CN108866336A - A method of recycling zinc from the pickle liquor of Gold Concentrate under Normal Pressure - Google Patents
A method of recycling zinc from the pickle liquor of Gold Concentrate under Normal Pressure Download PDFInfo
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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
- 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
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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
- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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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
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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Abstract
The present invention relates to a kind of methods that zinc is effectively recycled in pickle liquor from Gold Concentrate under Normal Pressure, including being fired the pickle liquor of the resulting cupric of acid leaching process to gold and silver concentrate through multi-stage oxidizing, charcoal adsorbs gold and silver, chelated zinc ions, extraction electrodeposition, chelate decomposition and etc., by the present invention in that forming highly stable chelate with the zinc ion of four picolyl ethylenediamine of chelating agent and divalent, copper can be contained at the same time, zinc ion is separated by the method that organic solvent extracts in the mixed solution of iron plasma, to which zinc ion is effectively used, compared with traditional Extraction electrodeposition technique, zinc is effectively recycled, and reduce the processing cost of pickle liquor, reduce the influence to ambient enviroment.
Description
Technical field
The present invention relates to effectively recycle in a kind of recovery method of metallic zinc more particularly to a kind of pickle liquor from Gold Concentrate under Normal Pressure
The method of zinc, belongs to field of chemical metallurgical technology.
Background technique
In recent years, in gold smelting field cupric gold and silver concentrate baking cyaniding technique, be to adopt the concentrate of cupric gold and silver
Slurry type feeding is roasted at a certain temperature with the oxygen in air after being sized mixing with water, and roasting gained high-temperature flue gas enters sulfuric acid
Production technology, gained calcining and dilute sulfuric acid carry out acidleach, output cupric pickle liquor, gained cupric acidleach under the conditions of certain acidleach
Enter extraction electrodeposition technique after liquid, extraction is the key step of modern wet-milling processing (Leaching-solvent Extraction-electrowinning Technology, L-SX-EW)
Suddenly.With the exploitation of efficient, stable copper extractant, the hydrometallurgy of copper has obtained huge development.Currently, the whole world 20%
Copper is produced by Extraction electrodeposition technique.
Although good recycling, the zinc contained in Gold Concentrate under Normal Pressure can be obtained by traditional Extraction electrodeposition technique in copper metal
The recycling of metal is but always a problem, and the zinc metal contained in Gold Concentrate under Normal Pressure is leached during acidleach with copper together, existing
In some technique, the raffinate waste liquid (containing remaining a small amount of copper simultaneously) containing zinc is by the way of lime neutralization
Reason not only causes the waste of zinc resource, but also neutralize higher cost, institute so that zinc enters the bottom ash of lime neutralization in this way
Bottom ash can partially be sold to cement plant and do raw materials for production, remainder can only be stored up, and not only take up a large amount of soils in this way, and right
Ambient enviroment causes to seriously affect, and with national conservation-minded society, the proposition of environment-friendly type social construction, carries out in cupric pickle liquor
The research and application of the effectively recycling, reduction outlet and neutralisation treatment cost direction of metallic zinc are rather important.
Summary of the invention
Deficiency present in recovery method of the present invention for metallic zinc in the pickle liquor of Gold Concentrate under Normal Pressure provides a kind of from aurin
The method of zinc is effectively recycled in the pickle liquor of mine.
The technical solution that the present invention solves above-mentioned technical problem is as follows:
A method of it recycling zinc from the pickle liquor of Gold Concentrate under Normal Pressure, includes the following steps:
1) multi-stage oxidizing:It is concatenated that the pickle liquor that gold and silver concentrate is fired the resulting cupric of acid leaching process is introduced several
In stirred tank, hydrogen peroxide and potassium permanganate are added into stirred tank, the additional amount of hydrogen peroxide is 3-5kg/m3, potassium permanganate plus
Entering amount is 0.5-1.0kg/m3, oxidated solution is obtained after oxidation 3-5 hours;
2) charcoal adsorbs gold and silver:So that oxidated solution obtained in step 1) is flowed through activated carbon adsorption device, controls oxidated solution
Flow velocity be 10-20m3/ h, liquid after output absorption after absorption, gold, silver are effectively adsorbed in active carbon at this time, the load gold and silver of output
Active carbon carries out smelting recycling, output gold and silver product;
3) chelated zinc ions:Four picolyl ethylenediamine of chelating agent, stirring is added after to the resulting absorption of step 2) in liquid
Mixing makes chelating agent and zinc ion forms chelate, and organic solvent is added in backward mixed system and is extracted, stirring fills it
Divide mixing, rear standing liquid separation obtains organic phase and water phase, and the chelate of zinc ion is present in organic phase;
4) extraction electrodeposition:Water phase obtained in step 3) is subjected to level-one extraction with copper extractant, obtains level-one raffinate
With the organic phase of load, the organic phase of load obtains level-one copper-rich liquid and regeneration organic phase after carrying out acidleach back extraction copper;Second level extraction
It takes, the level-one raffinate after dilution carries out second level extraction using regeneration organic phase, obtains second level raffinate and fractional load
Organic phase;The organic phase of fractional load obtains second level copper-rich liquid after acidleach is stripped copper, and level-one copper-rich liquid and second level copper-rich liquid close
Through electrodeposition process output tough cathode after and;
5) chelate decomposes:The acid adding into organic phase obtained by step 3), adjusting pH are 3-5, make four picolyl of chelating agent
Ethylenediamine at salt, after thereto plus water is extracted, stirring mixes them thoroughly, rear to stand liquid separation and obtain organic phase and water phase, has
Machine it is mutually purified after return step 3) in reuse, water phase is zinc solution;
Wherein, step 4) and step 5) are without sequencing.
Further, the additional amount of four picolyl ethylenediamine of chelating agent is 50~100mg/L in step 3).
Further, the pickle liquor of cupric described in step 1) 0.03-0.06g/m containing gold3, argentiferous 0.01-0.05g/m3, contain
Copper 1-10g/L, iron content 3-10g/L, 2-8kg/m containing zinc3。
Further, the pickle liquor of cupric described in step 1) obtains by the following method:
I is sized mixing roasting:Gold and silver concentrate is sized mixing with water, control pulp density is 50-70wt%, after ore pulp is placed in 500-
Roast to obtain high-temperature flue gas and calcining at 650 DEG C, roasting refer to gold and silver concentrate make in calciner inflammable substance sulphur, arsenic, carbon,
The clean-burning process of the elements such as selenium, gained high-temperature flue gas enter sulfuric acid production process output arsenic trioxide product and sulphuric acid production
Product;
II acidleach:Calcining is mixed with dilute sulfuric acid and is sized mixing, control pulp density is 30-35wt%, after ore pulp is placed in 50-
Acidleach is carried out under the conditions of 70 DEG C, after will separation of solid and liquid obtain the pickle liquor of acid leaching residue and cupric containing gold and silver, gained is containing gold and silver
Acid leaching residue enters recovery for Au and Ag system recycling gold and silver.
Further, the mass concentration of dilute sulfuric acid described in step II acid leaching process is 1-2.5wt%, leaching time control
It is 2-4 hours.
Further, copper extractant described in step 4) is oximes extractant, beta-diketon kind of extractants, ternary amine extraction
Agent and any one in compounding kind of extractants, the compounding preferred ketoxime of kind of extractants is compounded with aldoxime.
Further, organic solvent described in step 3) be ethyl acetate, acetone, THF, DMSO, benzene,toluene,xylene,
Any one in DMF.
Further, the stirred tank in step 1) is 3-5 concatenated stirred tanks, and the mixing speed control of stirred tank is 50-
80r/min。
Further, the control of adsorption process described in step 2) is 4-6 hours.
Four picolyl ethylenediamine Chinese name of Zinc Ions Chelated agent used in the present invention is:Tetra- (2- of N, N, N', N'-
Picolyl) ethylenediamine, CAS:16858-02-9.
The beneficial effects of the invention are as follows:
1) by the present invention in that forming highly stable chela with the zinc ion of four picolyl ethylenediamine of chelating agent and divalent
Close object, can at the same time containing copper, iron plasma mixed solution in by organic solvent extract method zinc ion is isolated
Come, so that zinc ion is effectively used, compared with traditional Extraction electrodeposition technique, has effectively recycled zinc, and reduce acid
The processing cost of immersion liquid reduces the influence to ambient enviroment;
2) due to the basic Whote-wet method closed cycle of whole set process process, the circulation comprehensive benefit of cupric pickle liquor is significantly improved
With efficiency, wastewater zero discharge is realized, reduces the pollution to ambient enviroment, finally improves the economic benefit of enterprise.
Specific embodiment
Principles and features of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
The 0.03-0.06g/m containing gold of the pickle liquor of raw material cupric used in the embodiment of the present invention3, argentiferous 0.01-
0.05g/m3, cupric 1-10g/l, iron content 3-10g/l, 2-8kg/m containing zinc3, production obtains by the following method:
I is sized mixing roasting:Gold and silver concentrate is sized mixing with water, control pulp density is 50-70wt%, after ore pulp is placed in 500-
Roast to obtain high-temperature flue gas and calcining at 650 DEG C, roasting refer to gold and silver concentrate make in calciner inflammable substance sulphur, arsenic, carbon,
The clean-burning process of the elements such as selenium, gained high-temperature flue gas enter sulfuric acid production process output arsenic trioxide product and sulphuric acid production
Product;
II acidleach:Calcining is mixed with the dilute sulfuric acid that mass concentration is 1-2.5wt% and is sized mixing, control pulp density is 30-
35wt%, after ore pulp is placed in 50-70 DEG C under the conditions of carry out acidleach, after acidleach 2-4 hours will separation of solid and liquid obtain containing gold and silver
The pickle liquor of acid leaching residue and cupric, acid leaching residue of the gained containing gold and silver enter recovery for Au and Ag system recycling gold and silver.
Embodiment 1:
A method of it recycling zinc from the pickle liquor of Gold Concentrate under Normal Pressure, includes the following steps:
1) multi-stage oxidizing:The pickle liquor that gold and silver concentrate is fired the resulting cupric of acid leaching process is introduced 3 concatenated to stir
It mixes in slot, hydrogen peroxide and potassium permanganate is added into stirred tank, the additional amount of hydrogen peroxide is 3kg/m3, the additional amount of potassium permanganate
For 1.0kg/m3, mixing speed 60r/min, oxidation 3 hours after oxidated solution;
2) charcoal adsorbs gold and silver:So that oxidated solution obtained in step 1) is flowed through activated carbon adsorption device, controls oxidated solution
Flow velocity be 15m3/ h, liquid after output absorption after circulation absorption 4 hours, gold, silver are effectively adsorbed in active carbon at this time, output
It carries gold and silver active carbon and carries out smelting recycling, output gold and silver product;
3) chelated zinc ions:Four picolyl ethylenediamine of chelating agent, chelating is added after to the resulting absorption of step 2) in liquid
The additional amount of agent is 80mg/L, and being stirred makes chelating agent and zinc ion form chelate, and acetic acid is added in backward mixed system
Ethyl ester is extracted, and stirring mixes them thoroughly, and rear standing liquid separation obtains organic phase and water phase, and the chelate of zinc ion, which is present in, to be had
In machine phase;
4) extraction electrodeposition:Water phase obtained in step 3) is subjected to level-one extraction with copper extractant Acorga M5640, is obtained
To the organic phase of level-one raffinate and load, the organic phase of load, which carries out obtaining level-one copper-rich liquid and regeneration after acidleach back extraction copper, to be had
Machine phase;Second level extraction, the level-one raffinate after dilution carry out second level extraction using regeneration organic phase, obtain second level raffinate
With the organic phase of fractional load;The organic phase of fractional load obtains second level copper-rich liquid, level-one copper-rich liquid and two after acidleach is stripped copper
Through electrodeposition process output tough cathode after grade copper-rich liquid merging;
5) chelate decomposes:Into organic phase obtained by step 3) plus the dilute hydrochloric acid of 1mol/L, adjusting pH are 3-5, make to chelate
Four picolyl ethylenediamine of agent at salt, after thereto plus the water of equal volume is extracted, stirring mixes them thoroughly, rear to stand
Liquid separation obtains organic phase and water phase, return step 3 after organic phase is purified) in reuse, water phase is liquor zinci chloridi.
Embodiment 2:
A method of it recycling zinc from the pickle liquor of Gold Concentrate under Normal Pressure, includes the following steps:
1) multi-stage oxidizing:The pickle liquor that gold and silver concentrate is fired the resulting cupric of acid leaching process is introduced 5 concatenated to stir
It mixes in slot, hydrogen peroxide and potassium permanganate is added into stirred tank, the additional amount of hydrogen peroxide is 5kg/m3, the additional amount of potassium permanganate
For 0.5kg/m3, mixing speed 50r/min, oxidation 5 hours after oxidated solution;
2) charcoal adsorbs gold and silver:So that oxidated solution obtained in step 1) is flowed through activated carbon adsorption device, controls oxidated solution
Flow velocity be 10m3/ h, liquid after output absorption after circulation absorption 5 hours, gold, silver are effectively adsorbed in active carbon at this time, output
It carries gold and silver active carbon and carries out smelting recycling, output gold and silver product;
3) chelated zinc ions:Four picolyl ethylenediamine of chelating agent, chelating is added after to the resulting absorption of step 2) in liquid
The additional amount of agent is 50mg/L, and being stirred makes chelating agent and zinc ion form chelate, and acetone is added in backward mixed system
It is extracted, stirring mixes them thoroughly, and rear standing liquid separation obtains organic phase and water phase, and the chelate of zinc ion is present in organic phase
In;
4) chelate decomposes:Into organic phase obtained by step 3) plus the dilute sulfuric acid of 1mol/L, adjusting pH are 3-5, make to chelate
Four picolyl ethylenediamine of agent at salt, after thereto plus isometric water is extracted, stirring mixes them thoroughly, rear to stand point
Liquid obtains organic phase and water phase, return step 3 after organic phase is purified) in reuse, water phase is solution of zinc sulfate.
5) extraction electrodeposition:Water phase obtained in step 3) is subjected to level-one extraction with copper extractant Lix984, obtains level-one
The organic phase of raffinate and load, the organic phase of load obtain level-one copper-rich liquid and regeneration organic phase after carrying out acidleach back extraction copper;
Second level extraction, the level-one raffinate after dilution carry out second level extraction using regeneration organic phase, obtain second level raffinate and portion
Divide the organic phase of load;The organic phase of fractional load obtains second level copper-rich liquid after acidleach is stripped copper, and level-one copper-rich liquid and second level are rich
Through electrodeposition process output tough cathode after copper liquid merging.
Embodiment 3:
A method of zinc effectively being recycled from the pickle liquor of cupric, is included the following steps:
1) multi-stage oxidizing:The pickle liquor that gold and silver concentrate is fired the resulting cupric of acid leaching process is introduced 3 concatenated to stir
It mixes in slot, hydrogen peroxide and potassium permanganate is added into stirred tank, the additional amount of hydrogen peroxide is 4kg/m3, the additional amount of potassium permanganate
For 0.8kg/m3, mixing speed 80r/min, oxidation 4 hours after oxidated solution;
2) charcoal adsorbs gold and silver:So that oxidated solution obtained in step 1) is flowed through activated carbon adsorption device, controls oxidated solution
Flow velocity be 20m3/ h, liquid after output absorption after circulation absorption 6 hours, gold, silver are effectively adsorbed in active carbon at this time, output
It carries gold and silver active carbon and carries out smelting recycling, output gold and silver product;
3) chelated zinc ions:Four picolyl ethylenediamine of chelating agent, chelating is added after to the resulting absorption of step 2) in liquid
The additional amount of agent is 100mg/L, and being stirred makes chelating agent and zinc ion form chelate, is added in backward mixed system organic
Solvent THF is extracted, and stirring mixes them thoroughly, and rear standing liquid separation obtains organic phase and water phase, and the chelate of zinc ion exists
In organic phase;
4) extraction electrodeposition:The resulting water phase of step 3) is subjected to level-one with the copper extractant SME529 that Shell company produces
Extraction, obtains the organic phase of level-one raffinate and load, and the organic phase of load obtains level-one copper-rich liquid after carrying out acidleach back extraction copper
With regeneration organic phase;Second level extraction, the level-one raffinate after dilution carry out second level extraction using regeneration organic phase, obtain two
The organic phase of grade raffinate and fractional load;The organic phase of fractional load obtains second level copper-rich liquid after acidleach is stripped copper, and level-one is rich
Copper liquid merge with second level copper-rich liquid after through electrodeposition process output tough cathode;
5) chelate decomposes:Into organic phase obtained by step 3) plus the dilute sulfuric acid of 1mol/L, adjusting pH are 3-5, make to chelate
Four picolyl ethylenediamine of agent at salt, after thereto plus water is extracted, stirring mixes them thoroughly, it is rear stand liquid separation obtain it is organic
Mutually and water phase, organic phase it is purified after return step 3) in reuse, water phase is solution of zinc sulfate.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. recycling the method for zinc in a kind of pickle liquor from Gold Concentrate under Normal Pressure, which is characterized in that include the following steps:
1) multi-stage oxidizing:The pickle liquor that gold and silver concentrate is fired the resulting cupric of acid leaching process is introduced into several concatenated stirrings
In slot, hydrogen peroxide and potassium permanganate are added into stirred tank, the additional amount of hydrogen peroxide is 3-5kg/m3, the additional amount of potassium permanganate
For 0.5-1.0kg/m3, oxidated solution is obtained after oxidation 3-5 hours;
2) charcoal adsorbs gold and silver:So that oxidated solution obtained in step 1) is flowed through activated carbon adsorption device, controls the stream of oxidated solution
Speed is 10-20m3/ h, liquid after output absorption after absorption, gold, silver are effectively adsorbed in active carbon at this time, the load gold and silver activity of output
Charcoal carries out smelting recycling, output gold and silver product;
3) chelated zinc ions:Four picolyl ethylenediamine of chelating agent is added after to the resulting absorption of step 2) in liquid, is stirred
So that chelating agent and zinc ion is formed chelate, organic solvent is added in backward mixed system and is extracted, stirring keeps it sufficiently mixed
It closes, rear standing liquid separation obtains organic phase and water phase, and the chelate of zinc ion is present in organic phase;
4) extraction electrodeposition:Water phase obtained in step 3) is subjected to level-one extraction with copper extractant, obtain level-one raffinate and is born
The organic phase of load, the organic phase of load obtain level-one copper-rich liquid and regeneration organic phase after carrying out acidleach back extraction copper;Second level extraction, warp
Level-one raffinate after crossing dilution obtains the organic of second level raffinate and fractional load using regeneration organic phase progress second level extraction
Phase;The organic phase of fractional load obtains second level copper-rich liquid after acidleach is stripped copper, and level-one copper-rich liquid passes through after merging with second level copper-rich liquid
Electrodeposition process output tough cathode;
5) chelate decomposes:The acid adding into organic phase obtained by step 3), adjusting pH are 3-5, make four picolyl second two of chelating agent
Amine at salt, after thereto plus water is extracted, stirring mixes them thoroughly, rear to stand liquid separation and obtain organic phase and water phase, organic phase
It is purified after return step 3) in reuse, water phase is zinc solution;
Wherein, step 4) and step 5) are without sequencing.
2. the method according to claim 1, wherein in step 3) four picolyl ethylenediamine of chelating agent addition
Amount is 50~100mg/L.
3. method according to claim 1 or 2, which is characterized in that the pickle liquor of cupric described in step 1) 0.03- containing gold
0.06g/m3, argentiferous 0.01-0.05g/m3, cupric 1-10g/l, iron content 3-10g/l, 2-8kg/m containing zinc3。
4. according to the method described in claim 3, it is characterized in that, the pickle liquor of cupric described in step 1) is by such as lower section
What method obtained:
I is sized mixing roasting:Gold and silver concentrate is sized mixing with water, control pulp density is 50~70wt%, after ore pulp is placed in 500~
Roast to obtain high-temperature flue gas and calcining at 650 DEG C, roasting refer to gold and silver concentrate make in calciner inflammable substance sulphur, arsenic, carbon,
The clean-burning process of the elements such as selenium, gained high-temperature flue gas enter sulfuric acid production process output arsenic trioxide product and sulphuric acid production
Product;
II acidleach:Calcining is mixed with dilute sulfuric acid and is sized mixing, control pulp density is 30-35wt%, after ore pulp is placed in 50~70
Acidleach is carried out under the conditions of DEG C, after will separation of solid and liquid obtain the pickle liquor of acid leaching residue and cupric containing gold and silver, acid of the gained containing gold and silver
Phase analysis enters recovery for Au and Ag system recycling gold and silver.
5. according to the method described in claim 4, it is characterized in that, the quality of dilute sulfuric acid described in step II acid leaching process is dense
Degree is 1-2.5wt%, and leaching time control is 2-4 hours.
6. method according to claim 1 or 2, which is characterized in that copper extractant described in step 4) is oximes extraction
Agent, beta-diketon kind of extractants, ternary amine extractant and compounding kind of extractants in any one, compound the preferred ketone of kind of extractants
Oxime is compounded with aldoxime.
7. method according to claim 1 or 2, which is characterized in that organic solvent described in step 3) be ethyl acetate,
Acetone, THF, DMSO, benzene,toluene,xylene, any one in DMF.
8. method according to claim 1 or 2, which is characterized in that the stirred tank in step 1) is 3-5 concatenated stirrings
Slot.
9. the method according to the description of claim 7 is characterized in that the mixing speed control of stirred tank is 50- in step 1)
80r/min。
10. method according to claim 1 or 2, which is characterized in that the control of adsorption process described in step 2) is 4-6
Hour.
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CN112575187A (en) * | 2020-11-24 | 2021-03-30 | 昆明理工大学 | Extraction system and extraction separation method for selective dezincification of waste pickle liquor |
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WO2015110702A1 (en) * | 2014-01-22 | 2015-07-30 | Outotec (Finland) Oy | Method for recovery of copper and zinc |
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