CN104269548B - A kind of method optimizing size distribution in nickel cobalt manganese persursor material preparation process - Google Patents

A kind of method optimizing size distribution in nickel cobalt manganese persursor material preparation process Download PDF

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Publication number
CN104269548B
CN104269548B CN201410424018.4A CN201410424018A CN104269548B CN 104269548 B CN104269548 B CN 104269548B CN 201410424018 A CN201410424018 A CN 201410424018A CN 104269548 B CN104269548 B CN 104269548B
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reactor
solution
reaction temperature
nickel cobalt
cobalt manganese
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CN104269548A (en
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张世龙
吉同棕
陈明峰
朱珠
王顺林
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Ningbo Jinhe New Materials Co Ltd
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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 present invention discloses a kind of method optimizing size distribution in nickel cobalt manganese persursor material preparation process, and described nickel cobalt manganese persursor material chemical formula is NixCoyMn1‑x‑y(OH)2, wherein 0.2 < x < 0.8,0.2 < y < 0.8；The device for making of described nickel cobalt manganese persursor material includes two reactors connected by overflow pipe；Described reactor I is provided with feed pipe I and agitating device I；Described reactor II is provided with feed pipe II and agitating device II.The preparation of described nickel cobalt manganese persursor material includes: 1) preparing the first solution, nickel and cobalt containing manganese three metal ion species total concentration is 1.0 1.5mol/L, complexing agent 1 5g/L；2) the second solution is prepared, containing 5 10mol/L NaOH；3) the first solution and the second solution are passed in reactor I by feed pipe I；Meanwhile, the first solution and the second solution are passed in reactor II by feed pipe II；Further, the technological parameter in reactor I and reactor II is controlled.The method can be obtained by the nickel cobalt manganese presoma of size distribution stable uniform by feasible process parameter control.

Description

A kind of method optimizing size distribution in nickel cobalt manganese persursor material preparation process
Technical field
The present invention relates to a kind of method optimizing size distribution, in particular it relates to a kind of nickel cobalt The method optimizing size distribution in manganese persursor material preparation process.
Background technology
The advantages such as it is high that lithium ion battery has voltage, and specific capacitance is big, safe and environment-friendly and by people Extensive concern.And lithium ion battery main is by positive electrode, negative material with the big portion of electrolyte three Being grouped into, wherein positive electrode plays a part most critical to promoting lithium ion battery combination property.
In existing market positive electrode, cobalt acid lithium, nickle cobalt lithium manganate and LiMn2O4 occupy leading substantially Share, the presoma cobalt/cobalt oxide/cobalt hydroxide of these positive electrodes, nickel cobalt manganese hydroxide and Mainly use liquid-phase coprecipitation in the producing country of Mn oxide/manganese hydroxide, control in process of production Size distribution processed, controls unnecessary little granule fines and bulky grain meal always row in course of reaction The most important problem.
In Chinese patent CN 201320092391.X discloses " reaction system that a kind of granularity is controlled " Mention the increase a series of equipment such as EGR, grading plant, clarifier to adjust size distribution, Owing to technique needs to increase input increases, operation complexity, it is unsuitable for industrialization production；(Chinese patent " a kind of continous way cobaltosic oxide device for making " disclosed in 201220518689.3 proposes three Reactor is together in series, and allows reaction particles grow step by step, owing to not having charging to continue to participate in reaction, grain There is certain limitation in degree dispersion of distribution control range)；Disclosed in Chinese patent 201310142370.4 " preparation method of a kind of small particle precursor of nickel-cobalt-lithium-manganese-oxide " proposes preparation method, does not but mention How Control granularity location mode.
Summary of the invention
The technical problem to be solved is to provide in nickel cobalt manganese persursor material preparation process excellent The method changing size distribution, the method can be obtained by size distribution by feasible process parameter control The nickel cobalt manganese persursor material of stable uniform.
The present invention solves above-mentioned technical problem and be the technical scheme is that a kind of nickel cobalt manganese presoma material The method optimizing size distribution in material preparation process, described nickel cobalt manganese persursor material chemical formula is NixCoyMn1-x-y(OH)2, wherein 0.2 < x < 0.8,0.2 < y < 0.8；Described nickel cobalt manganese persursor material NixCoyMn1-x-y(OH)2Prepared by following device for making: described device for making includes two by overflow The reactor of pipe series connection: reactor I and reactor II；Described reactor I is provided with feed pipe I and stirring Device I；Described reactor II is provided with feed pipe II and agitating device II；
Described nickel cobalt manganese persursor material NixCoyMn1-x-y(OH)2Preparation comprises the following steps:
1) preparing the first solution, described first solution nickel and cobalt containing manganese three metal ion species total concentration is 1.0-1.5mol/L, complexing agent 1-5g/L；
2) the second solution, described second solution NaOH Han 5-10mol/L are prepared；
3) by described first solution and the second solution by and the mode that flows be passed into by feed pipe I and to have adjusted In the reactor I of good mixing speed and reaction temperature；Meanwhile, by described first solution and the second solution By and the mode that flows be passed into by feed pipe II and to have mixed up the reactor II of mixing speed and reaction temperature In；
In described reactor I, the first solution feed rate is 30～200L/h, and agitating device I rotating speed is 300～600rpm, reaction temperature is 40-70 DEG C, and pH scope is 9.00-12.10；
Further, following parameter is controlled: make the first solution feed rate ratio in reactor II and reactor I Between 0.5-1.5, the rotating speed of agitating device make agitating device II be agitating device I 60%～100% Between, reactor II reaction temperature reduces 0-5 DEG C than reactor I reaction temperature, reactor II pH ratio Reactor I reduces 0.1-0.5.
In technique scheme, the first solution can use nickel sulfate, cobaltous sulfate, manganese sulfate or chlorine Change nickel, cobalt chloride, manganese chloride mixed preparing.
Described device for making also includes that aging reactor, described reactor II connect aging reactor by mozzle.
In one embodiment, described reactor I the first solution feed rate is 30L/h, stirring Device I rotating speed is 600rpm, and reaction temperature is 50 DEG C, and pH scope is between 12.00-12.10；Institute Stating reactor II the first solution feed rate is 20L/h, and agitating device II rotating speed is 450rpm, reaction Temperature is 45 DEG C, and pH scope is 11.80-11.90.
In another embodiment, described reactor I the first solution feed rate is 200L/h, stirs Mixing rotating speed is 300rpm, and reaction temperature is 55 DEG C, and pH scope is between 11.85-11.95；Described instead Answering still II the first solution feed rate is 150L/h, and speed of agitator is 200rpm, and reaction temperature is 50 DEG C, PH scope is 11.70-11.80.
In another embodiment, described reactor I the first solution feed rate is 100L/h, stirs Mixing rotating speed is 450rpm, and reaction temperature is 52 DEG C, and pH scope is between 11.90-12.00；Described instead Answering still II the first solution feed rate is 150L/h, and speed of agitator is 300rpm, and reaction temperature is 51 DEG C, PH scope is 11.85-11.90.
The size distribution that the present invention relates to, foundation is battery industry general testing graininess method---laser Diffractometry, according to size distribution Principle of Statistics, uses volumetrically weighted average to represent average.Respectively It is expressed as D0.1, D10, D50, D90, D100 and distribution span span etc..Wherein D10 Represent that the cumulative particle size distribution percentage of a sample reaches the granularity corresponding to 10%, D50, D90 Implication is analogized.Distribution span span is a kind of tolerance to the sample particle diameter dispersion of distribution:
Span=(D90-D10)/D50, the distribution of span more small grain size is the narrowest, otherwise the widest.
In sum, the invention has the beneficial effects as follows:
(1) present invention is by coupling together two reactors by overflow pipe, and feeds simultaneously Participate in reaction；And control reactor I and the relevant parameter of reactor II so that liquid phase reactor obtains During solid particle, form the size distribution of stable uniform.
(2) the present invention is especially suitable for preparing little particle nickel cobalt manganese persursor material, reactor I provides The process of the generation of particle nucleus, by the environment in regulation reactor II so that crystal is given birth to Long, finally give the optimized particle size results of distribution.
Brief description
Fig. 1 is the structural representation of embodiment 1 device for making.
Fig. 2 is the particle size distribution figure of reactor I in embodiment 2.
Fig. 3 is the particle size distribution figure of reactor II in embodiment 2.
Fig. 4 is the particle size distribution figure of reactor I in embodiment 3.
Fig. 5 is the particle size distribution figure of reactor II in embodiment 3.
Fig. 6 is the particle size distribution figure of reactor I in embodiment 4.
Fig. 7 is the particle size distribution figure of reactor II in embodiment 5.
The title that in figure, each parts are corresponding is: 1-reactor I；2-reactor II；3-feed pipe I；4- Agitating device I；5-feed pipe II；6-agitating device II；7-overflow pipe；8-mozzle；9-aging reactor.
Detailed description of the invention
In order to be more fully understood that present disclosure, it is described further below in conjunction with specific embodiment. Should be understood that these embodiments are only used for that the present invention is further described, rather than limit the present invention's Scope.In addition, it is to be understood that after having read content of the present invention, person skilled in art couple The present invention makes some nonessential change or adjustment, still falls within protection scope of the present invention.
Embodiment 1
Nickel cobalt manganese persursor material Ni of the present inventionxCoyMn1-x-y(OH)2In following device for making Preparation: the device for making used includes two reactors connected by overflow pipe 7: reactor I 1 With reactor II 2.Described reactor I is provided with feed pipe I 3 and agitating device I 4；Described reactor II is provided with feed pipe II 5 and agitating device II 6.
Described device for making also includes aging reactor 9, and described reactor II connects ageing by mozzle 8 Still 9.
Embodiment 2
1) prepare the first solution, described first solution sulfur acid nickel 0.3mol/L, cobaltous sulfate 0.3mol/L, Manganese sulfate 0.3mol/L, glycine 5g/L；
2) the second solution, described second solution NaOH Han 10mol/L are prepared；
3) by described first solution and the second solution by and the mode that flows be passed into by feed pipe I and to have adjusted In the reactor I of good mixing speed and reaction temperature；Meanwhile, by described first solution and the second solution By and the mode that flows be passed into by feed pipe II and to have mixed up the reactor II of mixing speed and reaction temperature In；
Control following parameter:
Reactor I the first solution feed rate is 30L/h, and speed of agitator is 600rpm, reaction temperature Being 50 DEG C, pH scope is between 12.00-12.10, and successive reaction a period of time takes in reactor I Sample test particle size results is D10=0.54um, and (distribution map is figure for D50=3.86um, D90=6.13um 1, there is too much little particle, be fine powder)；Reactor I flows into reactor II by overflow pipe, adjusts Joint reactor II the first solution feed rate is 20L/h, and speed of agitator is 450rpm, and reaction temperature is 45 DEG C, pH scope is 11.80-11.90, and successive reaction a period of time is sampling and testing in reactor II Particle size results is D10=2.51um, D50=4.56um, D90=8.04um (distribution map is Fig. 2).
Embodiment 3
1) prepare the first solution, described first solution sulfur acid nickel 0.5mol/L, cobaltous sulfate 0.5mol/L, Manganese sulfate 0.5mol/L, glycine 5g/L；
2) the second solution, described second solution NaOH Han 10mol/L are prepared；
3) by described first solution and the second solution by and the mode that flows be passed into by feed pipe I and to have adjusted In the reactor I of good mixing speed and reaction temperature；Meanwhile, by described first solution and the second solution By and the mode that flows be passed into by feed pipe II and to have mixed up the reactor II of mixing speed and reaction temperature In；
Control following parameter:
Reactor I charging rate is 200L/h, and speed of agitator is 300rpm, and reaction temperature is 55 DEG C, PH scope is between 11.85-11.95, and successive reaction a period of time is sampling and testing grain in reactor I Degree result is D0.1=0.22um, D10=0.45um, D50=3.64um, D90=6.46um, D100=28.39um (distribution map is as it is shown on figure 3, exist too much little particle and bulky grain simultaneously)；Instead Answering still I to flow into reactor II by overflow pipe, regulation reactor II the first solution feed rate is 150L/h, speed of agitator is 200rpm, and reaction temperature is 50 DEG C, and pH scope is 11.70-11.80, Successive reaction a period of time sampling and testing particle size results in reactor II is D0.1=2.26um, D10=3.77um, D50=4.85um, D90=7.68um, D100=12.53um (distribution map such as Fig. 4 Shown in).
Embodiment 4:
1) prepare the first solution, described first solution chloride containing nickel 0.2mol/L, 0.2 cobalt chloride mol/L, 0.2 manganese chloride mol/L；Glycine 2g/L；
2) the second solution, described second solution NaOH Han 10mol/L are prepared；
3) by described first solution and the second solution by and the mode that flows be passed into by feed pipe I and to have adjusted In the reactor I of good mixing speed and reaction temperature；Meanwhile, by described first solution and the second solution By and the mode that flows be passed into by feed pipe II and to have mixed up the reactor II of mixing speed and reaction temperature In；
Control following parameter:
Reactor I charging rate is 100L/h, and speed of agitator is 450rpm, and reaction temperature is 52 DEG C, PH scope is between 11.90-12.00, and successive reaction a period of time is sampling and testing grain in reactor I Degree result is D0.1=0.76um, D10=1.85um, D50=3.45um, D90=6.68um, D100=52.75um (distribution map is as shown in Figure 6)；Reactor I flows into reactor II by overflow pipe, Regulation reactor II the first solution feed rate is 150L/h, and speed of agitator is 300rpm, reaction temperature Degree is 51 DEG C, and pH scope is 11.85-11.90, and successive reaction a period of time samples in reactor II Test particle size results is D0.1=2.31um, D10=3.56um, D50=4.50um, D90=6.98um, D100=11.63um (distribution map is as shown in Figure 7).
As it has been described above, just can preferably realize the present invention.

Claims (5)

1. the method optimizing size distribution in nickel cobalt manganese persursor material preparation process, its feature exists In, described nickel cobalt manganese persursor material chemical formula is NixCoyMn1-x-y(OH)2, wherein 0.2 < x < 0.8, 0.2<y<0.8；Described nickel cobalt manganese persursor material NixCoyMn1-x-y(OH)2In following device for making Preparation: described device for making includes two reactors connected by overflow pipe: reactor I and reactor II；Described reactor I is provided with feed pipe I and agitating device I；Described reactor II is provided with feed pipe II With agitating device II；
Described nickel cobalt manganese persursor material NixCoyMn1-x-y(OH)2Preparation comprises the following steps:
1) preparing the first solution, described first solution nickel and cobalt containing manganese three metal ion species total concentration is 1.0-1.5mol/L, complexing agent 1-5g/L；
2) the second solution, described second solution NaOH Han 5-10mol/L are prepared；
3) by described first solution and the second solution by and the mode that flows be passed into by feed pipe I and to have adjusted In the reactor I of good mixing speed and reaction temperature；Meanwhile, by described first solution and the second solution By and the mode that flows be passed into by feed pipe II and to have mixed up the reactor II of mixing speed and reaction temperature In；
In described reactor I, the first solution feed rate is 30～200L/h, and agitating device I rotating speed is 300～600rpm, reaction temperature is 40-70 DEG C, and pH scope is 9.0-12.1；After reaction a period of time, Reactor I is made to flow into reactor II by overflow pipe；
Further, following parameter is controlled: make the first solution feed rate ratio in reactor II and reactor I Between 0.5-1.5, the rotating speed of agitating device make agitating device II be agitating device I 60%～100% Between, reactor II reaction temperature reduces 1-5 DEG C than reactor I reaction temperature, reactor II pH ratio Reactor I reduces 0.1-0.5.
2. a kind of nickel cobalt manganese persursor material preparation process as claimed in claim 1 optimizes granularity The method of distribution, it is characterised in that described device for making also includes aging reactor, described reactor II leads to Cross mozzle and connect aging reactor.
3. a kind of nickel cobalt manganese persursor material preparation process as claimed in claim 1 optimizes granularity The method of distribution, it is characterised in that described reactor I the first solution feed rate is 30L/h, stirring Device I rotating speed is 600rpm, and reaction temperature is 50 DEG C, and pH scope is between 12.00-12.10；Institute Stating reactor II the first solution feed rate is 20L/h, and agitating device II rotating speed is 450rpm, reaction Temperature is 45 DEG C, and pH scope is 11.80-11.90.
4. a kind of nickel cobalt manganese persursor material preparation process as claimed in claim 1 optimizes granularity The method of distribution, it is characterised in that described reactor I the first solution feed rate is 200L/h, stirs Mixing rotating speed is 300rpm, and reaction temperature is 55 DEG C, and pH scope is between 11.85-11.95；Described instead Answering still II the first solution feed rate is 150L/h, and speed of agitator is 200rpm, and reaction temperature is 50 DEG C, PH scope is 11.70-11.80.
5. a kind of nickel cobalt manganese persursor material preparation process as claimed in claim 1 optimizes granularity The method of distribution, it is characterised in that described reactor I the first solution feed rate is 100L/h, stirs Mixing rotating speed is 450rpm, and reaction temperature is 52 DEG C, and pH scope is between 11.90-12.00；Described instead Answering still II the first solution feed rate is 150L/h, and speed of agitator is 300rpm, and reaction temperature is 51 DEG C, PH scope is 11.85-11.90.
CN201410424018.4A 2014-08-26 2014-08-26 A kind of method optimizing size distribution in nickel cobalt manganese persursor material preparation process Expired - Fee Related CN104269548B (en)

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