CN110846520A - Method for removing iron in laterite-nickel ore leaching solution by using laterite-nickel ore nickel cobalt-depositing waste liquid slag - Google Patents
Method for removing iron in laterite-nickel ore leaching solution by using laterite-nickel ore nickel cobalt-depositing waste liquid slag Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- C22B47/00—Obtaining manganese
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- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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Abstract
The invention discloses a method for removing iron in a laterite-nickel ore leaching solution by using laterite-nickel ore nickel cobalt precipitation waste liquid slag. The method comprises the following steps: (1) mixing the solution obtained after the first-stage nickel and cobalt precipitation of the laterite-nickel ore with an alkali solution to react to obtain laterite-nickel ore waste liquid slag; (2) aerating, stirring and heating the laterite-nickel ore waste liquid slag to prepare laterite-nickel ore waste liquid slag slurry; (3) uniformly mixing the laterite nickel ore waste liquid slag slurry with the laterite nickel ore leaching solution, adding an alkali solution for reaction, and carrying out solid-liquid separation to obtain the iron-removed laterite nickel ore liquid and iron slag. The method can obviously improve the recovery rate of valuable metals in the liquid after the nickel and cobalt precipitation in one section, the waste liquid slag is used as an oxidant to be recycled, the waste liquid slag is used as the oxidant to replace other oxidants such as sodium chlorate and the like, the corrosion of a strong oxidant to equipment is reduced, the introduction of impurities into the leaching solution of the laterite-nickel ore is reduced, the waste liquid slag is used as an alkali to adjust the pH value of the leaching solution of the laterite-nickel ore, the production cost is reduced, and the economic benefit.
Description
Technical Field
The invention belongs to the field of nickel and cobalt hydrometallurgy metallurgy, and particularly relates to a method for removing iron in a laterite-nickel ore leaching solution by using laterite-nickel ore nickel and cobalt precipitation waste liquid slag.
Background
The laterite-nickel ore is generally smelted by a wet method, and generally, the laterite-nickel ore contains 0.5-2 g/L of manganese, a small amount of nickel-cobalt valuable metals and a large amount of impurity metals in the laterite-nickel ore hydrometallurgy wastewater. The conventional method for treating the waste liquid is lime water neutralization, so that a large amount of solid waste is generated, and the environment is greatly polluted and the resource is wasted.
The laterite nickel ore leaching solution contains 0.5-5 g/L of ferrous iron and 50-100 g/L of residual acid. The conventional treatment of ferrous oxide is to add sodium chlorate oxidant and the conventional treatment of neutralizing residual acid is to add lime water. The addition of sodium chlorate can introduce impurity element chloride ions, seriously corrode equipment, seriously pollute the natural environment and increase the production cost. A large amount of lime water is added to neutralize residual acid in the leaching solution of the laterite-nickel ore, so that a large amount of waste residues are generated, and a serious burden is generated on the environment.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide the method for removing iron in the laterite-nickel ore leaching solution by using the laterite-nickel ore nickel cobalt precipitation waste liquid slag, which can recover valuable metals nickel, cobalt and manganese in the laterite-nickel ore hydrometallurgy waste water and oxidize ferrous iron in the laterite-nickel ore leaching solution by using the recovered nickel, cobalt and manganese.
The method can obviously improve the recovery rate of the valuable metal in the liquid after one-stage nickel and cobalt precipitation, the waste liquid slag after nickel and cobalt precipitation of the laterite-nickel ore is prepared into the oxidant and recycled, the waste liquid slag is used as the oxidant to replace other oxidants such as sodium chlorate and the like in the prior art, the corrosion of a strong oxidant to equipment is reduced, the introduction of impurities in the leaching liquid of the laterite-nickel ore is reduced, the waste liquid slag is used as alkali to adjust the pH value of the leaching liquid of the laterite-nickel ore, the production cost is reduced, and the economic benefit is.
The purpose of the invention is realized by the following technical scheme:
a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag comprises the following steps:
(1) under the condition of aeration stirring, introducing hot steam into the first-stage nickel and cobalt precipitation liquid of the laterite-nickel ore to heat, adding an alkali solution and reacting to obtain a laterite-nickel ore waste liquid slag slurry;
(2) carrying out solid-liquid separation on the laterite-nickel ore waste liquid slag slurry in the step (1) to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid;
(3) adding water into the laterite-nickel ore waste liquid slag in the step (2), aerating and stirring, and introducing hot steam for heating to obtain laterite-nickel ore waste liquid slag slurry;
(4) and (3) adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry obtained in the step (3), adjusting the pH value to be 2.0-3.6, reacting, and carrying out solid-liquid separation to obtain a laterite nickel ore iron removal liquid and iron slag.
Preferably, the liquid obtained after the first-stage nickel and cobalt precipitation of the laterite-nickel ore in the step (1) is the hydrometallurgical wastewater of the laterite-nickel ore, and more preferably the hydrometallurgical nickel and cobalt precipitation wastewater of the laterite-nickel ore.
Preferably, the laterite-nickel ore primary nickel-cobalt precipitation solution in the step (1) contains divalent manganese ions. The divalent manganese ions are easily oxidized by the oxidizing agent after forming hydroxides.
Preferably, the reaction temperature in the step (1) is not higher than 90 ℃ and the time is 0.5-3 h; more preferably 40 to 90 ℃. The reaction temperature in the step (1) is the temperature for heating by introducing hot steam.
Preferably, the alkali solution in step (1) is NaOH, Ca (OH)2、NH4At least one of OH and CaO solution. The mass concentration of the alkali solution is 10-30 wt%. The addition of the alkali solution can prevent the local concentration from being too high in the process of adding the alkali, so that the alkali is consumed excessively.
Preferably, the pH value of the system after the alkali solution is added in the step (1) is 8.0-9.5. After the system (mixed solution) fully reacts under the condition that the pH value is 8.0-9.5, the laterite-nickel ore waste liquid (the liquid after the first-stage nickel and cobalt precipitation of the laterite-nickel ore) is precipitated in the form of hydroxide, so that valuable metals in the waste liquid are recovered.
Preferably, the gas for aeration stirring in steps (1) and (3) is at least one of air and oxygen. The aeration stirring replaces other mechanical stirring, the energy consumption is reduced, the air and oxygen are low in price, and the manganese hydroxide in the waste liquid slag can be oxidized.
Preferably, the pressure of the aeration stirring in the steps (1) and (3) is 0.5-7.0 mPa; and (4) the time of aeration stirring in the step (3) is 0.5-3 h. The aeration pressure and the reaction temperature are improved, the aeration time is prolonged, the oxidation rate is improved, the energy consumption is reduced, and the production efficiency is improved.
Preferably, the heating temperature of the steps (1) and (3) is 40-90 ℃.
Preferably, the mass ratio of the water to the laterite-nickel ore waste liquid slag in the step (3) is (1-5): 1.
preferably, the solid-liquid separation method in steps (2) and (4) is one of dense precipitation, horizontal filter pressing and belt filter pressing. Separating the laterite-nickel ore waste liquid slag and the laterite-nickel ore waste liquid by solid-liquid separation; and (4) separating iron-removed liquid and iron slag of the laterite nickel ore by solid-liquid separation.
Preferably, the molar ratio of manganese in the lateritic nickel ore waste liquid slag slurry to ferrous ions in the lateritic nickel ore leaching solution in the step (4) is (0.5-3): 1. and (4) the valence state of manganese in the manganese hydroxide in the laterite-nickel ore waste liquid slag slurry is trivalent, quadrivalent or other valence states, and ferrous ions in the solution are easily oxidized.
Preferably, the pH adjustment in the step (4) is performed by using an alkali solution, wherein the alkali solution is NaOH, Ca (OH)2、NH4At least one of OH and CaO solution. The mass concentration of the alkali solution is 10-30 wt%. The addition of the alkali solution can prevent the local concentration from being too high in the process of adding the alkali, so that the alkali is consumed excessively.
Preferably, the reaction temperature of the step (4) is not lower than 40 ℃, and the reaction time is not less than 15 minutes; more preferably, the reaction temperature in the step (4) is 40-90 ℃ and the reaction time is 0.5-3 h. The ferrous oxidation rate can be improved by increasing the reaction temperature and the reaction time.
Preferably, the reaction of step (4) is carried out at a constant temperature and pH, wherein the pH is 2.0.
Preferably, both steps (3) and (4) are carried out in an oxidation tank.
The invention relates to a method for removing iron in a leaching solution of a laterite-nickel ore by using nickel and cobalt precipitation waste liquid slag of the laterite-nickel ore, which comprises the steps of firstly mixing a first-stage nickel and cobalt precipitation liquid of the laterite-nickel ore with an alkali solution in an aeration stirring mode to form nickel and cobalt manganese hydroxides, and further oxidizing the nickel and cobalt manganese hydroxides by using air used for aeration to form oxidized waste liquid slag; and then adding the oxidized waste liquid slag into an oxidation tank, introducing steam for heating, then adding the laterite-nickel ore leachate and the oxidized waste liquid slag slurry for mixing, taking the waste liquid slag as an oxidant, oxidizing ferrous ions in the laterite-nickel ore leachate into ferric ions, taking the waste liquid slag as alkali to adjust the pH value of the laterite-nickel ore leachate, forming ferric hydroxide from the ferric ions, and finally separating from the solution by a solid-liquid separation method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
compared with the traditional method for treating wastewater and oxidizing ferrous ions in the laterite-nickel ore leaching solution, the method for removing iron in the laterite-nickel ore leaching solution by using the laterite-nickel ore nickel cobalt precipitation waste liquid slag provided by the invention reduces the loss of valuable metals and the introduction of impurities, reduces the corrosion of the impurities to equipment and the pollution to the environment, reduces the production cost, improves the recovery rate of the valuable metals and improves the economic benefit.
Drawings
FIG. 1 is a schematic flow chart of the method for removing iron in the lateritic nickel ore leaching solution by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
In the embodiment of the application, the liquid obtained after the first-stage nickel and cobalt precipitation of the laterite nickel ore is the nickel and cobalt precipitation wastewater obtained by hydrometallurgical nickel and cobalt precipitation of the laterite nickel ore; the laterite nickel ore leaching solution contains 0.5-5 g/L of ferrous iron and 50-100 g/L of residual acid.
Example 1
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 0.5mPa to ensure that the temperature of the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for the first time is raised to 40 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: adding a CaO aqueous solution with the mass concentration of 10% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel-cobalt-precipitated liquid to 8.0, and fully reacting at the reaction temperature of 40 ℃ for 3h to obtain the laterite-nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 1: 1 pulping, aerating and stirring for 3h by using air with the pressure of 0.5mPa, and introducing high-temperature steam to raise the temperature to 40 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 0.5 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding a CaO water solution with the mass concentration of 10% to adjust the pH of the system to be 2.0, and then carrying out heat preservation reaction at 40 ℃ for 3 hours to obtain the liquid slurry after deironing of the laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore ferrous removal solution obtained by the embodiment is 100%, the iron precipitation rate is 85%, the nickel loss rate is 0.02%, and the cobalt loss rate is 0.01%.
Example 2
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 7mPa to ensure that the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for one period is heated to 80 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: adding a CaO aqueous solution with the mass concentration of 30% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel-cobalt-precipitated liquid to 9.5, and fully reacting at the reaction temperature of 80 ℃ for 0.5h to obtain the laterite-nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 3: 1 pulping, carrying out aeration stirring for 0.5h by using air with the pressure of 7.0mPa, and introducing high-temperature steam to raise the temperature to 90 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 3.0 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding a CaO water solution with the mass concentration of 30% to adjust the pH of the system to be 4.5, and then carrying out heat preservation reaction at 90 ℃ for 0.5h to obtain the liquid slurry after removing iron from laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore ferrous removal solution obtained by the embodiment is 100%, the iron precipitation rate is 99%, the nickel loss rate is 0.12%, and the cobalt loss rate is 0.09%.
Example 3
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 7mPa to ensure that the temperature of the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for one time is raised to 40 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: adding a CaO aqueous solution with the mass concentration of 30% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel-cobalt-precipitated liquid to 8.5, reacting at the temperature of 40 ℃, and fully reacting for 1.0h to obtain the laterite-nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain waste liquid slag and waste water.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 5: 1 pulping, carrying out aeration stirring for 0.5h by using air with the pressure of 7.0mPa, and introducing high-temperature steam to raise the temperature to 90 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 2.0 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding a CaO water solution with the mass concentration of 10% to adjust the pH of the system to be 3.6, and then carrying out heat preservation reaction at 90 ℃ for 0.5h to obtain the liquid slurry after removing iron from laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore ferrous removal solution obtained by the embodiment is 100%, the iron precipitation rate is 99%, the nickel loss rate is 0.09%, and the cobalt loss rate is 0.04%.
Example 4
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 5mPa to ensure that the temperature of the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for one time is raised to 60 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: adding a CaO aqueous solution with the mass concentration of 30% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel-cobalt-precipitated liquid to 8.2, reacting at the reaction temperature of 40 ℃, and fully reacting for 1.0h to obtain the laterite-nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 2: 1, pulping, aerating and stirring for 1.0h by using air with the pressure of 5.0mPa, introducing high-temperature steam, and heating to 80 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 0.8 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding a CaO water solution with the mass concentration of 10% to adjust the pH of the system to be 3.6, and then carrying out heat preservation reaction at 80 ℃ for 1h to obtain the liquid slurry after deironing of the laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore ferrous removal solution obtained in the embodiment is 100%, the iron precipitation rate is 99%, the nickel loss rate is 0.07%, and the cobalt loss rate is 0.03%.
Example 5
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 5mPa to ensure that the temperature of the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for one time is raised to 60 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: adding a CaO aqueous solution with the mass concentration of 30% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel-cobalt-precipitated liquid to 8.0, and fully reacting at the reaction temperature of 60 ℃ for 1.0h to obtain the laterite-nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 2: 1 pulping, namely aerating and stirring air with the pressure of 5.0mPa for 1.0h, and introducing high-temperature steam to heat to 80 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 1.5 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding a CaO water solution with the mass concentration of 10% to adjust the pH of the system to be 3.6, and then carrying out heat preservation reaction at 80 ℃ for 1h to obtain the liquid slurry after deironing of the laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore ferrous removal solution obtained in the embodiment is 100%, the iron precipitation rate is 99%, the nickel loss rate is 0.07%, and the cobalt loss rate is 0.03%.
Example 6
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 5mPa to ensure that the temperature of the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for one time is raised to 60 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: and (2) adding a NaOH aqueous solution with the mass concentration of 10% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel and cobalt precipitation solution to 8.0, and fully reacting at the reaction temperature of 60 ℃ for 1.0h to obtain the laterite nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 2: 1 pulping, namely aerating and stirring air with the pressure of 5.0mPa for 1.0h, and introducing high-temperature steam to heat to 80 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 1.5 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding a NaOH aqueous solution with the mass concentration of 10% to adjust the pH of the system to be 3.6, and then carrying out heat preservation reaction at 80 ℃ for 1h to obtain the liquid slurry after deironing of the laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore post-ferrous removal solution obtained by the embodiment is 100%, the iron precipitation rate is 99%, the nickel loss rate is 0.15%, and the cobalt loss rate is 0.08%.
Example 7
The embodiment provides a method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag, which comprises the following steps:
(1) heating for a first period of time to precipitate nickel and cobalt solution: introducing high-temperature steam under the condition of air aeration stirring with the pressure of 5mPa to ensure that the temperature of the liquid after the nickel and cobalt are deposited on the laterite-nickel ore for one time is raised to 60 ℃.
(2) Adjusting the pH of the solution after the first-stage nickel and cobalt precipitation: and (2) adding a NaOH aqueous solution with the mass concentration of 30% into the step (1) under the aeration stirring condition in the step (1), adjusting the pH of the first-stage nickel and cobalt precipitation solution to 8.0, and fully reacting at the reaction temperature of 60 ℃ for 1.0h to obtain the laterite nickel ore waste liquid slag slurry.
(3) First solid-liquid separation: and (3) separating the laterite-nickel ore waste liquid slurry in the step (2) by adopting horizontal filter pressing to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid.
(4) Pulping waste liquid and slag: and (3) pumping the waste liquid slag of the laterite-nickel ore into an oxidation tank, wherein the mass ratio of water to the waste liquid slag of the laterite-nickel ore is 2: 1 pulping, namely aerating and stirring air with the pressure of 5.0mPa for 1.0h, and introducing high-temperature steam to heat to 80 ℃ to obtain the laterite-nickel ore waste liquid slag slurry.
(5) Oxidizing ferrous ions, adjusting pH: adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry in the step (4), wherein the molar weight of manganese in the laterite nickel ore waste liquid slag slurry is 1.5 times of the molar weight of ferrous ions in the laterite nickel ore leaching solution, adding NaOH aqueous solution with the mass concentration of 30% to adjust the pH of the system to be 3.6, and then carrying out heat preservation reaction at 80 ℃ for 1h to obtain the liquid slurry after deironing of the laterite nickel ore.
(6) Second solid-liquid separation: and (3) adopting the liquid slurry after the laterite nickel ore is subjected to iron removal in the horizontal filter pressing separation step (5) to obtain the liquid after the laterite nickel ore is subjected to iron removal and iron slag.
The ferrous oxidation rate of the laterite-nickel ore ferrous removal solution obtained by the embodiment is 100%, the iron precipitation rate is 99%, the nickel loss rate is 0.42%, and the cobalt loss rate is 0.15%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for removing iron in a lateritic nickel ore leaching solution by using lateritic nickel ore nickel cobalt precipitation waste liquid slag is characterized by comprising the following steps:
(1) under the condition of aeration stirring, introducing hot steam into the first-stage nickel and cobalt precipitation liquid of the laterite-nickel ore to heat, adding an alkali solution and reacting to obtain a laterite-nickel ore waste liquid slag slurry;
(2) carrying out solid-liquid separation on the laterite-nickel ore waste liquid slag slurry in the step (1) to obtain laterite-nickel ore waste liquid slag and laterite-nickel ore waste liquid;
(3) adding water into the laterite-nickel ore waste liquid slag in the step (2), aerating and stirring, and introducing hot steam for heating to obtain laterite-nickel ore waste liquid slag slurry;
(4) and (3) adding the laterite nickel ore leaching solution into the laterite nickel ore waste liquid slag slurry obtained in the step (3), adjusting the pH value to be 2.0-3.6, reacting, and carrying out solid-liquid separation to obtain a laterite nickel ore iron removal liquid and iron slag.
2. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 1, wherein the molar ratio of manganese in the lateritic nickel ore waste liquid slag slurry to ferrous ions in the leachate of the lateritic nickel ore in the step (4) is (0.5-3): 1.
3. the method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 2, wherein the pH value of the system after adding the alkali solution in the step (1) is 8.0-9.5.
4. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 2 or 3, characterized in that the reaction temperature in the step (1) is not higher than 90 ℃ and the time is 0.5-3 h; the reaction temperature of the step (4) is not lower than 40 ℃, and the reaction time is not less than 15 minutes.
5. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 4, wherein the reaction temperature in the step (1) is 40-90 ℃; the reaction temperature in the step (4) is 40-90 ℃, and the reaction time is 0.5-3 h.
6. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 4, characterized in that the lateritic nickel ore of the step (1) contains divalent manganese ions in the first-stage nickel cobalt precipitation liquid; the heating temperature in the steps (1) and (3) is 40-90 ℃; and (3) the mass ratio of the water to the laterite-nickel ore waste liquid slag is (1-5): 1.
7. the method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 4, wherein the alkali solution in the step (1) is NaOH, Ca (OH)2、NH4At least one of OH and CaO solution; the mass concentration of the alkali solution is 10-30 wt%;
adjusting the pH value in the step (4) is carried out by adopting an alkali solution, wherein the alkali solution is NaOH or Ca (OH)2、NH4At least one of OH and CaO solution; the mass concentration of the alkali solution is 10-30 wt%.
8. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 4, wherein the gas for aeration stirring in the steps (1) and (3) is at least one of air and oxygen; the pressure of the aeration stirring in the steps (1) and (3) is 0.5-7.0 mPa; and (4) the time of aeration stirring in the step (3) is 0.5-3 h.
9. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 4, characterized in that the reaction of the step (4) is carried out at a constant temperature and pH value, wherein the pH value is 2.0.
10. The method for removing iron in the leachate of the lateritic nickel ore by using the lateritic nickel ore nickel cobalt precipitation waste liquid slag according to the claim 4, characterized in that the solid-liquid separation method of the steps (2) and (4) is one of dense precipitation, horizontal filter pressing and belt filter pressing.
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| CN115109927A (en) * | 2021-03-17 | 2022-09-27 | 中国科学院过程工程研究所 | Method for removing manganese and magnesium from laterite-nickel ore hydrochloric acid leaching solution |
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| CN115109927A (en) * | 2021-03-17 | 2022-09-27 | 中国科学院过程工程研究所 | Method for removing manganese and magnesium from laterite-nickel ore hydrochloric acid leaching solution |
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