preferably 0.1 to 8 mm. If it is less than 1 mm, the cementation reaction is not always performed favorably, and the deposited metal peeled off from the metal particles cannot be easily recovered! / If exceeded, the number of metal particles that can be held in the reactor body decreases, and as a result, the total surface area of the metal particles may decrease and the efficiency of the precipitation reaction may decrease, and valuable metals or impurity metals for recovery purposes may be reduced. This is because other metals may be deposited on the metal particles.
  • the cross-sectional area of the reactor main body 5 is formed so as to increase toward the top, the force with which the above preferable effect is obtained is as described above.
  • the formation of the main body 5 is not an essential condition for the present invention.
  • the means for separating the deposited metal from the metal particles may be other means than the means using the ultrasonic wave in the first and second embodiments and the means using the electromagnet in the third embodiment.
  • FIG. 8 28 is the waste LCD layer described in FIG. 7, 29 is a tube pump, 30 is hydrochloric acid, 31 is a resin container, and 32 is a mesh tank. From analysis, the waste LCD contained 400 mgZkg of In. In the elution process, the waste LCD24kg is held in a cotton bag, and the bag is placed in a 100L resin container as shown in Fig. 8. It was put in a container 31, 14 L of hydrochloric acid was added, and circulation treatment was performed at room temperature using a tube pump 29.
  • the lid of the 100L resin container is equipped with a gasket, and a tube pump with a lid that can seal between the 100L resin container and the lid 29
  • the insertion part and the extraction part used were sealed with a caulking agent.

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Abstract

La présente invention concerne un procédé et un appareil de récupération d’indium sous forme d’un alliage ou d’une substance simple métallique comme matériau précieux à partir d’un affichage à cristaux liquides mis au rebut. Dans le procédé et l’appareil de récupération d’indium, il n’est pas nécessaire de récupérer l’indium sous forme d’hydroxyde d’indium, et l’on peut récupérer l’indium sous forme de métal précieux. En conséquence, à la différence du cas de l’hydroxyde d’indium, la récupération ne souffre pas d’une manipulation médiocre, et l’indium peut être facilement récupéré à travers un filtre ou similaire avec une récupération d’indium nettement améliorée. Le procédé de récupération d’indium est caractérisé en ce qu’il consiste à concasser un affichage à cristaux liquides mis au rebut contenant de l’oxyde d’étain d’indium, à dissoudre l’oxyde d’étain d’indium provenant de l’affichage à cristaux liquides mis au rebut et concassé avec un acide pour produire une solution contenant un composé d’indium, à laisser la solution couler dans un réacteur pour récupération et, de plus, à ajouter des particules d’un métal ayant une tendance à l’ionisation plus importante que l’indium dans le réacteur pour récupération, à fluidifier les particules de métal, à précipiter l’indium ou un alliage d’indium contenu dans la solution contenant un composé d’indium à la surface des particules de métal, avant de séparer l’indium ou l’alliage d’indium précipité des particules de métal grâce à un moyen de séparation, et à séparer l’indium ou l’alliage d’indium solide séparé du composant liquide et à le récupérer.
PCT/JP2006/314626 2005-08-04 2006-07-25 Procédé et appareil de récupération d’indium d’un affichage à cristaux liquides mis au rebut Ceased WO2007015392A1 (fr)

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JP2007529217A JPWO2007015392A1 (ja) 2005-08-04 2006-07-25 廃棄液晶ディスプレイからのインジウムの回収方法とその装置
US11/997,884 US20100101367A1 (en) 2005-08-04 2006-07-25 Method and apparatus for recovering indium from waste liquid crystal displays

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JP2005226920 2005-08-04

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JP2007270342A (ja) * 2006-03-06 2007-10-18 Kobelco Eco-Solutions Co Ltd インジウムの回収方法とその装置
JP2008208396A (ja) * 2007-02-23 2008-09-11 Kobelco Eco-Solutions Co Ltd インジウムの回収方法とその装置
JP2009155717A (ja) * 2007-12-28 2009-07-16 Dowa Eco-System Co Ltd インジウムの回収方法
JP2009191309A (ja) * 2008-02-14 2009-08-27 Sumitomo Metal Mining Co Ltd 粗インジウムの回収方法
JP2014040639A (ja) * 2012-08-23 2014-03-06 Sumitomo Electric Ind Ltd 金属の製造方法
WO2015128581A1 (fr) 2014-02-27 2015-09-03 Centre National De La Recherche Scientifique (Cnrs) Procede de traitement d'un support dont une face est au moins partiellement recouverte d'une couche d'oxydes indium-etain (ito)- dispositif associe

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CN101690936B (zh) * 2009-10-16 2011-06-15 清华大学 一种废薄膜晶体管液晶显示器资源化处理方法
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KR101289987B1 (ko) * 2011-06-29 2013-07-26 엘지디스플레이 주식회사 Ｌｃｄ 폐유리로부터의 유가금속 회수방법 및 그 공정
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JP5713946B2 (ja) * 2012-03-27 2015-05-07 三菱電機株式会社 酸化物半導体中の金属成分の回収方法
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CN103602815B (zh) * 2013-11-06 2015-12-09 四川长虹电器股份有限公司 从废液晶显示器中回收铟的方法
FR3025806B1 (fr) * 2014-09-15 2019-09-06 Bigarren Bizi Procede de traitement et d'extraction de dechets electroniques en vue de la recuperation des constituants inclus dans de tel dechets
CN104498721A (zh) * 2015-01-08 2015-04-08 中国科学院城市环境研究所 一种液晶面板无害化处理方法及系统
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007270342A (ja) * 2006-03-06 2007-10-18 Kobelco Eco-Solutions Co Ltd インジウムの回収方法とその装置
JP2008208396A (ja) * 2007-02-23 2008-09-11 Kobelco Eco-Solutions Co Ltd インジウムの回収方法とその装置
JP2009155717A (ja) * 2007-12-28 2009-07-16 Dowa Eco-System Co Ltd インジウムの回収方法
JP2009191309A (ja) * 2008-02-14 2009-08-27 Sumitomo Metal Mining Co Ltd 粗インジウムの回収方法
JP2014040639A (ja) * 2012-08-23 2014-03-06 Sumitomo Electric Ind Ltd 金属の製造方法
WO2015128581A1 (fr) 2014-02-27 2015-09-03 Centre National De La Recherche Scientifique (Cnrs) Procede de traitement d'un support dont une face est au moins partiellement recouverte d'une couche d'oxydes indium-etain (ito)- dispositif associe

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US20100101367A1 (en) 2010-04-29
CN101133172A (zh) 2008-02-27
CN100554454C (zh) 2009-10-28
TWI385255B (zh) 2013-02-11
TW200712219A (en) 2007-04-01
KR20080031661A (ko) 2008-04-10

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