CN110092421A - A kind of production method of the spherical basic cobaltous carbonate of size tunable - Google Patents
A kind of production method of the spherical basic cobaltous carbonate of size tunable Download PDFInfo
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- CN110092421A CN110092421A CN201910364718.1A CN201910364718A CN110092421A CN 110092421 A CN110092421 A CN 110092421A CN 201910364718 A CN201910364718 A CN 201910364718A CN 110092421 A CN110092421 A CN 110092421A
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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
- C01G51/06—Carbonates
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
Abstract
The invention discloses a kind of production method of the spherical basic cobaltous carbonate of size tunable, the substantially steps of this method are as follows: 1. prepare solution;2. magnetic induced forming core;3. grain length is big;4. filters pressing and washing;5. drying.This method reduces forming core degree of supersaturation by way of the externally-applied magnetic field when synthesizing basic cobaltous carbonate, shorten the induced nucleation phase, moment forms a large amount of basic cobaltous carbonate nucleus in the solution, simultaneously, it can be good at adjusting the quality of product by control mixing speed, reaction temperature, the adding speed of cobalt liquid, achieve the effect that particle uniformly, spherical morphology, so that cobalt content is reached 52% or more.The granularity of basic cobaltous carbonate product of the present invention is in standardized normal distribution, particle is uniform, good fluidity, D50 maximum is more than 40 μm, realize the uniformity and stability of large-scale continuous production large granular spherical basic cobaltous carbonate partial size, and it is simple process, easily operated, low in cost, and high-quality raw material is provided to produce high-end lithium battery.
Description
Technical field
The present invention relates to field of chemical preparation, and in particular to a kind of producer of the spherical basic cobaltous carbonate of size tunable
Method.
Background technique
Basic cobaltous carbonate [2CoCO3·3Co(OH)2·H2O] it is a kind of aubergine prism sprills, it is dissolved in diluted acid and liquid
Ammonia is practically insoluble in cold water, decomposes in the hot water, is mainly used in and prepares various cobalt products, for example, cobalt powder, cobaltosic oxide,
Cobalt oxide etc., the hot succession very big with the performance some of its presoma cobalt carbonate of the powder such as granularity, the pattern of these cobalt products
Property, and have extensive purposes in fields such as electronics, metallurgy, chemical industry, especially it is used as LITHIUM BATTERY Co in battery industry3O4Forerunner
Body.Meanwhile the preparation process of cobalt acid lithium shows that cobalt acid lithium, which can be improved, using big partial size spherical cobaltic-cobaltous oxide prepared now
The reactivity of journey improves discharge platform, therefore, big four oxidation three of big partial size spherical shape of preparation quality stabilization, spherical morphology, partial size
Cobalt precursor has become research hotspot.
In the development process of basic cobaltous carbonate production method, most original is to carry out production Co by semi-mechanized operation
[(OH)2]a[CO3] 1-a, but the production technology period is long, and washing step time-consuming takes 3-4 days at the soonest, and technological parameter is cumbersome
Complexity is not easy to grasp, meanwhile, drying time is long in the production technology, and temperature distribution is non-uniform, be easy to cause local temperature mistake
Height, product particle is small, reunites serious, spherical shape is poor.So then replaced by a kind of quick basic cobaltous carbonate production technology,
The processing step is substantially are as follows: dissolution, synthesis, filtering, washing, drying;Wherein, cobalt chloride and sodium carbonate dissolve in course of dissolution
Ratio example in mass ratio are as follows: CoCl2:H2O=1:4-8, Na2CO3:H2O=1:4-8;Wherein, aqueous slkali and chlorine in the synthesis process
Changing cobalt liquor takes spray mode to be added, and synthesising reacting time is 2-4 hours.This technological operation is simple, with short production cycle;But
It is that the properties of product produced are unstable, it is oxidizable, and also product particle is uneven, and granularity is small, granularity difficulty control, cobalt tenor
It can only achieve 46%-50%, therefore be unfavorable for efficiently refining production, be easy to produce great waste.Now, and one is developed
Kind produces basic cobaltous carbonate material in such a way that nanometer synthesizes, and the technology is although more advanced, guaranteed to product quality,
But production cost is but very high, requires precision to equipment and instrument, and it is costly, therefore, large area also is done without condition now
It promotes.
Summary of the invention
(1) technical problems to be solved
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of spherical basic cobaltous carbonates of size tunable
Production method.
(2) technical solution
In order to solve the above-mentioned technical problems, the present invention provides the lifes of the spherical basic cobaltous carbonate of such a size tunable
Production method, the specific steps of the production method are as follows:
Step 1: preparing solution;1. the preparation of cobalt liquor, by cobalt liquor it is purified after, be configured to Co2+Concentration is 0.5-
The soluble cobalt solution of 3mol/L;2. the preparation of precipitant solution prepares Na with soda ash2CO3Solution, then by Na2CO3Solution
Calcium ion and magnesium ion are removed through ion exchange, controls Na in solution after removing calcium ion and magnesium ion2CO3Concentration be 80g/
L-200g/L, and control the concentration of calcium constituent and magnesium elements in solution and be respectively less than 0.001g/L, then by Na2CO3Solution and deionization
Water is that 1:1 is added in reaction kettle as bottom water by volume, and heat temperature raising simultaneously stirs, and mixing speed is controlled in 300-
1000rpm;
Step 2: magnetic induced forming core;Before basic cobaltous carbonate forming core, field generator for magnetic is opened, according to size of current
Required magnetic field strength is regulated, sodium ascorbate is added into reaction kettle, by soluble cobalt solution and precipitant solution
It is added in reaction kettle in the form of cocurrent, by sodium ascorbate to prevent from being oxidized in synthesis;After the completion of forming core, in reaction kettle
Middle carry out ripening, digestion time are 0.5-1.5 hours, keep temperature constant;
Step 3: grain length is big;After the completion of ageing, soluble cobalt solution and precipitant solution are added in the form of cocurrent
In reaction kettle, it is 1-1.3 that precipitating reagent and the molar ratio of cobalt salt, which is added, in control, and control mixing speed is 100~500rpm, reaches institute
It needs to stop being added dropwise when granule size;
Step 4: filters pressing and washing;Filters pressing is carried out to reaction solution, solid product is obtained, uses deionized water again later
Solid product is washed, and is added to it sodium ascorbate in washing process, by sodium ascorbate to prevent from producing
Product oxidation;
Step 5: dry;After the completion of washing, solid product is placed in cyclone type flash drying equipment and is dried,
In the drying process, material is by Mechanical Crushing under the action of stirring crushing device, and water capacity is lower and the lesser material of particle
Rise together with swirling eddy, and separator is delivered to by discharge port and carries out gas solid separation, to obtain spherical basic cobaltous carbonate
Finished product.
Preferably, in step 1, the soluble cobalt solution is cobalt chloride, cobaltous sulfate or cobalt nitrate;The heating
The temperature of heating is controlled at 45-85 DEG C.
Preferably, in step 2, the current control of the field generator for magnetic is in 5-60A;Control the pH of reaction end
For 6.7-7.2;The additive amount for controlling sodium ascorbate is the 0.2-2% of cobalt metal element quality.
Preferably, in step 3, the pH for controlling reaction process is 7.2-7.5.
Preferably, in step 4, the dosage of the deionized water is that solid product per ton uses 8-20m3。
Preferably, in step 5, drying temperature is controlled at 100-130 DEG C.
This method reduces forming core degree of supersaturation by way of the externally-applied magnetic field when synthesizing basic cobaltous carbonate, shortens induction shape
The core phase, moment forms a large amount of basic cobaltous carbonate nucleus in the solution, meanwhile, pass through control mixing speed, reaction temperature, cobalt liquid
Adding speed can be good at adjust product quality, achieve the effect that particle uniformly, spherical morphology, so that cobalt content is reached
52% or more.Meanwhile addition additive sodium ascorbate can prevent the oxidation of product in reaction and wash water, due to product spherical shape
Well, particle is big, and strainability is good, the washing removal of impurity The book of Changes deionized water, and liquid is can be recycled by sewage treatment after wash water.
The granularity of basic cobaltous carbonate product of the present invention is in standardized normal distribution, and particle is uniform, good fluidity, and D50 maximum is more than 40 μm, real
Showed it is large-scale continuous production large granular spherical basic cobaltous carbonate partial size uniformity and stability, and simple process, easily
In operation, low in cost, and high-quality raw material is provided for the high-end lithium battery of production.
(3) beneficial effect
Compared with prior art, the present invention the production method simple process, based on homogeneous nucleation principle and utilizes " magnetic
Induction nucleation " technology is acted under the conditions of spraying dropwise addition by additional electromagnetic field, and it is critical to can reduce basic carbonate cobalt liquor
Degree of supersaturation accelerates basic cobaltous carbonate nucleation, shortens nucleation induction period, reaches the quick forming core of induction, and moment obtains a large amount of tiny
The consistent nucleus of crystalline form.Its mechanism is mainly Co under the influence of Lorentz force, in solution2+And CO3 2-、OH?It is ionized Deng band
The sub- direction of motion will deviate round about, increase Co2+And CO3 2-、OH?Interionic collision probability accelerates cenotype nucleus
Generation.It separates forming core independently with the stage of growing up, after the completion of forming core, passes through the reaction solution molecule of subsequent addition sufficiently right
Stream, reach and be adsorbed on plane of crystal, then binding molecule migrates into lattice under magnetic fields, thus allow crystal grain equably
It grows up, forms spherical morphology product.
xCo2++yCO3 2-+zOH-→Cox(OH)y(CO3)z↓ (1)
In growth process, it can be good at adjusting the matter of product by control mixing speed, reaction temperature, pH value in reaction
Amount, reaches evengranular effect, and be adjusted product particle size according to product specification, keeps its strainability good, wash water
Amount is few, meanwhile, additive sodium ascorbate is added when reaction and in wash water can prevent the oxidation of product, product quality can reach with
Lower standard: Co52% ± 0.5, H2O≤3%, Fe≤10ppm, Mg≤10ppm, NH4 +≤300ppm、Na≤100ppm、Cl≤
300ppm, Ca≤10ppm, Al≤5.0ppm, Cu≤5.0ppm, Mn≤5.0ppm, Ni≤5.0ppm, Zn≤5.0ppm, loose ratio
≥0.30g/cm3, and the granularity of basic cobaltous carbonate product is in standardized normal distribution, and particle is uniform, good fluidity, and D50 is maximum
More than 40 μm.Make entire production procedure easy to operate, at low cost in this way, while reducing labor intensity, and improves life
Efficiency, and non-environmental-pollution are produced, can be used for being widely applied.
Detailed description of the invention
Illustrate the specific embodiment of the invention or technical solution in the prior art in order to clearer, it below will be to specific
Embodiment describes required attached drawing in the prior art and is briefly described, it should be apparent that, it is described below
Attached drawing is only one embodiment of the present invention, to those skilled in the art, is not being made the creative labor
Under the premise of, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is the SEM figure that cobalt carbonate is prepared in embodiment 1.
Fig. 2 is the SEM figure that cobalt carbonate is prepared in embodiment 2.
Fig. 3 is the SEM figure that cobalt carbonate is prepared in embodiment 3.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below to this
Technical solution in invention specific embodiment carries out clear, complete description, with the present invention is further explained, it is clear that retouched
The specific embodiment stated is only a part of embodiment of the invention, rather than whole patterns.
Embodiment 1
Present embodiment is a kind of production method of the spherical basic cobaltous carbonate of size tunable, is included the following steps:
A. solution is prepared;1. CoCl is selected in the preparation of cobalt liquor2Solution is configured to Co as cobalt source2+Concentration is
The soluble cobalt solution of 0.5mol/L.2. the preparation of precipitant solution prepares Na with soda ash2CO3Solution, then by Na2CO3It is molten
Liquid removes calcium and magnesium ion through ion exchange, the Na after removing calcium and magnesium ion2CO3Solution concentration is controlled in 80g/L, wherein and Ca <
0.001g/L, Mg < 0.001g/L, then by Na2CO3Solution and deionized water are that 1:1 is added in reaction kettle the bottom of as by volume
Water heats up and stirs, and wherein in 300rpm, reaction temperature is 45 DEG C for mixing speed control;
B. magnetic induced forming core;Field generator for magnetic is opened, adjusting magnetic field generator size of current is 5A, and cobalt chloride is molten
Liquid and sodium carbonate liquor cocurrent form are added in reaction kettle, and the ascorbic acid of cobalt weight metal 0.2% is added into reaction kettle
Sodium, by sodium ascorbate to prevent from being oxidized in synthesis;Controlling solution terminal pH is 6.7, after the completion of forming core, in a kettle
Ripening is carried out, digestion time is 0.5 hour, and temperature keeps constant temperature;
C. crystal grain is grown up;After being aged, cobalt chloride solution and sodium carbonate liquor cocurrent form are added in reaction kettle, are added
Sodium carbonate and cobalt salt molar ratio are 1-1.3, control the pH of reaction process 7.2.It is big to reach required granularity by mixing speed 100rpm
Hour stops being added dropwise;
D. filters pressing and washing;It is washed with deionized after filters pressing, sodium ascorbate is added in washing process prevents product oxygen
Change, deionized water dosage is product 20m per ton3Deionized water.
E. it dries;Drying process will be completed in cyclone type flash drying equipment, and drying temperature is controlled at 130 DEG C, by going out
Material mouth is delivered to separator and carries out gas solid separation, completes finished product and collects and pack.
Embodiment 2
Present embodiment is a kind of production method of the spherical basic cobaltous carbonate of size tunable, is included the following steps:
A. solution is prepared;1. CoSO is selected in the preparation of cobalt liquor4Solution is configured to Co as cobalt source2+Concentration is 2mol/L
Soluble cobalt solution.2. the preparation of precipitant solution prepares Na with soda ash2CO3Solution, then by Na2CO3Solution is through ion
Exchange removal calcium and magnesium ion, the Na after removing calcium and magnesium ion2CO3Solution concentration is controlled in 150g/L, wherein Ca < 0.001g/
L, Mg < 0.001g/L, then by Na2CO3Solution and deionized water are that 1:1 is added in reaction kettle as bottom water by volume, and heating is simultaneously
Stirring, wherein in 500rpm, reaction temperature is 60 DEG C for mixing speed control;
B. magnetic induced forming core;Field generator for magnetic is opened, adjusting magnetic field generator size of current is 25A, by cobalt chloride
Solution and sodium carbonate liquor cocurrent form are added in reaction kettle, and the Vitamin C of cobalt weight metal 0.8% is added into reaction kettle
Sour sodium, by sodium ascorbate to prevent from being oxidized in synthesis;Controlling solution terminal pH is 7.0, after the completion of forming core, in reaction kettle
Middle carry out ripening, digestion time are 1 hour, and temperature keeps constant temperature;
C. crystal grain is grown up;After being aged, cobalt chloride solution and sodium carbonate liquor cocurrent form are added in reaction kettle, are added
Sodium carbonate and cobalt salt molar ratio are 1-1.3, control the pH of reaction process 7.3.It is big to reach required granularity by mixing speed 300rpm
Hour stops being added dropwise;
D. filters pressing and washing;It is washed with deionized after filters pressing, sodium ascorbate is added in washing process prevents product oxygen
Change, deionized water dosage is product 15m per ton3Deionized water.
E. it dries;Drying process will be completed in cyclone type flash drying equipment, and drying temperature is controlled at 115 DEG C, by going out
Material mouth is delivered to separator and carries out gas solid separation, completes finished product and collects and pack.
Embodiment 3
Present embodiment is a kind of production method of the spherical basic cobaltous carbonate of size tunable, is included the following steps:
A. solution is prepared;1. Co (NO is selected in the preparation of cobalt liquor3)3Solution is configured to Co as cobalt source2+Concentration is
The soluble cobalt solution of 2.5mol/L.2. the preparation of precipitant solution prepares Na with soda ash2CO3Solution, then by Na2CO3It is molten
Liquid removes calcium and magnesium ion through ion exchange, the Na after removing calcium and magnesium ion2CO3Solution concentration is controlled in 200g/L, wherein and Ca <
0.001g/L, Mg < 0.001g/L, then by Na2CO3Solution and deionized water are that 1:1 is added in reaction kettle the bottom of as by volume
Water heats up and stirs, and wherein in 1000rpm, reaction temperature is 85 DEG C for mixing speed control;
B. magnetic induced forming core;Field generator for magnetic is opened, adjusting magnetic field generator size of current is 60A, by cobalt chloride
Solution and sodium carbonate liquor cocurrent form are added in reaction kettle, and the ascorbic acid of cobalt weight metal 2% is added into reaction kettle
Sodium, by sodium ascorbate to prevent from being oxidized in synthesis;Controlling solution terminal pH is 7.2, after the completion of forming core, in a kettle
Ripening is carried out, digestion time is 1.5 hours, and temperature keeps constant temperature;
C. crystal grain is grown up;After being aged, cobalt chloride solution and sodium carbonate liquor cocurrent form are added in reaction kettle, are added
Sodium carbonate and cobalt salt molar ratio are 1-1.3, control the pH of reaction process 7.5.It is big to reach required granularity by mixing speed 500rpm
Hour stops being added dropwise;
D. filters pressing and washing;It is washed with deionized after filters pressing, sodium ascorbate is added in washing process prevents product oxygen
Change, deionized water dosage is product 8m per ton3Deionized water.
E. it dries;Drying process will be completed in cyclone type flash drying equipment, and drying temperature is controlled at 100 DEG C, by going out
Material mouth is delivered to separator and carries out gas solid separation, completes finished product and collects and pack.
The foregoing describe technical characteristics of the invention and basic principle and associated advantages, for those skilled in the art
For, it is clear that the present invention is not limited to the details of above-mentioned exemplary embodiment, and without departing substantially from design of the invention or
In the case where essential characteristic, the present invention can be realized in other specific forms.Therefore, in all respects, should all incite somebody to action
Above-mentioned specific embodiment regards exemplary as, and is non-limiting, the scope of the present invention by appended claims and
It is not that above description limits, it is intended that all changes that come within the meaning and range of equivalency of the claims are included
In the present invention.
Although not each embodiment is only in addition, it should be understood that this specification is described according to each embodiment
It contains an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art answer
When considering the specification as a whole, the technical solution in each embodiment may also be suitably combined to form art technology
The other embodiments that personnel are understood that.
Claims (6)
1. a kind of production method of the spherical basic cobaltous carbonate of size tunable, which is characterized in that the specific steps of the production method
Are as follows:
Step 1: preparing solution;1. the preparation of cobalt liquor, by cobalt liquor it is purified after, be configured to Co2+Concentration is 0.5-3mol/L
Soluble cobalt solution;2. the preparation of precipitant solution prepares Na with soda ash2CO3Solution, then by Na2CO3Solution is through ion
Exchange removal calcium ion and magnesium ion control Na in solution after removing calcium ion and magnesium ion2CO3Concentration be 80g/L-200g/
L, and control the concentration of calcium constituent and magnesium elements in solution and be respectively less than 0.001g/L, then by Na2CO3Solution and deionized water press body
Product is than being that 1:1 is added in reaction kettle as bottom water, and heat temperature raising simultaneously stirs, and mixing speed is controlled in 300-1000rpm;
Step 2: magnetic induced forming core;Before basic cobaltous carbonate forming core, field generator for magnetic is opened, is added into reaction kettle anti-
Bad hematic acid sodium, soluble cobalt solution and precipitant solution are added in reaction kettle in the form of cocurrent;After the completion of forming core, anti-
It answers and carries out ripening in kettle, digestion time is 0.5-1.5 hours, keeps temperature constant;
Step 3: grain length is big;After the completion of ageing, soluble cobalt solution is added in the form of cocurrent with precipitant solution and is reacted
In kettle, it is 1-1.3 that precipitating reagent and the molar ratio of cobalt salt, which is added, in control, and control mixing speed is 100~500rpm, reaches required grain
Stop being added dropwise when spending size;
Step 4: filters pressing and washing;Filters pressing is carried out to reaction solution, obtains solid product, later again with deionized water to solid
Body product is washed, and sodium ascorbate is added to it in washing process;
Step 5: dry;After the completion of washing, solid product is placed in cyclone type flash drying equipment and is dried, dry
During dry, material is by Mechanical Crushing under the action of stirring crushing device, and water capacity is lower and the lesser material of particle is with rotation
Turn air-flow to rise together, and separator is delivered to by discharge port and carries out gas solid separation, to obtain spherical basic cobaltous carbonate finished product.
2. a kind of production method of the spherical basic cobaltous carbonate of size tunable according to claim 1, which is characterized in that
In step 1, the soluble cobalt solution is cobalt chloride, cobaltous sulfate or cobalt nitrate;The temperature control of the heat temperature raising exists
45-85℃。
3. a kind of production method of the spherical basic cobaltous carbonate of size tunable according to claim 1, which is characterized in that
In step 2, the current control of the field generator for magnetic is in 5-60A;The pH for controlling reaction end is 6.7-7.2;It controls anti-bad
The additive amount of hematic acid sodium is the 0.2-2% of cobalt metal element quality.
4. a kind of production method of the spherical basic cobaltous carbonate of size tunable according to claim 1, which is characterized in that
In step 3, the pH for controlling reaction process is 7.2-7.5.
5. a kind of production method of the spherical basic cobaltous carbonate of size tunable according to claim 1, which is characterized in that
In step 4, the dosage of the deionized water is that solid product per ton uses 8-20m3。
6. a kind of production method of the spherical basic cobaltous carbonate of size tunable according to claim 1, which is characterized in that
In step 5, drying temperature is controlled at 100-130 DEG C.
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CN112158892A (en) * | 2020-08-27 | 2021-01-01 | 格林美股份有限公司 | Preparation method of cobalt carbonate for lithium ion battery |
CN112158892B (en) * | 2020-08-27 | 2022-09-02 | 格林美股份有限公司 | Preparation method of cobalt carbonate for lithium ion battery |
CN111825125A (en) * | 2020-09-16 | 2020-10-27 | 金驰能源材料有限公司 | Doped basic cobalt carbonate/cobalt carbonate composite precursor and preparation method and application thereof |
CN112846213A (en) * | 2021-01-05 | 2021-05-28 | 有研工程技术研究院有限公司 | Preparation method of low-oxygen high-dispersion nano spherical cobalt powder |
CN114873653A (en) * | 2022-05-11 | 2022-08-09 | 金驰能源材料有限公司 | Basic cobalt carbonate and preparation method thereof |
CN114873653B (en) * | 2022-05-11 | 2023-10-13 | 金驰能源材料有限公司 | Basic cobalt carbonate and preparation method thereof |
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