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CN109592720A - Ternary precursor solution purification method - Google Patents

Ternary precursor solution purification method Download PDF

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Publication number
CN109592720A
CN109592720A CN201811409265.1A CN201811409265A CN109592720A CN 109592720 A CN109592720 A CN 109592720A CN 201811409265 A CN201811409265 A CN 201811409265A CN 109592720 A CN109592720 A CN 109592720A
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Prior art keywords
ternary precursor
precursor solution
time
solution
purification method
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CN109592720B (en
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罗钢
邓睿超
訚硕
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Hunan Zhongwei Amperex Technology Ltd
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Hunan Zhongwei Amperex Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/40Complex oxides containing nickel and at least one other metal element
    • C01G53/42Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
    • C01G53/44Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention provides ternary precursor solution purification methods, this method first adjusts the pH of ternary precursor solution with oxalic acid, first time temperature programming after hydrogen peroxide will be added in treated solution again, then to second of temperature programming after solution progress first time filtering, finally by treated, solution carries out second being aged after filtering.Ternary precursor solution purification method provided by the present invention, it solves in the prior art, it is difficult to effectively exclude the problem of trace impurity interferes persursor material performance in raw material when preparing ternary precursor, every impurity content complies with the national standard requirements, purification process process of the invention is uncomplicated, low energy consumption for cost, is conducive to promote and apply.In purification process, after hydrogen peroxide heating filtering for the first time is added, then second of temperature programming is carried out, may advantageously facilitate the precipitation of microelement in solution, promote the degree of purification of solution.

Description

Ternary precursor solution purification method
Technical field
The invention belongs to technical field of lithium ion, and in particular to ternary precursor solution purification method.
Background technique
Lithium ion battery is the best secondary accumulator battery of current comprehensive performance, since specific energy is high, have extended cycle life, put certainly The features such as electric small, memory-less effect and good safety, be widely used in portable electronic device, electric car, electric bicycle, The multiple fields such as military equipment, peak regulation energy storage and distributed energy storage.
Positive electrode is the critical material of lithium ion battery, largely determines the performance of battery.It is common just Pole material has cobalt acid lithium, LiMn2O4, LiFePO4 and ternary material (LiNixCoyM1-x-yO2, M is Mn or Al).Ternary material tool There are the advantages such as the cost more balanced, energy density, circulation and security performance, becomes the products such as electric car, electric bicycle Main selection, especially in passenger car field, ternary material relies on its higher superiority of effectiveness, gradually surmount LiFePO4 and LiMn2O4 becomes the selection of mainstream vehicle enterprise.The performance and cost of ternary material depend primarily on production technology and equipment.Nickel cobalt manganese Hydroxide solubility product is small, and settling rate is fast, and solution degree of supersaturation is high, and crystal nucleation is fast, and colloidal precipitation easy to form, pattern is not It is easy to control, and Mn (OH)2Big two orders of magnitude of the more other two kinds of hydroxide of solubility product are straight using nickel cobalt manganese metal salt and alkali Reversed to be difficult to synthesis with spherical morphology presoma, realization is uniform to be co-precipitated, therefore in the synthesis of hydroxide precursor When, the degree of supersaturation, pH value of precipitating ion, ammonia concn, temperature and stirring rate in reaction system need to be controlled, further, since The presence of impurity can reduce coulombic efficiency, weaken the first discharge specific capacity of material, cause irreversible capacitance loss, therefore go Except the trace impurity in raw material is also particularly critical to the performance for improving persursor material.
In the prior art, it is difficult to effectively exclude the trace impurity in raw material in industry when preparing ternary precursor to preceding Drive the interference of body material property, it is therefore desirable to a kind of purification process for ternary precursor solution.
Summary of the invention
To solve in the prior art, when preparing ternary precursor, it is difficult to which trace impurity is to forerunner effectively in exclusion raw material The problem of body material property interferes, the purpose of the present invention is to provide ternary precursor solution purification methods.
To achieve the above object, the invention adopts the following technical scheme:
Ternary precursor solution purification method, step include:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution is carried out second being aged after filtering.
Preferably, the range of step (1) described pH is 3.0~6.5.
Preferably, the concentration of step (2) described hydrogen peroxide is 0.02~0.2mol/L, and the addition flow that hydrogen peroxide is added is 70~600L/min.
Preferably, the heating rate of step (2) the first time temperature programming is 0.5~1.5 DEG C/min, and outlet temperature is 60 DEG C, the soaking time after reaching the outlet temperature is 10~30min.
Preferably, step (3) first time is filtered into natural filtration.
It is further preferred that the filter cloth mesh number of the natural filtration is 3000~6000.
Preferably, the heating rate of step (3) second of temperature programming is 1.5~2.5 DEG C/min, and outlet temperature is 70 DEG C, the soaking time after reaching the outlet temperature is 30~60min.
Preferably, step (4) described be filtered into for the second time is filtered under diminished pressure.
It is further preferred that the pressure being filtered under diminished pressure is 0.1~2MPa.
Preferably, the time of step (4) described ageing is 90~240min, and the temperature of the ageing is 35~60 DEG C.
Preferably, the method also includes before step (1), ternary precursor solution is heated up to 15~35 DEG C.
Beneficial effects of the present invention
1, ternary precursor solution purification method provided by the present invention solves in the prior art, prepares ternary forerunner Be difficult to effectively exclude in raw material the problem of trace impurity interferes persursor material performance when body, after processing Fe in solution, The content of the foreign ions such as Cu, Na, Zn, Ca, Mg is all satisfied requirements of the national standard;
2, purification process provided by the present invention, process is uncomplicated, and low energy consumption for cost, is conducive to promote and apply;
3, ternary precursor solution purification method provided by the present invention, after the temperature programming of hydrogen peroxide first time is added, First time natural filtration is first carried out, which can remove impurity therein and the concentration that product is precipitated, production concentration is precipitated The generation that contamination precipitation can be promoted to react is reduced, second of temperature programming is carried out again later, makes remaining micro member in solution It is plain to be further precipitated, while the degree of purification for promoting solution gets a promotion, first kept the temperature after second of temperature programming to terminal again into Row ageing, ensure that the abundant precipitation of impurity;
4, in purification process of the invention, the temperature being finally aged is lower than the outlet temperature of second of temperature programming, favorably In making full use of thermal energy, energy consumption is saved, reduces real cost of production.
Specific embodiment
The following is specific embodiments of the present invention, and further retouches to technical solution of the present invention work in conjunction with the embodiments It states, however, the present invention is not limited to these examples.
Embodiment 1
Ternary precursor solution purification method, step include:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution is carried out second being aged after filtering.
Wherein, the range of step (1) described pH is 3.0~6.5.
The concentration of step (2) described hydrogen peroxide is 0.02mol/L, and the addition flow that hydrogen peroxide is added is 70L/min, step (2) heating rate of the first time temperature programming is 0.5 DEG C/min, and outlet temperature is 60 DEG C, after reaching the outlet temperature Soaking time be 10~30min.
Step (3) first time is filtered into filter-cloth filtering, and the mesh number of the filter cloth is 3000, step (3) described second The heating rate of secondary program heating is 1.5 DEG C/min, and outlet temperature is 70 DEG C, and the soaking time after reaching the outlet temperature is 30min。
Step (4) described be filtered into for the second time is filtered under diminished pressure, and the pressure being filtered under diminished pressure is 0.1MPa.Step (4) is described old The time of change is 90min, and the temperature of the ageing is 35 DEG C.
Embodiment 2
Ternary precursor solution purification method, step include:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution is carried out second being aged after filtering.
Wherein, the range of step (1) described pH is 3.0~6.5.
The concentration of step (2) described hydrogen peroxide is 0.2mol/L, and the addition flow that hydrogen peroxide is added is 600L/min, step (2) heating rate of the first time temperature programming is 0.5 DEG C/min, and outlet temperature is 60 DEG C, after reaching the outlet temperature Soaking time be 10~30min.
Step (3) first time is filtered into filter-cloth filtering, and the mesh number of the filter cloth is 6000, step (3) described second The heating rate of secondary program heating is 2.5 DEG C/min, and outlet temperature is 70 DEG C, and the soaking time after reaching the outlet temperature is 60min。
Step (4) described be filtered into for the second time is filtered under diminished pressure, and the pressure being filtered under diminished pressure is 2MPa, step (4) described ageing Time be 240min, the temperature of the ageing is 60 DEG C.
Embodiment 3
Ternary precursor solution purification method, step include:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution is carried out second being aged after filtering.
Wherein, the range of step (1) described pH is 3.0~6.5.
The concentration of step (2) described hydrogen peroxide is 0.1mol/L, and the addition flow that hydrogen peroxide is added is 300L/min, step (2) heating rate of the first time temperature programming is 0.5 DEG C/min, and outlet temperature is 60 DEG C, after reaching the outlet temperature Soaking time be 10~30min.
Step (3) first time is filtered into filter-cloth filtering, and the mesh number of the filter cloth is 5000, step (3) described second The heating rate of secondary program heating is 2.0 DEG C/min, and outlet temperature is 70 DEG C, and the soaking time after reaching the outlet temperature is 45min。
Step (4) described be filtered into for the second time is filtered under diminished pressure, and the pressure being filtered under diminished pressure is 1MPa, step (4) described ageing Time be 160min, the temperature of the ageing is 50 DEG C.
Embodiment 4
Ternary precursor solution purification method, step include:
(1) ternary precursor solution is heated up to 15~35 DEG C, the pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution is carried out second being aged after filtering.
Wherein, the range of step (1) described pH is 3.0~6.5.
The concentration of step (2) described hydrogen peroxide is 0.1mol/L, and the addition flow that hydrogen peroxide is added is 300L/min, step (2) heating rate of the first time temperature programming is 1 DEG C/min, and outlet temperature is 60 DEG C, after reaching the outlet temperature Soaking time is 20min.
Step (3) first time is filtered into filter-cloth filtering, and the mesh number of the filter cloth is 5000, step (3) described second The heating rate of secondary program heating is 2.0 DEG C/min, and outlet temperature is 70 DEG C, and the soaking time after reaching the outlet temperature is 45min。
Step (4) described be filtered into for the second time is filtered under diminished pressure, and the pressure being filtered under diminished pressure is 1MPa, step (4) described ageing Time be 160min, the temperature of the ageing is 60 DEG C.
Comparative example 1
Ternary precursor solution purification method, step include:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) by step (2), treated is aged after solution is filtered.
Wherein, the range of step (1) described pH is 3.0~6.5.
The concentration of step (2) described hydrogen peroxide is 0.1mol/L, and the addition flow that hydrogen peroxide is added is 300L/min, step (2) heating rate of described program heating is 1 DEG C/min, and outlet temperature is 70 DEG C, when heat preservation after reaching the outlet temperature Between be 45min, described be filtered into of step (3) is filtered under diminished pressure, and the pressure being filtered under diminished pressure is 1MPa, and the time of the ageing is 160min, the temperature of the ageing are 60 DEG C.
Comparative example 2
Ternary precursor solution purification method, step include:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution second is carried out to filter.
Wherein, the range of step (1) described pH is 3.0~6.5.
The concentration of step (2) described hydrogen peroxide is 0.1mol/L, and the addition flow that hydrogen peroxide is added is 300L/min, step (2) heating rate of the first time temperature programming is 1 DEG C/min, and outlet temperature is 60 DEG C, after reaching the outlet temperature Soaking time is 20min.
Step (3) first time is filtered into filter-cloth filtering, and the mesh number of the filter cloth is 3000, step (3) described second The heating rate of secondary program heating is 2.0 DEG C/min, and outlet temperature is 70 DEG C, and the soaking time after reaching the outlet temperature is 45min。
Step (4) described be filtered into for the second time is filtered under diminished pressure, and the pressure being filtered under diminished pressure is 1MPa.
Detect example
Using the method for Examples 1 to 4 and comparative example 1,2, to anode material for lithium-ion batteries ternary precursor solution into It has gone purifying, has had detected the content of the foreign ions such as Fe, Cu, Na, Zn, Ca and Mg in purified solution, the results are shown in Table 1.
1 foreign ion testing result of table
Requirement in standard GB/T/T 26300-2010 " nickel-cobalt-manganese ternary complex hydroxide " to impurity element is Cu Wt%≤0.01 wt%≤0.005, Fe, Na wt%≤0.03, Zn wt%≤0.01, Ca wt%≤0.03, Mg wt% ≤0.03。
As can be found from Table 1, the solution handled using 1 purification process of comparative example, Cu, Na, Zn and Mg impurity content exceeding index, The solution handled using 2 purification process of comparative example, the impurity content exceeding index of Cu, Na, Zn and Ca, and use the embodiment of the present invention 1 ~4 ternary precursor solution Fe, Cu, Na, Zn, Ca and Mg after purification complies with the national standard requirements.
Ternary precursor solution purification method provided by the present invention, solves in the prior art, prepares ternary precursor When be difficult to effectively exclude in raw material the problem of trace impurity interferes persursor material performance, after processing Fe, Cu in solution, The content of the foreign ions such as Na, Zn, Ca, Mg is all satisfied requirements of the national standard.Purification process process is uncomplicated, cost energy consumption It is low, it is conducive to promote and apply.In purification process, after hydrogen peroxide heating filtering for the first time is added, then second of temperature programming is carried out, The precipitation that may advantageously facilitate microelement in solution promotes the degree of purification of solution.

Claims (10)

1. ternary precursor solution purification method, which is characterized in that step includes:
(1) pH of ternary precursor solution is adjusted with oxalic acid;
(2) first time temperature programming after hydrogen peroxide is added into step (1) treated solution;
(3) after step (2) treated solution being carried out first time filtering, second of temperature programming;
(4) step (3) treated solution is carried out second being aged after filtering.
2. ternary precursor solution purification method described in claim 1, which is characterized in that the range of step (1) described pH is 3.0 ~6.5.
3. ternary precursor solution purification method described in claim 1, which is characterized in that the concentration of step (2) described hydrogen peroxide For 0.02~0.2mol/L, the addition flow that hydrogen peroxide is added is 70~600L/min.
4. ternary precursor solution purification method described in claim 1, which is characterized in that step (2) the first secondary program liter The heating rate of temperature is 0.5~1.5 DEG C/min, and outlet temperature is 45 DEG C, and the soaking time after reaching the outlet temperature is 10 ~30min.
5. ternary precursor solution purification method described in claim 1, which is characterized in that step (3) first time is filtered into Natural filtration.
6. ternary precursor solution purification method described in claim 1, which is characterized in that step (3) the second secondary program liter The heating rate of temperature is 1.5~2.5 DEG C/min, and outlet temperature is 70 DEG C, and the soaking time after reaching the outlet temperature is 30 ~60min.
7. ternary precursor solution purification method described in claim 1, which is characterized in that step (4) is described to be filtered into for the second time It is filtered under diminished pressure.
8. ternary precursor solution purification method described in claim 7, which is characterized in that the pressure being filtered under diminished pressure is 0.1 ~2MPa.
9. ternary precursor solution purification method described in claim 1, which is characterized in that the time of step (4) described ageing is 90~240min, the temperature of the ageing are 35~60 DEG C.
10. ternary precursor solution purification method described in claim 1, which is characterized in that the method also includes in step (1) Before, ternary precursor solution is heated up to 15~35 DEG C.
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CN102008939A (en) * 2010-11-15 2011-04-13 西北农林科技大学 Method for preparing aluminum-manganese composite oxide modified molecular sieve
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116040694A (en) * 2022-12-27 2023-05-02 中冶瑞木新能源科技有限公司 Production method of ternary precursor

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