CN107828975A - The technique of Centrifugical extraction copper in a kind of leachate from heterogenite - Google Patents
The technique of Centrifugical extraction copper in a kind of leachate from heterogenite 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- 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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22B3/30—Oximes
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- 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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Abstract
The invention discloses a kind of technique of Centrifugical extraction copper in leachate from heterogenite, the extraction tank for the PVC material for replacing using at present by using glass steel material centrifuge, it is used in series extracting with stripping process using multiple Centrifugical extractions, the extraction yield and back extraction ratio of copper are improved, while decreases wastewater treatment;Blank organic phase C u < 50mg/L can be recycled.Centrifugical extraction and centrifugation Stripping times are short, are separated and mass-transfer efficiency is high, and level retains that liquid measure is few, and occupation area of equipment is small, and operating cost is low, suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of technique of Centrifugical extraction copper in leachate from heterogenite, belong to technical field of wet metallurgy.
Background technology
The conventional extraction equipment of hydrometallurgy has mixing clarification extraction box, extraction tower and centrifugal extractor etc..Mixing clarification
Extraction box is made up of mixing chamber and clarifying chamber, and aqueous phase and organic phase are carried out in mixing chamber stirring reaction, mixed phase into clarifying chamber
Two-phase laminated flow, the mixing chamber that aqueous phase and organic phase after separation separately flow into adjacent level realize counter current multi-stage extraction process.Mixing
Clarification extraction box planar development floor space is big, and clarifying chamber's organic solvent storage is big.Extraction tower is vertically arranged extraction equipment,
Mostly cylindrical, light phase enters from bottom of towe, is overflowed by tower top, and heavy phase adds from tower top to be flowed out by bottom of towe, and both do inverse in tower
To flowing, sometimes for efficiency is improved, accelerate stirring or vibrations easily cause emulsification, so operation has strict demand, tower equipment
It is limited to extract series, is difficult to apply more than 10 grades, two phase materials are entered in gravitational field in mixer-settler, tower equipment
Row separation.Centrifugical extraction is using rotary drum powerful centrifugal force field caused by rotation at a high speed, makes density different and immiscible two
Kind liquid is completed to mix and separated in the presence of shearing force caused by drum rotating and centrifugal force, and the phase materials of Centrifugical extraction two connect
It is short to touch the time, is separated and mass-transfer efficiency is high, and level retains that liquid measure is few, and production capacity is big, is widely used in hydrometallurgy, at waste water
The multiple fields such as reason, biology, pharmacy, petrochemical industry, chemical industry, spices, dyestuff, atomic energy.
With valuable metals such as copper, the copper that more than 90% is there are about during sulfuric acid leaching enters majority together with cobalt in heterogenite
Enter solution, existing separation of Cu and Co uses extracting process more, and extracting system mainly uses the extraction tank of PVC materials, and extraction tank takes up an area face
Product is big, and extraction time length, organic consumption is big, and environmental pollution is serious, and the third phase cleared up in groove is difficult and potential safety hazard be present.
The content of the invention
The technical problem to be solved in the present invention is the technique of the Centrifugical extraction copper from heterogenite leachate, by using glass
Steel material centrifuge replaces the extraction tank of the PVC material used at present, is extracting and is using multiple Centrifugical extractions in stripping process
It is used in series, improves the extraction yield and back extraction ratio of copper, Centrifugical extraction organic phase and aqueous phase split-phase are thorough, the iron containing copper liquid of back extraction
Powder reduction prepares copper sponge, and copper sponge precipitation upper liquid contains Fe2+ and sulfuric acid, returns to the leaching process of heterogenite, control solution
PH=1.0~2.0, Fe2+:1~2g/l, cobalt slag Co≤0.2% can be made, reduce the usage amount for leaching reducing agent and sulfuric acid, simultaneously
Decrease wastewater treatment;Blank organic phase C u < 50mg/L can be recycled.Centrifugical extraction and centrifugation Stripping times are short, phase point
High from mass-transfer efficiency, level retains that liquid measure is few, and occupation area of equipment is small, and operating cost is low, suitable for large-scale production.
The technique of Centrifugical extraction copper in the leachate from heterogenite, it is comprised the following steps that:
1) heterogenite is more than 25% through wet ball-milling 85~90% by -100 mesh, pulp density, adds sulfuric acid and sponge
60~80 DEG C, 1~2h of time of copper precipitation upper liquid reducing leaching temperature, controls solution PH=1.0~2.0, Fe2+:1~2g/
L, sampling analysis Co≤0.2%.
2) by step (1) obtained by leachate, add alkali to adjust PH=3~3.5, blast air, add hydrogen peroxide or addition
Sodium chlorate aoxidizes, and reacts 1-2h, 60~80 DEG C of temperature, controls solution Fe≤0.03g/l, and filter.
3) by step (2) except iron liquid and aldoxime kind of extractants 15~40%, remaining is that sulfonated kerosene adds glass steel
Matter centrifugal extractor, extraction series n=2~6, extraction temperature is 30 DEG C~50 DEG C, compared to O:A=1:1~2, flow ratio:O:A=1
~2:1,5~20s of extraction time, at different levels are connected using polyethylene pipe, and raffinate returns to cobalt production process.
4) by the copper-rich organic phase of step (3) using 1.5~2.5mol/l sulfuric acid as back washing agent, series n=2~6 are stripped, instead
It is 10 DEG C~40 DEG C to extract temperature, compared to O:A=1~2:1, stream compares O:A=7~10:1, Stripping times are 10~30s, are contained
Copper solution and blank organic phase, the mg/L of blank organic phase < containing Cu 50 can return to extraction process recycling.
5) step (4) back extraction is prepared into copper sponge containing copper liquid using iron powder reducing, iron powder adds coefficient 1.0-1.2, sponge
Copper precipitation upper liquid, which returns to leach, to be used.
Further, step (1) copper sponge precipitation upper liquid refers to the liquid filtered after iron powder reducing copper solution, contain
Co3+ in heterogenite can be reduced to Co2+ by Fe2+, Fe2+, be advantageous to the leaching of cobalt.Chemical equation:
Cu2++Fe=Fe2++Cu Fe2++Co3+=Co2++Fe3+
Further, step (2) mode of oxidizing aoxidizes one of which to blast air, adding hydrogen peroxide or adding sodium chlorate
Or various ways combination.
Further, step (3) the aldoxime kind of extractants is:Lix984 (5-nonyl salicyl aldooxime and 2- hydroxyl -5- nonyls
Base acetophenone ketoxime presses volume 1:1 mixing), Lix973 (5-nonyl salicyl aldooxime and 2- hydroxyl -5- nonyl acetophenone ketoximes are pressed,
Volume ratio 7:3 compositions), N902 (2- hydroxyl -5- nonylsalicylaldoximes), M5640 it is one or more, extraction series n=2~6,
It is preferred that 3 grades, 5~20s of extraction time, preferably 10~15s.Extractive reaction equation (HR is extractant):
2HR (org)+Cu2+=CuR2 (org)+2H+
Further, step (4) copper-rich organic phase is using 1.5~2.5mol/l sulfuric acid as back washing agent, preferably 2.0mol/l sulphur
Acid, back extraction series n=2~6, preferably 2 grades, Stripping times are 10~30s, preferably 10~15s.It is stripped equation:
CuR2 (org)+2H+=2HR (org)+Cu2+
The present invention has the advantages that relative to prior art:.
1) Centrifugical extraction copper is used, extraction level retains that liquid measure is few, saves the expense of substantial amounts of extractant;Cost is low.Centrifugation
Extracter vertical direct coupled motor drives, is compact-sized, and floor space is small.
2) copper-rich organic phase is stripped using sulfuric acid centrifugal, and Stripping times are short, and back extraction ratio is high, back extraction blank organic phase < containing Cu
50mg/L can be recycled, and the addition iron powder containing copper liquid of back extraction prepares copper sponge, and copper sponge precipitation upper liquid contains Fe2+ and sulphur
Acid, the leaching process of cobalt is returned to, the usage amount for leaching reducing agent and sulfuric acid can be reduced, while decrease wastewater treatment, reduced
Production cost.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Glass steel material centrifugal extractor (CTL550-N) used is commercially available, and mixing flux is imported and exported for 15~40m3/hAppearance and size 1000mm × 1000mm × 2200mm.
Embodiment 1
1) heterogenite (composition Co:10.2%, Cu:4.4%, Fe:2.34%, Mg:1.21%, Ca:0.003%), through wet
Formula ball milling 85% is more than 25% by -100 mesh, pulp density, adds sulfuric acid and copper sponge precipitation upper liquid reducing leaching temperature
70 DEG C, time 1.5h, control solution PH=1.5, Fe2+:The filtering of 1.5g/l, sampling analysis residue Co≤0.18%.
2) by step (1) obtained by leachate, add alkali to adjust PH=3.5, blast air oxidation, react 1h, 75 DEG C of temperature,
During sampling analysis solution Fe≤0.03g/l, filtering.
3) solution after the iron removaling of step (2) is added into centrifugation together with extractant 15%Lix984+85% sulfonated kerosenes
Extracter, in 36 DEG C of three-level counter-current extraction Centrifugical extractions, compared to O:A=1.2:1, stream compares O:A=1:1, extraction time 10s, extraction
Extraction raffinate Cu < 0.2g/l, raffinate return to cobalt production process.
4) by the copper-rich organic phase of step (3) using 2mol/l sulfuric acid as back washing agent, series n=2 is stripped, is stripped temperature 25
DEG C, compared to O:A=1~2:1, stream compares O:A=7:1, Stripping times 10s, obtain copper-containing solution and blank organic phase, and blank has
Machine mutually returns to extraction process recycling.
5) step (4) back extraction is prepared into copper sponge containing copper liquid using iron powder reducing, iron powder adds coefficient 1.1, and copper sponge sinks
Shallow lake upper liquid is returned to leach and used.
Embodiment 2
1) heterogenite (composition Co:10.2%, Cu:4.4%, Fe:2.34%, Mg:1.21%, Ca:0.003%), through wet
Formula ball milling 90% is more than 27% by -100 mesh, pulp density, adds sulfuric acid and copper sponge precipitation upper liquid reducing leaching temperature
75 DEG C, time 1.5h, control solution PH=1.3, Fe2+:When 1.2g/l, sampling analysis residue Co≤0.15%, filtering.
2) by step (1) obtained by leachate, add alkali adjust PH=3.0, add hydrogen peroxide oxidation, react 1.5h, temperature
60~80 DEG C, the Fe≤0.03g/l filterings of control solution.
3) by step (2) except iron liquid and extractant 15%Lix973+85% sulfonated kerosenes add centrifugal extractor, 30
DEG C three-level counter-current extraction Centrifugical extraction, compared to O:A=1.2:1, stream compares O:A=1:1, extraction time 10s, raffinate Cu <
0.1g/l, raffinate return to cobalt production process.
4) by the copper-rich organic phase of step (3) using 2mol/l sulfuric acid as back washing agent, series n=2 is stripped, back extraction temperature is 25
DEG C, compared to O:A=1~2:1, stream compares O:A=7:1, Stripping times 10s, obtain copper-containing solution and blank organic phase, and blank has
Machine mutually returns to extraction process recycling.
5) step (4) back extraction is prepared into copper sponge containing copper liquid using iron powder reducing, iron powder adds coefficient 1.1, and copper sponge sinks
Shallow lake upper liquid is returned to leach and used.
Embodiment 3
1) heterogenite (composition Co:10.2%, Cu:4.4%, Fe:2.34%, Mg:1.21%, Ca:0.003%), through wet
Formula ball milling 90% is more than 28% by -100 mesh, pulp density, adds sulfuric acid and copper sponge precipitation upper liquid reducing leaching temperature
70 DEG C, reaction time 1.5h, solution PH=1.2, Fe2+ < 1.5g/l are controlled, sampling analysis residue Co≤0.13% filters.
2) by step (1) obtained by leachate, add alkali adjust PH=3.0, add sodium chlorate oxidation, react 1.5h, temperature
60~80 DEG C, the Fe≤0.03g/l filterings of control solution.
3) by step (2) except iron liquid and extractant 15%N902+85% sulfonated kerosenes add centrifugal extractor, at 30 DEG C
Three-level counter-current extraction Centrifugical extraction, compared to O:A=1.2:1, stream compares O:A=1:1, extraction time 10s, raffinate Cu < 0.3g/
L, raffinate return to cobalt production process.
4) by the copper-rich organic phase of step (3) using 2mol/l sulfuric acid as back washing agent, series n=2 is stripped, back extraction temperature is 25
DEG C, compared to O:A=1~2:1, stream compares O:A=7:1, Stripping times 10s, obtain copper-containing solution and blank organic phase, and blank has
Machine mutually returns to extraction process recycling.
5) step (4) back extraction is prepared into copper sponge containing copper liquid using iron powder reducing, iron powder adds coefficient 1.1, and copper sponge sinks
Shallow lake upper liquid is returned to leach and used.
Embodiment 4
1) heterogenite (composition Co:10.2%, Cu:4.4%, Fe:2.34%, Mg:1.21%, Ca:0.003%), through wet
Formula ball milling 90% is more than 30% by -100 mesh, pulp density, adds sulfuric acid and copper sponge precipitation upper liquid reducing leaching temperature
70 DEG C, reaction time 1.5h, control solution PH=1.2, Fe2+ < 1.5g/l, sampling analysis residue Co≤0.16%, filtering.
2) by step (1) obtained by leachate, add alkali to adjust PH=3.2, blast air oxidation, react 1.5h, temperature 70
DEG C, filter during sampling analysis solution Fe≤0.03g/l.
3) by step (2) except iron liquid and extractant 15%M5640+85% sulfonated kerosenes add centrifugal extractor, 30
DEG C three-level counter-current extraction Centrifugical extraction, compared to O:A=1.2:1, stream compares O:A=1:1, extraction time 10s, raffinate Cu <
0.2g/l, raffinate return to cobalt production process.
4) by the copper-rich organic phase of step (3) using 2mol/l sulfuric acid as back washing agent, series n=2 is stripped, back extraction temperature is 25
DEG C, compared to O:A=1~2:1, stream compares O:A=7:1, Stripping times 10s, obtain copper-containing solution and blank organic phase, and blank has
Machine mutually returns to extraction process recycling.
5) step (4) back extraction is prepared into copper sponge containing copper liquid using iron powder reducing, iron powder adds coefficient 1.1, and copper sponge sinks
Shallow lake upper liquid is returned to leach and used.
Comparative example 1
1) heterogenite is more than 27% through wet ball-milling 90% by -100 mesh, pulp density, adds sulfuric acid and sodium sulfite
Reduction, 75 DEG C, reaction time 1.5h of temperature, control solution PH=1.2, Fe2+ < 1.5g/l, sampling analysis residue Co≤
0.2%, filtering.
2) by step (1) obtained by leachate, add alkali adjust PH=3.2, blast air oxidation and add sodium chlorate, reaction
1.5h, temperature 70 C, the Fe≤0.03g/l filterings of control solution.
3) by step (2) except iron liquid and extractant 15%Lix984+85% sulfonated kerosenes add extraction tank, at 30 DEG C three
Stage countercurrent extraction extraction, compared to O:A=1.2:1, stream compares O:A=1:1, extraction time 5min, raffinate Cu < 0.5g/l, raffinate
Liquid returns to cobalt production process.
4) copper-rich organic phase obtained by step (3) is subjected to one-level clarification, extraction tank Gravity Separation speed is slow, and contains the 3rd
Mutually need to separate, third phase also needs regular press filtration to separate.
5) by the clarification copper-rich organic phase of step (4) using 2mol/l sulfuric acid as back washing agent, series n=2 is stripped, is stripped temperature
For 25 DEG C, compared to O:A=1~2:1, stream compares O:A=7:1, Stripping times 5min, copper-containing solution and blank organic phase are obtained,
Blank organic phase returns to extraction process and recycled.
6) step (4) back extraction is prepared into electro deposited copper containing copper liquid, containing copper liquid continuing return be stripped process circulate after electrodeposition makes
With.
Cobalt content sampling analysis result in leaching cobalt slag cobalt content and raffinate in 1~embodiment of the embodiment of the present invention 4
It is as follows:
Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 |
Cobalt slag cobalt content | 0.18% | 0.15% | 0.13% | 0.16% | 0.2% |
Raffinate copper content | 0.2g/l | 0.1g/l | 0.3g/l | 0.2g/l | 0.5g/l |
Extraction time | 10s | 10s | 10s | 10s | 5min |
Stripping times | 10s | 10s | 10s | 10s | 5min |
Extract series | 3 | 3 | 3 | 3 | 3 |
It is stripped series | 2 | 2 | 2 | 2 | 2 |
Clarify series | 0 | 0 | 0 | 0 | 1 |
Applicant states, the foregoing is only the embodiment of the present invention, but protection scope of the present invention not office
It is limited to this, person of ordinary skill in the field is it will be clearly understood that any belong to those skilled in the art and taken off in the present invention
In the technical scope of dew, the change or replacement that can readily occur in, all fall within protection scope of the present invention and it is open within the scope of.
Claims (5)
1. the technique of Centrifugical extraction copper in a kind of leachate from heterogenite, it is comprised the following steps that:
(1) heterogenite is more than 25% through wet ball-milling 85% above by -100 mesh, pulp density, adds sulfuric acid and copper sponge sinks
Shallow lake upper liquid reducing leaching, 60~80 DEG C, 1~2h of time of temperature, control solution PH=1.0~2.0, Fe2+:1~2g/l, sampling
Analyze Co≤0.2%, filtering;
(2) by step (1) obtained by leachate, add alkali adjust PH=3~3.5, oxidation, react 1-2h, 60~80 DEG C of temperature, control
Solution Fe≤0.03g/l processed, and filter;
(3) by step (2) except iron liquid and aldoxime kind of extractants 15~40%, remaining is that sulfonated kerosene adds glass steel material together
Centrifugal extractor, extraction series n=2~6, extraction temperature is 30~50 DEG C, compared to O:A=1:1~2, flow ratio:O:A=1~2:
1,5~20s of extraction time, at different levels are connected using polyethylene pipe, and raffinate returns to cobalt production process;
(4) by the copper-rich organic phase of step (3) with 1.5~2.5mol/l sulfuric acid back washing agents, back extraction series n=2~6, back extraction temperature
Spend for 10~40 DEG C, compared to O:A=1~2:1, stream compares O:A=7~10:1, Stripping times are 10~30s, obtain copper-containing solution
With blank organic phase, blank organic phase < containing Cu 50mg/L can return to extraction process recycling;
(5) step (4) back extraction is prepared into copper sponge containing copper liquid using iron powder reducing, iron powder adds coefficient 1.0-1.2, and copper sponge sinks
Shallow lake upper liquid is returned to leach and used.
2. the technique of Centrifugical extraction copper in a kind of leachate from heterogenite according to claims 1, it is characterised in that:Step
Suddenly (1) copper sponge precipitation upper liquid refers to the liquid filtered after iron powder reducing copper solution, contain Fe2+, Fe2+By in heterogenite
Co3+It is reduced to Co2+, chemical equation:
Cu2++ Fe=Fe2++Cu Fe2++Co3+=Co2++Fe3+。
3. the technique of Centrifugical extraction copper in a kind of leachate from heterogenite according to claims 1, it is characterised in that:Step
Suddenly (2) mode of oxidizing combines to blast air, adding hydrogen peroxide or adding sodium chlorate oxidation one or more of which mode.
4. the technique of Centrifugical extraction copper in a kind of leachate from heterogenite according to claims 1, it is characterised in that:Step
Suddenly (3) described aldoxime kind of extractants is:(5-nonyl salicyl aldooxime presses volume to Lix984 with 2- hydroxyl -5- nonyl acetophenones ketoximes
1:1 mixing), Lix973 (press, volume ratio 7 by 5-nonyl salicyl aldooxime and 2- hydroxyl -5- nonyl acetophenone ketoximes:3 composition), N902
(2- hydroxyls -5-nonyl salicyl aldooxime), M5640 are one or more, extraction series n=2~6, preferably 3 grades, and extraction time 5~
20s, preferably 10~15s;Extractive reaction equation (HR is extractant):
2HR(org)+Cu2+=CuR2(org)+2H+。
5. the technique of Centrifugical extraction copper in a kind of leachate from heterogenite according to claims 1, it is characterised in that:Step
Suddenly (4) copper-rich organic phase is using 1.5~2.5mol/l sulfuric acid as back washing agent, preferably 2.0mol/l sulfuric acid, back extraction series n=2~6,
It is preferred that 2 grades, Stripping times are 10~30s, preferably 10~15s;It is stripped equation:
CuR2(org)+2H+=2HR(org)+Cu2+。
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Cited By (4)
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---|---|---|---|---|
CN109234525A (en) * | 2018-11-16 | 2019-01-18 | 温州大学 | A kind of inexpensive leaching method of heterogenite |
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