CN102251253A - Method for extracting and separating nickel, iron and copper from electrolyte - Google Patents
Method for extracting and separating nickel, iron and copper from electrolyte Download PDFInfo
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- CN102251253A CN102251253A CN2011101739977A CN201110173997A CN102251253A CN 102251253 A CN102251253 A CN 102251253A CN 2011101739977 A CN2011101739977 A CN 2011101739977A CN 201110173997 A CN201110173997 A CN 201110173997A CN 102251253 A CN102251253 A CN 102251253A
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Abstract
The invention relates to an electrolyte, particularly a method for extracting and separating nickel, iron and copper from electrolyte, which comprises the following steps: adding oxydol into the electrolyte to carry out previous oxidation treatment on the electrolyte; adding ammonium fluoride shielding iron ions into the electrolyte subjected to previous oxidation treatment; regulating the pH value of the electrolyte to 4-5 with ammonia water, extracting copper ions for the first time with an extractant/kerosene mixed solution, regulating the pH value of the electrolyte to 4-5 with ammonia water, extracting copper ions for the second time with an extractant/kerosene mixed solution, regulating the pH value of the raffinate to 10-11 with ammonia water, precipitating, filtering to remove iron, and extracting nickel for the first time with an extractant/kerosene mixed solution so that copper and nickel are extracted, and cobalt ions and the like are left in the water phase; back extracting copper with an H2SO4 solution; and back extracting nickel with an H2SO4 solution. After the back extraction operation, metallic ions in the extractant are completely eluted, thereby completing the extraction and separation of nickel, iron and copper in the electrolyte.
Description
Technical field
The present invention relates to a kind of electrolytic solution, especially relate to the extraction separating method of nickel, iron, copper in a kind of electrolytic solution.
Background technology
Though China's copper natural resources shortage but is one of main refined matte producing country in the world.Because high-technology field will continue to increase to the demand of nickel, so nickel industry will have boundless development prospect.Simultaneously, the development of the production technique of nickel is subjected to more and more stricter requirement on environmental protection.Therefore, develop a kind of from the electrolytic solution waste liquid technology of extracting and separating copper, nickel, iron, not only can efficent use of resources, also be of value to environment protection simultaneously.
Solvent extraction is one of separation method commonly used in the analytical chemistry in modern age, its advantage be simple, fast, easy handling and automatization.Because the development of Synthetic Organic Chemistry and the achievement that obtains, alternative extraction agent type constantly increases, therefore alternative extraction system is also many, reach high extraction efficiency and selectivity easily, solvent extraction simultaneously can combine with atomic absorption method, x ray fluorescence spectrometry, emission spectrometry etc., separating resulting is done accurately measured.(assay laboratory, 1998,17 (2): 30-32.) discover such as the Li whole people at (NH4)
2SO
4Exist down, dimethylglyoxime generates huge legendary turtle compound precipitation with nickel can be extracted flotation between ethanol and water two-phase, and the huge legendary turtle compound of cobalt and dimethylglyoxime generation is by alcohol extraction, Fe
3+Stay aqueous phase, realized separating Ni in the same system
2+, Co
2+, Fe
3+, the result is good.Jiang Xiongxun etc. (the journal .2007 of Scientific and Technological Institutes Of Zhejiang, 19 (3)) do extraction agent selectivity from the catalytic reduction ammonia leach liquor of oceanic multi-metal nodule copper nickel that comes together altogether with the kerosin of LIX84, and cobalt is stayed in the raffinate.
For the complicated nickel electrolyte that contains Determination of Multi-Impurities is carried out separation of metal ions, need carry out the research of corresponding technology, and behavior, isolation technique, the reaction mechanism of impurity element in the corresponding solution system behind the different process processing nickel raw material be carried out systematic study seek the optimal separation condition.
LIX984N is ketone-aldoxime mixing kind of extractants, is that 1: 1 LIX860 (5-nonyl salicylaldoxime) and LIX84 (2-hydroxyl-5-nonylacetophenone oxime) are with the mixture of high flash point kerosene as thinner.Outward appearance is an amber color liquid, density (25 ℃) 0.90～0.92g/cm
3, flash-point is greater than 160 ℃.Because ketoxime can improve the balance between aldoxime and copper, the hydrogen ion, assist the collection effect better, so LIX984N have the extracting power of aldoxime and the good back extraction performance and the physicals of dynamics and ketoxime concurrently.1%LIX984N is 0.556g/L to the extraction saturated capacity of copper.In the extraction process, extractive reaction functional group in the structural formula is hydroxyl (O H) and oximido (=N-O H), promptly form covalent linkage and coordinate bond with being extracted metal ion respectively, thereby form the extracted species that can be dissolved in organic solvent with chela ring structure by hydroxyl oxygen atom and oximido nitrogen-atoms.
Summary of the invention
The object of the present invention is to provide the extraction separating method of nickel, iron, copper in a kind of electrolytic solution.
Described electrolytic solution is that main component is copper, nickel, iron ion, contains the little cobalt ion, and the initial pH of solution is about 0.5 electrolytic solution.
The present invention includes following steps:
1) in electrolytic solution, adds hydrogen peroxide, electrolytic solution is carried out pre-oxidation handle;
In step 1), the volume ratio of described electrolytic solution and hydrogen peroxide can be electrolytic solution: hydrogen peroxide=(1～3): 10.
2) in the electrolytic solution of handling through pre-oxidation, add Neutral ammonium fluoride and shelter iron ion;
In step 2) in, the add-on of described Neutral ammonium fluoride and the proportioning of electrolytic solution can be (5～10) g: (10～30) ml, and wherein Neutral ammonium fluoride is calculated by mass, and electrolytic solution by volume calculates.
3) adopt ammoniacal liquor to regulate pH value to 4～5 of electrolytic solution, use extraction agent and the 1st extracting copper ion of kerosene mixing solutions, adopt ammoniacal liquor to regulate pH value to 4～5 of electrolytic solution again, use extraction agent and the 2nd extracting copper ion of kerosene mixing solutions, then raffinate is regulated pH value to 10～11 with ammoniacal liquor, and the sedimentation and filtration deironing, use the 1st extraction of nickel of extraction agent and kerosene mixing solutions again, copper, nickel are extracted cobalt ion etc. and then stay aqueous phase;
In step 3), it is 5%～15% LIX984N that described the 1st extracting copper ionic extraction agent can adopt concentration; It is 5%～15% LIX984N that the extraction agent of described the 1st extraction of nickel can adopt concentration; It is 5%～15% LIX984N that described the 2nd extracting copper ionic extraction agent can adopt concentration; It is 5%～15% LIX984N that the extraction agent of described the 2nd extraction of nickel can adopt concentration; (the O: A) can be 1 that compares of described extraction liquid and kerosene mixing solutions; The time of described the 1st extraction of nickel can be 3min; The time of described the 2nd extraction of nickel can be 3min.
4) use H
2SO
4Solution back extraction copper;
In step 4), described H
2SO
4The concentration of solution can be 1～2mol/ml; Described back extraction copper preferably adopts back extraction copper 3 times, and the time of described back extraction copper can be 1～5min; Describedly compare with vitriolic that (O: A) can be 1.5, described 3 back extraction copper obtain single copper ion solution.
5) use H
2SO
4Solution back extraction nickel;
In step 5), described H
2SO
4The concentration of solution can be 0.5～1.5mol/ml; Described back extraction nickel can adopt back extraction nickel 2 times, and the time of described back extraction nickel can be 1～5min.
6) through after the operation of stripping, the metal ion in the extraction agent is finished the extracting and separating of nickel in the electrolytic solution, iron, copper fully by wash-out.The clarification extraction agent that obtains can reuse.
The extracting metals reaction is in ammonia gonosome of the present invention is:
HR(o)+Me(NH
3)
n 2+＝MeR(org)+nNH
3(a)+H
+
By following formula following relational expression: 1gD=1gK-1g (the 1+ ∑ β that can derive
i[NH
3]
n)+2lg[HR]
(o)+ 2pH
(a)
In the formula: D is a distribution ratio, and K is the extraction equilibrium constant, β
iBe metal complex ion stability constant, N is a ligancy.
The principal element of visible influences metal ion distribution ratio is extractant concentration, water pH, ammonia concentration and temperature, compare etc. (referring to document: mining metallurgical engineering .1995,15 (4); Mining and metallurgy .2003,12 (3); Non-ferrous metal (smelting part) .2002.2.1; Transactions ofNonferrous Metals Society ofChina[J] .2003,13 (4)).
The present invention adopts LIX984N (can available from Kening Co.,Ltd) as extraction agent, adopts kerosene as thinner, shelters iron with ammonium fluoride under acidic conditions, makes its extraction that does not influence copper, regulates the pH value and do not precipitate in acid range.As long as copper is extracted, metal content can reduce greatly, is difficult for during precipitated iron adsorbing.At this moment just can pass through the strong aqua heightening pH value, make the iron precipitation, and overanxious removing.
The organic phase of extraction agent after the pickling back extraction is clear, pure, with former extraction agent color and luster basically identical, can recycle, and extracts again.
The complicated nickel electrolyte that contains Determination of Multi-Impurities is carried out the separation of metal ions field, be specifically related to when electrolytic solution copper concentration big, the concentration of iron and nickel near the time, will inevitably cause copper to be adsorbed loss if directly precipitate deironing, become key so how to handle iron.In order to address this problem, the method for extracting and separating has not only been adopted in this experiment, need not separate and simple covering method is fast eliminated the interference in the reaction but also used, thereby reach the purpose that improves reaction preference.
Description of drawings
Fig. 1 compares curve for the copper extraction phase.In Fig. 1, (O: A), ordinate zou is copper percentage extraction (%) to X-coordinate in order to compare; Comparing is the volume ratio of oil phase and water, and the copper percentage extraction is the extraction efficiency of cupric ion.
Fig. 2 is a nickel extractant concentration curve.In Fig. 2, X-coordinate is LIX984N concentration (%), and ordinate zou is nickel percentage extraction (%).
Fig. 3 compares curve for the nickel extraction phase.In Fig. 3, (O: A), ordinate zou is nickel percentage extraction (%) to X-coordinate in order to compare.
Fig. 4 is a copper back extraction time curve.In Fig. 4, X-coordinate is time (min), and ordinate zou is copper back extraction ratio (%).
Fig. 5 is the curve of comparing of copper stripping efficiency.In Fig. 5, (O: A), ordinate zou is copper back extraction ratio (%) to X-coordinate in order to compare.
Fig. 6 is the sulfuric acid concentration curve of copper back extraction.In Fig. 6, X-coordinate is sulphuric acid soln concentration (mol/L), and ordinate zou is copper back extraction ratio (%).
Fig. 7 is a nickel back extraction time curve.In Fig. 7, X-coordinate is time (min), and ordinate zou is nickel back extraction ratio (%).
Fig. 8 is the sulfuric acid concentration curve of nickel back extraction.In Fig. 8, X-coordinate is sulphuric acid soln concentration (mol/L), and ordinate zou is nickel back extraction ratio (%).
Fig. 9 is the curve of comparing of back extraction nickel.In Fig. 9, (O: A), ordinate zou is nickel back extraction ratio (%) to X-coordinate in order to compare.
Embodiment
Earlier electrolytic solution is carried out oxide treatment with hydrogen peroxide; Under acidic conditions, shelter iron with Neutral ammonium fluoride; Former used for electrolyte ammoniacal liquor is regulated pH value to 4.Measure the wherein content of each metal ion with the inductively coupled plasma atomic emission spectrum.Can see Table 1 with the bath composition after the strong aqua adjusting pH value.
Table 1
With 10%LIX984N kerosene mixing solutions and electrolytic solution among the embodiment 1 be by volume mix at 1: 1 after, in separating funnel, shake 3min, so should in advance the electrolysis dilution be regulated pH with strong aqua for 10 times again, emmission spectrum is surveyed its extraction efficiency.The single extraction rate of copper is as shown in table 2.
Table 2
Compare the influence of copper percentage extraction.10%LIX984N kerosene diluent, organic phase and water volume ratio O: A=1: 1, water pH=4.0.Concussion time 5min.Compare (O: A) be set to: 0.5: 1,1: 1,1.5: 1,2: 1,2.5: 1.Extraction results is as shown in table 3.To be in a ratio of X-coordinate, raffinate residual metallic ionic concn is an ordinate zou, does logarithmic curve chart as shown in Figure 1.The result shows that under experiment condition, the extraction that compares copper, nickel has certain influence, and the extraction efficiency of comprehensive copper and purity are considered, got to compare 0.5 to 1 and be advisable.
Table 3
Residual solution behind collection copper is regulated pH value to 10, iron removal by filtration with strong aqua.And measurement metal ion content wherein.Measuring result is as shown in table 4.
Table 4
The pH of electrolytic solution is adjusted to 10, organic phase and water volume ratio O: A=1: 1.The extraction time is adopted 5min.LIX984N concentration is respectively: 5%, 10%, 15%.Extraction results is as shown in table 5.With LIX984N concentration is X-coordinate, and the nickel ion percentage extraction is an ordinate zou, graphic representation as shown in Figure 2: the result shows that under experiment condition, LIX984N concentration is just can reach the highest extraction efficiency more than 10%.
Table 5
Compare the influence of nickel percentage extraction.With 10%LIX984N kerosene diluent, the water pH=10.0. extraction time is adopted 5min.Compare (O: A) be 10: 40,10: 20,10: 10,10: 12.5,10: 10.Shown in the extraction results table 6, to be in a ratio of X-coordinate, the nickel ion extraction efficiency is an ordinate zou, does graphic representation as shown in Figure 3.The result shows that under experiment condition, LIX984N is O mutually: peak about A=0.5.Because nickel concentration is very low, comprehensive O: the degree of the low more organic phase enriching nickel of A value is high more, help the consideration of stripping more, and compare and get O: A=0.5 is comparatively suitable.
Table 6
Reextraction is to obtain single metal ion.Feed liquid: best pH, optimum reacting time, optimum extractant concentration, the best are compared the metal load organic phase that the collection of secondary under condition copper, one-level collection nickel obtains and are used for the back extraction experiment in the extraction test.Record Cu in the raffinate
2+, Ni
2+Isoionic concentration is calculated loaded metal ion concentration in the organic phase according to C (org)={ C (a, stoste)-C (a, extraction back) }/2.The concentration of metal ion is as shown in table 7 in the organic phase.Because in the extraction process, little ammonia is carried and is total to collection secretly and enters organic phase, thus before back extraction, must remove through washing, otherwise ammonia enters strip liquor, not only increases the consumption of acid, and the back process engineering is caused detrimentally affect.It is washing composition that tap water is adopted in this experiment, compares 5: 1, mixing time is 10min, room temperature, about 1min of the time that is separated, through secondary washing except that ammonia.Adopt sulfuric acid back extraction copper, nickel from load organic phases.Mainly reach back extraction purpose, separating copper nickel by the control sulfuric acid concentration.Copper adopts compares O: A=2: 1, three grade of back extraction; Nickel adopts O: A=2: 1, and the secondary back extraction.
Table 7
Time is to the influence of copper back extraction ratio.Back extraction condition: 1.8mol/L H
2SO
4, O: A=2: 1, the back extraction time is respectively 2min, 5min, 10min.According to formula: back extraction ratio=(strip liquor copper content * 3/2)/(organic phase copper content * 100) calculates stripping efficiency.Extraction results is as shown in table 8, is X-coordinate with time, and stripping efficiency is an ordinate zou, and curve plotting as shown in Figure 4.The result shows that under experiment condition, the back extraction speed of copper is quite fast, reaches the highest about 3min, reaches capacity after the 5min.Substantially do not contain other elements in the elutant.Explanation is higher in this experiment condition back extraction copper efficient, gained copper purity height.
Table 8
Compare the influence of stripping efficiency.Back extraction condition: 1.8mol/L H
2SO
4Solution, time 5min compares to set gradually and is O: A=1.5: 1,2: 1,2.5: 1.Back extraction ratio=(strip liquor copper content * 3)/(comparing * organic phase copper content * 100) calculated stripping efficiency according to this formula.The result is as shown in table 9, is X-coordinate with O: A, and stripping efficiency is an ordinate zou, draws logarithmic plot as shown in Figure 5.The result shows that under experiment condition, O: A is low more, and stripping efficiency is high more.But the low enrichment that is unfavorable for metal ion of O: A, be controlled at O so compare: A=1.5: 1 is advisable.
Table 9
H
2SO
4Concentration is to the influence of stripping efficiency.Back extraction condition: O: A=2: 1, time 5min, sulfuric acid concentration set gradually and are 1.60mol/L, 1.80mol/L, 2.00mol/L.The back extraction result is as shown in table 10, is X-coordinate with the sulfuric acid concentration, and stripping efficiency is an ordinate zou, draws coordinate diagram as shown in Figure 6, and the result shows that under experiment condition, extraction efficiency was the highest when sulfuric acid concentration was 1.80mol/L.
Table 10
Time is to the influence of the anti-rate of nickel.Back extraction condition: 1.8mol/L H
2SO
4, O: A=2: 1, the time sets gradually and is 1min, 3min, 5min, 10min.Extraction results is as shown in table 11, is X-coordinate with time, and stripping efficiency is an ordinate zou, and curve plotting figure as shown in Figure 7.The result shows that under experiment condition, the speed of back extraction nickel is very fast, reaches capacity substantially about 3min.In the elutant except that nickel other elements dense very little, so just make higher, the gained nickel purity height of this experiment condition back extraction nickel efficient.
Table 11
H
2SO
4Concentration is to the influence of nickel stripping efficiency, back extraction condition: O: A=2: 1, and time 5min, sulfuric acid concentration set gradually and are 0.60mol/L, 1.00mol/L, 1.50mol/L, 1.80mol/L.The back extraction result is as shown in table 12, is X-coordinate with the sulfuric acid concentration, and stripping efficiency is an ordinate zou, and curve plotting figure as shown in Figure 8.The result shows that under experiment condition, when sulfuric acid concentration was 0.60mol/L, stripping efficiency was the highest.And sulfuric acid concentration is too high or too low all can to influence back extraction ratio.
Table 12
Compare the influence of stripping efficiency.Back extraction condition: 1.8mol/L H
2SO
4, time 5min, O: A set gradually into: 0.215,0.424,0.632,0.840.Extraction results is as shown in table 13, and (O: A) be X-coordinate, stripping efficiency is an ordinate zou, and curve plotting figure as shown in Figure 9 to compare.The result shows that under experiment condition, O: A is that 0.840 o'clock stripping efficiency is the highest.Can guarantee higher stripping efficiency like this, can keep elutant that higher nickel enrichment is arranged again.
Table 13
Claims (10)
1. the extraction separating method of nickel, iron, copper in the electrolytic solution is characterized in that may further comprise the steps:
1) in electrolytic solution, adds hydrogen peroxide, electrolytic solution is carried out pre-oxidation handle;
2) in the electrolytic solution of handling through pre-oxidation, add Neutral ammonium fluoride and shelter iron ion;
3) adopt ammoniacal liquor to regulate pH value to 4～5 of electrolytic solution, use extraction agent and the 1st extracting copper ion of kerosene mixing solutions, adopt ammoniacal liquor to regulate pH value to 4～5 of electrolytic solution again, use extraction agent and the 2nd extracting copper ion of kerosene mixing solutions, then raffinate is regulated pH value to 10～11 with ammoniacal liquor, and the sedimentation and filtration deironing, use the 1st extraction of nickel of extraction agent and kerosene mixing solutions again, copper, nickel are extracted cobalt ion etc. and then stay aqueous phase;
4) use H
2SO
4Solution back extraction copper;
5) use H
2SO
4Solution back extraction nickel;
6) through after the operation of stripping, the metal ion in the extraction agent is finished the extracting and separating of nickel in the electrolytic solution, iron, copper fully by wash-out.
2. the extraction separating method of nickel, iron, copper is characterized in that in step 1) in a kind of electrolytic solution as claimed in claim 1, and the volume ratio of described electrolytic solution and hydrogen peroxide is an electrolytic solution: hydrogen peroxide=1～3: 10; In step 2) in, the add-on of described Neutral ammonium fluoride and the proportioning of electrolytic solution are (5～10) g: (10～30) ml, and wherein Neutral ammonium fluoride is calculated by mass, and electrolytic solution by volume calculates.
3. the extraction separating method of nickel, iron, copper is characterized in that in step 3) in a kind of electrolytic solution as claimed in claim 1, and described the 1st extracting copper ionic extraction agent employing concentration is 5%～15% LIX984N; The extraction agent employing concentration of described the 1st extraction of nickel is 5%～15% LIX984N; Described the 2nd extracting copper ionic extraction agent employing concentration is 5%～15% LIX984N, and the extraction agent employing concentration of described the 2nd extraction of nickel is 5%～15% LIX984N.
4. the extraction separating method of nickel, iron, copper is characterized in that in step 3) in a kind of electrolytic solution as claimed in claim 1, (the O: be 1 A) that compares of described extraction liquid and kerosene mixing solutions.
5. the extraction separating method of nickel, iron, copper is characterized in that in step 3) in a kind of electrolytic solution as claimed in claim 1, and the time of described the 1st extraction of nickel is 3min; The time of described the 2nd extraction of nickel is 3min.
6. the extraction separating method of nickel, iron, copper is characterized in that in step 4) in a kind of electrolytic solution as claimed in claim 1, described H
2SO
4The concentration of solution is 1～2mol/ml.
7. the extraction separating method of nickel, iron, copper is characterized in that in step 4) in a kind of electrolytic solution as claimed in claim 1, and described back extraction copper adopts 3 back extraction copper, and the time of described back extraction copper is 1～5min.
8. the extraction separating method of nickel, iron, copper is characterized in that in step 4) in a kind of electrolytic solution as claimed in claim 1, describedly compares (O: be 1.5 A) with vitriolic.
9. the extraction separating method of nickel, iron, copper is characterized in that in step 5) in a kind of electrolytic solution as claimed in claim 1, described H
2SO
4The concentration of solution is 0.5～1.5mol/ml.
10. the extraction separating method of nickel, iron, copper is characterized in that in step 5) in a kind of electrolytic solution as claimed in claim 1, and described back extraction nickel adopts 2 back extraction nickel, and the time of described back extraction nickel is 1～5min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374727A (en) * | 2013-07-05 | 2013-10-30 | 浙江科菲冶金科技股份有限公司 | Selective separation method of copper and iron in sulphuric acid system cobalt leachate |
| CN104030487A (en) * | 2014-06-11 | 2014-09-10 | 深圳市天净环境科技发展有限公司 | Method for processing chemical nickel-plating wastewater |
| CN104451191A (en) * | 2014-12-03 | 2015-03-25 | 紫金矿业集团股份有限公司 | Dilution extraction process capable of improving copper recovery rate |
| CN106906369A (en) * | 2015-12-22 | 2017-06-30 | 北京有色金属研究总院 | The technique that a kind of utilization synergic solvent extraction technology reclaims copper, zinc, nickel, cadmium from heavy metal wastewater thereby |
| CN110029371A (en) * | 2019-04-25 | 2019-07-19 | 江西自立环保科技有限公司 | A kind of method of copper electrolyte open circuit iron ion |
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| CN1493705A (en) * | 2003-09-02 | 2004-05-05 | 夏培富 | Preparation method of primary extraction copper, nickel to produce its salt product and its formulation |
| CN101824550A (en) * | 2009-03-02 | 2010-09-08 | 姚龚斌 | Extracting and purifying technology of high purity nickel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374727A (en) * | 2013-07-05 | 2013-10-30 | 浙江科菲冶金科技股份有限公司 | Selective separation method of copper and iron in sulphuric acid system cobalt leachate |
| CN103374727B (en) * | 2013-07-05 | 2016-03-16 | 浙江科菲科技股份有限公司 | The selective separation method of copper and iron in a kind of sulfuric acid system cobalt leach liquor |
| CN104030487A (en) * | 2014-06-11 | 2014-09-10 | 深圳市天净环境科技发展有限公司 | Method for processing chemical nickel-plating wastewater |
| CN104451191A (en) * | 2014-12-03 | 2015-03-25 | 紫金矿业集团股份有限公司 | Dilution extraction process capable of improving copper recovery rate |
| CN106906369A (en) * | 2015-12-22 | 2017-06-30 | 北京有色金属研究总院 | The technique that a kind of utilization synergic solvent extraction technology reclaims copper, zinc, nickel, cadmium from heavy metal wastewater thereby |
| CN106906369B (en) * | 2015-12-22 | 2018-10-26 | 北京有色金属研究总院 | A kind of technique recycling copper, zinc, nickel, cadmium from heavy metal wastewater thereby using synergic solvent extraction technology |
| CN110029371A (en) * | 2019-04-25 | 2019-07-19 | 江西自立环保科技有限公司 | A kind of method of copper electrolyte open circuit iron ion |
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