CN101532095A - Method for producing electrodeposited cobalt by non-hydrochloric acid electrolyte - Google Patents
Method for producing electrodeposited cobalt by non-hydrochloric acid electrolyte Download PDFInfo
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- CN101532095A CN101532095A CN200910020258A CN200910020258A CN101532095A CN 101532095 A CN101532095 A CN 101532095A CN 200910020258 A CN200910020258 A CN 200910020258A CN 200910020258 A CN200910020258 A CN 200910020258A CN 101532095 A CN101532095 A CN 101532095A
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 84
- 239000010941 cobalt Substances 0.000 title claims abstract description 84
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 81
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 40
- 239000003792 electrolyte Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000004070 electrodeposition Methods 0.000 claims abstract description 25
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000006298 dechlorination reaction Methods 0.000 claims abstract description 5
- 238000000053 physical method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 34
- 239000008151 electrolyte solution Substances 0.000 claims description 25
- 238000005137 deposition process Methods 0.000 claims description 13
- 239000012074 organic phase Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 8
- 230000007704 transition Effects 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 6
- 229940044175 cobalt sulfate Drugs 0.000 claims description 6
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 6
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 6
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 abstract description 19
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 230000009466 transformation Effects 0.000 abstract 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000002386 leaching Methods 0.000 description 4
- 239000007764 o/w emulsion Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 206010067868 Skin mass Diseases 0.000 description 2
- UBFQFXPUZDMELL-UHFFFAOYSA-N [S]C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)Cl Chemical compound [S]C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)C(Cl)(Cl)Cl UBFQFXPUZDMELL-UHFFFAOYSA-N 0.000 description 2
- -1 amine salt Chemical class 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000010349 cathodic reaction Methods 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
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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
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- Electrolytic Production Of Metals (AREA)
Abstract
The invention relates to a method for producing electrodeposited cobalt, which belongs to the technical field of production methods of the electrodeposited cobalt. The method for producing the electrodeposited cobalt by a non-hydrochloric acid electrolyte is characterized in that the method comprises the steps of: the preparation of a CoCl2 solution, extraction and transformation, dechlorination, the removal of an organic substance by a physical method, the preparation of a cobalt electrolyte, and the production of the electrodeposited cobalt. The method adds an acid fog inhibitor into the electrolyte to ensure that the expansive force on the surface of the electrolyte is reduced and oxygen precipitated by an anode smoothly passes through the liquid level so as to prevent acid from being brought into production field. The method effectively improves work environment and prevent the pollution to the ambient environment. The method for producing the electrodeposited cobalt by the non-hydrochloric acid electrolyte, due to adopting solution transformation and chlorine washing processes, ensures that Cl<-> in the electrolyte is lower than 0.1g.l<-1>, and basically meets the requirement of no precipitation of chlorine gas during the electrodeposition.
Description
One, technical field
The present invention relates to a kind of method of production electrodeposited cobalt, belong to the production method technical field of electrodeposited cobalt.
Two, background technology
At present, the commercial run of production electrodeposited cobalt commonly used is: through pyrometallurgical smelting process, behind the rough cobalt positive plate of output, carry out the electrolysis process refining, and use the soluble anode technology and produce the electrolytic cobalt product.The production technique that this process combination has adopted pyrogenic process and hydrometallurgy to produce electrolytic cobalt.Because of complex process, metal recovery rate is low, and fund input is big, is unfavorable for shortcomings such as environment protection, and is progressively substituted by the electrowinning with insoluble anode technology of full hydrometallurgy; In recent years, the domestic suitability for industrialized production of carrying out electrodeposited cobalt in hydrochloric acid system that has is put into practice.But, therefore, must seal and set up supporting chlorine absorption system to production environment and just can produce because the production electrodeposited cobalt has a large amount of chlorine and overflows (be about cobalt weight metal 1.2 times) at anode in hydrochloric acid system; So not only can increase running cost greatly, and constitute the environment potential greatly dangerous.
Three, summary of the invention
The object of the invention is to solve the problem that above-mentioned prior art exists, avoid the production of electrodeposited cobalt to cause to the substantial pollution of environment with to producers' the safety danger side of body, my company tests and research of technique by a large amount of, found electrodeposited cobalt produce in mutual restriction rule and parameter between the various processing parameters change electrolytic deposition process current efficiency, the interaction of electrodeposited cobalt quality and influence factor, simultaneously, the selection of additive and dosage are determined etc. that the item technology carried out sufficient special experimental study, research and develop the proprietary technology of production electrodeposited cobalt from non-hydrochloric acid electrolyte, and be successfully applied to suitability for industrialized production.
The method of producing electrodeposited cobalt by non-hydrochloric acid electrolyte of the present invention, special character are, comprise following operation
1, produces CoCl
2Solution
1) cobalt raw material input pulverizer is pulverized;
2) grinding machine for grinding processing;
3) fine powder after the grinding drops into oxidation leaching in the leaching vat, must extract preceding solution;
4) remove metal and nonmetallic impurity with chemical process, promptly remove impurity such as calcium, magnesium;
5) solvent extraction:, get CoCl with the extraction agent extraction
2Solution;
6) adopt the resins exchange removal of impurities, carry out deep purifying.
2, abstraction and type-reverting
CoCl
2Solution is after extraction agent separates nickel, cobalt Co, and cobalt is still with CoCl
2Form exists, and in order to guarantee the environmental quality of electrolytic deposition process, it must be made the transition to non-hydrochloric acid system, and processing method adopts abstraction and type-reverting; Use the P507 extraction agent, it has the big advantage of saturated capacity; Can be with CoCl
2Collection is gone into its organic phase; Select 2.5N H again
2SO
4With the cobalt back extraction, can obtain cobalt sulfate solution.
3, dechlorination
Cl anion is stayed aqueous phase in extraction process, gone out groove for fear of appearance in extraction process by mechanical entrapment, and adopt 1.2N H
2SO
4Be washing composition, in extraction box, the cobalt organic phase of carrying before the back extraction advanced the multi-stage countercurrent washing, fully wash-out carry in the cobalt organic phase with Cl
-, make CoSO after the back extraction
4Solution is chloride to reach electrodeposition safety in production requirement.
4, physical method is removed organism
Through washing the CoSO of chlorine after transition
4Solution contains band with suspension, emulsification and dissolve the organism that three kinds of states exist.In order to eliminate the harm that organism is produced the cobalt electrodeposition.Adopt ultrasonic degreasing technique to carry out fluid and separate, make to contain organic solution, through ultrasonic dehydration, oil in water emulsion forms thin oil droplet and is dispersed in the cobalt liquor.In solution, dissolve in air then.Dissolve in the tiny oil droplet of gas and dispersive and be combined into the steam bubble of density less than solution.Come out and break away from solution by gravity separation, remove the solution behind the oil in water emulsion,, grain is removed through littler dissolving oil absorption through fibrous nodules, fiber yarn absorption.Make the cobalt liquor organic content reach the production requirement of cobalt electrodeposition.
5, cobalt electrolytic solution preparation
Through the cobalt sulfate solution of ultrasonic oil removing, major ingredient is Co55-65gL
-1Cl
-＜0.1gL
-1), through adjusting PH, add additive boric acid (tensio-active agent), perchloro-butyl sulphur is washed amine salt FC-1100 (acid fog inhibitor), be warming up to 55-65 ℃ after, flow into electrolyzer through header tank continuously.
Major ingredient Co:55-65g/l in the cobalt electrolytic solution, Cl
-≤ 0.1g/l import and has installed in the electrolyzer of cathode and anode through adding additive, acid fog inhibitor, adjustment pH value, the back of heating up, and constantly circulates and heat up and adjust pH value to make after parameters stablizes, and the connection direct supply carries out the electrodeposition production process of cobalt.
6, electrodeposited cobalt production
The electrolytic solution for preparing continuously flows into the electrolyzer that installs cathode and anode, after every processing parameter is stable, connects direct supply and carries out the electrodeposition production of cobalt, and the electrodeposition production of cobalt divides two portion's steps to finish.
1) starting sheet is made; To plant plate and insert in the electrolyzer, Co in the electrolytic solution of energising back
++Separate out on kind of a plate (negative electrode) surface,, plant plate and go out groove when thickness reaches 0.3-0.5mm.
2) carry out starting sheet and peel off, penetrate current conducting rod after acidleach is handled and continue,, carry out electrodeposition as negative electrode into groove; After direct supply was connected, electric current caused electrode generation chemical transformation by non-electrolysis of hydrochloric acid liquid, and the yin, yang ion moves to the two poles of the earth respectively in the electrolytic solution, and had produced oxidation, reduction reaction because of electron exchange occurs; Electrodeposition is to negative electrode thickness 3-10mm, and product goes out groove, finishes electrodeposited cobalt production (relevant electrodeposition parameter is attached).
In order to keep the concentration of cobalt ion in the electrolytic deposition process, guarantee that electrodeposition carries out smoothly, need to add new electrolytic solution continuously and replenish cobalt ion.Therefore, must accurately carry out the balance of electrolytic deposition process liquor capacity and metal concentration continuously, produce unusual fluctuations to prevent liquor capacity or concentration of metal ions; Simultaneously, because the anodic reaction process has O
2Separate out, cause H+ concentration increase (acidity raising) in the solution; Therefore, before entering new circulation, antianode liquid will carry out the pH value adjustment.
The new electrolytic solution that replenishes mixes with the anolyte process behind the adjustment PH, pumps into high-order circulation groove again, after rising to certain temperature, relies on the header tank potential difference, and the speed of separating out of pressing the electrolytic deposition process cobalt evenly replenishes electrolytic solution continuously around every negative electrode.
The cobalt electrodeposition is decided negative electrode after the production cycle to giving, and can cut off the electricity supply and lifts out groove; The electrodeposited cobalt product can be put in storage for sale after scalding and checking.
The present invention adds acid fog inhibitor FC-1100 in electrolytic solution, the electrolyte surface expansive force is reduced, and the anode precipitated oxygen passes liquid level smoothly, has avoided bringing acid into production scene.Effectively improved Working environment and prevented pollution surrounding enviroment.
The method of producing electrodeposited cobalt by non-hydrochloric acid electrolyte of the present invention is owing to adopt solution to make the transition, wash chlorine technology, (Cl in the electrolytic solution
-) be lower than 0.1gl
-1, in electrolytic deposition process, reach no chlorine substantially and separate out requirement.
Four, description of drawings
Fig. 1: be the method process flow sheet of embodiment of the invention producing electrodeposited cobalt by non-hydrochloric acid electrolyte.
Five, embodiment
Followingly provide the specific embodiment of the present invention with reference to accompanying drawing 1, the invention will be further described.
Embodiment
The method of the producing electrodeposited cobalt by non-hydrochloric acid electrolyte of present embodiment mainly comprises following operation
1) cobalt raw material input pulverizer is pulverized;
2) grinding machine for grinding processing;
3) fine powder after the grinding drops into oxidation leaching in the leaching vat, must extract preceding solution;
4) remove metal and nonmetallic impurity with chemical process, remove impurity such as calcium, magnesium;
5) solvent extraction:, get CoCl with the extraction of P204 extraction agent
2Solution;
6) adopt the resins exchange removal of impurities, carry out deep purifying.
7) abstraction and type-reverting
CoCl
2Solution is after extraction agent P507 separates nickel, cobalt Co, and cobalt is still with CoCl
2Form exists, and in order to guarantee the environmental quality of electrolytic deposition process, it must be made the transition to non-hydrochloric acid system, and method adopts abstraction and type-reverting.With CoCl
2Collection is gone into organic phase, and method is selected 2.5N H
2SO
4With the cobalt back extraction, can obtain cobalt sulfate solution.
8) dechlorination
Cl anion is stayed aqueous phase in extraction process, for fear of being entrained with liquid level by mechanical movement, adopt 1.2N H
2SO
4As washing composition, in extraction box, the cobalt organic phase of carrying before the back extraction is advanced the multi-stage countercurrent washing, fully wash-out carries the Cl that is had in the cobalt organic phase
-, make the CoSO after the back extraction
4The solution chlorinity is removed low and is satisfied the electrodeposition production requirement.
9) physical method is removed organism
Through washing the CoSO of chlorine after transition
4Solution contains suspension, emulsification and dissolves the organism that three kinds of states exist.In order to eliminate the harm that organism is produced the cobalt electrodeposition.Adopt ultrasonic degreasing technique to carry out fluid and separate, contain organic solution, through ultrasonic dehydration, oil in water emulsion forms thin oil droplet and is dispersed in the cobalt liquor.In solution, dissolve in air then.Dissolve in the tiny oil droplet of gas and dispersive and be combined into the steam bubble of density less than solution.Come out and break away from solution by gravity separation, remove the solution behind the oil in water emulsion,, grain is removed through littler dissolving oil absorption through fibrous nodules, fiber yarn absorption.Make the cobalt liquor organic content reach the production requirement of cobalt electrodeposition.
10) cobalt electrolytic solution preparation
Through the cobalt sulfate solution of ultrasonic oil removing, major ingredient is Co55-65gL
-1Cl-＜0.1gL
-1), through adjusting PH, add additive boric acid (tensio-active agent), perchloro-butyl sulphur is washed amine salt (acid fog inhibitor), be warming up to 55-65 ℃ after, flow into electrolyzer through header tank continuously.
11) electrodeposited cobalt production
Preparation back electrolytic solution continuously flows in the electrolyzer that installs cathode and anode, after every processing parameter is stable, connects direct supply and carries out the electrodeposition production of cobalt, and the electrodeposition production of cobalt divides two portion's steps to finish.
1, starting sheet is made; To plant plate and insert in the electrolyzer, Co in the electrolytic solution of energising back
++ separate out on kind of a plate (negative electrode) surface, when thickness reaches 0.3-0.5mm, plant plate and go out groove.
2, carry out starting sheet and peel off, penetrate current conducting rod after acidleach is handled and continue,, carry out electrodeposition as negative electrode into groove; After direct supply was connected, electric current caused electrode generation chemical transformation by non-electrolysis of hydrochloric acid liquid, and the yin, yang ion moves to the two poles of the earth respectively in the electrolytic solution, and had produced oxidation, reduction reaction because of electron exchange occurs; Electrodeposition is to negative electrode thickness 3-10mm, and product goes out groove, finishes electrodeposited cobalt production (relevant electrodeposition parameter is attached).
The reaction that takes place on negative electrode and anode is as follows:
1) cathodic reaction: Co
+++ 2e---Co
2) anodic reaction: 4OH
--2e---O
2↑+2H
2O
More than reaction makes electric energy change the chemical energy of producing the electrodeposition product into.
In order to keep the concentration of cobalt ion in the electrolytic deposition process, guarantee that electrodeposition carries out smoothly, need to add new electrolytic solution continuously and replenish cobalt ion.Therefore, must accurately carry out the balance of electrolytic deposition process liquor capacity and metal concentration continuously, produce unusual fluctuations to prevent liquor capacity or concentration of metal ions; Simultaneously, because the anodic reaction process has O
2Separate out, cause H+ concentration increase (acidity raising) in the solution; Therefore, before entering new circulation, antianode liquid will carry out the pH value adjustment.
The new electrolytic solution that replenishes mixes with the anolyte process behind the adjustment PH, pumps into high-order circulation groove again, after rising to certain temperature, relies on the header tank potential difference, and the speed of separating out of pressing the electrolytic deposition process cobalt evenly replenishes electrolytic solution continuously around every negative electrode.
The cobalt electrodeposition is decided negative electrode after the production cycle to giving, and can cut off the electricity supply and lifts out groove; The electrodeposited cobalt product can be put in storage for sale after scalding and checking.
The present invention adds acid fog inhibitor FC-1100 in electrolytic solution, the electrolyte surface expansive force is reduced, and the anode precipitated oxygen passes liquid level smoothly, and the environmental issue of having avoided acid molecule being brought into the production scene takes place.Effectively improved Working environment and prevented pollution surrounding enviroment.
The method of producing electrodeposited cobalt by non-hydrochloric acid electrolyte of the present invention owing to adopt solution to make the transition, wash chlorine technology, makes (Cl in the electrolytic solution
-) be lower than 0.1gl
-1, in electrolytic deposition process, reach no chlorine substantially and separate out requirement.
Main technologic parameters and technical indicator
1, electrolytic solution is formed Co:35-40g/l, Cl
-:≤0.1g/l, additive 1:201 * 7 (series), additive 2:FC-1100;
2, be 100--120mm with pole span; 3, current density is 180-300A/m
2
4, temperature is 30-50 ℃; 5, PH is 1.0-4.0;
6, bath voltage is 3-4.5V; 7, current efficiency is 90--95%;
8, the production cycle is 6-10 days.
Claims (6)
1, the method for producing electrodeposited cobalt by non-hydrochloric acid electrolyte is characterized in that comprising that following operation produces CoCl
2------physical method is removed organism--preparation of cobalt electrolytic solution--electrodeposited cobalt production to abstraction and type-reverting to solution in dechlorination.
2,, it is characterized in that described abstraction and type-reverting is according to the method for the described producing electrodeposited cobalt by non-hydrochloric acid electrolyte of claim 1
CoCl
2Solution is after extraction agent separates nickel, cobalt Co, and cobalt is still with CoCl
2Form exists, and needs it is made the transition to non-hydrochloric acid system, with CoCl
2Collection is gone into organic phase, and method is selected 2.5N H
2SO
4With the cobalt back extraction, obtain cobalt sulfate solution.
3,, it is characterized in that described dechlorination technology is for adopting 1.2N H according to the method for the described producing electrodeposited cobalt by non-hydrochloric acid electrolyte of claim 1
2SO
4Be washing composition, in extraction box, the cobalt organic phase of carrying before the back extraction advanced the multi-stage countercurrent washing, fully wash-out carry in the cobalt organic phase with Cl
-, make CoSO after the back extraction
4The chloride reduction of solution is also satisfied the electrodeposition production requirement.
4,, it is characterized in that described cobalt electrolytic solution is prepared as according to the method for the described producing electrodeposited cobalt by non-hydrochloric acid electrolyte of claim 1
Through the cobalt sulfate solution of ultrasonic oil removing, major ingredient is Co55-65gL
-1Cl
-＜0.1gL
-1, through adjusting PH, add and add tensio-active agent, acid fog inhibitor, be warming up to 55-65 ℃ after, flow into electrolyzer through header tank continuously.
5,, it is characterized in that described electrodeposited cobalt production is according to the method for the described producing electrodeposited cobalt by non-hydrochloric acid electrolyte of claim 1
The electrolytic solution of preparation continuously flows into the electrolyzer that installs cathode and anode, after every processing parameter is stable, connects direct supply and carries out the electrodeposition production of cobalt.
6, according to the method for the described producing electrodeposited cobalt by non-hydrochloric acid electrolyte of claim 5, it is characterized in that
For keeping the concentration of cobalt ion in the electrolytic deposition process, need to add new electrolytic solution continuously and replenish cobalt ion; Before entering new circulation, antianode liquid will carry out the pH value adjustment; The new electrolytic solution that replenishes mixes with the anolyte process behind the adjustment PH, pumps into high-order circulation groove again, after rising to certain temperature, relies on the header tank potential difference, and the speed of separating out of pressing the electrolytic deposition process cobalt evenly replenishes electrolytic solution continuously around every negative electrode.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101831547A (en) * | 2010-05-26 | 2010-09-15 | 江苏凯力克钴业股份有限公司 | Method for purifying cobalt solution |
| CN102206761A (en) * | 2010-03-29 | 2011-10-05 | 北京品一材料科技有限责任公司 | Production method of high purity cobalt |
| CN102330111A (en) * | 2011-09-22 | 2012-01-25 | 浙江华友钴业股份有限公司 | Method for preparing electric deposited cobalt |
| CN102797019A (en) * | 2011-05-25 | 2012-11-28 | 南通新玮镍钴科技发展有限公司 | Method for preparing micro spheroidal metallic cobalt powder |
| CN102943177A (en) * | 2012-10-29 | 2013-02-27 | 浙江特力再生资源有限公司 | Method for recovering cooper and silicon powder from organosilicon waste residue |
| CN103409772A (en) * | 2013-08-13 | 2013-11-27 | 四川省尼科国润新材料有限公司 | Enclosed frame-type circulatory system apparatus for electrodeposition nickel or electrodeposition cobalt electrolyte |
| CN103958416A (en) * | 2011-12-26 | 2014-07-30 | 住友金属矿山株式会社 | Method for producing cobalt sulfate |
| CN105935779A (en) * | 2016-06-22 | 2016-09-14 | 荆门市格林美新材料有限公司 | Cobalt powder preparing method |
| CN106835194A (en) * | 2017-01-12 | 2017-06-13 | 江苏凯力克钴业股份有限公司 | A kind of cobalt chloride electrodeposition process |
| CN107815540A (en) * | 2017-12-13 | 2018-03-20 | 栗秀臣 | A kind of method of hydrometallurgy metal nickel cobalt and its salt product |
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2009
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| CN103409772A (en) * | 2013-08-13 | 2013-11-27 | 四川省尼科国润新材料有限公司 | Enclosed frame-type circulatory system apparatus for electrodeposition nickel or electrodeposition cobalt electrolyte |
| CN103409772B (en) * | 2013-08-13 | 2017-07-21 | 四川省尼科国润新材料有限公司 | A kind of circulating system device of closed frame electro deposited nickel or electrodeposited cobalt electrolyte |
| CN105935779A (en) * | 2016-06-22 | 2016-09-14 | 荆门市格林美新材料有限公司 | Cobalt powder preparing method |
| CN106835194A (en) * | 2017-01-12 | 2017-06-13 | 江苏凯力克钴业股份有限公司 | A kind of cobalt chloride electrodeposition process |
| CN107815540A (en) * | 2017-12-13 | 2018-03-20 | 栗秀臣 | A kind of method of hydrometallurgy metal nickel cobalt and its salt product |
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| CN101532095B (en) | 2010-06-30 |
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