CN113718115A - Novel iron removal and purification process method for cobalt system - Google Patents
Novel iron removal and purification process method for cobalt system Download PDFInfo
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- 238000006460 hydrolysis reaction Methods 0.000 description 1
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- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a novel iron removal and purification process method for a cobalt system, which comprises the following steps: the method comprises the following steps: dissolving cobalt raw material, heating, adding proper amount of oxidant, and adding Fe into the solution2+Oxidation to Fe3+. Step two: then slowly adding the slurried liquid of the purchased cobalt hydroxide raw material, and adding a sodium carbonate solution after reaction. Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally. Most of the cobalt raw materials used in the invention are purchased cobalt hydroxide powder, and the cobalt raw materials are utilized to replace soda ash for neutralization and iron removal by utilizing the property of the cobalt hydroxide powder that can be synthesized with acidThe sulfuric acid produced in the process can be fully utilized while the consumption of the sodium carbonate is saved, and meanwhile, the process is simple to operate and is very suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of novel iron removal and purification processes of a cobalt system, in particular to a novel iron removal and purification process method of the cobalt system.
Background
Cobalt, element symbol Co, silver-white ferromagnetic metal, the surface of which is silver white with light pink color, is located in 4 th period and VIII group in the periodic table, has an atomic number of 27, an atomic weight of 58.9332, and is a close-packed hexagonal crystal, and the common valence is +2 and + 3. Cobalt is a shiny, steel grey metal, relatively hard and brittle, ferromagnetic, and disappears magnetically when heated to 1150 ℃. It is stable in humid air and does not react with water at normal temperature. When heated to 300 ℃ or higher in air, CoO is generated by oxidation, and when the furnace is in white heat, Co3O4 is generated by combustion. The fine metal cobalt powder prepared by the hydrogen reduction method can spontaneously generate cobalt oxide in the air. Cobalt is an important raw material for producing heat-resistant alloy, hard alloy, anticorrosive alloy, magnetic alloy and various cobalt salts.
Because the raw materials used in the smelting process of cobalt metal are accompanied by more iron impurities which can only be removed in the wet smelting process, most of the raw materials adopt a sodium iron vanadium iron removing and purifying process, in the process, sodium carbonate is mainly used as a neutralizing agent to neutralize sulfuric acid generated in the iron removing process, but the process has large consumption of sodium carbonate, and the generated sulfuric acid is not effectively utilized, so that the iron removing cost is high.
In the prior art, the iron removal cost in the cobalt metal smelting process is high, so a novel iron removal purification process method of a cobalt system needs to be designed to solve the problems.
Disclosure of Invention
The invention aims to provide a novel iron removal and purification process method for a cobalt system, which aims to solve the problem of high iron removal cost in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: dissolving cobalt raw material, heating, adding proper amount of oxidant, and adding Fe into the solution2+Oxidation to Fe3+。
Step two: then slowly adding the slurried liquid of the purchased cobalt hydroxide raw material, and adding a sodium carbonate solution after reaction.
Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
Preferably, in the first step, 500g of the cobalt hydroxide raw material and 2000ml of pure water are weighed, stirred and slurried.
Preferably, in the first step, the cobalt raw material is dissolved and heated to +/-85 ℃, and the cobalt raw material is dissolved and heated by a water bath.
Preferably, the oxidizing agent in the first step is sodium chlorate.
Preferably, the second step comprises 500g of cobalt hydroxide and has a density of about 3.6g/cm for thin-wall cultivation. Melting point 1100-1200 deg.C, and adding 2000ml of pure water, stirring, and stirring to obtain solution with pH of 2.0-2.5.
Preferably, in the second step, the slurried cobalt hydroxide raw material solution is reacted for 4 hours, and the pH value of the sodium carbonate solution is slowly added to 3.0-3.5.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the novel iron removal purification process method for the cobalt system, in the cobalt hydrometallurgy industry, most of used cobalt raw materials are purchased cobalt hydroxide powder, and the cobalt raw materials are utilized to replace sodium carbonate to neutralize sulfuric acid generated in the iron removal process by utilizing the property of the cobalt hydroxide powder, so that the use amount of the sodium carbonate is saved, the sulfuric acid generated in the iron removal process is fully utilized, the content of liquid iron after iron removal is less than 0.05g/L, and the requirement of the iron removal process is met. Meanwhile, the process is simple to operate and is very suitable for industrial production.
Drawings
FIG. 1 is a schematic view of the operation flow structure of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-1, an embodiment of the present invention is shown:
the first embodiment is as follows:
a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: weighing 500g of cobalt hydroxide raw material, stirring 2000ml of pure water to prepare slurry, heating the dissolved cobalt raw material to +/-85 ℃, heating the dissolved cobalt raw material to water bath heating, stably controlling the temperature by using the water bath heating energy, enabling the temperature rise range to be relatively stable, enabling the cobalt raw material to be uniformly heated, adding appropriate amount of sodium chlorate, and adding Fe in the solution2+Oxidation to Fe3+。
Step two: and slowly adding 500g of the slurried cobalt hydroxide raw material purchased from outside, and carrying out high-speed cultivation with the density of about 3.6 g/cm. Melting point 1100-1200 deg.C, adding 2000ml pure water, stirring, reacting for 4 hr, adding sodium carbonate solution, and controlling pH to 3.0-3.5.
Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
Dissolving a purchased cobalt hydroxide raw material in water and sulfuric acid, controlling the pH value to be 1.5-2.0 after dissolving, heating to 85 ℃, adding a proper amount of sodium chlorate, and completely oxidizing Fe2+ in the dissolved solution into Fe3 +; adding a proper amount of water into a purchased cobalt hydroxide raw material to obtain slurry, slowly adding the slurry into oxidized liquid before iron removal, controlling the pH value of the reaction process to be 2.0-2.5, maintaining the reaction temperature, after reacting for 4 hours, stopping adding the purchased cobalt hydroxide slurry if the pH value of the solution does not change obviously, slowly adding soda ash, adjusting the pH value of the solution to be 3.0-3.5, and clarifying or filter-pressing to realize solid-liquid separation, thus finishing the iron removal process.
Example two:
a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: the cobalt-containing waste material method is characterized in that various cobalt-containing waste materials are dissolved by nitric acid and hydrochloric acid, the obtained cobalt chloride solution is purified and deironized by hydrogen peroxide, and sodium carbonate or ammonia water is added when necessary to ensure complete purification. Adding sodium hydroxide into the purified cobalt chloride solution to generate cobalt hydroxide, and then washing and centrifugally separating to obtain a cobalt hydroxide product.
Step two: the sulfate or nitrate of the divalent cobalt reacts with alkali to generate the cobalt hydroxide. 100g of CoSO4 & 7H2O was dissolved in water to form a nearly saturated solution, and a basic solution of 42g of sodium hydroxide in 60mL of water was added with heating and stirring. The precipitation reaction is carried out in a long beaker, which is beneficial to the clarification of the mixed liquid. The precipitate formed initially was blue in color and rapidly turned red when placed on a water bath and heated. After clarification, the precipitate is washed several times by decantation with water, filtered off with suction on a Buchner funnel and washed with water until the wash water is neutral. Finally, drying is carried out in a vacuum drier filled with concentrated H2SO 4.
Step three: reacting metallic cobalt with dilute nitric acid at the temperature of 60-70 ℃, supplementing lost water after the reaction is basically stopped, separating redundant metal, adding CoCO3 to make the solution approach to neutrality, preserving the temperature for 2-3 h at the temperature, and filtering to remove insoluble substances. Then slowly adding 2% ammonia water under the condition of continuously stirring and heating to make the initially formed blue precipitate be promptly changed into purple, then changed into rose-red precipitate. After the reaction was complete and clarified, the solution was aspirated off with a pipette and washed with water until the aqueous solution was neutral, the precipitate was filtered off rapidly and dried in a vacuum desiccator with concentrated H2SO 4.
Step four: 500g of cobalt hydroxide, 2000ml of pure water, 18.4mol/L of sulfuric acid, sodium chloride and sodium carbonate are prepared by preparing two groups of cobalt hydroxide slurry solutions, the first group of cobalt hydroxide slurry solutions is prepared by adding sulfuric acid, 4Co (OH) 3+ 4H 2SO4 =4 CoSO4 + 10H2O + O2. The generated oxygen is discharged and collected by adopting an upward air discharging method, the pH value of the cobalt sulfate aqueous solution is controlled to be 1.5-2.0, after the sufficient reaction, sodium carbonate is added into the cobalt sulfate aqueous solution for the sufficient reaction, 2H2O + O2+4e- =4OH-, 2Fe-4e- =2Fe2+, and the generated iron ion precipitate is extracted by extraction.
Example three:
a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: weighing 500g of cobalt hydroxide raw material, stirring 1000ml of pure water to prepare slurry, heating the dissolved cobalt raw material to +/-85 ℃, heating the dissolved cobalt raw material to water bath heating, stably controlling the temperature by using the water bath heating energy, enabling the temperature rise range to be relatively stable, enabling the cobalt raw material to be uniformly heated, adding appropriate amount of sodium chlorate, and adding Fe in the solution2+Oxidation to Fe3+。
Step two: and slowly adding 500g of the slurried cobalt hydroxide raw material purchased from outside, and carrying out high-speed cultivation with the density of about 3.6 g/cm. Melting point 1100-1200 deg.C, adding 2000ml pure water, stirring, reacting for 4 hr, adding sodium carbonate solution, and controlling pH to 3.0-3.5.
Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
Example four:
a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: weighing 500g of cobalt hydroxide raw material, stirring 2000ml of pure water to prepare slurry, heating the dissolved cobalt raw material to +/-85 ℃, heating the dissolved cobalt raw material to water bath heating, stably controlling the temperature by using the water bath heating energy, enabling the temperature rise range to be relatively stable, enabling the cobalt raw material to be uniformly heated, adding appropriate amount of sodium chlorate, and adding Fe in the solution2+Oxidation to Fe3+。
Step two: and slowly adding 500g of the slurried cobalt hydroxide raw material purchased from outside, and carrying out high-speed cultivation with the density of about 3.6 g/cm. Melting point 1100-1200 deg.C, adding 2000ml of pure water, stirring, adding sodium carbonate solution, and controlling pH value of the solution to 3.0-3.5.
Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
Example five:
a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: weighing 500g of cobalt hydroxide raw material, stirring 2000ml of pure water to prepare pulp, heating the dissolved cobalt raw material to 100 ℃ by adopting water bath heating, stably controlling the temperature by using the water bath heating energy, ensuring that the temperature rise range is relatively stable, uniformly heating the cobalt raw material, adding proper sodium chlorate, and adding Fe in the solution2+Oxidation to Fe3+。
Step two: and slowly adding 500g of the slurried cobalt hydroxide raw material purchased from outside, and carrying out high-speed cultivation with the density of about 3.6 g/cm. Melting point 1100-1200 deg.C, adding 2000ml pure water, stirring, reacting for 4 hr, adding sodium carbonate solution, and controlling pH to 3.0-3.5.
Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
Example six:
a novel iron removal and purification process method for a cobalt system comprises the following steps:
the method comprises the following steps: weighing 500g of cobalt hydroxide raw material, stirring 2000ml of pure water to prepare slurry, heating the dissolved cobalt raw material to +/-85 ℃, heating the dissolved cobalt raw material to water bath heating, stably controlling the temperature by using the water bath heating energy, enabling the temperature rise range to be relatively stable, enabling the cobalt raw material to be uniformly heated, adding appropriate amount of sodium chlorate, and adding Fe in the solution2+Oxidation to Fe3+。
Step two: and slowly adding 500g of the slurried cobalt hydroxide raw material purchased from outside, and carrying out high-speed cultivation with the density of about 3.6 g/cm. Melting point 1100-1200 deg.C, adding 2000ml pure water, stirring, reacting for 4h, adding sodium carbonate solution, and controlling pH to 6.0-6.5.
Step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
Compared with the novel iron removal and purification process method of six cobalt systems, the novel iron removal and purification process method of six cobalt systems has ideal effect, wherein iron ions can be removed in cobalt metal smelting, in the first embodiment, the property of comprehensive acid is utilized, in the iron removal process of sodium iron vanadium, the cobalt raw material is utilized to replace sulfuric acid generated in the process of neutralizing iron removal by soda, so that the soda is saved, the added sulfuric acid can be fully utilized, the waste of resources is reduced, meanwhile, the operation is relatively simple in process production, and the first embodiment is the best iron removal and purification process method.
Through comparing the first embodiment with the second embodiment, the operation is relatively simple by using the purchased cobalt hydroxide in the use of raw materials, the second embodiment adopts nitric acid, sulfuric acid and hydrochloric acid to dissolve the cobalt hydroxide, converts the cobalt hydroxide into a cobalt chloride solution, and removes iron by using hydrogen peroxide, so that a large amount of strong acid is involved in the reaction, and the strong acid causes various inconveniences in the later treatment, and the protein and the cutin are dissolved or solidified by the strong acid to form tissue burns with obvious boundaries. When orally taken, the oral cavity, esophagus and gastric mucosa are corroded, and when severe, the oral cavity, esophagus and gastric mucosa can be perforated. When the poison is in the form of gas and acid mist, respiratory mucosa damage is generated. High concentrations of strong acid can damage the skin and penetrate into the subcutaneous tissue causing necrosis. Concentrated sulfuric acid has strong water absorption, and can cause corrosion and burn when contacting with skin mucosa, and ulcer and scorch in severe cases. Concentrated nitric acid is contacted with air to release nitrogen dioxide, is inhaled into lung and contacted with water to generate nitric acid, and is easy to cause pulmonary edema. The contact of the concentrated hydrochloric acid causes skin, oral cavity and nasal mucosa ulcer, trachea and bronchitis, blepharospasm and corneal ulcer, the harm brought by the second embodiment is relatively large, and the strong acid is relatively complicated in the later treatment.
In the third example, by weighing 500g of cobalt hydroxide raw material and stirring with 1000ml of pure water, when the dosage of the pure water is changed from 1:4 to 1:2, the concentration of the reagent is larger, the sealing in the solution is relatively larger, and the reaction rate of the sulfuric acid and the cobalt hydroxide is prolonged when the sulfuric acid is adjusted to react. This in turn leads to a low reaction rate at the same time in the reaction between the reagents. By comparing the first embodiment with the fourth embodiment, when the slurry of the cobalt hydroxide raw material cannot be subjected to the control of the pH value and directly added into the sodium carbonate solution, the pH value in the later period cannot be controlled accurately, at this time, the sodium carbonate solution is added excessively, and the solution cannot be subjected to sufficient reaction before the sodium carbonate is explored and added, so that iron ions cannot be sufficiently separated out, and a certain deviation exists in iron removal in the later period.
When the PH of the novel iron removal purification process of the cobalt system is increased in the fifth embodiment and the sixth embodiment, the reaction rate is gradually decreased along with the increase of the PH when the sodium carbonate solution is adjusted, the reaction is incomplete in the redox reaction, ferrous ions cannot be rapidly converted into iron ions, a large amount of iron cannot be precipitated when the sodium carbonate is adjusted, and the iron ion removal effect is poor in the later treatment.
This novel deironing purification technology method of cobalt system will purchase the cobalt hydroxide raw materials outward and will go into water and stir the pulp, stir and dissolve through adding sulphuric acid, after the stirring, sodium chlorate is as the catalyst for lead to ferrous ion redox in the cobalt hydroxide solution and become ferric ion, the cobalt hydroxide pulp liquid of same concentration of ratio once more, mix it together, control its PH concentration, treat to react completely the back through the two hydrolysis reaction between sodium carbonate and the ferric ion, its reaction equation is as follows: 2Fe3+ + 3CO3^2- + 3H2O = =2Fe (OH)3 ↓ + 3CO2 ℃, (iron hydroxide precipitation) in the way of sedimentation and filter pressing, solid-liquid separation, and then realized the deironing.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. A novel iron removal and purification process method of a cobalt system is characterized in that: the method comprises the following steps:
the method comprises the following steps: dissolving cobalt raw material, heating, adding proper amount of oxidant, and adding Fe into the solution2+Oxidation to Fe3+；
Step two: slowly adding the slurried liquid of the purchased cobalt hydroxide raw material, and adding a sodium carbonate solution after reaction;
step three: and finally, realizing solid-liquid separation through free settling or filter pressing, wherein the separated solution is a solution after iron removal and can be used for a subsequent extraction process, the separated slag is yellow sodium iron vanadium slag and a small part of outsourcing cobalt hydroxide raw material which is not completely dissolved, and after the separated slag is dissolved and washed, the cobalt content in the tailing reaches below 0.4 percent and the solution is directly added externally.
2. The novel iron removal and purification process method for the cobalt system as claimed in claim 1, wherein the process method comprises the following steps: in the first step, 500g of cobalt hydroxide and 2000ml of pure water are weighed and stirred to prepare slurry.
3. The novel iron removal and purification process method for the cobalt system as claimed in claim 1, wherein the process method comprises the following steps: in the first step, the cobalt raw material is dissolved and heated to +/-85 ℃, and the cobalt raw material is dissolved and heated by using a water bath.
4. The novel iron removal and purification process method for the cobalt system as claimed in claim 1, wherein the process method comprises the following steps: in the first step, the oxidant is sodium chlorate.
5. The novel iron removal and purification process method for the cobalt system as claimed in claim 1, wherein the process method comprises the following steps: and in the second step, 500g of cobalt hydroxide is obtained, the density is about 3.6g/cm, the melting point is 1100-1200 ℃, the cobalt hydroxide is amphoteric hydroxide, 2000ml of pure water is added, stirring and pulping are carried out, and the pH value of the solution is 2.0-2.5.
6. The novel iron removal and purification process method for the cobalt system as claimed in claim 1, wherein the process method comprises the following steps: in the second step, the slurried cobalt hydroxide raw material solution reacts for 4 hours, and the pH value of the sodium carbonate solution is slowly added to 3.0-3.5.
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