CN106365211A - Preparation method of NCA precursor - Google Patents
Preparation method of NCA precursor Download PDFInfo
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- CN106365211A CN106365211A CN201610770151.4A CN201610770151A CN106365211A CN 106365211 A CN106365211 A CN 106365211A CN 201610770151 A CN201610770151 A CN 201610770151A CN 106365211 A CN106365211 A CN 106365211A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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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
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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
- C01P2004/01—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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2006/11—Powder tap density
Abstract
The invention discloses a preparation method of an NCA precursor. The preparation method comprises the following steps: mixing water-soluble salt of Ni and water-soluble salt of Co, and preparing into an aqueous solution to obtain a mixed ion solution, wherein in the mixed ion solution, the concentration of mixed ions comprising Ni<2+> and Co<2+> is in the range of 0.8-2.3 mol/L; preparing a mixed alkali liquid: preparing a sodium hydroxide solution with the concentration of 0.5-4.0 mol/L first, then adding a certain amount of aluminum sulfate solid with the concentration of 0.2-0.5 mol/L, completely dissolving, adding ammonia water with the concentration of 0.05-1.0 mol/L to obtain the mixed alkali solution II; continuously adding the mixed ion solution into a reactor, performing an equimolar synthesis reaction on the mixed ion solution and the mixed alkali solution, and constantly adjusting the flow rate to stabilize the pH during the reaction; performing solid-liquid separation on a synthetic product in the step, washing obtained solid, and drying to obtain a ternary cathode material NCA precursor.
Description
Technical field
The present invention relates to nca forerunner's Antibody Production Techniques, more particularly, to a kind of preparation method of nca presoma.
Background technology
Conventional nca forerunner's Antibody Production Techniques lead to aluminum in the nickel cobalt aluminum hydroxide prepared due to the defect of batching mode
Uneven inside and outside content, density and pattern fluctuation larger so that nca material technique in sintering process cannot be stablized, need pin
Different sintering process are adjusted to different production batch, have impact on quality stability and production efficiency.
The invention of this technology, can be conducive to stablizing course of reaction, aluminium salt is added in alkali liquor and carries out precipitation again
Make the aluminium content in granule more uniform, and more efficiently complexation aluminium ion, the nickel cobalt aluminum hydroxide content produced
Stable, physicochemical property is good so that follow-up sintering circuit stablizes controlled, and the nca anode material for lithium-ion batteries sintering out
Chemical property more excellent.
Content of the invention
Problem to be solved by this invention be stablize aluminum ions precipitation process so as to be evenly embedded into and be coated on nickel,
Around cobalt ion, to reach each element stable content of precipitation product nickel cobalt aluminium hydroxide, it is evenly distributed.
The present invention is dissolved in sodium hydroxide lye using aluminum sulfate and adds appropriate ammonia, then with nickel sulfate, sulphuric acid
Cobalt mixed solution carries out precipitation, and uniformly, stable performance, in order to realize for the aluminium-hydroxide powder constituent content obtaining after reaction
Above-mentioned purpose, the technical scheme is that
1st, a kind of preparation method of nca presoma, the method comprises the steps:
(1) water soluble salt of the water soluble salt of ni, co is mixed and be configured to aqueous solution, obtain mixed ion solutions；Wherein institute
State mixed ion solutions and include ni2+And co2+Hybrid ionic concentration in the range of 0.8～2.3mol/l；
(2) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 0.5～4.0mol/l, is subsequently adding a certain amount of
Aluminum sulfate solid, concentration be 0.1～0.4mol/l, after being completely dissolved, add ammonia, concentration be 0.05～1.0mol/l, extremely
The configuration of this mixed ammonium/alkali solutions completes；
(3) configure mixed ammonium/alkali solutions, first configuration concentration is the sodium hydroxide solution of 0.5～4.0mol/l, be subsequently adding certain
The aluminum sulfate solid of amount, concentration is 0.2～0.5mol/l, after being completely dissolved, adds ammonia, and concentration is 0.05～1.0mol/l,
So far mixed ammonium/alkali solutions configuration completes；
(4) described to (1) mixed ion solutions are added continuously in reactor carry out with mixed ammonium/alkali solutions and mixed ammonium/alkali solutions
Equimolar synthetic reaction, mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and are carried out with the order of mixed ammonium/alkali solutions, and constantly
Adjust flow with the ph value of stable reaction；
(5) synthetic product of step (4) is carried out solid-liquid separation, gained solid is through washing, being dried to obtain tertiary cathode material
Nca presoma.Gained ternary precursor nickel cobalt aluminium hydroxide narrow diameter distribution, component is uniform, and size tunable, sulfate
Impurity is low.
Mixed ion solutions described in step (4) with 300～600l/h flow be added continuously in reactor with mixed base
Solution and mixed ammonium/alkali solutions carry out equimolar synthetic reaction, and mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and use mixed base again
The order of solution is carried out, and constantly regulate flow is with the ph value of stable reaction, and described temperature of reactor is 30～60 DEG C, stirring
Speed is 600～1200r/min.
Nickel, cobalt, the molar ratio of aluminum are: 0.8:0.15:0.05, its molecular formula is: ni0.8co0.15al0.05(oh)2.05.
Patent advantage
The present invention is dissolved in sodium hydroxide lye using aluminum sulfate and adds appropriate ammonia, using aluminum sulfate as alkali liquor group
Become part, then carry out coprecipitation reaction with nickel sulfate, cobaltous sulfate mixed solution, the aluminium hydrate powder last element obtaining after reaction contains
Uniformly, impurity is low, every stable physical-chemical indexes for amount.
Using this kind of batching mode, aluminium ion precipitation uniformly, stable content, in the nca granular precursor prepared aluminum from
Sub is evenly distributed, stable content, and the nca material electrochemical performance sintering out is good.
Figure of description
Fig. 1 schemes for sem of the present invention.
Specific embodiment
Embodiment 1
The invention provides a kind of preparation method of nca presoma, the method comprises the steps:
(1) water soluble salt of the water soluble salt of ni, co is mixed and be configured to aqueous solution, obtain mixed ion solutions, wherein institute
State mixed ion solutions and include ni2+And co2+Hybrid ionic concentration be 1.5mol/l；
(2) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 3.0mol/l, is subsequently adding a certain amount of sulfur
Sour aluminum solid, concentration is 0.2mol/l, after being completely dissolved, adds ammonia, and concentration is 0.1mol/l, and so far mixed ammonium/alkali solutions are joined
Put and complete；
(3) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 3.0mol/l, is subsequently adding a certain amount of sulfur
Sour aluminum solid, concentration is 0.3mol/l, after being completely dissolved, adds ammonia, and concentration is 0.1mol/l, and so far mixed ammonium/alkali solutions are joined
Put and complete；
(4) by described to (1) mixed ion solutions with 400l/h flow be added continuously in reactor with mixed ammonium/alkali solutions and mixing
Aqueous slkali carries out equimolar synthetic reaction, and mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and use the suitable of mixed ammonium/alkali solutions again
Sequence is carried out, and constantly regulate flow is with the ph value of stable reaction, and described temperature of reactor is 40 DEG C, and mixing speed is 800r/
min；
(5) synthetic product of step (4) is carried out solid-liquid separation, gained solid is through washing, being dried to obtain tertiary cathode material
Nca presoma, gained ternary precursor nickel cobalt aluminium hydroxide narrow diameter distribution, component is uniform, and size tunable, sulfate
Impurity is low.
Embodiment 2
The invention provides a kind of preparation method of nca presoma, the method comprises the steps:
(1) water soluble salt of the water soluble salt of ni, co is mixed and be configured to aqueous solution, obtain mixed ion solutions；Wherein institute
State mixed ion solutions and include ni2+And co2+Hybrid ionic concentration in the range of 1.0mol/l；
(2) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 2mol/l, is subsequently adding a certain amount of sulphuric acid
Aluminum solid, concentration is 0.3mol/l, after being completely dissolved, adds ammonia, and concentration is 0.3mol/l, so far mixed ammonium/alkali solutions configuration
Complete；
(3) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 2.0mol/l, is subsequently adding a certain amount of sulfur
Sour aluminum solid, concentration is 0.4mol/l, after being completely dissolved, adds ammonia, and concentration is 0.4mol/l, and so far mixed ammonium/alkali solutions are joined
Put and complete；
(4) by described to (1) mixed ion solutions with 500l/h flow be added continuously in reactor with mixed ammonium/alkali solutions and mixing
Aqueous slkali carries out equimolar synthetic reaction, and mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and use the suitable of mixed ammonium/alkali solutions again
Sequence is carried out, and constantly regulate flow is with the ph value of stable reaction, and described temperature of reactor is 50 DEG C, and mixing speed is 800r/
min；
(5) synthetic product of step (4) is carried out solid-liquid separation, gained solid is through washing, being dried to obtain tertiary cathode material
Nca presoma.Gained ternary precursor nickel cobalt aluminium hydroxide narrow diameter distribution, component is uniform, and size tunable, sulfate
Impurity is low.
Embodiment 3
The invention provides a kind of preparation method of nca presoma, the method comprises the steps:
(1) water soluble salt of the water soluble salt of ni, co is mixed and be configured to aqueous solution, obtain mixed ion solutions；Wherein institute
State mixed ion solutions and include ni2+And co2+Hybrid ionic concentration in the range of 1.5mol/l；
(2) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 3.0mol/l, is subsequently adding a certain amount of sulfur
Sour aluminum solid, concentration is 0.25mol/l, after being completely dissolved, adds ammonia, and concentration is 0.25mol/l, so far mixed ammonium/alkali solutions
Configuration completes；
(3) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 3.0mol/l, is subsequently adding a certain amount of sulfur
Sour aluminum solid, concentration is 0.4mol/l, after being completely dissolved, adds ammonia, and concentration is 0.25mol/l, so far mixed ammonium/alkali solutions
Configuration completes；
(4) by described to (1) mixed ion solutions with 500l/h flow be added continuously in reactor with mixed ammonium/alkali solutions and mixing
Aqueous slkali carries out equimolar synthetic reaction, and mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and use the suitable of mixed ammonium/alkali solutions again
Sequence is carried out, and constantly regulate flow is with the ph value of stable reaction, and described temperature of reactor is 50 DEG C, and mixing speed is 1200r/
min；
(5) synthetic product of step (4) is carried out solid-liquid separation, gained solid is through washing, being dried to obtain tertiary cathode material
Nca presoma.Gained ternary precursor nickel cobalt aluminium hydroxide narrow diameter distribution, component is uniform, and size tunable, sulfate
Impurity is low.
Experimental data statistical table
| Project | Experiment 1 | Experiment 2 | Experiment 3 | Experiment 4 | Experiment 5 | Experiment 6 |
| Salt flow (l/h) | 457 | 452 | 452 | 455 | 454 | 453 |
| Salinity (mol/l) | 2.0 | 2.1 | 2.2 | 2.3 | 2.1 | 2.2 |
| Flux of alkaline liquor (l/h) | 451 | 454 | 451 | 454 | 456 | 454 |
| Flux of alkaline liquor (l/h) | 454 | 452 | 451 | 454 | 452 | 456 |
| Alkali liquor () concentration (mol/l) | 4.0 | 4.2 | 4.4 | 4.6 | 4.2 | 4.4 |
| Ph value | 11.4 | 11.3 | 11.3 | 11.4 | 11.5 | 11.4 |
| Reaction temperature (DEG C) | 56 | 56.5 | 56 | 56.3 | 56.2 | 56.3 |
| Granularity d10(µm) | 6.3 | 6.5 | 6.3 | 6.7 | 6.4 | 6.5 |
| Granularity d50(µm) | 11.4 | 11.2 | 11.5 | 11.4 | 11.6 | 11.1 |
| Granularity d90(µm) | 23.2 | 23.6 | 23.8 | 24.1 | 24.5 | 24.2 |
| Tap density (g/cm3) | 2.01 | 2.1 | 2.08 | 2.12 | 2.15 | 2.17 |
| so4 2-% | 0.45 | 0.43 | 0.46 | 0.52 | 0.51 | 0.5 |
Claims (3)
1. a kind of preparation method of nca presoma, the method comprises the steps:
(1) water soluble salt of the water soluble salt of ni, co is mixed and be configured to aqueous solution, obtain mixed ion solutions；Wherein institute
State mixed ion solutions and include ni2+And co2+Hybrid ionic concentration in the range of 0.8～2.3mol/l；
(2) mixed ammonium/alkali solutions are configured, first configuration concentration is the sodium hydroxide solution of 0.5～4.0mol/l, is subsequently adding a certain amount of
Aluminum sulfate solid, concentration be 0.1～0.4mol/l, after being completely dissolved, add ammonia, concentration be 0.05～1.0mol/l, extremely
The configuration of this mixed ammonium/alkali solutions completes；
(3) configure mixed ammonium/alkali solutions, first configuration concentration is the sodium hydroxide solution of 0.5～4.0mol/l, be subsequently adding certain
The aluminum sulfate solid of amount, concentration is 0.2～0.5mol/l, after being completely dissolved, adds ammonia, and concentration is 0.05～1.0mol/l,
So far mixed ammonium/alkali solutions configuration completes；
(4) described to (1) mixed ion solutions are added continuously in reactor carry out with mixed ammonium/alkali solutions and mixed ammonium/alkali solutions
Equimolar synthetic reaction, mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and are carried out with the order of mixed ammonium/alkali solutions, and constantly
Adjust flow with the ph value of stable reaction；
(5) synthetic product of step (4) is carried out solid-liquid separation, gained solid is through washing, being dried to obtain tertiary cathode material
Nca presoma, gained ternary precursor nickel cobalt aluminium hydroxide narrow diameter distribution, component is uniform, and size tunable, sulfate
Impurity is low.
2. the preparation method of a kind of nca presoma according to claim 1, is characterized in that: mix described in step (4) from
Sub- solution is added continuously in reactor to carry out with mixed ammonium/alkali solutions and mixed ammonium/alkali solutions etc. rub with 300～600l/h flow
That synthetic reaction, mixed ammonium/alkali solutions are finished according to mixed ammonium/alkali solutions and are carried out with the order of mixed ammonium/alkali solutions, and constantly regulate
Flow is 30～60 DEG C with the ph value of stable reaction, described temperature of reactor, and mixing speed is 600～1200r/min.
3. the preparation method of a kind of nca presoma according to claim 1, is characterized in that: nickel, cobalt, the molar ratio of aluminum
For: 0.8:0.15:0.05, its molecular formula is: ni0.8co0.15al0.05(oh)2.05.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467069A (en) * | 2018-04-12 | 2018-08-31 | 安徽同心化工有限公司 | The nickel cobalt aluminium ternary material precursor and its preparation process of a kind of extremely low impurity content and application |
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| CN104934595A (en) * | 2015-05-08 | 2015-09-23 | 广州锂宝新材料有限公司 | Methods for preparing nickel-cobalt-aluminum precursor material and nickel-cobalt-aluminum cathode material with gradient distribution of aluminum element |
| CN105390667A (en) * | 2015-12-14 | 2016-03-09 | 山东精工电子科技有限公司 | Method for preparing spherical lithium battery cathode material LiNixCoyAl1xyO2 based on normal distribution of aluminum concentration |
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2016
- 2016-08-31 CN CN201610770151.4A patent/CN106365211A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103296263A (en) * | 2012-12-28 | 2013-09-11 | 深圳市天骄科技开发有限公司 | Preparation method of lithium-ion battery positive electrode material spherical nickel-cobalt-lithium aluminate |
| CN103553152A (en) * | 2013-10-22 | 2014-02-05 | 金天能源材料有限公司 | High-density spherical nickel-cobalt-aluminum precursor material and preparation method thereof |
| CN104649336A (en) * | 2015-02-09 | 2015-05-27 | 深圳市贝特瑞新能源材料股份有限公司 | Preparation method of spherical nickel-cobalt-aluminum hydroxide precursor |
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| CN105390667A (en) * | 2015-12-14 | 2016-03-09 | 山东精工电子科技有限公司 | Method for preparing spherical lithium battery cathode material LiNixCoyAl1xyO2 based on normal distribution of aluminum concentration |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467069A (en) * | 2018-04-12 | 2018-08-31 | 安徽同心化工有限公司 | The nickel cobalt aluminium ternary material precursor and its preparation process of a kind of extremely low impurity content and application |
| CN108467069B (en) * | 2018-04-12 | 2020-02-07 | 安徽同心新材料科技有限公司 | Nickel-cobalt-aluminum ternary material precursor with extremely low impurity content and preparation process and application thereof |
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Application publication date: 20170201 |