CN108118151B - 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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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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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)3The liquid phase is Mn-removed2+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 invention relates to a method for removing Mn in cobalt sulfate solution by controlling potential oxidation2+Belonging to the technical field of wet metallurgy.
Background
CoSO4·7H2The O product has wide application in industry and is used as a paint drier in the coating industry. The ceramic industry is used as a colored porcelain glaze. The chemical industry is used to make cobalt-containing pigments and as a raw material for the production of various cobalt salts. The battery industry is used as an additive to alkaline batteries and lithopone. In addition, the method can also be used for electroplating cobalt, preparing storage batteries, cobalt pigments, ceramics, enamels and glaze colors, and used as catalysts, foam stabilizers, driers and the like.
Because of the shortage of cobalt earth ore at home and abroad, the developed and utilized cobalt resource is very little, most of cobalt metal is associated in other metal minerals and is produced in the form of cobalt slag enrichment in the process of extracting main metal, and domestic cobalt smelting production raw materials are mainly from secondary cobalt precipitation slag of metal minerals with high cobalt content. The crude cobalt sulfate solution obtained by leaching the cobalt slag through sulfuric acid often has high content of metal impurities, and if the cobalt sulfate solution is not subjected to pre-impurity removal treatment, the cobalt sulfate solution directly enters P204 for extraction and impurity removal, so that the P204 load is too large, the operation cost is high, and meanwhile, the extraction capacity of the P204 is influenced, particularly Mn2+The cobalt sulfate solution with high content directly enters a P204 extraction system, the influence on the extraction capacity of the P204 is very obvious, the metal impurities in the purified cobalt sulfate solution exceed the standard, and the produced product is unqualified, so that the Mn in the crude cobalt sulfate solution is treated before the purified cobalt sulfate solution enters the P204 extraction system2+It is necessary to perform preliminary removal.
Mn in the sulfuric acid system most frequently used in industry2+The removing method comprises the steps of adopting potassium permanganate and H2O2Removing Mn by oxidizing with equal oxidant2+The oxidability of potassium permanganate is too strong and is not easy to control in the oxidation reaction process, and Mn is oxidized2+While adding Co2+Also largely oxidized, the cobalt loss is too high, MnO in slag is removed by oxidation2And Co (OH)3Too high to be sold or recycled. Adding H2O2The consumption of the oxidation demanganization is too large, the cost is too high, and the cobalt sulfate solution can be diluted at the same time, which is not beneficial to the subsequent process production.
Disclosure of Invention
The inventionAims to overcome the problem of removing Mn by oxidation in the crude cobalt sulfate solution2+The prior art has the defects that the prior art provides a method for removing Mn in a cobalt sulfate solution by controlling potential oxidation2+Can increase Mn2+Removal rate of and reduction of Co2+The loss rate of the Mn-free catalyst is reduced, the load of P204 extraction in the subsequent working procedure is reduced, the extraction cost of P204 is reduced, and Mn is removed by oxidation2+The process achieves the effect of no waste residue and waste liquid discharge, and is green, environment-friendly and zero-emission.
The invention provides a method for removing Mn in cobalt sulfate solution by controlling potential oxidation2+Method from S2O8 2--H2The O is E-pH diagram showing S2O8 2-Has an oxidation-reduction potential of 2.08V, so that metal ions having an oxidation-reduction potential of less than 2.08V can be oxidized by S2O8 2-And (4) oxidizing. From Me-H2The E-pH diagram of O is shown, Mn2+，Co2+The maximum potential of the oxide is about 1.3V and 1.8V respectively; mn2+Oxidation to MnO2The lowest oxidation potential of the catalyst is 0.4V, and the invention makes full use of Na2S2O8(2.08V)，Mn2+(1.3V)，Co2+(1.8V) difference in maximum Redox potential in aqueous solution, CoSO4Potential and pH of the solution with Na2S2O8Oxidation for removing Mn in cobalt sulfate solution2+. The method comprises the following specific steps: selection of Na2S2O8As an oxidizing agent, crude CoSO was continuously stirred4The solution is always kept at pH 5.0-5.5, temperature 55-60 ℃ and oxidation potential 0.4-1.3V, Na is added at constant speed in sections2S2O8Solution, 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)3The liquid phase is Mn-removed2+After CoSO4And (3) solution.
The solid phase contains MnO2And Co (OH)3By oxidation of manganeseThe slag demanganization slag is used as an oxidant in the process of oxidizing and deironing the electrolytic nickel system or sold as manganese concentrate; the liquid phase enters a P204 extraction system to carry out deep extraction and separation on trace metal impurities in the solution, and then Ni and Co are extracted and separated through P507 to obtain pure cobalt sulfate solution for producing CoSO4·7H2O products or electrocobalts; crude CoSO obtained4Mn in solution2+The removal rate of (1) was 99.5%, Co2+The loss rate of (A) can be controlled within 5%.
Crude CoSO in said step4Mn in solution2+The concentration is 0.4-5 g/L.
Crude CoSO in said step4Co in solution2+The concentration is 55-60 g/L.
Crude CoSO in said step4The pH of the solution was adjusted to 5% by sodium hydroxide solution. The sodium hydroxide solution is prepared by adopting industrial-grade sodium hydroxide with the NaOH content of 96 percent.
The rotating speed of stirring in the step is 250-300 r/min.
In said step Na2S2O8The concentration of (A) is 0.1 mol/L; the Na is2S2O8The solution adopts Na2S2O8Technical grade Na with content of 99%2S2O8And (4) preparing.
The reaction time in said step is preferably 1 h.
The invention adopts Na for controlling solution potential2S2O8Oxidation for removing Mn in cobalt sulfate solution2+The method has no acid mist pollution to the operation environment, and can improve Mn2+Removal rate of and reduction of Co2+While reducing the load of P204 extraction in the subsequent step, reducing the cost of P204 extraction, and containing MnO2And Co (OH)3The manganese-removing slag can be recycled as an oxidant in the process of oxidizing and removing iron in an electrolytic nickel system, or can be sold as manganese concentrate. The method has the advantages of practicability, simple process and easy operation and control, and can realize the oxidation removal of Mn while reducing the production cost2+The process has no waste residue and waste liquid discharge effect, is green and environment-friendly, and has zero dischargeDischarge, has the advantages of high efficiency, environmental protection and strong practicability.
Drawings
FIG. 1 is a schematic view of a process flow for purifying a crude cobalt sulfate solution in example 1 of the present invention;
FIG. 2 shows the removal of Mn from cobalt sulfate solution according to the present invention2+And (4) an oxidation test device.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
In the embodiment of the invention, the oxidation potential of the rough cobaltous sulfate solution is controlled to be 0.4-1.3V;
the crude cobalt sulfate solution in the embodiment of the invention is obtained by leaching cobalt hydroxide slag produced by certain nickel production enterprises in Yunnan with 60g/L industrial sulfuric acid, wherein the concentration of cobalt is 55-60 g/L.
The sodium hydroxide solution adopted in the embodiment of the invention is commercial industrial sodium hydroxide, and the solution prepared by industrial sodium hydroxide with the NaOH content of 96 percent is adopted.
Na used in the examples of the present invention2S2O8The solution is commercial industrial Na2S2O8By using Na2S2O8Technical grade Na with content of 99%2S2O8And (4) preparing a solution.
Crude CoSO used in the examples of the invention4Mn in solution2+The content is 0.4-5 g/L;
in the embodiment of the invention, the rotating speed of the DF-1 constant-temperature magnetic stirrer in the reaction process is 250-300 r/min
In the embodiment of the invention, the reaction time is 0.5-1 h;
in the embodiment of the invention, the reaction temperature is 55-60 ℃;
examples of the present invention Na2S2O8The amount of oxidant added is controlled to crude CoSO4Mn in solution2+3.5 to 4 times of the theoretical molar content.
Example 1:
as shown in FIGS. 1 and 2, using Na2S2O8(2.08V)，Mn2+(1.3V)，Co2+(1.8V) difference in maximum Redox potential in aqueous solution, CoSO4Potential and pH of the solution with Na2S2O8Oxidation for removing Mn in cobalt sulfate solution2+Extracting the demanganized cobalt sulfate solution by P204 to separate trace metal impurities in the solution, and extracting and separating Ni and Co by P507 to obtain pure cobalt sulfate solution for producing CoSO4·7H2O products or cobalt carbide; the main component of the oxidation precipitation slag is MnO2And Co (OH)3The method can be used as an oxidant for recycling in an oxidation iron removal process of an electro-nickel hydrometallurgy system, or can be sold as manganese slag, and the method comprises the following specific steps:
(1) will contain Co2+：55g/L，Mn2+: adding 0.4g/L of crude cobalt sulfate solution into a beaker, adding sodium hydroxide solution to adjust the pH value of the solution to 5.0-5.5, starting a DF-1 constant-temperature magnetic stirrer in the adding process at the rotating speed of 250r/min, and starting a water bath kettle to heat to 60 ℃;
(2) using 0.1mol/L Na2S2O8Starting an oxidation-reduction potential tester as an oxidant, controlling the oxidation potential within the range of 0.4-1.3V, and adding Na into the crude cobalt sulfate solution at a constant speed in a segmented manner according to the potential change condition2S2O8The oxidant pays attention to the change condition of the pH value of the solution at any time in the reaction process, and the pH value is ensured to be between 5.0 and 5.5, and Na is contained2S2O8The amount of oxidant added is controlled to crude CoSO4Mn in solution2+3.5 times the theoretical molar content, a reaction time of 1h, during which step crude CoSO was obtained4Mn in solution2+The removal rate of (C) was 99.2%, Co2+The loss rate of (A) can be controlled to be 4.1%;
(3) removing Mn from the oxide in the step (2)2+The liquid is filtered for liquid-solid separation, and Mn is removed from the liquid phase2+The latter solution enters the next stage of P204 extraction process to carry out deep extraction and impurity removal on the residual trace metal impurities in the solution; the solid phase is MnO-containing2And Co (OH)3Removing manganese slag.
Example 2:
by using Na2S2O8(2.08V)，Mn2+(1.3V)，Co2+(1.8V) difference in maximum Redox potential in aqueous solution, CoSO4Potential and pH of the solution with Na2S2O8Oxidation for removing Mn in cobalt sulfate solution2+Extracting the demanganized cobalt sulfate solution by P204 to separate trace metal impurities in the solution, and extracting and separating Ni and Co by P507 to obtain pure cobalt sulfate solution for producing CoSO4·7H2O products or cobalt carbide; the main component of the oxidation precipitation slag is MnO2And Co (OH)3The method can be used as an oxidant for recycling in an oxidation iron removal process of an electro-nickel hydrometallurgy system, or can be sold as manganese slag, and the method comprises the following specific steps:
(1) will contain Co2+：57g/L，Mn2+: 2.2g/L of crude cobalt sulfate solution is added into a beaker, sodium hydroxide solution is added to adjust the pH value of the solution to be between 5.0 and 5.5, a DF-1 constant-temperature magnetic stirrer is started in the adding process, the rotating speed is 260r/min, and a water bath kettle is started to heat to 60 ℃;
(2) using 0.1mol/L Na2S2O8Starting an oxidation-reduction potential tester as an oxidant, controlling the oxidation potential within the range of 0.4-1.3V, and adding Na into the crude cobalt sulfate solution at a constant speed in a segmented manner according to the potential change condition2S2O8The oxidant pays attention to the change condition of the pH value of the solution at any time in the reaction process, and the pH value is ensured to be between 5.0 and 5.5, and Na is contained2S2O8The amount of oxidant added is controlled to crude CoSO4Mn in solution2+3.8 times the theoretical molar content, a reaction time of 1h, during which step crude CoSO was obtained4Mn in solution2+The removal rate of (1) was 99.4%, Co2+The loss rate of (A) can be controlled to be 4.3%;
(3) removing Mn from the oxide in the step (2)2+The liquid is filtered for liquid-solid separation, and Mn is removed from the liquid phase2+The latter liquid enters the next stage of P204 extraction process to remove the residual trace metal impurities in the solutionCarrying out deep extraction and impurity removal; the solid phase is MnO-containing2And Co (OH)3Removing manganese slag.
Example 3:
by using Na2S2O8(2.08V)，Mn2+(1.3V)，Co2+(1.8V) difference in maximum Redox potential in aqueous solution, CoSO4Potential and pH of the solution with Na2S2O8Oxidation for removing Mn in cobalt sulfate solution2+Extracting the demanganized cobalt sulfate solution by P204 to separate trace metal impurities in the solution, and extracting and separating Ni and Co by P507 to obtain pure cobalt sulfate solution for producing CoSO4·7H2O products or cobalt carbide; the main component of the oxidation precipitation slag is MnO2And Co (OH)3The method can be used as an oxidant for recycling in an oxidation iron removal process of an electro-nickel hydrometallurgy system, or can be sold as manganese slag, and the method comprises the following specific steps:
(1) will contain Co2+：60g/L，Mn2+: adding 5.0g/L of crude cobalt sulfate solution into a beaker, adding sodium hydroxide solution to adjust the pH value of the solution to 5.0-5.5, starting a DF-1 constant-temperature magnetic stirrer in the adding process at the rotating speed of 300r/min, and starting a water bath kettle to heat to 58 ℃;
(2) using 0.1mol/L Na2S2O8Starting an oxidation-reduction potential tester as an oxidant, controlling the oxidation potential within the range of 0.4-1.3V, and adding Na into the crude cobalt sulfate solution at a constant speed in a segmented manner according to the potential change condition2S2O8The oxidant pays attention to the change condition of the pH value of the solution at any time in the reaction process, and the pH value is ensured to be between 5.0 and 5.5, and Na is contained2S2O8The amount of oxidant added is controlled to crude CoSO4Mn in solution2+4 times the theoretical molar content, a reaction time of 1h, during which the crude CoSO is obtained4Mn in solution2+The removal rate of (1) was 99.5%, Co2+The loss rate of (A) can be controlled to be 4.8%;
(3) removing Mn from the oxide in the step (2)2+Filtering the liquid to separate liquid from solid, and removing the liquid from the liquidMn2+The latter solution enters the next stage of P204 extraction process to carry out deep extraction and impurity removal on the residual trace metal impurities in the solution; the solid phase is MnO-containing2And Co (OH)3Removing manganese slag.
Example 4:
by using Na2S2O8(2.08V)，Mn2+(1.3V)，Co2+(1.8V) difference in maximum Redox potential in aqueous solution, CoSO4Potential and pH of the solution with Na2S2O8Oxidation for removing Mn in cobalt sulfate solution2+Extracting the demanganized cobalt sulfate solution by P204 to separate trace metal impurities in the solution, and extracting and separating Ni and Co by P507 to obtain pure cobalt sulfate solution for producing CoSO4·7H2O products or cobalt carbide; the main component of the oxidation precipitation slag is MnO2And Co (OH)3The method can be used as an oxidant for recycling in an oxidation iron removal process of an electro-nickel hydrometallurgy system, or can be sold as manganese slag, and the method comprises the following specific steps:
(1) will contain Co2+：56g/L，Mn2+: adding 0.8g/L crude cobalt sulfate solution into a beaker, adding sodium hydroxide solution to adjust the pH value of the solution to 5.0-5.5, starting a DF-1 constant-temperature magnetic stirrer in the adding process at the rotating speed of 250r/min, and starting a water bath kettle to heat to 55 ℃;
(2) using 0.1mol/L Na2S2O8Starting an oxidation-reduction potential tester as an oxidant, controlling the oxidation potential within the range of 0.4-1.3V, and adding Na into the crude cobalt sulfate solution at a constant speed in a segmented manner according to the potential change condition2S2O8The oxidant pays attention to the change condition of the pH value of the solution at any time in the reaction process, and the pH value is ensured to be between 5.0 and 5.5, and Na is contained2S2O8The amount of oxidant added is controlled to crude CoSO4Mn in solution2+3.5 times the theoretical molar content, a reaction time of 1h, during which step crude CoSO was obtained4Mn in solution2+The removal rate of (C) was 99.3%, Co2+The loss rate of (A) can be controlled to be 4.6%;
(3) removing Mn from the oxide in the step (2)2+The liquid is filtered for liquid-solid separation, and Mn is removed from the liquid phase2+The latter solution enters the next stage of P204 extraction process to carry out deep extraction and impurity removal on the residual trace metal impurities in the solution; the solid phase is MnO-containing2And Co (OH)3Removing manganese slag.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (5)
1. Potential-controlled oxidation removal of Mn in cobalt sulfate solution2+The method is characterized by the specific steps
The method comprises the following steps: 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)3The liquid phase is Mn-removed2+After CoSO4A solution; crude CoSO4Mn in solution2+The concentration is 0.4-5 g/L, Co2+The concentration is 55-60 g/L.
2. The method of claim 1 for the removal of Mn from a cobalt sulfate solution by controlled potential oxidation2+The method of (2), characterized by: in said step Na2S2O8The concentration of the solution was controlled at 0.1 mol/L.
3. The method of claim 1 for the removal of Mn from a cobalt sulfate solution by controlled potential oxidation2+The method of (2), characterized by: crude CoSO in said step4The pH value of the solution is adjusted by sodium hydroxideThe solution was adjusted to a concentration of 5%.
4. The method of claim 1 for the removal of Mn from a cobalt sulfate solution by controlled potential oxidation2+The method of (2), characterized by: in the step, the stirring speed in the reaction process is controlled to be 250-300 r/min.
5. The method of claim 1 for the removal of Mn from a cobalt sulfate solution by controlled potential oxidation2+The method of (2), characterized by: the reaction time in the step is controlled to be 1 h.
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| WO2004009232A1 (en) * | 2002-06-11 | 2004-01-29 | Enviroscrub Technologies Corporation | Disassociation processing of metal oxides |
| CN101974691A (en) * | 2010-11-10 | 2011-02-16 | 白银有色集团股份有限公司 | Method for recovering cobalt in cobalt-containing waste residues from zinc smelting |
| CN103088215A (en) * | 2012-10-16 | 2013-05-08 | 赣州市豪鹏科技有限公司 | Method for separating nickel-cobalt and manganese in nickel-cobalt-manganese material with high manganese-cobalt ratio |
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| WO2004009232A1 (en) * | 2002-06-11 | 2004-01-29 | Enviroscrub Technologies Corporation | Disassociation processing of metal oxides |
| CN101974691A (en) * | 2010-11-10 | 2011-02-16 | 白银有色集团股份有限公司 | Method for recovering cobalt in cobalt-containing waste residues from zinc smelting |
| CN103088215A (en) * | 2012-10-16 | 2013-05-08 | 赣州市豪鹏科技有限公司 | Method for separating nickel-cobalt and manganese in nickel-cobalt-manganese material with high manganese-cobalt ratio |
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