CN115353160B - Preparation method of battery-grade nickel-cobalt-manganese ternary sulfate solution - Google Patents
Preparation method of battery-grade nickel-cobalt-manganese ternary sulfate solution Download PDFInfo
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- CN115353160B CN115353160B CN202211155269.8A CN202211155269A CN115353160B CN 115353160 B CN115353160 B CN 115353160B CN 202211155269 A CN202211155269 A CN 202211155269A CN 115353160 B CN115353160 B CN 115353160B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a preparation method of a battery-grade nickel-cobalt-manganese ternary sulfate solution, which comprises the following steps: s1, uniformly mixing concentrated sulfuric acid and pure water to obtain a sulfuric acid solution; s2, adding nickel and cobalt into the sulfuric acid solution, continuously stirring, introducing steam, heating and keeping the temperature at 80-90 ℃ for reaction for 6-8h; s3, slowly adding manganese, adjusting the pH to 5-5.5 after the reaction is completed, filtering, and demagnetizing to obtain the battery grade nickel-cobalt-manganese ternary sulfate solution. The method has the advantages of short time consumption and accurate batching.
Description
Technical Field
The invention relates to a preparation method of a battery-grade nickel-cobalt-manganese ternary sulfate solution, and belongs to the field of material science.
Background
The raw materials used for preparing the nickel-cobalt-manganese ternary battery anode precursor material mainly comprise sulfate or sulfate solution. The sulfate (nickel sulfate, cobalt sulfate and manganese sulfate) solution is prepared by mainly dissolving and finely filtering sulfate. However, the process of the preparation method is long, or the ingredients are inaccurate due to the deviation of the water content of sulfate or the deviation of a mass flowmeter.
Therefore, there is an urgent need to develop a preparation method of nickel-cobalt-manganese ternary sulfate solution with short time consumption and accurate ingredients.
Disclosure of Invention
The invention provides a preparation method of a battery-grade nickel-cobalt-manganese ternary sulfate solution, which can effectively solve the problems.
The invention is realized in the following way:
the preparation method of the battery grade nickel-cobalt-manganese ternary sulfate solution comprises the following steps:
s1, uniformly mixing concentrated sulfuric acid and pure water to obtain a sulfuric acid solution;
S2, adding nickel and cobalt into the sulfuric acid solution, continuously stirring, introducing steam, heating and keeping the temperature at 80-90 ℃ for reaction for 6-8h;
s3, slowly adding manganese, adjusting the pH to 5-5.5 after the reaction is completed, filtering, and demagnetizing to obtain the battery grade nickel-cobalt-manganese ternary sulfate solution.
In some embodiments, in step S1, the sulfuric acid solution has a volume concentration of 4-6%.
In some embodiments, in step S2, the induced air is also turned on at the same time, reacting to the disappearance of the bubbles.
In some embodiments, in step S3, the slow manganese addition is preferably performed at a rate that does not overflow.
In some embodiments, in step S3, the adjusting pH is: if the pH of the solution is more than or equal to 5.5, adding a small amount of hydrogen peroxide, and if the pH of the solution is less than 5, adding 10wt% of sodium hydroxide at the same time, and adjusting the pH to 5-5.5.
In some embodiments, in step S3, the filtering is a post-press fine filtration.
The beneficial effects of the invention are as follows:
According to the invention, nickel, cobalt and manganese metals are directly used for batching, dissolving and removing impurities, and the battery-grade sulfate solution with qualified metal quantity proportion is prepared at one time, so that inaccurate batching caused by sulfate water content deviation or inaccurate batching caused by mass flowmeter deviation in the traditional method is avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of preparation of a battery grade nickel cobalt manganese ternary sulfate solution provided by an embodiment of the invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The embodiment of the invention provides a preparation method of a battery-grade nickel-cobalt-manganese ternary sulfate solution, which comprises the following steps:
s1, uniformly mixing concentrated sulfuric acid and pure water to obtain a sulfuric acid solution;
S2, adding nickel and cobalt into the sulfuric acid solution, continuously stirring, introducing steam, heating and keeping the temperature at 80-90 ℃ for reaction for 6-8h;
s3, slowly adding manganese, adjusting the pH to 5-5.5 after the reaction is completed, filtering, and demagnetizing to obtain the battery grade nickel-cobalt-manganese ternary sulfate solution.
In the embodiment of the invention, the metal simple substance is directly used, for example, the metal nickel is nickel bean or nickel powder (99.8%), the metal cobalt is cobalt bean or cobalt powder (99.8%), the metal manganese is manganese powder (99.5%), other auxiliary materials are not required to be added, the impurity is controllable, the requirement of preparing the battery-level ternary precursor on the impurity can be met, the one-time batching qualification rate is high, and the influence of factors such as raw material purity, moisture, accuracy of a mass flowmeter, temperature and the like is avoided; the metal proportion of the three-way precursor products can be adjusted according to the needs, such as 811/622/523 and the like.
According to the embodiment of the invention, according to the reactivity of nickel, cobalt and manganese, the method is divided into two sections, so that the alkali consumption is reduced, the reaction rate is improved, the prepared solution can be directly used for preparing ternary precursors for production, the processes of intermediate batching, detection and the like are reduced, and the production efficiency is improved.
In some embodiments, in step S1, the sulfuric acid solution has a volume concentration of 4-6%, which is determined according to the sulfate concentration required for precursor production.
In some embodiments, in step S2, the induced air is also turned on at the same time, reacting to the disappearance of the bubbles.
In some embodiments, in step S3, the slow manganese addition is preferably performed at a rate that does not overflow.
In some embodiments, in step S3, the adjusting pH is: if the pH of the solution is more than or equal to 5.5, adding a small amount of hydrogen peroxide, if the pH of the solution is less than 5, adding 10wt% of sodium hydroxide at the same time, and adjusting the pH to 5-5.5, wherein the pH can hydrolyze iron or aluminum introduced in the raw materials or the production process to become ferric hydroxide and aluminum hydroxide precipitate, so that the iron hydroxide and the aluminum hydroxide precipitate are separated.
In some embodiments, in step S3, the filtering is performed after the filter pressing, and this process is a impurity removal process, so as to ensure that the finished product meets the usage standard of the precursor.
Example 1
Taking nickel cobalt manganese 523 as an example, the raw materials of the ternary precursor are fed in two times.
The production raw materials are as follows: raw materials with mole fraction ratio: 1000kg of nickel beans, 400kg of cobalt beans, 560kg of manganese powder, 2400L of concentrated sulfuric acid, pure water, 28v/v% hydrogen peroxide and 10wt% sodium hydroxide.
(1) Preparing liquid: 50000L of pure water was added to the reaction vessel, 2400L of 98% concentrated sulfuric acid was slowly added to the pure water, and stirring was started during the process (time period was 0.5 h).
(2) Feeding 1: 1000kg of nickel beans and 400kg of cobalt beans are put into a reaction kettle for reaction, stirring is continuously carried out in the process, steam is introduced for heating, the temperature is kept at 80-90 ℃, and air introduction is started at the same time, the reaction is carried out until the acidity of the solution is about 1mol/L, and bubbles in the reaction kettle disappear (the reaction time is 6-8 h).
(3) Feeding 2: 560kg of manganese powder is slowly put into the reaction kettle in the last step, the speed is not increased, and after the material is put, the reaction is carried out until no bubbles are generated (a small amount of acid can be supplemented when the reaction is too slow, and the reaction time is about 4-8 h).
(4) Detecting the pH of the solution, and if the pH of the solution is more than or equal to 5, adding a small amount of hydrogen peroxide and then carrying out the next step; if the pH value of the solution is less than 5, adding hydrogen peroxide and 10wt% of liquid alkali at the same time to regulate the pH value to be more than or equal to 5 (reaction for 0-1 h).
(5) The solution is subjected to filter pressing, precise filtration, a pipeline demagnetizer and then transferred to a finished product storage tank, and sampling and inspection analysis (time consumption is 1.5 h).
The inspection method of the present embodiment is to perform inspection using ICP or atomic absorption spectroscopy.
The total time taken for this example was 12-19h.
The detection data are shown in Table 1.
Table 1 ternary nickel cobalt manganese feed liquid detection data
From the data in Table 1, it can be seen that the method of this example can control the ratio of nickel, cobalt and manganese and the final product can meet the usage standard of the precursor (GB/T26300-2020), and can directly perform precursor production.
Comparative example 1
Taking nickel cobalt manganese 523 as an example, three-way precursor raw materials are fed.
The production raw materials are as follows: raw materials with mole fraction ratio: 1000kg of nickel beans, 400kg of cobalt beans, 560kg of manganese powder, 2400kg of concentrated sulfuric acid, pure water, 28v/v% hydrogen peroxide and 10wt% sodium hydroxide.
(1) Preparing liquid: 50000L of pure water was added to the reaction vessel, 3000L of 98% concentrated sulfuric acid was slowly added to the pure water, and stirring was started during the process (time period was 0.5 h).
(2) Feeding: 2500kg of nickel beans are put into a reaction kettle, stirring is continuously carried out in the process, steam is introduced to heat the reaction kettle to keep the temperature at 80-90 ℃, and induced air is started at the same time, the reaction is carried out until the acidity of the solution is about 1mol/L, and bubbles in the reaction kettle disappear (the reaction time is 6-8 h).
(3) Detecting the pH of the solution, and if the pH of the solution is more than or equal to 5.5, adding a small amount of hydrogen peroxide, and then performing the next step; if the pH value of the solution is less than 5, adding hydrogen peroxide and 10wt% of liquid alkali at the same time to regulate the pH value to be more than or equal to 5 (reaction for 1-2 h).
(4) The nickel sulfate solution is subjected to filter pressing, precise filtration and pipeline demagnetizer and then transferred into a nickel sulfate finished product storage tank, and sampling and inspection analysis (time is 1.5 h).
(5) Repeating the steps 1-4, putting 2500kg of cobalt beans into a reaction kettle, preparing a cobalt sulfate solution, transferring the cobalt sulfate solution into a cobalt sulfate finished product storage tank, and sampling and inspecting for analysis (taking 9-12 h).
(6) Repeating the steps 1-4, putting 2500kg of manganese powder into a reaction kettle, preparing a manganese sulfate solution, transferring the manganese sulfate solution into a manganese sulfate finished product storage tank, and sampling and inspecting for analysis (which takes 7-10 h).
(7) And (3) batching: 1000kg of nickel sulfate, 400kg of cobalt sulfate and 560kg of manganese sulfate are taken after the concentration of the nickel cobalt manganese sulfate solution is calculated, and are mixed in a reaction kettle to prepare materials (the time is 0.5 h).
(8) And (5) transferring the mixture liquid to a finished product storage tank (consuming 1.5 h) after the mixture liquid is qualified for inspection and analysis.
The test method of this comparative example is the same as that of example 1.
The total time taken for this comparative example was 29-36h.
Comparative example 2
Taking nickel cobalt manganese 523 as an example, the raw materials of the ternary precursor are fed at one time.
The production raw materials are as follows: raw materials with mole fraction ratio: 1000kg of nickel beans, 400kg of cobalt beans, 560kg of manganese powder, 2400kg of concentrated sulfuric acid, pure water, 28v/v% hydrogen peroxide and 10wt% sodium hydroxide.
(1) Preparing liquid: 50000L of pure water was added to the reaction vessel, 2400L of 98% concentrated sulfuric acid was slowly added to the pure water, and stirring was started during the process (time period was 0.5 h).
(2) Feeding 1: 1000kg of nickel beans, 400kg of cobalt beans and 560kg of manganese powder are put into a reaction kettle for reaction, the stirring is continuously carried out in the process, the temperature is kept at 80-90 ℃ by introducing steam and heating, and meanwhile, the air introduction is started, the reaction is carried out until no obvious solid exists in the solution, and bubbles in the reaction kettle disappear (a small amount of acid can be supplemented when the reaction is too slow, and the reaction time is 16-24 h).
(3) Detecting the pH of the solution, and if the pH of the solution is more than or equal to 5.5, adding a small amount of hydrogen peroxide, and then performing the next step; if the pH value of the solution is less than 5, adding hydrogen peroxide and 10% of liquid alkali at the same time to regulate the pH value to be more than or equal to 5 (reaction for 0-1 h).
(4) Carrying out filter pressing on the solution, carrying out precise filtration, and transferring the solution into a finished product storage tank after a pipeline demagnetizer; sample and send analysis (1.5 h).
The test method of this comparative example is the same as that of example 1.
The total time spent for this comparative example was 20-27h.
Analysis of example 1, comparative examples 1 and 2 together found that the total consumption of example 1 was significantly lower than that of comparative examples 1 and 2. The analytical reasons are considered as follows: in example 1, the reaction rate was also fast in the case of low acid concentration due to strong metal activity of manganese powder, and the solution of charge 2 had the effect of adjusting pH at the same time, and the free acid in the solution after the reaction was small, and the time for adjusting pH was shortened. In comparative example 1, it took about 12 hours to prepare a single sulfate solution, it took 4.5 hours to detect a large amount of trisulfate solution, in order to ensure that the reaction rate was excessive each time the acid was excessive, the excessive acid in the solution was still much after the metal dissolution reaction was completed, the amount of alkali was large for adjusting the pH, and the time was long. In comparative example 2, since the manganese powder has strong metal activity, the manganese powder can react preferentially and react vigorously together, the feeding time can be longer to ensure safety, if acid is not added in the reaction process, the concentration of acid in the liquid after the manganese powder reacts is reduced, the reaction rate of nickel beans, cobalt beans and the reaction time is reduced, and the reaction time is prolonged.
In addition, in example 1, the pH adjustment time was short, and the alkali consumption was smaller than in comparative examples 1 and 2. In comparative example 1, in order to increase the rate and acid utilization rate in the actual production, a multistage gradient reaction was used to prepare a sulfate solution, and the equipment required for the production was large in area, and this problem was not found in example 1.
In summary, example 1 was fed in two runs, which was less time-consuming than both three runs and one run, and also less alkali consumption, with unexpected technical results and significant technical advances.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the battery grade nickel-cobalt-manganese ternary sulfate solution is characterized by comprising the following steps of:
s1, uniformly mixing concentrated sulfuric acid and pure water to obtain a sulfuric acid solution;
S2, adding nickel and cobalt into the sulfuric acid solution, continuously stirring, introducing steam, heating and keeping the temperature at 80-90 ℃ for reaction for 6-8h;
s3, slowly adding manganese, after the reaction is completed, regulating the pH to 5-5.5, filtering, and demagnetizing to obtain a battery-level nickel-cobalt-manganese ternary sulfate solution;
in the step S1, the volume concentration of the sulfuric acid solution is 4-6%;
In step S3, the pH adjustment is: if the pH of the solution is more than or equal to 5.5, adding a small amount of hydrogen peroxide, and if the pH of the solution is less than 5, adding 10wt% of sodium hydroxide at the same time, and adjusting the pH to 5-5.5.
2. The method for preparing a battery grade nickel cobalt manganese ternary sulfate solution according to claim 1, wherein in step S2, induced air is also started at the same time, and the reaction is carried out until bubbles disappear.
3. The method for producing a ternary sulfate solution of nickel, cobalt, and manganese in a battery grade according to claim 1, wherein in step S3, the slow manganese addition is preferably performed at a rate that does not overflow.
4. The method for preparing a battery grade nickel cobalt manganese ternary sulfate solution according to claim 1, wherein in step S3, the filtration is a fine filtration after press filtration.
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| CN109825714A (en) * | 2019-03-20 | 2019-05-31 | 兰州金川新材料科技股份有限公司 | A kind of method that nickel protoxide reclaimed materials is used to synthesize lithium electricity anode material precursor raw material |
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| KR101539749B1 (en) * | 2013-06-11 | 2015-07-28 | 주식회사 포스코 | Method for producing manganese precursors for lithium ion batteries, and manganese precursors for lithium ion batteries produced by the method |
| JP6365838B2 (en) * | 2014-11-28 | 2018-08-01 | 三菱マテリアル株式会社 | Cobalt nickel leaching method |
| CN105206889B (en) * | 2015-07-29 | 2018-10-26 | 浙江三晟化工有限公司 | A kind of processing method of waste and old nickle cobalt lithium manganate ternary cell positive material |
| CN110372038A (en) * | 2019-08-15 | 2019-10-25 | 衢州华友资源再生科技有限公司 | A kind of method of raw material containing manganese preparation LITHIUM BATTERY manganese sulfate and its LITHIUM BATTERY manganese sulfate of preparation |
| CN110607439A (en) * | 2019-09-12 | 2019-12-24 | 金川集团股份有限公司 | Spherical nickel protoxide sectional oxidation acid leaching treatment method |
| CN112159897B (en) * | 2020-09-09 | 2022-07-15 | 广东邦普循环科技有限公司 | Method for purifying nickel-cobalt-manganese leaching solution |
| CN113184927A (en) * | 2021-04-29 | 2021-07-30 | 金川集团镍盐有限公司 | Method for producing nickel sulfate solution by using nickel powder |
| CN113184928B (en) * | 2021-06-18 | 2023-04-21 | 芜湖佳纳新能源材料有限公司 | Preparation method of nickel sulfate solution |
| CN113562783B (en) * | 2021-07-30 | 2023-05-12 | 福建常青新能源科技有限公司 | Preparation method of nickel sulfate solution |
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