CN108118151A - Potential-controlled oxidation removal of Mn in cobalt sulfate solution2+Method (2) - Google Patents
Potential-controlled oxidation removal of Mn in cobalt sulfate solution2+Method (2) Download PDFInfo
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- CN108118151A CN108118151A CN201711439622.4A CN201711439622A CN108118151A CN 108118151 A CN108118151 A CN 108118151A CN 201711439622 A CN201711439622 A CN 201711439622A CN 108118151 A CN108118151 A CN 108118151A
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- solution
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- cobalt sulfate
- oxidation
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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
- 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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- 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
- C22B47/00—Obtaining manganese
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for removing Mn in cobalt sulfate solution by controlling potential oxidation2+Belonging to the technical field of wet metallurgy. Selection of Na2S2O8As an oxidizing agent, crude CoSO was continuously stirred4The solution is maintained at pH 5.0-5.5, temperature 55-60 deg.C, oxidation potential 0.4-1.3V, Na is added at constant speed and in stages2S2O8Solution, Na2S2O8The amount of oxidant added is controlled to crude CoSO4Mn in solution2+3.5 to 4 times of theoretical molar content, reacting for 0.8 to 1.2 hours, and filtering to obtain the product containing MnO2And Co (OH)3Oxidizing demanganization slag, liquid phaseFor removing Mn2+After CoSO4And (3) solution. The main component of the oxidation manganese removal slag is MnO2And Co (OH)3The manganese slag can be recycled as an oxidant in an oxidation iron removal process in an electro-nickel hydrometallurgy system, or can be sold as manganese slag. The method is used for adding Mn in the cobalt sulfate solution2+After the preliminary removal, the load and the operation cost of the P204 extraction are reduced, and meanwhile, the effects of no waste residue and waste liquid discharge are achieved, so that the method is green, environment-friendly and zero-discharge.
Description
Technical field
The present invention relates to Mn in a kind of controlling potential oxidation removal cobalt sulfate solution2+Method, belong to hydrometallurgical technology
Field.
Background technology
CoSO4·7H2Purposes than wide, is used as paint drier to O products in coatings industry in the industry.Ceramic industry
As painted china glaze.Chemical industry is for pigment of the manufacture containing cobalt and as the raw material for producing various cobalt salts.Battery industry
Additive as alkaline battery and lithopone.It additionally can be used for electroplating cobalt, accumulator processed, cobalt pigment, ceramics, enamel, glaze
It is color and as catalyst, foam stabiliser, drier etc..
Since domestic and international earthy cobalt lacks, the cobalt resource that can be developed is considerably less, and cobalt metal majority is association at other
In metalliferous mineral, output, domestic cobalt smelt raw materials for production main source in the form of cobalt slag enriched substance in main metal process is extracted
In the secondary heavy cobalt slag of the higher metalliferous mineral containing cobalt.The crude cobalt sulfate solution obtained from cobalt slag by sulfuric acid leaching is often
Metals content impurity is higher, if cobalt sulfate solution is handled without pre- removal of impurities, is just directly entered P204 abstraction impurity removals, can lead
Cause P204 loads too big, operating cost is high, while can influence the extracting power of P204, special Mn2+The higher cobaltous sulfate of content is molten
Liquid is directly entered P204 extracting systems, and the influence to the extracting power of P204 is fairly obvious, causes purified cobalt sulfate solution
In metal impurities it is exceeded, the product produced is unqualified, molten to crude cobaltous sulfate so into before P204 extracting systems
Mn in liquid2+Carry out preliminary removing be very it is necessary to.
It is industrially commonly used to Mn under sulfuric acid system2+Removal methods be, using potassium permanganate, H2O2Wait oxidants
Oxidation removal Mn2+, the oxidisability of potassium permanganate is too strong, is difficult to control in oxidation reaction process, in oxidation Mn2+While will
Co2+Also a large amount of oxidations, cobalt damage too high, the MnO in oxidation removal slag2With Co (OH)3Content it is all too high, it is difficult to sale or return
It receives and utilizes.Add H2O2Demanganize is aoxidized, consumption is too big, and cost is too high, while can dilute cobalt sulfate solution, is unfavorable for subsequent technique
Production.
The content of the invention
The purpose of the invention is to overcome to aoxidize de- Mn in above-mentioned crude cobalt sulfate solution2+Existing for prior art not
Foot, provides Mn in a kind of controlling potential oxidation removal cobalt sulfate solution2+Method, this method can improve Mn2+Removal efficiency and
Reduce Co2+Loss late, while reduce the load of back segment process P204 extractions, reduce the extraction cost of P204, aoxidize de- Mn2+
Process achievees the effect that no waste residue, discharging of waste liquid, environmentally protective, zero-emission.
The present invention provides Mn in a kind of controlling potential oxidation removal cobalt sulfate solution2+Method, from S2O8 2--H2O systems E-pH
Figure understands S2O8 2-Oxidation-reduction potential for 2.08V, therefore oxidation-reduction potential is less than the gold with oxidation-reduction quality of 2.08V
Belonging to ion can be by S2O8 2-It is aoxidized.From Me-H2Knowable to O systems E-pH figures, Mn2+, Co2+The maximum potential aoxidized respectively may be about
1.3V,1.8V；Mn2+It is oxidized to MnO2Minimum oxidizing potential for 0.4V, the present invention makes full use of Na2S2O8(2.08V), Mn2+
(1.3V), Co2+The difference of the highest oxidation reduction potential in aqueous solution of (1.8V) controls CoSO4Solution potential and pH value,
Use Na2S2O8Mn in oxidation removal cobalt sulfate solution2+.Specific steps include：Select Na2S2O8As oxidant, it is stirred continuously thick
CoSO processed4Solution and remain solution pH be 5.0~5.5, temperature is 55~60 DEG C, 0.4~1.3V of oxidizing potential, at the uniform velocity
And it is segmented and adds in Na2S2O8Solution, Na2S2O8Oxidant addition is controlled in crude CoSO4Mn in solution2+Theoretical molar content
3.5~4 times, reaction 0.8~1.2 it is small when, after filtering obtain contain MnO2With Co (OH)3Oxidation demanganization slag, liquid phase for removing
Mn2+CoSO afterwards4Solution.
Above-mentioned solid phase contains MnO2With Co (OH)3Oxidation demanganization slag demanganization slag as electricity nickel system oxidation iron removal step
Oxidant is used or sold as manganic concerntrate；Liquid phase enters P204 extracting systems and carries out trace meter in depth extract and separate solution
Impurity using P507 extract and separates Ni, Co, obtains pure cobalt sulfate solution and is used for producing CoSO4·7H2O products or electricity
Cobalt；The crude CoSO finally obtained4Mn in solution2+Removal efficiency be 99.5%, Co2+Loss late can control 5% with
It is interior.
Crude CoSO in the step4Mn in solution2+Concentration is 0.4~5g/L.
Crude CoSO in the step4Co in solution2+Concentration is 55~60g/L.
Crude CoSO in the step4The pH value of solution is adjusted by sodium hydroxide solution, concentration 5%.The hydroxide
Sodium solution uses NaOH content to be prepared for 96% industrial sodium hydroxide.
The rotating speed stirred in the step is 250~300r/min.
Na in the step2S2O8Concentration be 0.1mol/L；The Na2S2O8Solution uses Na2S2O8Content is 99% work
Industry grade Na2S2O8It prepares.
The reaction time is preferably 1h in the step.
The present invention is using control solution potential Na2S2O8Mn in oxidation removal cobalt sulfate solution2+, this method operating environment
Without acid mist pollution, Mn can be improved2+Removal efficiency and reduce Co2+Loss late, while reduce the negative of back segment process P204 extractions
Lotus reduces the extraction cost of P204, containing MnO2With Co (OH)3Demanganization slag can be as the oxidation of electric nickel system oxidation iron removal step
Agent is recycled or sold as manganic concerntrate.The method of the present invention is with more practicability, simple for process, control easy to operate,
Reach oxidation de- Mn while production cost is reduced2+Effect of the process without waste residue, discharging of waste liquid, environmentally protective, zero-emission, tool
There is the advantages of efficient, environmentally friendly, highly practical.
Description of the drawings
Fig. 1 is the crude cobalt sulfate solution purification process flow diagram of the embodiment of the present invention 1；
Fig. 2 is the cobalt sulfate solution removing Mn of the present invention2+Oxidation test device.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Crude cobalt sulfate solution oxidizing potential control is in 0.4~1.3V in the embodiment of the present invention；
Crude cobalt sulfate solution in the embodiment of the present invention is the cobalt hydroxide slag using Yunnan nickel manufacturing enterprise output,
It leaches and obtains by the industrial sulphuric acid of 60g/L, cobalt concentration is 55~60g/L.
The sodium hydroxide solution used in the embodiment of the present invention uses NaOH content as 96% for industrial sodium hydroxide purchased in market
Industrial sodium hydroxide prepare solution.
The Na used in the embodiment of the present invention2S2O8Solution is industry Na purchased in market2S2O8, using Na2S2O8Content is 99%
Technical grade Na2S2O8The solution of preparation.
The crude CoSO used in the embodiment of the present invention4Mn in solution2+Content is 0.4~5g/L；
The rotating speed of DF-1 constant temperature blender with magnetic force is 250~300r/min in reaction process in the embodiment of the present invention
The reaction time is 0.5~1h in the embodiment of the present invention；
Reaction temperature is 55~60 DEG C in the embodiment of the present invention；
Na in the embodiment of the present invention2S2O8Oxidant addition is controlled in crude CoSO4Mn in solution2+Theoretical molar contains
3.5~4 times of amount.
Embodiment 1：
As illustrated in fig. 1 and 2, Na is utilized2S2O8(2.08V), Mn2+(1.3V), Co2+The highest in aqueous solution of (1.8V)
The difference of oxidation-reduction potential controls CoSO4Solution potential and pH value, use Na2S2O8Mn in oxidation removal cobalt sulfate solution2+, sulphur
After sour cobalt demanganize liquid using P204 extraction carry out extract and separate solution in trace metal impurities, using P507 extract and separates Ni,
Co obtains pure cobalt sulfate solution and is used for producing CoSO4·7H2O products or electric cobalt；The main component of oxidation precipitation slag is
MnO2With Co (OH)3, iron removal by oxidation process that can be as oxidant in electric nickel hydrometallurgy system recycled or
It is sold as manganese slag, specific steps include：
(1) Co will be contained2+：55g/L, Mn2+：It is added in the crude cobalt sulfate solution of 0.4g/L in beaker, and adds in hydroxide
Sodium solution adjusts the pH value of solution between 5.0~5.5, and adition process opens DF-1 constant temperature blender with magnetic force, rotating speed 250r/
Min, and open water-bath and be heated to 60 DEG C；
(2) 0.1mol/L Na are used2S2O8As oxidant, oxidation reduction potential determination instrument is opened, controls oxidizing potential
In the range of 0.4~1.3V, according to potential change situation, at the uniform velocity, segmentation add in Na into crude cobalt sulfate solution2S2O8
Oxidant, concern solution ph obtains situation of change at any time during the reaction, between ensureing pH value 5.0~5.5, Na2S2O8Oxidation
Agent addition is controlled in crude CoSO4Mn in solution2+3.5 times of theoretical molar content, reaction time 1h, among the step
Crude CoSO4Mn in solution2+Removal efficiency be 99.2%, Co2+Loss late can control 4.1%；
(3) Mn is taken off to the oxidation in step (2)2+Liquid is filtered solid-liquor separation, and liquid phase takes off de- Mn2+Liquid enters next afterwards
Section P204 extraction process carries out depth abstraction impurity removal to remaining trace metal impurities in solution；Solid phase is containing MnO2With Co (OH)3
Demanganization slag.
Embodiment 2：
Utilize Na2S2O8(2.08V), Mn2+(1.3V), Co2+The highest oxidation reduction potential in aqueous solution of (1.8V)
Difference, control CoSO4Solution potential and pH value, use Na2S2O8Mn in oxidation removal cobalt sulfate solution2+, liquid after cobaltous sulfate demanganize
It is extracted using P204 and carries out trace metal impurities in extract and separate solution, using P507 extract and separates Ni, Co, obtained pure
Cobalt sulfate solution is used for producing CoSO4·7H2O products or electric cobalt；The main component of oxidation precipitation slag is MnO2With Co (OH)3, can
It is recycled as iron removal by oxidation process of the oxidant in electric nickel hydrometallurgy system or is gone out as manganese slag
It sells, specific steps include：
(1) Co will be contained2+：57g/L, Mn2+：It is added in the crude cobalt sulfate solution of 2.2g/L in beaker, and adds in hydroxide
Sodium solution adjusts the pH value of solution between 5.0~5.5, and adition process opens DF-1 constant temperature blender with magnetic force, rotating speed 260r/
Min, and open water-bath and be heated to 60 DEG C；
(2) 0.1mol/L Na are used2S2O8As oxidant, oxidation reduction potential determination instrument is opened, controls oxidizing potential
In the range of 0.4~1.3V, according to potential change situation, at the uniform velocity, segmentation add in Na into crude cobalt sulfate solution2S2O8
Oxidant, concern solution ph obtains situation of change at any time during the reaction, between ensureing pH value 5.0~5.5, Na2S2O8Oxidation
Agent addition is controlled in crude CoSO4Mn in solution2+3.8 times of theoretical molar content, reaction time 1h, among the step
Crude CoSO4Mn in solution2+Removal efficiency be 99.4%, Co2+Loss late can control 4.3%；
(3) Mn is taken off to the oxidation in step (2)2+Liquid is filtered solid-liquor separation, and liquid phase takes off de- Mn2+Liquid enters next afterwards
Section P204 extraction process carries out depth abstraction impurity removal to remaining trace metal impurities in solution；Solid phase is containing MnO2With Co (OH)3
Demanganization slag.
Embodiment 3：
Utilize Na2S2O8(2.08V), Mn2+(1.3V), Co2+The highest oxidation reduction potential in aqueous solution of (1.8V)
Difference, control CoSO4Solution potential and pH value, use Na2S2O8Mn in oxidation removal cobalt sulfate solution2+, liquid after cobaltous sulfate demanganize
It is extracted using P204 and carries out trace metal impurities in extract and separate solution, using P507 extract and separates Ni, Co, obtained pure
Cobalt sulfate solution is used for producing CoSO4·7H2O products or electric cobalt；The main component of oxidation precipitation slag is MnO2With Co (OH)3, can
It is recycled as iron removal by oxidation process of the oxidant in electric nickel hydrometallurgy system or is gone out as manganese slag
It sells, specific steps include：
(1) Co will be contained2+：60g/L, Mn2+：It is added in the crude cobalt sulfate solution of 5.0g/L in beaker, and adds in hydroxide
Sodium solution adjusts the pH value of solution between 5.0~5.5, and adition process opens DF-1 constant temperature blender with magnetic force, rotating speed 300r/
Min, and open water-bath and be heated to 58 DEG C；
(2) 0.1mol/L Na are used2S2O8As oxidant, oxidation reduction potential determination instrument is opened, controls oxidizing potential
In the range of 0.4~1.3V, according to potential change situation, at the uniform velocity, segmentation add in Na into crude cobalt sulfate solution2S2O8
Oxidant, concern solution ph obtains situation of change at any time during the reaction, between ensureing pH value 5.0~5.5, Na2S2O8Oxidation
Agent addition is controlled in crude CoSO4Mn in solution2+4 times of theoretical molar content, reaction time 1h are thick among the step
CoSO processed4Mn in solution2+Removal efficiency be 99.5%, Co2+Loss late can control 4.8%；
(3) Mn is taken off to the oxidation in step (2)2+Liquid is filtered solid-liquor separation, and liquid phase takes off de- Mn2+Liquid enters next afterwards
Section P204 extraction process carries out depth abstraction impurity removal to remaining trace metal impurities in solution；Solid phase is containing MnO2With Co (OH)3
Demanganization slag.
Embodiment 4：
Utilize Na2S2O8(2.08V), Mn2+(1.3V), Co2+The highest oxidation reduction potential in aqueous solution of (1.8V)
Difference, control CoSO4Solution potential and pH value, use Na2S2O8Mn in oxidation removal cobalt sulfate solution2+, liquid after cobaltous sulfate demanganize
It is extracted using P204 and carries out trace metal impurities in extract and separate solution, using P507 extract and separates Ni, Co, obtained pure
Cobalt sulfate solution is used for producing CoSO4·7H2O products or electric cobalt；The main component of oxidation precipitation slag is MnO2With Co (OH)3, can
It is recycled as iron removal by oxidation process of the oxidant in electric nickel hydrometallurgy system or is gone out as manganese slag
It sells, specific steps include：
(1) Co will be contained2+：56g/L, Mn2+：It is added in the crude cobalt sulfate solution of 0.8g/L in beaker, and adds in hydroxide
Sodium solution adjusts the pH value of solution between 5.0~5.5, and adition process opens DF-1 constant temperature blender with magnetic force, rotating speed 250r/
Min, and open water-bath and be heated to 55 DEG C；
(2) 0.1mol/L Na are used2S2O8As oxidant, oxidation reduction potential determination instrument is opened, controls oxidizing potential
In the range of 0.4~1.3V, according to potential change situation, at the uniform velocity, segmentation add in Na into crude cobalt sulfate solution2S2O8
Oxidant, concern solution ph obtains situation of change at any time during the reaction, between ensureing pH value 5.0~5.5, Na2S2O8Oxidation
Agent addition is controlled in crude CoSO4Mn in solution2+3.5 times of theoretical molar content, reaction time 1h, among the step
Crude CoSO4Mn in solution2+Removal efficiency be 99.3%, Co2+Loss late can control 4.6%；
(3) Mn is taken off to the oxidation in step (2)2+Liquid is filtered solid-liquor separation, and liquid phase takes off de- Mn2+Liquid enters next afterwards
Section P204 extraction process carries out depth abstraction impurity removal to remaining trace metal impurities in solution；Solid phase is containing MnO2With Co (OH)3
Demanganization slag.
The specific embodiment of the present invention is explained in detail above in association with attached drawing, but the present invention is not limited to above-mentioned
Embodiment, within the knowledge of a person skilled in the art, can also be before present inventive concept not be departed from
Put that various changes can be made.
Claims (7)
1. a kind of Mn in controlling potential oxidation removal cobalt sulfate solution2+Method, it is characterised in that specific steps include：Selection
Na2S2O8As oxidant, crude CoSO is stirred continuously4Solution and remain solution pH be 5.0~5.5, temperature be 55~
60 DEG C, 0.4~1.3V of oxidizing potential, at the uniform velocity and be segmented add in Na2S2O8Solution, Na2S2O8Oxidant addition is controlled crude
CoSO4Mn in solution2+3.5~4 times of theoretical molar content obtain when reaction 0.8~1.2 is small, after filtering and contain MnO2With
Co(OH)3Oxidation demanganization slag, liquid phase for removing Mn2+CoSO afterwards4Solution.
2. Mn in controlling potential oxidation removal cobalt sulfate solution according to claim 12+Method, it is characterised in that：Institute
State crude CoSO in step4Mn in solution2+Concentration is 0.4~5g/L.
3. Mn in controlling potential oxidation removal cobalt sulfate solution according to claim 12+Method, it is characterised in that：Institute
State crude CoSO in step4Co in solution2+Concentration is 55~60g/L.
4. Mn in controlling potential oxidation removal cobalt sulfate solution according to claim 12+Method, it is characterised in that：Institute
State Na in step2S2O8The concentration of solution is controlled in 0.1mol/L.
5. Mn in controlling potential oxidation removal cobalt sulfate solution according to claim 12+Method, it is characterised in that：Institute
State crude CoSO in step4The pH value of solution is adjusted by sodium hydroxide solution, concentration 5%.
6. Mn in controlling potential oxidation removal cobalt sulfate solution according to claim 12+Method, it is characterised in that：Institute
Reaction process mixing speed in step is stated to control in 250~300r/min.
7. Mn in controlling potential oxidation removal cobalt sulfate solution according to claim 12+Method, it is characterised in that：Institute
Reaction time control is stated in step in 1h.
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| CN201711439622.4A CN108118151B (en) | 2017-12-27 | 2017-12-27 | Potential-controlled oxidation removal of Mn in cobalt sulfate solution2+Method (2) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112522515A (en) * | 2020-11-17 | 2021-03-19 | 天津三环化工有限公司 | Method for treating waste residue containing metal manganese |
| CN116445728A (en) * | 2023-06-13 | 2023-07-18 | 矿冶科技集团有限公司 | Process method for removing manganese in solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116445728A (en) * | 2023-06-13 | 2023-07-18 | 矿冶科技集团有限公司 | Process method for removing manganese in solution |
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| CN108118151B (en) | 2020-04-14 |
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