CN112646976B - Method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore and application - Google Patents
Method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore and application Download PDFInfo
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- CN112646976B CN112646976B CN202011498900.5A CN202011498900A CN112646976B CN 112646976 B CN112646976 B CN 112646976B CN 202011498900 A CN202011498900 A CN 202011498900A CN 112646976 B CN112646976 B CN 112646976B
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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
- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- C22B47/00—Obtaining manganese
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention provides a method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore and application, relates to the technical field of metallurgy, and comprises the following steps: mixing the waste lithium ion battery black powder and nickel cobalt sulfide ore to prepare ore pulp; adding an auxiliary leaching agent and a leaching agent into the ore pulp, and adjusting the pH value of the ore pulp; introducing oxygen-containing gas; controlling the leaching condition of the system and synergistically leaching the valuable metal ions. The method utilizes the oxidability of battery black powder and the reducibility of nickel cobalt sulfide ore, adopts the leaching aid as an intermediate carrier and a catalyst, and the leaching aid plays a role in transferring electrons, thereby accelerating the solid-solid reaction kinetic process and achieving the effect of synergistically leaching metal ions. The synergistic leaching method provided by the invention has the advantages of less consumption of chemical reagents, low cost, simple operation, environmental friendliness, easy realization of industrial application and the like.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore and application.
Background
At present, hydrometallurgy is widely used for recycling waste lithium ion batteries due to the advantages of mild conditions, high metal leaching rate and the like.
The traditional treatment of the nickel cobalt sulfide ore has the defects of complex process, high treatment cost, heavy environmental pollution, low metal recovery rate and the like.
The recovery of valuable components of the waste lithium ion battery and the high-efficiency utilization of the traditional nickel sulfide cobalt mineral products are very important. Therefore, how to accelerate the chemical reaction process under mild conditions and improve the recovery rate of metal ions has important industrial significance.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore, which utilizes the oxidability of the waste lithium ion battery black powder and the reducibility of the nickel cobalt sulfide ore, adopts a leaching aid as an intermediate carrier and a catalyst, synergistically treats the waste lithium ion battery black powder and the nickel cobalt sulfide ore, and can efficiently recover target metal ions under the conditions of normal pressure and low temperature.
The second purpose of the invention is to provide the application of the method in preparing the ternary precursor, and the method has the advantages of less consumption of chemical reagents, low cost, environmental friendliness, easiness in industrial application and the like.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the invention provides a method for synergistically leaching nickel, cobalt and manganese by using waste lithium ion battery black powder and nickel cobalt sulfide ore, which comprises the following steps:
providing black powder of waste lithium ion batteries and ore pulp of nickel cobalt sulfide ore;
adding an auxiliary leaching agent and a leaching agent into the ore pulp;
introducing oxygen-containing gas into the leached ore pulp;
and carrying out liquid-solid separation to obtain the nickel-cobalt-manganese leaching solution.
The waste lithium ion battery is a nickel cobalt lithium manganate battery.
The invention adopts mineral powder obtained by crushing and finely grinding nickel cobalt sulfide ore;
preferably, the granularity of the mineral powder of the nickel-cobalt sulfide ore is-0.074 mm and accounts for more than 80%.
Furthermore, the mass ratio of the battery black powder to the nickel cobalt sulfide ore is 1-10: 10-1.
Preferably, the mass fraction of the ore pulp is 15% -33%.
Preferably, the leaching aid comprises one or more of iron ions, copper ions, silver ions, manganese ions;
further preferably, the addition amount of the auxiliary leaching agent is 2-10 g/L.
Preferably, the leaching agent is sulfuric acid;
preferably, the leaching agent adjusts the pH value of the ore pulp to be not more than 2.0.
Preferably, the leaching reaction temperature is 50-95 ℃, and the reaction time is 1-10 h.
In a second aspect, the invention provides the use of a method for preparing a ternary precursor.
Compared with the prior art, the invention has the following beneficial effects:
the invention skillfully creates the condition for reaction, namely, the oxidizability of the black powder of the waste lithium ion battery and the reducibility of the nickel cobalt sulfide ore are utilized to carry out the synergistic leaching of nickel, cobalt and manganese, thereby avoiding the need of adding additional chemical reagents in the traditional treatment of single raw material, and particularly avoiding the use of hydrogen peroxide which is a hazardous chemical product and an easily-explosive product.
The invention skillfully adopts the leaching aid as the intermediate carrier and the catalyst, accelerates the solid-solid reaction kinetic process, ensures the high-efficiency leaching of valuable metals such as nickel, cobalt, manganese and the like in the raw materials, wherein the leaching rate of nickel is more than 96 percent, the leaching rate of cobalt is more than 98 percent, and the leaching rate of manganese is more than 98 percent.
The method has the advantages of low cost, simple operation, environmental protection, easy realization of industrial application and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a flowchart provided in embodiment 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. 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.
According to the first aspect of the invention, the method for synergistically leaching nickel, cobalt and manganese by utilizing the black powder of the waste lithium ion battery and the nickel cobalt sulfide ore comprises the following steps:
providing the black powder of the waste lithium ion battery and the ore pulp of the nickel cobalt sulfide ore;
adding an auxiliary leaching agent and a leaching agent into the ore pulp;
introducing oxygen-containing gas into the leached ore pulp;
and carrying out liquid-solid separation to obtain the nickel-cobalt-manganese leaching solution.
The spent lithium ion battery comprises a nickel cobalt lithium manganate battery.
Black powder of waste lithium ion battery
The waste lithium ion battery black powder is a material obtained after disassembly, module discharge, crushing and sorting of the waste lithium ion battery.
Cobalt nickel sulfide ore
The nickel-cobalt sulfide ore comprises nickel sulfide and cobalt sulfide, wherein the powder of the nickel sulfide is black and has reducibility; cobalt sulfide is insoluble in water, soluble in acid and reductive.
The invention adopts ore powder obtained by crushing and finely grinding nickel cobalt sulfide ore.
Preferably, the granularity of the mineral powder of the nickel-cobalt sulfide ore is-0.074 mm and accounts for more than 80%.
The invention ensures that the granularity of the mineral powder of the nickel-cobalt sulfide ore, which is-0.074 mm, accounts for more than 80 percent, thereby not only obtaining higher leaching rate, but also improving the leaching rate of target metal ions.
Furthermore, the mass ratio of the waste lithium ion battery black powder to the nickel cobalt sulfide ore is 1-10: 10-1.
The oxidized nickel cobalt lithium manganate battery black powder reacts with the reduced nickel cobalt sulfide ore, so that the purpose of synergistically leaching nickel, cobalt and manganese is achieved, and the need of adding an additional chemical reagent in the traditional treatment process is avoided.
Typical but non-limiting mass ratios of spent lithium ion battery black powder to nickel cobalt sulfide ore are, for example, 1:10, 2:9, 3:8, 4:7, 5:6, 6:5, 7:4, 8:3, 9:2, 10: 1.
The specific mass ratio of the waste lithium ion battery black powder to the nickel cobalt sulfide ore provided by the invention ensures the full reaction of the battery black powder and the nickel cobalt sulfide ore.
Ore pulp
Mineral slurry is a liquid mixture of solid raw materials such as ore, ore soil and the like added with water and other auxiliary agents in industrial production for extracting target elements.
Preferably, the mass fraction of the ore pulp is 15% -33%.
The mass fraction of the slurry is the ratio of the weight of the solids in the slurry to the total weight of the solids and liquid in the slurry.
The ore pulp concentration is too small, the ion concentration in the leaching solution is not high, and the improvement of the ore treatment capacity is not facilitated; the ore pulp has too high concentration, sticky ore pulp, difficult stirring and large energy consumption loss.
Typical but non-limiting concentrations of the pulp are for example 15%, 18%, 21%, 24%, 27%, 30%, 33%.
Infusion aid
The leaching aid plays a role in transferring electrons and quickens the reaction rate.
Preferably, the leaching aid comprises one or more of iron ions, copper ions, silver ions, manganese ions;
further preferably, the concentration of the leaching aid is 2-10 g/L.
Typical but non-limiting concentrations of the leaching aid are, for example, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L, 10 g/L.
Leaching agent
The pH value is controlled by using a leaching agent.
Preferably, the leaching agent is sulfuric acid;
preferably, the leaching agent adjusts the pH value of the ore pulp to be not more than 2.0.
The method utilizes the oxidizability of the black powder of the waste lithium ion battery and the reducibility of the nickel cobalt sulfide ore to carry out synergistic leaching, adopts the leaching aid as an intermediate carrier and a catalyst, accelerates the solid-solid reaction kinetic process, and ensures the efficient leaching of valuable metals such as nickel, cobalt, manganese and the like in the raw materials.
With Fe 2+ For example, using Fe 2+ The carrier used as the electron transfer catalyzes oxidation-reduction reaction, accelerates the kinetic process of solid-solid reaction, and the process takes place as follows:
Li z Ni 1-x-y Co x Mn y O 2 +NiS+Fe 2+ +O 2 +H 2 SO 4 →Li 2 SO 4 +NiSO 4 +CoSO 4 +MnSO 4 +H 2 O+Fe 3+ +S
typical but non-limiting amounts of the leaching aid are, for example, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L, 10 g/L.
Typical but not limiting pH values of the pulp are e.g. 0.5, 1, 1.5, 2.
Preferably, the leaching reaction temperature is 50-95 ℃, and the reaction time is 1-10 h.
Suitable reaction temperatures and reaction times may allow for more efficient leaching of the target metal ion.
Typical but non-limiting reaction temperatures for leaching are for example 50 ℃, 65 ℃, 80 ℃, 95 ℃.
Typical but non-limiting reaction times for leaching are, for example, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10 h.
The invention provides a method for synergistically leaching nickel, cobalt and manganese by using waste lithium ion battery black powder and nickel cobalt sulfide ore, which can realize the purpose of efficiently recovering target metal ions under the mild conditions of normal pressure and low temperature by controlling the proportion and reaction conditions of the waste lithium ion battery black powder and the nickel cobalt sulfide ore.
According to the second aspect of the invention, the invention provides the application of the method for synergistically leaching nickel, cobalt and manganese by using the waste lithium ion battery black powder and the nickel cobalt sulfide ore in preparing the ternary precursor.
The nickel-cobalt-manganese leaching solution is utilized to prepare the ternary precursor through coprecipitation, and the method has the advantages of less consumption of chemical reagents, low cost, environmental friendliness, easiness in industrial application and the like.
The invention is further illustrated by the following examples. The materials in the examples are prepared according to known methods or are directly commercially available, unless otherwise specified.
The process of the present invention is further illustrated by the following non-limiting examples to facilitate understanding of the present invention and its advantages, but not to limit the scope of the present invention, which is defined by the claims.
Example 1
The typical main element analysis of black powder of a waste lithium ion battery in a certain domestic factory is shown in the following table:
| element(s) | Ni | Co | Mn | Li | Al | Cu | Ca |
| Content/% | 20.65 | 9.78 | 20.83 | 5.0 | 0.76 | 0.039 | 0.083 |
The nickel sulfide cobalt-nickel ore contains 14.07% of nickel, 0.46% of cobalt and 35.43% of sulfur.
Mixing the black powder 100g and the nickel cobalt sulfide 30g to prepare ore pulp with the mass fraction of 25%, controlling the concentration of iron ions of the leaching aid to be 5g/L and the pH value to be 1.5, leaching in a water bath at the temperature of 98 ℃ for 3 hours, wherein the oxygen flow is 17m 3 /h。
As a result: the leaching rate of nickel is 96 percent, the leaching rate of cobalt is 98 percent, and the leaching rate of manganese is 98 percent. The flow chart is shown in figure 1.
Example 2
The black powder of the waste lithium ion battery in a certain domestic plant contains 19.49 percent of nickel, 19.29 percent of cobalt and 17.78 percent of manganese, and the black powder of the waste lithium ion battery in a certain domestic plant contains 14.07 percent of nickel, 0.46 percent of cobalt and 35.43 percent of sulfur in nickel sulfide cobalt nickel ore in a certain domestic plant.
Taking 35g of nickel cobalt sulfide ore to prepare ore pulp with the mass fraction of 20% from 100g of black powder, controlling the ferrous ion concentration of the leaching aid to be 8g/L and the pH value to be 1.2, leaching for 6 hours in a water bath at 90 ℃, wherein the oxygen flow is 10m 3 /h。
As a result: the leaching rate of nickel is 97%, the leaching rate of cobalt is 99% and the leaching rate of manganese is 99%.
Comparative example 1
The components of certain nickel sulfide ores are as follows:
| element(s) | Ni | Cu | Ca | Mg | S | Al | Co | Cr | Fe | K |
| Content/% | 6.415 | 0.957 | 0.401 | 1.804 | 19.762 | 0.067 | 0.307 | 0.008 | 42.780 | 0.003 |
| Element(s) | Mn | Na | P | Pb | Sr | Ti | V | Zn | As | |
| Content/%) | 0.009 | 0.012 | 0.046 | 0.012 | 0.000 | 0.027 | 0.009 | 0.005 | 0.0002 |
The atmospheric leaching test conditions were as follows: the nickel sulfide concentrate ore with the particle size of-0.020 mm accounts for more than 80%, the oxygen flow rate is 300mL/min, the reaction temperature is 95 ℃, the chloride ion concentration is 50g/L, the liquid-solid ratio is 5: 1, sulfuric acid is added to control the pH value in the reaction process to be less than 1.0, and the reaction time is 15 hours. The reaction results are given in the following table:
from the results, the conventional nickel sulfide concentrate leaching needs to leach for a long time under the condition of extremely fine ore granularity to obtain the ideal leaching effect, and chloride ions are added as a leaching aid, and are extremely corrosive to equipment in an acid system.
Comparative example 2
Taking 100g of black powder, adding water, stirring and slurrying, wherein the solid-to-liquid ratio is 3:1, the unit is mL/g, the reaction temperature is 80 ℃, introducing sulfur dioxide gas, the adding amount of sulfur dioxide is 60mL/min, slowly adding concentrated sulfuric acid, controlling the end point pH to be 1.5, leaching for 3h, after leaching, carrying out liquid-solid separation, and drying filter residues and analyzing.
In this process, SO 2 Acting as a reducing agent to reduce the high valence ions in the black powder to low valence ions, e.g. Co 3+ Reduction to Co 2+ 。
Weighing the slag and analyzing the contents of Ni, Co, Mn and Li, wherein the leaching rates of Ni, Co, Mn and Li are 93.14%, 92.21%, 94.37% and 93.95%
In this reaction, additional introduction of SO is required 2 As a reducing agent.
Comparative example 3
The black powder of the waste lithium ion battery in a certain domestic factory contains 19.49 percent of nickel, 19.29 percent of cobalt, 17.78 percent of manganese, 14.07 percent of nickel, 0.46 percent of cobalt and 35.43 percent of sulfur. Taking 100g of the black powder, taking 35g of nickel-cobalt concentrate, the liquid-solid ratio of 4:1, the unit of mL/g, the ore pulp concentration of 20 percent, adding sulfuric acid to control the pH value to be 1.2, leaching for 6 hours in a water bath at the temperature of 90 ℃, wherein the oxygen flow is 10m 3 H is used as the reference value. The leaching rate of nickel is 78.68 percent, the leaching rate of cobalt is 91.22 percent, and the leaching rate of manganese is 88.06 percent.
Analysis of
According to data results of experimental examples and comparative examples, waste lithium ion battery black powder and nickel cobalt sulfide ore are mixed according to a specific proportion, the pH value of ore pulp is adjusted by reasonably controlling the mass fraction of the ore pulp and the addition amount of an auxiliary leaching agent and a leaching agent, oxygen-containing gas is introduced, and appropriate reaction temperature and time are controlled at the same time, so that target metal ions can be efficiently and synergistically leached, wherein the nickel leaching rate is more than 96%, the cobalt leaching rate is more than 98%, and the manganese leaching rate is more than 98%.
The invention skillfully creates the condition for reaction generation, namely, the oxidizability of the black powder of the waste lithium ion battery and the reducibility of the nickel cobalt sulfide ore are utilized to carry out the synergistic leaching of nickel cobalt manganese.
The invention skillfully adopts the leaching aid as the intermediate carrier and the catalyst, accelerates the solid-solid reaction kinetic process, ensures the high-efficiency leaching of valuable metals such as nickel, cobalt, manganese and the like in the raw materials, wherein the leaching rate of nickel is more than 96 percent, the leaching rate of cobalt is more than 98 percent, and the leaching rate of manganese is more than 98 percent.
The method has the advantages of low cost, simple operation, environmental protection, easy realization of industrial application and the like.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. A method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore is characterized by comprising the following steps:
providing the black powder of the waste lithium ion battery and the ore pulp of the nickel cobalt sulfide ore;
adding an auxiliary leaching agent and a leaching agent into the ore pulp, and introducing oxygen-containing gas;
carrying out liquid-solid separation to obtain a nickel-cobalt-manganese leaching solution;
the waste lithium ion battery comprises a waste nickel cobalt lithium manganate battery;
the granularity of the mineral powder of the nickel-cobalt sulfide ore is-0.074 mm and accounts for more than 80 percent;
the mass ratio of the waste lithium ion battery black powder to the nickel cobalt sulfide ore is 1-10: 10-1;
the mass fraction of the ore pulp is 15-33%;
the leaching aid is ferrous ions;
the addition amount of the auxiliary infusion is 2-10 g/L;
the leaching agent regulates the pH value of ore pulp to be not more than 2.0;
the leaching reaction temperature is 50-95 ℃, and the reaction time is 1-10 h.
2. The method of claim 1, wherein the leaching agent is sulfuric acid.
3. Use of a method according to claim 1 or 2 for the preparation of a ternary precursor.
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