CN113897499A - Method for removing iron by cobalt solution goethite method - Google Patents
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- CN113897499A CN113897499A CN202111183390.7A CN202111183390A CN113897499A CN 113897499 A CN113897499 A CN 113897499A CN 202111183390 A CN202111183390 A CN 202111183390A CN 113897499 A CN113897499 A CN 113897499A
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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
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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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- 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 iron by a cobalt solution goethite method, which comprises the following steps: the method comprises the steps of adding pure water into a first reaction kettle to serve as base liquid, and enabling the amount of the pure water to be based on that the pure water just submerges a first stirring paddle of the reaction kettle and starts stirring to fully stir the base liquid; heating the solution in the kettle to 55-70 ℃, starting stirring, adding a cobalt solution and a nickel solution in a dispersing manner, oxidizing by using chlorine to remove cobalt materials, and adjusting the pH value to 2.0-2.5 by using a neutralizing agent A; adding the slurry into a second reaction kettle by using a disperser when the slurry in the first reaction kettle reaches 65-75% of the liquid level of the reaction kettle, and simultaneously adding a neutralizer B, and adjusting the pH value of the system to 3.0-3.5; thirdly, when the slurry in the second reaction kettle reaches 65-75% of the liquid level of the reaction kettle, enabling the slurry to flow into the third reaction kettle for goethite iron removal aging reaction, and after the reaction is finished, carrying out solid-liquid separation to respectively obtain the cobalt solution and goethite slag after iron removal. The invention is simple and efficient and has low cost.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for removing iron by a cobalt solution goethite method.
Background
The cobalt solution goethite method has the advantages of less iron slag removal amount, good slag filtering performance and low slag carried metal. The traditional goethite method iron removal of the cobalt solution adopts a method of taking sodium hypochlorite, sodium chlorate, oxygen or air and the like as oxidants to oxidize iron, the cost of the sodium chlorate, the oxygen and other oxidants is high, the air oxidation rate is low, a large amount of alkalis are required to be added in the iron removal process of the goethite method to neutralize acid generated during the formation of goethite, the cost of sodium hydroxide, sodium carbonate and the like is high, the calcium alkalis are low in price but slow in dissolution speed, a sulfuric acid system generates a large amount of calcium sulfate precipitates, and the recovery rate of valuable metals is low due to the fact that slag carries valuable metals; the burden of slag filtration and washing is large, and the labor intensity is high. Therefore, the use of a large amount of oxidant and neutralizer in the goethite process iron removal leads to high iron removal cost or large slag amount and high loss of valuable metals. Therefore, each method has the disadvantages of long process and high cost.
Because the nickel ore is associated with the cobalt ore, the nickel solution generally contains a small amount of element cobalt, and in order to recover the cobalt, the cobalt is generally extracted after the cobalt is enriched in nickel metallurgy. Usually, the method for removing cobalt from a small amount of cobalt contained in the nickel solution by using chlorine gas to oxidize Co2+Preferential oxidation to Co3+And Co is reacted with3+Hydrolysis to form poorly soluble Co (OH)3Precipitating to achieve the aim of removing cobalt. The conventional material treatment method is reduction acid leaching, and a reducing agent and acid are added in the leaching process; and the material is usually used as a cobalt raw material to extract valuable metals nickel and cobalt in the material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a simple and efficient method for removing iron by using a cobalt solution goethite method with low cost.
In order to solve the problems, the method for removing iron by the cobalt solution goethite method comprises the following steps:
the method comprises the steps of adding pure water into a first reaction kettle to serve as base liquid, and enabling the amount of the pure water to be based on that the pure water just submerges a first stirring paddle of the reaction kettle and starts stirring to fully stir the base liquid; heating the solution in the kettle to 55-70 ℃, starting stirring at the stirring frequency of 50-100 Hz, dispersedly adding a cobalt solution and a nickel solution, removing cobalt materials by chlorine oxidation, keeping the content of free iron ions in the kettle to be less than 1g/L by the flow of the cobalt solution, and adjusting the pH value to 2.0-2.5 by using a neutralizing agent A; the flow of the cobalt-removing material by chlorine oxidation of the nickel solution is calculated according to the following formula: m = S × (1.0 to 1.01)59b/(56 × a%), wherein: m is the flow of the cobalt-removing material by the oxidation of the chlorine in the nickel solution, and the unit is kg/min; s is the flow rate of the cobalt solution in unit time, and the unit is L/min; a is the cobalt content in the cobalt-removing material by the chlorine oxidation of the nickel solution, and the unit is; b is the iron content in the cobalt solution, and the unit is g/L; 59 is the atomic weight of cobalt; 56 is the atomic weight of iron;
adding the slurry into a second reaction kettle by using a disperser when the slurry in the first reaction kettle reaches 65-75% of the liquid level of the reaction kettle, and simultaneously adding a neutralizer B into the second reaction kettle by using the disperser in a dispersing way, so as to adjust the pH value of the system to 3.0-3.5;
thirdly, when the slurry in the second reaction kettle reaches 65-75% of the liquid level of the reaction kettle, enabling the slurry to flow into a third reaction kettle for goethite iron removal aging reaction, and after the reaction is finished, carrying out solid-liquid separation to respectively obtain an iron-removed cobalt solution and goethite slag; after the liquid level of the system is stable, the solution enters from the top and goes out from the bottom, or the solution is dispersedly added below the liquid level and enters from the bottom and goes out from the top, so that the continuous iron removal by the goethite method is realized.
The method comprises the step of oxidizing the nickel solution with chlorine gas to remove cobalt, wherein the material mainly containing nickel and cobalt is generated after the cobalt is removed by the nickel solution with the chlorine gas as an oxidant.
The neutralizing agent A in the step refers to one of hydroxide and carbonate of sodium or calcium, or one of sulfuric acid and hydrochloric acid.
The neutralizing agent B in the step II is one of hydroxide and carbonate of sodium or calcium.
The condition of the aging reaction in the step three is that the temperature is 55-70 ℃ and the time is 10-60 min.
Compared with the prior art, the invention has the following advantages:
1. the method takes the cobalt-removing material oxidized by the chlorine in the nickel solution as the oxidant for removing iron by the goethite method in the cobalt solution, and simultaneously the material is alkaline and can also be used as the neutralizer for removing iron by the goethite method, thereby not only saving the treatment process of the material, but also saving the reagent consumption of acid and a reducing agent for treatment, and simultaneously saving the oxidant and the neutralizer for removing iron by goethite.
2. The oxidation-reduction potential of the trivalent cobalt is far higher than that of iron, the oxidizability is strong, the oxidation rate is high, and the utilization rate is high.
3. The iron oxide and iron oxide removal by the traditional goethite method are carried out in a first step, and the pH value is adjusted to generate goethite, two steps are required, while the nickel solution, the chlorine gas oxidation cobalt removal material is used as an oxidant, and the iron oxide and the pH value adjustment to generate the goethite are combined into one step, so that the labor intensity is reduced, the equipment consumption is reduced, the process flow is shortened, the economic cost is reduced, and the aim of reducing the treatment cost is fulfilled.
4. The method uses the material for removing cobalt by oxidizing the chlorine in the nickel solution to remove iron in the cobalt solution, wherein nickel and cobalt do not influence the system, and the method can also improve the concentration of the cobalt solution and improve the treatment efficiency.
Detailed Description
A method for removing iron by a cobalt solution goethite method comprises the following steps:
the method comprises the steps of adding pure water into a first reaction kettle to serve as base liquid, and enabling the amount of the pure water to be based on that the pure water just submerges a first stirring paddle of the reaction kettle and starts stirring to fully stir the base liquid; and then heating the solution in the kettle to 55-70 ℃, starting stirring at the stirring frequency of 50-100 Hz, dispersedly adding a cobalt solution and a nickel solution, removing cobalt materials by chlorine oxidation, keeping the content of free iron ions in the kettle to be less than 1g/L by the flow of the cobalt solution, and adjusting the pH value to 2.0-2.5 by adopting a neutralizing agent A. The cobalt solution is added in a dispersing way by adopting any one of a shower head, a venturi or a dispersion disc; feeding the cobalt-removing material by oxidizing the chlorine gas in the nickel solution by using a vibrating screen, wherein the flow of the cobalt-removing material by oxidizing the chlorine gas in the nickel solution is calculated according to the following formula: m = S × (1.0 to 1.01)59b/(56 × a%), wherein: m is the flow of the cobalt-removing material by the oxidation of the chlorine in the nickel solution, and the unit is kg/min; s is the flow rate of the cobalt solution in unit time, and the unit is L/min; a is the cobalt content in the cobalt-removing material by the chlorine oxidation of the nickel solution, and the unit is; b is the iron content in the cobalt solution, and the unit is g/L; 59 is the atomic weight of cobalt; 56 is the atomic weight of iron.
Wherein: the material for removing cobalt by oxidizing the nickel solution with chlorine gas is the material mainly containing nickel and cobalt generated after the cobalt is removed by using the chlorine gas as an oxidant in the nickel solution.
The neutralizer A is one of hydroxide and carbonate of sodium or calcium, or one of sulfuric acid and hydrochloric acid.
The slurry in the first reaction kettle is added to the second reaction kettle when 65-75% of the liquid level of the reaction kettle is reached, and the neutralizing agent B is added to the second reaction kettle in a dispersing mode through the disperser, so that the pH value of the system is adjusted to 3.0-3.5.
Wherein: the disperser is any one of a shower head, a venturi or a dispersion plate.
The neutralizing agent B is one of hydroxide and carbonate of sodium or calcium.
Thirdly, when the slurry in the second reaction kettle reaches 65-75% of the liquid level of the reaction kettle, enabling the slurry to flow into the third reaction kettle, and carrying out goethite iron removal aging reaction at 55-70 ℃ for 10-60 min. After the reaction is finished, carrying out solid-liquid separation to respectively obtain a cobalt solution after iron removal and goethite slag; after the liquid level of the system is stable, the solution enters from the top and goes out from the bottom, or the solution is dispersedly added below the liquid level and enters from the bottom and goes out from the top, so that the continuous iron removal by the goethite method is realized.
[ working principle ]
The reaction formula of a sulfuric acid system in the iron removal process of the existing goethite method is as follows:
2CoSO4+Cl2+6H2O=2Co(OH)3↓+H2SO4+2HCl （1）
to promote the reaction to the right, nickel carbonate (or Na) is added2CO3) Neutralization of acid produced by hydrolysis reaction:
4H++2HCl+3NiCO3=2Ni2++NiCl2+3H2O+3CO2↑ （2）
combining the two reactions, the total reaction in the cobalt removing process is as follows:
2CoSO4+Cl2+3NiCO3+3H2O=2Co(OH)3↓+2NiSO4+2NiCl2+3CO2↑ （3）
redox equation and potential for cobalt and iron:
Co(OH)3+3H++e= Co2++3H2O E=1.981-0.1774pH （4）
Fe3++e-=Fe2+ 0.771 （5）
the reaction formula of the goethite method iron removal is as follows:
Fe3++2H2O——FeOOH+3H+ （6）
from formula (4), Co3+The potential is 1.803 when the pH =1.0, the potential is 1.626 when the pH =2.0, so that the trivalent cobalt has strong oxidizability, the potential for oxidizing the divalent iron into the trivalent iron is 0.771, and the oxidation-reduction potential of the trivalent cobalt is far higher than that of the iron, so that the oxidation and the alkalinity of the trivalent cobalt are theoretically feasible for oxidizing the iron and precipitating the iron, and the addition amount of the divalent iron oxide of the trivalent cobalt is almost not required to be excessive and is 1.0-1.01 times of the theoretical amount.
The invention adopts nickel solution chlorine gas oxidation cobalt removal materials of Jinchuan company, and the main components are shown in table 1.
TABLE 1 main chemical composition of cobalt removal material by chlorine oxidation of nickel solution
From formula (4) and formula (6), Co3+Oxidation of Fe2+And the acid generated in the iron precipitation process is equal to the consumed acid, if the pH value of the reaction system of the first reaction kettle is increased to 2.5, a small amount of sulfuric acid or hydrochloric acid is added to adjust the acidity of the iron removal system, and if the pH value of the reaction system is lower than 2.0, an alkali is added to adjust the pH value of the system to 2.0-2.5.
If the material for removing cobalt by the oxidation of the chlorine in the nickel solution is not used as a material for removing iron, a reducing agent is added for acid leaching, and a reagent is consumed in the process, so that the process flow is increased, and the process reduces the treatment cost of the nickel-cobalt raw material at the same time, thereby achieving two purposes.
In the following formula, cobalt solution is used as leaching solution of various cobalt raw materials, the cobalt concentration in the leaching solution is 30-80 g/L, and the iron concentration is 1-30 g/L.
Embodiment 1 a method for removing iron from cobalt solution by goethite method, comprising the following steps:
the method comprises the steps that pure water is added into a first reaction kettle and is submerged in a first stirring paddle of the reaction kettle; and then heating the solution in the reaction kettle to 60 ℃, starting stirring, dispersing the cobalt solution into the reaction kettle by using a disperser at the flow rate of 100L/min, wherein the iron concentration is 4.56g/L, dispersing and adding a nickel solution chlorine gas at the speed of 2.388kg/min to oxidize and remove cobalt material ferrous oxide, and slowly adjusting the cobalt solution in the reaction kettle to 2.0-2.5 by using 200g/L sodium hydroxide solution.
The slurry in the first reaction kettle is added into the second reaction kettle at the flow speed of 100L/min when reaching 65% of the liquid level of the reaction kettle, and the sodium hydroxide solution of 200g/L is added into the second reaction kettle in a dispersing mode through the disperser at the flow rate of 10-12L/min, so that the pH value of the system is adjusted to 3.3, and then the pH value is kept.
Thirdly, when the slurry in the second reaction kettle reaches 65% of the liquid level of the reaction kettle, the slurry flows into the third reaction kettle at the flow rate of 100L/min, goethite iron removal aging reaction is carried out at the temperature of 60 ℃, and the reaction time is 30 min. After the liquid level in the reaction kettle reaches 65%, liquid begins to be discharged, solid-liquid separation is carried out, and the cobalt solution and goethite slag after iron removal are respectively obtained; and (4) the liquid after iron removal enters the next working procedure. After the liquid level of the system is stable, the solution enters from the top and goes out from the bottom, or the solution is dispersedly added below the liquid level and enters from the bottom and goes out from the top, so that the continuous iron removal by the goethite method is realized.
The recovery rate of cobalt is 99.74 percent, and the concentration of iron in the cobalt solution is reduced to 0.0015 g/L.
Embodiment 2 a method for removing iron from cobalt solution by goethite method, comprising the following steps:
the method comprises the steps that pure water is added into a first reaction kettle and is submerged in a first stirring paddle of the reaction kettle; and then heating the solution in the reaction kettle to 60 ℃, starting stirring, dispersing the cobalt solution into the reaction kettle at a flow rate of 90L/min by using a disperser, wherein the iron concentration is 4.91g/L, dispersing and adding a nickel solution chlorine gas at a speed of 2.29kg/min to oxidize and remove cobalt material ferrous oxide, and slowly adjusting the pH value of the cobalt solution in the reaction kettle to 2.0-2.5 by using a 200g/L sodium hydroxide solution.
The slurry in the first reaction kettle is added into the second reaction kettle at the flow rate of 90L/min when reaching 70% of the liquid level of the reaction kettle, and the sodium hydroxide solution of 200g/L is added into the second reaction kettle in a dispersing mode through the disperser at the flow rate of 10-12L/min, so that the pH value of the system is adjusted to 3.3, and then the pH value is kept.
Thirdly, when the slurry in the second reaction kettle reaches 70% of the liquid level of the reaction kettle, the slurry flows into the third reaction kettle at the flow rate of 90L/min, goethite iron removal aging reaction is carried out at the temperature of 60 ℃, and the reaction time is 40 min. After the liquid level in the reaction kettle reaches 70%, liquid begins to be discharged, solid-liquid separation is carried out, and the cobalt solution and goethite slag after iron removal are respectively obtained; and (4) the liquid after iron removal enters the next working procedure. After the liquid level of the system is stable, the solution enters from the top and goes out from the bottom, or the solution is dispersedly added below the liquid level and enters from the bottom and goes out from the top, so that the continuous iron removal by the goethite method is realized.
The recovery rate of cobalt is 99.78%, and the concentration of iron in the cobalt solution is reduced to 0.0013 g/L.
Embodiment 3 a method for removing iron from cobalt solution by goethite method, comprising the following steps:
the method comprises the steps that pure water is added into a first reaction kettle and is submerged in a first stirring paddle of the reaction kettle; and then heating the solution in the reaction kettle to 70 ℃, starting stirring, dispersing the cobalt solution into the reaction kettle by using a disperser at the flow rate of 120L/min, wherein the iron concentration is 23.5g/L, simultaneously dispersing and adding a nickel solution chlorine gas at the speed of 14.62g/min to oxidize and remove cobalt material ferrous oxide, and slowly adjusting the pH value of the cobalt solution in the reaction kettle to 2.0-2.5 by using 93% concentrated sulfuric acid.
Adding the slurry into a second reaction kettle at a flow rate of 100L/min by using a disperser when the slurry in the first reaction kettle reaches 70% of the liquid level of the reaction kettle; and (3) adding the cobalt solution subjected to iron removal into the second reaction kettle, heating until the solution temperature in the reaction kettle reaches 70 ℃, adding the cobalt solution into the second reaction kettle by using a disperser at a flow rate of 120L/min, simultaneously adding 200g/L of sodium hydroxide solution into the second reaction kettle by using a disperser at a flow rate of 10-12L/min in a concurrent flow manner, adjusting the pH value of the system to 3.1, and then maintaining the pH value.
Thirdly, when the slurry in the second reaction kettle reaches 70% of the liquid level of the reaction kettle, the slurry flows into the third reaction kettle at the flow rate of 100L/min, goethite iron removal aging reaction is carried out at 70 ℃, and the reaction time is 50 min. After the liquid level in the reaction kettle reaches 70%, liquid begins to be discharged, solid-liquid separation is carried out, and the cobalt solution and goethite slag after iron removal are respectively obtained; and (4) the liquid after iron removal enters the next working procedure. After the liquid level of the system is stable, the solution enters from the top and goes out from the bottom, or the solution is dispersedly added below the liquid level and enters from the bottom and goes out from the top, so that the continuous iron removal by the goethite method is realized.
The recovery rate of cobalt is 99.84%, and the concentration of iron in the leaching solution can be reduced to 0.0010 g/L.
Claims (5)
1. A method for removing iron by a cobalt solution goethite method comprises the following steps:
the method comprises the steps of adding pure water into a first reaction kettle to serve as base liquid, and enabling the amount of the pure water to be based on that the pure water just submerges a first stirring paddle of the reaction kettle and starts stirring to fully stir the base liquid; heating the solution in the kettle to 55-70 ℃, starting stirring at the stirring frequency of 50-100 Hz, dispersedly adding a cobalt solution and a nickel solution, removing cobalt materials by chlorine oxidation, keeping the content of free iron ions in the kettle to be less than 1g/L by the flow of the cobalt solution, and adjusting the pH value to 2.0-2.5 by using a neutralizing agent A; the flow of the cobalt-removing material by chlorine oxidation of the nickel solution is calculated according to the following formula: m = S × (1.0 to 1.01)59b/(56 × a%), wherein: m is the flow of the cobalt-removing material by the oxidation of the chlorine in the nickel solution, and the unit is kg/min; s is the flow rate of the cobalt solution in unit time, and the unit is L/min; a is the cobalt content in the cobalt-removing material by the chlorine oxidation of the nickel solution, and the unit is; b is the iron content in the cobalt solution, and the unit is g/L; 59 is the atomic weight of cobalt; 56 is the atomic weight of iron;
adding the slurry into a second reaction kettle by using a disperser when the slurry in the first reaction kettle reaches 65-75% of the liquid level of the reaction kettle, and simultaneously adding a neutralizer B into the second reaction kettle by using the disperser in a dispersing way, so as to adjust the pH value of the system to 3.0-3.5;
thirdly, when the slurry in the second reaction kettle reaches 65-75% of the liquid level of the reaction kettle, enabling the slurry to flow into a third reaction kettle for goethite iron removal aging reaction, and after the reaction is finished, carrying out solid-liquid separation to respectively obtain an iron-removed cobalt solution and goethite slag; after the liquid level of the system is stable, the solution enters from the top and goes out from the bottom, or the solution is dispersedly added below the liquid level and enters from the bottom and goes out from the top, so that the continuous iron removal by the goethite method is realized.
2. The method for removing iron by goethite with cobalt solution as claimed in claim 1, wherein: the method comprises the step of oxidizing the nickel solution with chlorine gas to remove cobalt, wherein the material mainly containing nickel and cobalt is generated after the cobalt is removed by the nickel solution with the chlorine gas as an oxidant.
3. The method for removing iron by goethite with cobalt solution as claimed in claim 1, wherein: the neutralizing agent A in the step refers to one of hydroxide and carbonate of sodium or calcium, or one of sulfuric acid and hydrochloric acid.
4. The method for removing iron by goethite with cobalt solution as claimed in claim 1, wherein: the neutralizing agent B in the step II is one of hydroxide and carbonate of sodium or calcium.
5. The method for removing iron by goethite with cobalt solution as claimed in claim 1, wherein: the condition of the aging reaction in the step three is that the temperature is 55-70 ℃ and the time is 10-60 min.
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