CN109762993A - A method of it gives up from ITO and recycles indium metal in target - Google Patents
A method of it gives up from ITO and recycles indium metal in target Download PDFInfo
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- CN109762993A CN109762993A CN201910161292.XA CN201910161292A CN109762993A CN 109762993 A CN109762993 A CN 109762993A CN 201910161292 A CN201910161292 A CN 201910161292A CN 109762993 A CN109762993 A CN 109762993A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
It gives up the method that indium metal is recycled in target the invention discloses a kind of from ITO, ITO is given up after target is crushed by ball mill and is uniformly mixed preparation particulate material with reducing agent graphite powder, graphite surface wetting agent, particulate material is subjected to redox reaction at high temperature, generate indium stannum alloy, indium stannum alloy is cast into the progress of indium sheet tin, and electrolysis obtains indium metal twice, and the redox reaction carries out in reduction furnace.The present invention avoids chemical contamination under the premise of keeping indium metal high-recovery, simplifies operating process, can operate continuously, and is suitble to large-scale production.
Description
Technical field
It gives up the method for recycling indium metal in target the present invention relates to a kind of from indium tin oxide, belongs to metallurgy of rare metal neck
Domain.
Background technique
The slave ITO(indium tin oxide of mainstream currently on the market) in the method for recycling indium metal be chemical method, this method will
ITO gives up after target crushes and uses salt Ore Leaching, adjusts salting liquid pH value and forms stannic hydroxide, separation of solid and liquid obtains indiumchloride solution, chlorine
Change solution of indium aluminium sheet or zinc dust precipitation obtains sponge indium, electrolysis obtains smart indium after ingot casting.Chemical method disadvantage: this process is chemistry
Operation generates acid mist pollution, while needing using a large amount of hydrochloric acid and caustic soda, and the last a large amount of side product chlorinated aluminium of also generation
Or liquor zinci chloridi needs to handle, when furthermore separating stannic hydroxide and indiumchloride solution, because the colloid property of stannic hydroxide makes
It must be separated by solid-liquid separation difficulty, while influencing the yield of indium.In order to evade the defect of above-mentioned technology, the researcher of related fields is extensive
It inquired into and obtains the technology of indium metal using reduction method, but in the reduction method of the prior art, the rate of recovery of indium always can not be with
Chemical method competition.
Summary of the invention
It gives up the method that indium metal is recycled in target the technical problem to be solved by the invention is to provide a kind of from ITO, using carbon
Indium tin oxide is reduced into indium stannum alloy by thermal reduction, improves going back for indium using the cooling absorption indium steam of the feed particles of low temperature
Former recovery rate, then the method by being electrolysed twice obtain smart indium, while can shorten the time of reduction reaction.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
A method of give up from ITO and recycle indium metal in target, by ITO give up target by after ball mill crushing with reducing agent graphite powder,
Graphite surface wetting agent is uniformly mixed preparation particulate material, and particulate material is carried out to redox reaction at high temperature and generates the conjunction of indium tin
Gold, is cast into indium sheet tin for indium stannum alloy and carries out electrolysis twice and obtain indium metal, the redox reaction in reduction furnace into
Row.
Technical solution of the present invention further improvement lies in that: the reduction furnace include boiler tube and be fixedly installed in boiler tube and
Boiler tube is divided into reaction zone, the furnace of alloy storage area is confered, the setting of the upper end of boiler tube convenient for the feed opening of charging, confer by the furnace
It is furnished with alloy solution and hole is confered by the intransitable furnace of particulate material, heating device, boiler tube are set outside the boiler tube of reaction zone lower part
Setting is in the discharging gate of tea mouth shape on the side wall of bottom end.
Technical solution of the present invention further improvement lies in that: the tube wall of the boiler tube is set as cylindrical drum, the diameter of boiler tube
For 50~400mm, boiler tube uses high temperature ceramic material, and height of the heating device top apart from feed opening is greater than 0.5m, and furnace is confered
Using graphite material, it is 2mm that furnace, which confers furnace and confers the diameter in hole,.
Technical solution of the present invention further improvement lies in that: the diameter of the boiler tube is 100~200mm, and boiler tube is using rigid
Beautiful or recrystallized silicon carbide material.
Technical solution of the present invention further improvement lies in that: specific step is as follows:
A, prepared by particulate material: ITO is given up into target and water is added in ball mill and is pulverized and mixed, grinding particle size is 60~200 mesh,
It is mixed that smashed ITO powder and reducing agent graphite powder, graphite surface wetting agent are mixed in a certain ratio uniformly obtained slurry, slurry
The conjunction time is 2h, and particulate material is made using the method for rolling or suppressing after slurry is dried, and the particle diameter of particulate material is 2
~6mm, particulate material, which is dried, makes the moisture content of particulate material less than 0.2%；
B, it reacts: particulate material obtained being added in reduction furnace and is heated, reacted in reduction furnace reaction zone and generate the conjunction of indium tin
Gold, indium stannum alloy, which is in a liquid state and is confered by furnace, flows into alloy storage area；
C, cast: indium stannum alloy is cast into plate after discharging gate is discharged；
D, it is electrolysed: being that anode is electrolysed by plate indium stannum alloy, current density is controlled in 100-300A/m2, voltage, which controls, to exist
0.2-0.5V obtains thick indium in cathode, and the progress re-electrolysis of thick indium is obtained smart indium.
Technical solution of the present invention further improvement lies in that: in the step A ITO give up target grinding particle size be 60~100 mesh,
The mixing molar ratio of ITO powder and graphite powder is 1:2, and the particle diameter of particulate material is 3~4mm, and drying device is using spray drying
Machine, graphite surface lubricant is using any one in ethyl alcohol, acetone and nonionic surfactant.
Technical solution of the present invention further improvement lies in that: in the step B heating use resistance heating or heating in medium frequency,
Heating temperature is 1200~1500 DEG C.
Technical solution of the present invention further improvement lies in that: in the step B heating temperature be 1300~1400 DEG C.
Technical solution of the present invention further improvement lies in that: in the step C plate indium stannum alloy with a thickness of 0.5~
5mm。
Technical solution of the present invention further improvement lies in that: plate indium stannum alloy with a thickness of 2~3mm in the step C.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
The present invention crushes the ITO target that gives up, and the granularity of crushing is smaller, and the speed of carbon thermal reduction is faster, grinding particle size preferably 60
~100 mesh, less than 60 mesh, grinding time is longer, less economical；Greater than 100 mesh, the speed of carbon thermal reduction is slow.
The particulate material particle diameter of preparation is 2~6mm, and preferably 3~4mm, particle is too small, and the carbon monoxide for restoring generation is logical
Road is easy to be blocked, the cost that particle large increase is granulated.
Heating temperature is 1200~1500 DEG C, is lower than 1200 DEG C, the speed of reduction is too slow；Higher than 1500 DEG C, boiler tube is reduced
Service life, and the volatilization loss of indium increases, and furnace temperature is preferably kept in 1300~1400 DEG C.
The taper cone barrel that the tube wall of boiler tube is set as cylindrical drum or upper end is big, lower end is small enables particulate material freely downward
Flowing, convenient for carrying out redox reaction in heating zone, height of the heating device top apart from feed opening is greater than 0.5m, that is, heats
The height of area (reaction zone that heating device is heated) above particulate material is maintained at 0.5 meter or more, so that indium steam has long enough
Path carry out cooling absorption.
The diameter of boiler tube is 50~400mm, and preferably 100~200mm, diameter is less than 100mm, and production efficiency is low, and diameter is big
It is poor in 200mm core reduction effect.
The diameter that furnace confers hole is 2mm, and alloy solution can cannot be passed through by particulate material, and main function is to maintain not also
Former particulate material is separated with reducing metal, and the indium stannum alloy restored in use is confered in hole from furnace to be flowed down, and is not restored
Particulate material then on furnace is confered, this process is continuous process, it is only necessary to which constantly adding particulate material on top can be realized continuously
Operation is suitble to large-scale production.
Discharging gate is upwarped in tea mouth shape, and effect is the oxidation that isolation air prevents metal and graphite.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of reduction furnace of the present invention；
Wherein, 1, discharging gate, 2, boiler tube, 3, heating device, 4, furnace confer, 5, alloy storage area, 6, reaction zone, 7, feed opening.
Specific embodiment
The present invention is described in further details below with reference to embodiment:
As shown in Figure 1, a kind of give up the method for recycling indium metal in target from ITO, by ITO give up target crushed by ball mill after with and also
Former agent graphite powder, graphite surface wetting agent are uniformly mixed preparation particulate material, and particulate material is carried out redox reaction at high temperature,
Indium stannum alloy is generated, indium stannum alloy is cast into the progress of indium sheet tin, and electrolysis obtains indium metal twice, and the redox reaction exists
It is carried out in reduction furnace.
The reduction furnace includes boiler tube 2 and the furnace being fixedly installed in boiler tube 2 confers 4, and the upper end setting of boiler tube 2 is convenient for charging
Feed opening 7, the taper cone barrel that the tube wall of boiler tube 2 is set as cylindrical drum or upper end is big, lower end is small, the diameter of boiler tube 2 is 50~
400mm, preferably 100~200mm, boiler tube 2 use high temperature ceramic material, and preferably corundum and recrystallized silicon carbide, the furnace confers 4
Boiler tube 2 is divided for 5 two parts of reaction zone 6 and alloy storage area, furnace, which is confered, to be evenly equipped with alloy solution and cannot be led to by particulate material on 4
The furnace crossed confers hole, heating device 3 is arranged outside the boiler tube 2 of 6 lower part of reaction zone, the position that reaction zone 6 is equipped with heating device 3 is heating
Area, heating device 3 are cooling zone with the reaction zone 6 of upper bit, and height of 3 top of heating device apart from feed opening is greater than 0.5m,
That is the height of cooling zone particulate material is maintained at 0.5 meter or more, so that indium steam has sufficiently long path to carry out cooling absorption, makes indium
Evaporation less than 0.2%, on 2 bottom end side wall of boiler tube setting be in tea mouth shape discharging gate 1.
Specific step is as follows:
A, prepared by particulate material: ITO is given up into target and water is added in ball mill and is pulverized and mixed, grinding particle size is 60~200 mesh,
It is preferred that 60~100 mesh, smashed ITO powder and reducing agent graphite powder, graphite surface wetting agent are mixed in a certain ratio uniformly
The mixing molar ratio of obtained slurry, ITO powder and graphite powder is 1:2, incorporation time 2h, drying, using the side for rolling or suppressing
Particulate material is made in method, and the particle diameter of particulate material is 2~6mm, and preferably 3~4mm is dried again, so that particulate material moisture content is small
In 0.2%, drying device uses spray dryer or baking oven, preferably spray drying machine, and graphite surface lubricant uses ethyl alcohol, third
Ketone or nonionic surfactant；
B, it reacts: particulate material obtained is added to reduction furnace, heat, heating uses resistance heating or heating in medium frequency, heating temperature
Degree is 1200~1500 DEG C, preferably 1300~1400 DEG C, reacts in reduction furnace reaction zone 6 and generates indium stannum alloy, indium stannum alloy is in
Liquid confers 4 inflow alloy storage areas 5 by furnace；
C, cast: indium stannum alloy is discharged through discharging gate 1, and casting is cast into plate, plate indium stannum alloy with a thickness of 0.5~
5mm, preferably 2~3mm；
D, it is electrolysed: being that anode is electrolysed by plate indium stannum alloy, current density is controlled in 100-300A/m2, voltage, which controls, to exist
0.2-0.5V obtains thick indium in cathode, and the progress re-electrolysis of thick indium is obtained the high purity indium of 99.995% or more purity, indium it is comprehensive
It closes the rate of recovery and reaches 96% or more.
Embodiment 1:
Useless 200 kilograms of the target of ITO containing tin oxide 10% is crushed to 5 millimeters hereinafter, 200 lift ball mills of loading, are added deionized water
100 kilograms, 300 kilograms of zirconia ball of 15 millimeters of diameter are added, ball milling 24 hours, are with laser particle analyzer detection granularity d50
5.6 micron.17.4 kilograms of graphite powder, 1 kilogram of OP-10 surfactant is added to ball mill, ball milling 2 hours, extracts slurry mistake out
100 mesh screens.Slurry is dried with spray dryer, 220 degree of inlet air temperature, 110 degree of leaving air temp.Powder after drying
It being rolled and is granulated using granulating disc, sieving is made 3~4 mm granules material and enters baking process, it is dried 24 hours at 120 degree,
So that the moisture content of particulate material is less than 0.2%.
Particulate material is encased in reduction furnace of the invention, 1350 degree of furnace temperature, starts to calculate after feeding discharging and stablizing,
The particulate material being added in 24 hours weighs 123.62 kilograms, and indium stannum alloy out weighs 100.85 kilograms, by these indium stannum alloys electricity
Solution obtains 89.38 kilograms of thick indium of 99.5% purity, then these thick indiums are electrolysed to obtain 99.997% 88.49 kilograms of purity essence indium.
Calculating comprehensive recovery is 96.16%.
Embodiment 2:
Useless 200 kilograms of the target of ITO containing tin oxide 10% is crushed to 5 millimeters hereinafter, 200 lift ball mills of loading, are added deionized water
100 kilograms, 300 kilograms of zirconia ball of 15 millimeters of diameter are added, ball milling 24 hours, are with laser particle analyzer detection granularity d50
5.6 micron.17.4 kilograms of graphite powder, 1 kilogram of OP-10 surfactant is added to ball mill, ball milling 2 hours, extracts slurry mistake out
60 mesh screens.Slurry is dried with spray dryer, 220 degree of inlet air temperature, 110 degree of leaving air temp.Powder after drying
It being rolled and is granulated using granulating disc, sieving is made 3~4 mm granules material and enters baking process, it is dried 24 hours at 120 degree,
So that the moisture content of particulate material is less than 0.2%.
Particulate material is packed into reduction furnace of the invention, 1200 degree of furnace temperature, starts to calculate after feeding discharging and stablizing, 24
The particulate material being added in hour weighs 65.32 kilograms, and indium stannum alloy out weighs 53.23 kilograms, these indium stannum alloys are electrolysed
To 47.12 kilograms of thick indium of 99.5% purity, then these thick indiums are electrolysed to obtain 99.997% 46.71 kilograms of purity essence indium.It calculates
Comprehensive recovery is 96.07%.
Compared with Example 1, the comprehensive recovery of indium does not have significant change to embodiment 2, but because temperature is low, reduction
Rate can be decreased obviously.
Embodiment 3:
Useless 200 kilograms of the target of ITO containing tin oxide 10% is crushed to 5 millimeters hereinafter, 200 lift ball mills of loading, are added deionized water
100 kilograms, 300 kilograms of zirconia ball of 15 millimeters of diameter are added, ball milling 24 hours, are with laser particle analyzer detection granularity d50
5.6 micron.17.4 kilograms of graphite powder, 1 kilogram of OP-10 surfactant is added to ball mill, ball milling 2 hours, extracts slurry mistake out
200 mesh screens.Slurry is dried with spray dryer, 220 degree of inlet air temperature, 110 degree of leaving air temp.Powder after drying
It being rolled and is granulated using granulating disc, sieving is made 3~4 mm granules material and enters baking process, it is dried 24 hours at 120 degree,
So that the moisture content of particulate material is less than 0.2%.
Particulate material is packed into reduction furnace of the invention, 1500 degree of furnace temperature, starts to calculate after feeding discharging and stablizing, 24
The particulate material being added in hour weighs 302.43 kilograms, and indium stannum alloy out weighs 248.95 kilograms, these indium stannum alloys are electrolysed
220.54 kilograms of thick indium of 99.5% purity are obtained, then these thick indiums are electrolysed to obtain 99.997% 216.15 kilograms of purity essence indium.
Calculating comprehensive recovery is 96.09%.
Compared with Example 1, the comprehensive recovery of indium does not have significant change to embodiment 3, but production efficiency significantly improves.
Comparative example 1:
Useless 200 kilograms of the target of ITO containing tin oxide 10% is crushed to 5 millimeters hereinafter, 200 lift ball mills of loading, are added deionized water
100 kilograms, 300 kilograms of zirconia ball of 15 millimeters of diameter are added, ball milling 24 hours, are with laser particle analyzer detection granularity d50
5.6 micron.17.4 kilograms of graphite powder, 1 kilogram of OP-10 surfactant is added to ball mill, ball milling 2 hours, extracts slurry mistake out
100 mesh screens.Slurry is dried with spray dryer, 220 degree of inlet air temperature, 110 degree of leaving air temp.Powder after drying
It being rolled and is granulated using granulating disc, sieving is made 3~4 mm granules material and enters baking process, it is dried 24 hours at 120 degree,
So that the moisture content of particulate material is less than 0.2%.
Particulate material is packed into reduction furnace of the invention, 1000 degree of furnace temperature, is kept for 48 hours, flowed out without indium stannum alloy.
Comparative example 1 when heating temperature is reduced to 1000 degree compared with Example 1 reduction reaction can not just carry out at all, temperature arrives
1200 degree just have receptible production efficiency, and temperature is higher, and production efficiency is higher, but more than 1500 degree, it is difficult to it is suitable to find
Furnace lining material, energy consumption increase, it is not necessary that
Comparative example 2:
Useless 200 kilograms of the target of ITO containing tin oxide 10% is crushed to 5 millimeters hereinafter, 200 lift ball mills of loading, are added deionized water
100 kilograms, 300 kilograms of zirconia ball of 15 millimeters of diameter are added, ball milling 24 hours, are with laser particle analyzer detection granularity d50
5.6 micron.17.4 kilograms of graphite powder, 1 kilogram of OP-10 surfactant is added to ball mill, ball milling 2 hours, extracts slurry mistake out
100 mesh screens.Slurry is dried with spray dryer, 220 degree of inlet air temperature, 110 degree of leaving air temp.Powder after drying
It being rolled and is granulated using granulating disc, sieving is made 3~4 mm granules material and enters baking process, it is dried 24 hours at 120 degree,
So that the moisture content of particulate material is less than 0.2%.
Particulate material is packed into intermittent common carbothermic reduction furnace, the ITO particulate material being added at one time weighs 10 kilograms, obtains
Indium stannum alloy weigh 6.46 kilograms, these indium stannum alloys are electrolysed to obtain 5.73 kilograms of thick indium of 99.5% purity, then these are thick
Indium is electrolysed to obtain 99.997% 5.67 kilograms of purity essence indium.Calculating comprehensive recovery is 76.2%.
Compared with Example 1, using ordinary reduction furnace, indium volatilization is larger, and the comprehensive recovery of indium is very low for comparative example 2.
The present invention obtains the high purity indium of 99.995% or more purity, the granularity of particulate material preferably 60~100 mesh, heating temperature
It is preferred that 1300~1400 DEG C, the reaction time is reduced, production efficiency is improved, so that the comprehensive recovery of indium reaches 96% or more.
The present invention, which can be realized, avoids chemical contamination under the premise of keeping indium metal high-recovery, simplifies operating process, connects simultaneously
Continuous operation, is suitble to large-scale production.
Claims (10)
1. a kind of give up the method for recycling indium metal in target from ITO, it is characterised in that: by ITO give up target crushed by ball mill after and
Reducing agent graphite powder, graphite surface wetting agent are uniformly mixed preparation particulate material, and it is anti-that particulate material is carried out to redox at high temperature
Indium stannum alloy should be generated, indium stannum alloy is cast into the progress of indium sheet tin, and electrolysis obtains indium metal, the redox reaction twice
It is carried out in reduction furnace.
It a kind of gives up the method that indium metal is recycled in target from ITO 2. according to claim 1, it is characterised in that: the reduction
Furnace includes boiler tube (2) and the furnace for being fixedly installed in boiler tube (2) and be divided into boiler tube (2) reaction zone (6), alloy storage area (5)
Confer (4), the setting of the upper end of boiler tube (2) convenient for charging feed opening (7), the furnace confer be evenly equipped on (4) alloy solution by
The intransitable furnace of particulate material confers hole, and heating device (3), boiler tube (2) bottom end side is arranged in the boiler tube (2) of reaction zone (6) lower part outside
Setting is in the discharging gate (1) of tea mouth shape on wall.
It a kind of gives up the method that indium metal is recycled in target from ITO 3. according to claim 2, it is characterised in that: the boiler tube
(2) tube wall is set as cylindrical drum, and the diameter of boiler tube (2) is 50~400mm, and boiler tube (2) uses high temperature ceramic material, heating
Height of device (3) top apart from feed opening is greater than 0.5m, and furnace confers (4) using graphite material, and furnace confers the diameter that furnace on (4) confers hole
For 2mm.
It a kind of gives up the method that indium metal is recycled in target from ITO 4. according to claim 3, it is characterised in that: the boiler tube
(2) diameter is 100~200mm, and boiler tube (2) uses corundum or recrystallized silicon carbide material.
It a kind of gives up the method that indium metal is recycled in target from ITO 5. according to claim 2, it is characterised in that: specific steps
It is as follows:
A, prepared by particulate material: ITO is given up into target and water is added in ball mill and is pulverized and mixed, grinding particle size is 60~200 mesh,
It is mixed that smashed ITO powder and reducing agent graphite powder, graphite surface wetting agent are mixed in a certain ratio uniformly obtained slurry, slurry
The conjunction time is 2h, and particulate material is made using the method for rolling or suppressing after slurry is dried, and the particle diameter of particulate material is 2
~6mm, particulate material, which is dried, makes the moisture content of particulate material less than 0.2%；
B, it reacts: particulate material obtained being added in reduction furnace and is heated, reacted in reduction furnace reaction zone (6) and generate indium tin
Alloy, indium stannum alloy, which is in a liquid state and confers (4) by furnace, flows into alloy storage area (5)；
C, cast: indium stannum alloy is cast into plate after discharging gate (1) is discharged；
D, it is electrolysed: being that anode is electrolysed by plate indium stannum alloy, current density is controlled in 100-300A/m2, voltage, which controls, to exist
0.2-0.5V obtains thick indium in cathode, and the progress re-electrolysis of thick indium is obtained smart indium.
It a kind of gives up the method that indium metal is recycled in target from ITO 6. according to claim 5, it is characterised in that: the step A
Middle ITO gives up target grinding particle size as 60~100 mesh, and the mixing molar ratio of ITO powder and graphite powder is 1:2, the particle diameter of particulate material
For 3~4mm, drying device uses spray dryer, and graphite surface lubricant uses ethyl alcohol, acetone and nonionic surfactant
In any one.
It a kind of gives up the method that indium metal is recycled in target from ITO 7. according to claim 5, it is characterised in that: the step B
Middle heating uses resistance heating or heating in medium frequency, and heating temperature is 1200~1500 DEG C.
It a kind of gives up the method that indium metal is recycled in target from ITO 8. according to claim 7, it is characterised in that: the step B
Middle heating temperature is 1300~1400 DEG C.
It a kind of gives up the method that indium metal is recycled in target from ITO 9. according to claim 5, it is characterised in that: the step C
Middle plate indium stannum alloy with a thickness of 0.5~5mm.
It a kind of gives up the method that indium metal is recycled in target from ITO 10. according to claim 9, it is characterised in that: the step
Plate indium stannum alloy with a thickness of 2~3mm in C.
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| CN110408958A (en) * | 2019-08-28 | 2019-11-05 | 广东先导稀材股份有限公司 | Method for separating and recovering tin and indium from indium-tin alloy |
| CN110408958B (en) * | 2019-08-28 | 2021-08-13 | 广东先导稀材股份有限公司 | Method for separating and recovering tin and indium from indium-tin alloy |
| CN114808036A (en) * | 2022-04-21 | 2022-07-29 | 柳州华锡有色设计研究院有限责任公司 | Method for recovering high-purity tin-indium alloy from ITO target waste |
| CN114808036B (en) * | 2022-04-21 | 2023-12-05 | 柳州华锡有色设计研究院有限责任公司 | Method for recycling high-purity tin-indium alloy from ITO target scrap |
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