CN108565455A - A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor - Google Patents
A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor Download PDFInfo
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- CN108565455A CN108565455A CN201810542026.7A CN201810542026A CN108565455A CN 108565455 A CN108565455 A CN 108565455A CN 201810542026 A CN201810542026 A CN 201810542026A CN 108565455 A CN108565455 A CN 108565455A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection 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
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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
Abstract
The invention discloses a kind of methods that non-nitrogen containing complexing agent assists preparing spherical nickel cobalt manganese ternary precursor, including:Nickel salt, cobalt salt, manganese salt are configured to the nickel cobalt manganese mixing salt solution that metal ion total concentration is 1.0~2.0mol/L;The nickel cobalt manganese mixing salt solution, sodium hydroxide solution, non-nitrogen containing complexing agent are added into reaction kettle simultaneously, and under the conditions of protecting gas shielded, controlling reaction temperature is 53~57 DEG C, and the pH value for controlling mixture in reaction kettle maintains 10.9~11.1;After these three solution persistently add 6 hours, stops liquid feeding, and be aged 10 hours, then be separated by solid-liquid separation, obtain spherical nickel cobalt manganese ternary precursor Ni1‑x‑yCoxMny(OH)2.The high spherical nickel cobalt manganese ternary precursor of compactness can not only be made in the present invention, and used complexing agent is not tasteless, nontoxic, nitrogenous, can improve production environment, mitigate the pollution processing load in production waste water.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparing technical fields more particularly to a kind of non-nitrogen containing complexing agent to assist
The method for preparing spherical nickel cobalt manganese ternary precursor.
Background technology
Anode material for lithium-ion batteries is one of four important components of lithium ion battery, to the electrification of lithium ion battery
Performance and security performance play the role of vital.With the fast development of electric vehicle, to lithium ion battery correlation
Electrode material proposes higher performance requirement.Due to nickle cobalt lithium manganate (LiNi1-x-yCoxMnyO2) ternary material have Gao Rong
The advantages that amount, long circulation life, and the ratio that nickel, three kinds of cobalt, manganese elements is adjusted flexibly can be needed according to application, therefore should
Material has become the main product of current electronic automobile-used power lithium-ion battery positive electrode.
Currently, cobalt nickel lithium manganate ternary material in the market mainly has LiNi1/3Co1/3Mn1/3O2(111)、
LiNi0.4Co0.2Mn0.4O2(424)、LiNi0.5Co0.2Mn0.3O2(523) and LiNi0.6Mn0.2Co0.2O2(622), these material bases
This is all by spherical nickel cobalt manganese ternary precursor Ni1-x-yCoxMny(OH)2It is prepared through high-temperature calcination after being mixed with lithium salts.
And spherical nickel cobalt manganese ternary precursor Ni1-x-yCoxMny(OH)2Preparation method be all and to be adopted using control crystallisation
It is complexing agent with ammonium hydroxide, such as:The Chinese patents such as CN105731553A, CN106684351A, CN106920934A are to use
This method;Not only ammonium hydroxide smell is big for this method, and production environment is bad, and produces ammonia-nitrogen content height, control expense in waste water
Greatly, therefore it is badly in need of developing a kind of preparation method without spherical nickel cobalt manganese ternary precursor of the ammonium hydroxide as complexing agent.
In the prior art,《The research of lithium ion battery new electrode materials》(Wang Chuanbao, Nanjing Aero-Space University,
2012) it proposes and a kind of the side of spherical nickel cobalt manganese ternary precursor is prepared as complexing agent using EDTA (ethylenediamine tetra-acetic acid)
The higher spherical nickel cobalt manganese ternary precursor of compactness can be successfully made, since EDTA does not have smell, production environment in method
Very big improvement has been obtained, but has still contained nitrogen in EDTA, the ammonia-nitrogen content produced in waste water is still higher, waste water treatment
The big puzzlement of difficulty does not solve still.
Invention content
For above-mentioned shortcoming in the prior art, the present invention provides a kind of non-nitrogen containing complexing agents to assist preparing spherical shape
The method of nickel-cobalt-manganese ternary presoma can not only be made the high spherical nickel cobalt manganese ternary precursor of compactness, and be used
Complexing agent is not tasteless, nontoxic, nitrogenous, can improve production environment, mitigates the pollution processing load in production waste water.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor, includes the following steps:
Step A, according to nickel salt:Cobalt salt:Manganese salt=1:1:1 or 4:2:4 or 5:2:3 or 6:2:2 or 8:1:1 molar ratio,
Nickel salt, cobalt salt, manganese salt are configured to the nickel cobalt manganese mixing salt solution that metal ion total concentration is 1.0~2.0mol/L;
Step B, under agitation, by the nickel cobalt manganese mixing salt solution, the hydroxide of a concentration of 1.0~4.0mol/L
Sodium solution, a concentration of 0.2~0.8mol/L non-nitrogen containing complexing agent simultaneously added into reaction kettle, and protection gas shielded condition
Under, controlling reaction temperature is 53~57 DEG C, while adjusting the addition of sodium hydroxide solution, makes the pH value of mixture in reaction kettle
Maintain 10.9~11.1;After these three solution persistently add 6 hours, stop liquid feeding, and be aged 10 hours, then carry out solid-liquid
Separation, to which spherical nickel cobalt manganese ternary precursor Ni be made1-x-yCoxMny(OH)2。
Preferably, the non-nitrogen containing complexing agent is at least one of sodium gluconate, sodium citrate.
Preferably, the protection gas uses at least one of nitrogen or inert gas.
Preferably, in stepb, it is washed and is dried successively after separation of solid and liquid.
A kind of spherical nickel cobalt manganese ternary precursor prepares spherical nickel cobalt manganese ternary using above-mentioned non-nitrogen containing complexing agent auxiliary
The method of presoma is prepared.
As seen from the above technical solution provided by the invention, non-nitrogen containing complexing agent auxiliary provided by the invention prepares ball
The method of shape nickel-cobalt-manganese ternary presoma is in protection compression ring border, by nickel cobalt manganese mixing salt solution, the hydroxide of specific proportioning
Sodium solution, non-nitrogen containing enveloping agent solution are added into reaction kettle simultaneously, and by controlling stirring intensity, reaction temperature, reaction kettle
Interior mixture ph is reacted, aged after reaction and separation of solid and liquid, to can be obtained particle good sphericity, jolt ramming
The high spherical nickel cobalt manganese ternary precursor Ni of density1-x-yCoxMny(OH)2.The present invention provides a kind of non-nitrogen containing complexing agent auxiliary
It is tasteless, nontoxic, not nitrogenous to prepare complexing agent used in the method for spherical nickel cobalt manganese ternary precursor, production ring can be improved
Border mitigates the pollution processing load in production waste water, and control crystallisation process route phase is complexed with ammonium hydroxide in the prior art
Seemingly, upgrading, which substitutes, is easy, without increasing extras.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, other are can also be obtained according to these attached drawings
Attached drawing.
Fig. 1 is spherical nickel cobalt manganese ternary precursor Ni in the embodiment of the present invention 10.6Co0.2Mn0.2(OH)2Scanning electron microscope shine
Piece.
Fig. 2 is nickel-cobalt-manganternary ternary anode material LiNi in the embodiment of the present invention 10.6Co0.2Mn0.2O2Stereoscan photograph.
Fig. 3 is nickel-cobalt-manganternary ternary anode material LiNi in the embodiment of the present invention 10.6Co0.2Mn0.2O2First run charge and discharge it is bent
Line.
Specific implementation mode
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
Below to non-nitrogen containing complexing agent provided by the present invention assist prepare spherical nickel cobalt manganese ternary precursor method into
Row detailed description.The content not being described in detail in the present invention belongs to the prior art well known to professional and technical personnel in the field.
A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor, includes the following steps:
Step A, according to nickel salt:Cobalt salt:Manganese salt=1:1:1 or 4:2:4 or 5:2:3 or 6:2:2 or 8:1:1 molar ratio,
Nickel salt, cobalt salt, manganese salt are configured to the nickel cobalt manganese mixing salt solution that metal ion total concentration is 1.0~2.0mol/L.
Step B, in high-speed stirred, (high-speed stirred refers to that agitating paddle is stirred with the rotating speed of 500~1500r/min
Mix) under the conditions of, by the nickel cobalt manganese mixing salt solution, the sodium hydroxide solution of a concentration of 1.0~4.0mol/L, a concentration of 0.2
These three solution of the non-nitrogen containing complexing agent of~0.8mol/L are added into reaction kettle simultaneously, and under the conditions of protecting gas shielded, control
Reaction temperature processed is 53~57 DEG C, while adjusting the addition of sodium hydroxide solution, and the pH value of mixture in reaction kettle is made to maintain
10.9~11.1, after these three solution persistently add 6 hours, stop liquid feeding, continues stirring ageing 10 hours, then consolidated
Liquid separation, washing and drying, to which spherical nickel cobalt manganese ternary precursor Ni be made1-x-yCoxMny(OH)2。
Wherein, the non-nitrogen containing complexing agent is at least one of sodium gluconate, sodium citrate;The protection gas can be adopted
With at least one of nitrogen or inert gas;Filtering or suction filtration can be used in the separation of solid and liquid;The washing can be used
Pure water is washed.
Compared with prior art, non-nitrogen containing complexing agent auxiliary provided by the present invention prepares spherical nickel cobalt manganese ternary precursor
Method at least have the advantages that:
(1) made in the method for non-nitrogen containing complexing agent auxiliary preparation spherical nickel cobalt manganese ternary precursor provided by the present invention
It is tasteless, nontoxic, not nitrogenous with complexing agent, production environment can be improved, mitigate the pollution processing load in production waste water.
(2) non-nitrogen containing complexing agent provided by the present invention auxiliary prepare the method for spherical nickel cobalt manganese ternary precursor with it is existing
Ammonium hydroxide complexing control crystallisation process route is similar in technology, and upgrading, which substitutes, to be easy, without increasing extras.
(3) non-nitrogen containing complexing agent auxiliary provided by the present invention prepares the method and process letter of spherical nickel cobalt manganese ternary precursor
It is single, it is very suitable for a large amount of, the continuous production of industry.
(4) method that non-nitrogen containing complexing agent auxiliary provided by the present invention prepares spherical nickel cobalt manganese ternary precursor, system
For the spherical nickel cobalt manganese ternary precursor Ni gone out1-x-yCoxMny(OH)2Particle good sphericity, tap density can reach 2.4g/cm3,
It can be used for preparing the nickel-cobalt-manganternary ternary anode material LiNi of excellent electrical property1-x-yCoxMnyO2, therefore can be widely applied to high specific energy
Secondary cell field.
To sum up, the high spherical nickel cobalt manganese ternary precursor of compactness, Er Qiesuo can not only be made in the embodiment of the present invention
It is tasteless using complexing agent, nontoxic, not nitrogenous, production environment can be improved, mitigate the pollution processing load in production waste water.
In order to more clearly from show technical solution provided by the present invention and generated technique effect, below with tool
The method that body embodiment prepares spherical nickel cobalt manganese ternary precursor to the non-nitrogen containing complexing agent auxiliary of the present invention is described in detail.
Embodiment 1
A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor, includes the following steps:
Step a1, according to nickel salt:Cobalt salt:Manganese salt=6:2:2 molar ratio, by nickel salt, cobalt salt, manganese salt be configured to metal from
The nickel cobalt manganese mixing salt solution of a concentration of 2.0mol/L of subpopulation.
Step b1, under the conditions of the high-speed stirred that low whipping speed is 600r/min, using metering pump respectively by the nickel cobalt
The sodium citrate solution of manganese mixing salt solution, the sodium hydroxide solution of a concentration of 2.0mol/L and a concentration of 0.5mol/L simultaneously to
It is pumped into sealing reaction kettle, and under the conditions of nitrogen protection, controlling reaction temperature is 53~57 DEG C, while it is molten to adjust sodium hydroxide
The addition of liquid makes the pH value of mixture in reaction kettle maintain 10.9~11.1;Wait for that these three solution average rates are pumped into 6 hours
Afterwards, stop liquid feeding, and continue stirring ageing 10 hours, then take out reaction solution from reaction kettle, filtered, washed and done successively
It is dry, to which fully dry spherical nickel-cobalt spherical nickel cobalt manganese ternary precursor Ni as shown in Figure 1 be made0.6Co0.2Mn0.2
(OH)2。
Specifically, by spherical nickel-cobalt spherical nickel cobalt manganese ternary precursor fully dry obtained by the embodiment of the present invention 1
Ni0.6Co0.2Mn0.2(OH)2It is sufficiently mixed with lithium carbonate, makes Li:(Ni+Co+Mn)=1.08 it (is calculated according to molar ratio),
Then it is calcined in Muffle furnace, rises to 550 DEG C with the heating rate of 5 DEG C/min, keep the temperature 5h, then with the heating rate of 5 DEG C/min
850 DEG C are warming up to, 12h is kept the temperature, is then naturally cooling to room temperature, and roasted, be ground up, sieved, to obtain as shown in Figure 2
Nickel-cobalt-manganternary ternary anode material LiNi0.6Co0.2Mn0.2O2。
Further, to the nickel-cobalt-manganternary ternary anode material LiNi obtained by the embodiment of the present invention 10.6Co0.2Mn0.2O2Into
Row charge and discharge electro-detection, so as to obtain first run charging and discharging curve as shown in Figure 3.It can be seen that by Fig. 1, Fig. 2 and Fig. 3:This
Spherical nickel-cobalt spherical nickel cobalt manganese ternary precursor Ni obtained by inventive embodiments 10.6Co0.2Mn0.2(OH)2Good sphericity, jolt ramming
Density is up to 2.4g/cm3, at room temperature when 0.2C charge and discharge, specific discharge capacity reaches 172mAh/g or more.
Embodiment 2
A kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor, includes the following steps:
Step a2, according to nickel salt:Cobalt salt:Manganese salt=6:2:2 molar ratio, by nickel salt, cobalt salt, manganese salt be configured to metal from
The nickel cobalt manganese mixing salt solution of a concentration of 2.0mol/L of subpopulation.
Step b2, under the conditions of the high-speed stirred that low whipping speed is 600r/min, using metering pump respectively by the nickel cobalt
Manganese mixing salt solution, the sodium hydroxide solution of a concentration of 2.0mol/L, a concentration of 0.8mol/L sodium gluconate solution simultaneously
It is pumped into sealing reaction kettle, and under the conditions of nitrogen protection, controlling reaction temperature is 53~57 DEG C, while adjusting sodium hydroxide
The addition of solution makes the pH value of mixture in reaction kettle maintain 10.9~11.1;Wait for that these three solution average rates are pumped into 6 hours
Afterwards, stop liquid feeding, and continue stirring ageing 10 hours, then take out reaction solution from reaction kettle, filtered, washed and done successively
It is dry, to which fully dry spherical nickel-cobalt spherical nickel cobalt manganese ternary precursor Ni be made0.6Co0.2Mn0.2(OH)2。
Specifically, by spherical nickel-cobalt spherical nickel cobalt manganese ternary precursor fully dry obtained by the embodiment of the present invention 2
Ni0.6Co0.2Mn0.2(OH)2It is sufficiently mixed with lithium carbonate, makes Li:(Ni+Co+Mn)=1.08 it (is calculated according to molar ratio),
Then it is calcined in Muffle furnace, rises to 550 DEG C with the heating rate of 5 DEG C/min, keep the temperature 5h, then with the heating rate of 5 DEG C/min
850 DEG C are warming up to, 12h is kept the temperature, room temperature is then naturally cooling to, and roasted, be ground up, sieved, to obtain nickel cobalt manganese three
First positive electrode LiNi0.6Co0.2Mn0.2O2.Spherical nickel-cobalt spherical nickel cobalt manganese ternary precursor obtained by the embodiment of the present invention 2
Ni0.6Co0.2Mn0.2(OH)2Good sphericity, tap density is up to 2.4g/cm3, at room temperature when 0.2C charge and discharge, specific discharge capacity reaches
To 170mAh/g or more.
To sum up, the high spherical nickel cobalt manganese ternary precursor of compactness, Er Qiesuo can not only be made in the embodiment of the present invention
It is tasteless using complexing agent, nontoxic, not nitrogenous, production environment can be improved, mitigate the pollution processing load in production waste water.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (5)
1. a kind of method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor, which is characterized in that including following
Step:
Step A, according to nickel salt:Cobalt salt:Manganese salt=1:1:1 or 4:2:4 or 5:2:3 or 6:2:2 or 8:1:1 molar ratio, by nickel
Salt, cobalt salt, manganese salt are configured to the nickel cobalt manganese mixing salt solution that metal ion total concentration is 1.0~2.0mol/L;
Step B, under agitation, the nickel cobalt manganese mixing salt solution, the sodium hydroxide of a concentration of 1.0~4.0mol/L is molten
Liquid, a concentration of 0.2~0.8mol/L non-nitrogen containing complexing agent added simultaneously into reaction kettle, and under the conditions of protecting gas shielded,
Controlling reaction temperature is 53~57 DEG C, while adjusting the addition of sodium hydroxide solution, and the pH value of mixture in reaction kettle is made to tie up
It holds 10.9~11.1;After these three solution persistently add 6 hours, stop liquid feeding, and be aged 10 hours, then carry out solid-liquid point
From to which spherical nickel cobalt manganese ternary precursor Ni be made1-x-yCoxMny(OH)2。
2. the method that non-nitrogen containing complexing agent auxiliary according to claim 1 prepares spherical nickel cobalt manganese ternary precursor, special
Sign is that the non-nitrogen containing complexing agent is at least one of sodium gluconate, sodium citrate.
3. the method that non-nitrogen containing complexing agent auxiliary according to claim 1 or 2 prepares spherical nickel cobalt manganese ternary precursor,
It is characterized in that, the protection gas uses at least one of nitrogen or inert gas.
4. the method that non-nitrogen containing complexing agent auxiliary according to claim 1 or 2 prepares spherical nickel cobalt manganese ternary precursor,
It is characterized in that, in stepb, is washed and dried successively after separation of solid and liquid.
5. a kind of spherical nickel cobalt manganese ternary precursor, which is characterized in that described in any one of the claims 1 to 4
The method that non-nitrogen containing complexing agent auxiliary prepares spherical nickel cobalt manganese ternary precursor is prepared.
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