CN105668650B - The preparation method of low sodium cobaltosic oxide - Google Patents
The preparation method of low sodium cobaltosic oxide Download PDFInfo
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- CN105668650B CN105668650B CN201610169885.7A CN201610169885A CN105668650B CN 105668650 B CN105668650 B CN 105668650B CN 201610169885 A CN201610169885 A CN 201610169885A CN 105668650 B CN105668650 B CN 105668650B
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- C01—INORGANIC CHEMISTRY
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- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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Abstract
The invention discloses a kind of preparation method of low sodium cobaltosic oxide, including：Preparation process, mixes progress complex reaction with complexing agent by cobalt salt and obtains cobalt salt complex solution；Reactions steps, cobalt salt complex solution, sodium hydroxide solution and air are passed through in reaction unit under agitation and fully reacted, reaction temperature is 85 ~ 95 DEG C, and pH is 9.0 ~ 9.8, is reacted the sediment of acquisition after terminating through centrifuge washing and the dry low sodium cobaltosic oxide of acquisition.The present invention prepares cobaltosic oxide battery material presoma using high temperature, low pH method, and the primary particle of the presoma of formation is larger, can effectively reduce Na between particle+Be mingled with, effectively reduce Na+Content；Such as coordinate reinforcing to wash, can also further reduce the Na for remaining in particle surface+Content.In addition, the cobaltosic oxide battery material presoma regular appearance that the method for the invention is obtained, yield is high, Na in existing cobaltosic oxide battery material is overcome+The problem of too high levels and high cost.
Description
Technical field
The present invention relates to technical field of lithium ion, more particularly to a kind of preparation method of low sodium cobaltosic oxide.
Background technology
Lithium ion battery because its voltage is high, energy density is high, have extended cycle life, enjoy favor the advantages of environmental pollution is small,
In recent years, with the further growth of small movable battery requirements, it is good to be that lithium ion battery industrial expansion is created
Opportunity.Positive electrode is the core and key of lithium ion battery.Wherein LiCoO2Stability Analysis of Structures, specific capacity are high, combination property is dashed forward
Go out, be the positive electrode that current commercial Li-ion battery is generally used with good chemical property.
The Na in the cobaltosic oxide battery material presoma of hydroxide intermediate processing production is taken at present+Content is general
In 100-300ppm or so.Na+Too high levels, easily cause cobaltosic oxide precursor poor fluidity, for anode material
The internal resistance of battery can be increased after material.Although Na in ammoniacal liquor or ammonium salt precipitation method production cobaltosic oxide product+Content is low, product matter
Amount is preferable, but produces substantial amounts of ammonia nitrogen waste water, and production cost is high, and to the seriously polluted of environment.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of low sodium cobaltosic oxide, to reduce particle
Between Na+Be mingled with, obtain even particle distribution, good fluidity and Na+The low low sodium cobaltosic oxide material of mass concentration.
The technical problems to be solved by the invention are achieved by the following technical programs：A kind of low sodium cobaltosic oxide
Preparation method, comprises the following steps：
Preparation process, mixes progress complex reaction with complexing agent by cobalt salt and obtains cobalt salt complex solution；
Reactions steps, reaction dress is passed through by cobalt salt complex solution, sodium hydroxide solution and air under agitation
Put it is interior fully reacted, reaction temperature be 85 ~ 95 DEG C, pH be 9.2 ~ 9.8, reaction terminate after by the sediment of acquisition through centrifugation
Washing and the dry low sodium cobaltosic oxide of acquisition.
Further, in preparation process, the cobalt salt is cobalt chloride or cobaltous sulfate, and the complexing agent is selected from EDTA, two
At least one of monoethanolamine, triethanolamine and DTPA.
Further, in reactions steps, reaction temperature is 85 ~ 95 DEG C, and pH is 9.2 ~ 9.8, and the reaction time is 5 ~ 20h,
Mixing speed is 180 ~ 215r/min.
Further, the preparation process also includes sodium hydroxide is dissolved in into water and sodium hydroxide solution is obtained, and controls
The mass percent of sodium hydroxide is 25-32%.
Further, in preparation process, cobalt salt concentration is 30 ~ 150g/L, and the addition of complexing agent is the total matter of cobalt ions
The 1 ~ 6% of amount.
Further, in reactions steps, the centrifuge washing is the hot water centrifuge washing more than 5 times with more than 90 DEG C.
Further, in reactions steps, the temperature of the drying is 70 ~ 100 DEG C, and drying time is 2 ~ 8h.
Further, sodium ion mass concentration is less than 100ppm in the low sodium cobaltosic oxide.
Further, in reactions steps, the uninterrupted of the cobalt salt complex solution is 120 ~ 200L/h；Air leads to
Enter amount for 15 ~ 35 m3/h。
Further, in reactions steps, pure water is added first into reaction unit and EDTA is mixed, and is warming up to 85
~95℃。
The present invention has the advantages that：The present invention prepares cobaltosic oxide battery material using high temperature, low pH method
Material precursor, the primary particle of the presoma of formation is larger, can effectively reduce Na between particle+Be mingled with, effectively reduce
Na+Content；Such as coordinate reinforcing to wash, can also further reduce the Na for remaining in particle surface+Content.In addition, side of the present invention
The cobaltosic oxide battery material presoma regular appearance that method is obtained, yield is high.
Brief description of the drawings
Fig. 1 is the flow chart of low sodium cobaltosic oxide preparation method of the invention.
Fig. 2 is the surface topography schematic diagram of cobaltosic oxide made from embodiment 1.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combine, the present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
As shown in figure 1, the present invention provides a kind of preparation method of low sodium cobaltosic oxide, comprise the following steps：
a）Prepare cobalt salt-complexing agent cobalt salt complex solution：By cobalt salt and complexing agent be mixed to get cobalt salt concentration for 30 ~
150g/L cobalt salt complex solution, the addition of its complexing agent is preferably the 1 ~ 6% of cobalt ions gross mass；The cobalt salt can
Using cobalt chloride or cobaltous sulfate, it is preferred to use cobalt chloride；The complexing agent can select EDTA（I.e.：Tetraacethyl diaminourea second
Alkane）, diethanol amine, triethanolamine, DTPA（Diethylenetriamine pentacarboxylic acid salt）At least one of, it is preferred to use EDTA.
b）Prepare sodium hydroxide solution：Sodium hydroxide is formulated as the sodium hydroxide solution that mass percent is 25 ~ 32%.
c）Prepare cobaltosic oxide：Cobalt salt complex solution, the step b that preparation process is prepared）The hydrogen-oxygen prepared
Compound solution and air take cocurrent mode to be passed into reaction unit to be reacted under agitation, and reaction temperature is 85
~ 95 DEG C, pH is 9.0 ~ 9.8, reaction terminate after by the sediment of acquisition through more than 90 DEG C of hot water centrifuge washing at least 5 times, it is excellent
Choosing washing 8 times, and in 70 ~ 100 DEG C of 2 ~ 8h of drying and processing, Na is made+Mass concentration is in below 100ppm and the electricity of regular appearance
Pond grade cobaltosic oxide battery material presoma.
In step c）In, the reaction unit is preferably reactor, control cobalt salt complex solution uninterrupted for 120 ~
200L/h, air intake is 15 ~ 35 m3/h；Control during the course of the reaction in reaction unit agitating paddle mixing speed be 180 ~
215r/rpm, the reaction time is 5 ~ 20h.
Above step a）With step b）It is a part for preparation process, has no strict tandem and distinguish, even, also
Can be using the direct commercially suitable hydroxide solution of concentration come step of replacing b）.
Preferably, in step c）In, pure water is added first into reaction unit to its internal agitating paddle bottom, is then added
Complexing agent is mixed, and is warming up to 85 ~ 95 DEG C, then carries out follow-up operation.The complexing agent added in this step is molten with preparing cobalt salt
The complexing agent added during liquid is consistent.
The present invention prepares cobaltosic oxide battery material presoma using high temperature, low pH method, the presoma of formation
Primary particle is larger, can effectively reduce Na between particle+Be mingled with, effectively reduce Na+Content；Reinforcing is such as coordinated to wash, also
The Na for remaining in particle surface can further be reduced+Content.In addition, the cobaltosic oxide battery material that the method for the invention is obtained
Material precursor regular appearance, yield is high, overcomes Na in existing cobaltosic oxide battery material+Too high levels and high cost
Problem.
The specific implementation process of the present invention is further illustrated below by way of several embodiments.
Embodiment 1：
a）Compound concentration is 30g/L cobalt chloride-EDTA solution, and EDTA additions are the 1.27% of cobalt ions gross mass；
b）Prepare the sodium hydroxide solution that mass fraction is 32%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g EDTA, 85 DEG C are warming up to.Temperature herein
Degree refers to reaction temperature, and reaction temperature should be first warming up to before starting the reaction, maintains constant reaction temperature, adds preparation
Cobalt chloride-EDTA, liquid caustic soda etc. reacted.Under agitation by above-mentioned steps a）Cobalt chloride-EDTA the solution of preparation, step
Rapid b）The sodium hydroxide solution and air cocurrent of preparation are passed through in reactor, control the cobalt liquid-EDTA liquid inventory sizes to be
120L/h, air mass flow 15m3/ h, speed of agitator is 180 turns/min, and the temperature of maintenance reaction process is 85 DEG C, and pH is 9.5, instead
5h is answered, finely dispersed black precipitate is obtained, through 95 DEG C of hot water centrifuge washings, 70 DEG C of dryings obtain the spherical Co of black3O4Powder
Body, its surface topography are as shown in Fig. 2 the weight/mass percentage composition of its cobalt is 72.5%, Na+Mass concentration size is 78ppm.
Embodiment 2：
a）Compound concentration is 60g/L cobalt chloride-diethanolamine solution, and diethanol amine addition is cobalt ions gross mass
1.0%；
b）Prepare the sodium hydroxide solution that mass fraction is 25%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g diethanol amine, 90 DEG C are warming up to.In stirring
Under the conditions of by above-mentioned steps a）Cobalt chloride-diethanolamine solution, the step b of preparation）The sodium hydroxide solution and air of preparation
Cocurrent is passed through in reactor, and it is 150L/h, air mass flow 15m to control cobalt liquid-EDTA liquid inventories size3/ h, speed of agitator is
190 turns/min, the temperature of maintenance reaction process is 90 DEG C, and pH is 9.0, reacts 8h, finely dispersed black precipitate is obtained, through 95
DEG C hot water centrifuge washing, 80 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 72.8%, Na+
Mass concentration size is 102ppm, and its surface topography is similar with Fig. 2.
Embodiment 3：
a）Compound concentration is 90g/L cobalt chloride-triethanolamine solution, and triethanolamine addition is cobalt ions gross mass
2%；
b）Prepare the sodium hydroxide solution that mass fraction is 30%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g triethanolamines, 95 DEG C are warming up to.In stirring
Under the conditions of by above-mentioned steps a）Cobalt chloride-triethanolamine solution, the step b of preparation）The sodium hydroxide solution and air of preparation
Cocurrent is passed through in reactor, and it is 150L/h, air mass flow 25m to control cobalt liquid-EDTA liquid inventories size3/ h, speed of agitator is
215 turns/min, the temperature of maintenance reaction process is 95 DEG C, and pH is 9.2, reacts 15h, obtains finely dispersed black precipitate, is passed through
95 DEG C of hot water centrifuge washings, 100 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 72.6%,
Na+Mass concentration size is 82ppm, and its surface topography is similar with Fig. 2.
Embodiment 4：
a）Compound concentration is 120g/L cobaltous sulfate-DTPA solution, and DTPA additions are the 6% of cobalt ions gross mass；
b）Prepare the sodium hydroxide solution that mass fraction is 28%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g DTPA, 90 DEG C are warming up to.In stirring bar
By above-mentioned steps a under part）Cobaltous sulfate-DTPA solution, the step b of preparation）The sodium hydroxide solution and air cocurrent of preparation are passed through
In reactor, it is 180L/h, air mass flow 30m to control cobaltous sulfate-DTPA liquid inventories size3/ h, speed of agitator be 200 turns/
Min, the temperature of maintenance reaction process is 90 DEG C, and pH is 9.8, reacts 20h, finely dispersed black precipitate is obtained, through 95 DEG C of heat
Water centrifuge washing, 85 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 72.1%, Na+Quality
Concentration is 110ppm, and its surface topography is similar with Fig. 2.
Embodiment 5
a）Compound concentration is 150g/L cobalt chloride-EDTA solution, and EDTA additions are the 4% of cobalt ions gross mass；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g EDTA, 85 DEG C are warming up to.In stirring bar
By above-mentioned steps a under part）Cobalt chloride-EDTA the solution of preparation, the mass fraction directly bought from the market are 32% hydroxide
Sodium solution and air cocurrent are passed through in reactor, and it is 200L/h, air mass flow to control cobalt liquid-EDTA liquid inventories size
35m3/ h, speed of agitator is 200 turns/min, and the temperature of maintenance reaction process is 85 DEG C, and pH is 9.6, reacts 12h, is disperseed
Uniform black precipitate, through 95 DEG C of hot water centrifuge washings, 80 DEG C of dryings obtain the spherical Co of black3O4Powder, the quality of its cobalt
Percentage composition is 72.6%, Na+Mass concentration size is 95ppm, and its surface topography is similar with Fig. 2.
Comparative example 1：
a）Compound concentration is 60g/L cobalt chloride-EDTA solution, and EDTA additions are the 3.5% of cobalt ions gross mass；
b）Prepare the sodium hydroxide solution that mass fraction is 25%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g EDTA, 40 DEG C are warming up to.In stirring bar
By above-mentioned steps a under part）Cobalt chloride-EDTA solution, step b）The sodium hydroxide solution and air cocurrent of preparation are passed through reaction
In kettle, it is 150L/h, air mass flow 15m to control cobalt liquid-EDTA liquid inventories size3/ h, speed of agitator is 190 turns/min, dimension
The temperature for holding course of reaction is 40 DEG C, and pH is 9.0, reacts 8h, obtains finely dispersed black precipitate, is washed through 95 DEG C of hot water centrifugations
Wash, 80 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 72.1%, Na+Mass concentration size
For 395ppm.
Comparative example 2：
a）Compound concentration is 150g/L cobalt chloride-EDTA solution, and EDTA additions are 4 % of cobalt ions gross mass；
b）Prepare the sodium hydroxide solution that mass fraction is 32%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g EDTA, 70 DEG C are warming up to.In stirring bar
By cobalt chloride-EDTA solution, the step b of above-mentioned preparation process under part）The sodium hydroxide solution and air cocurrent of preparation are passed through instead
Answer in kettle, it is 200L/h, air mass flow 35m to control cobalt liquid-EDTA liquid inventories size3/ h, speed of agitator is 200 turns/min,
The temperature of maintenance reaction process be 70 DEG C, pH is 9.6, react 12h, obtain finely dispersed black precipitate, through 95 DEG C of hot water from
The heart is washed, and 80 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 71.8%, Na+Mass concentration
Size is 257ppm.
Comparative example 3：
a）Compound concentration is 90g/L cobalt chloride-EDTA solution, and EDTA additions are the 2.5% of cobalt ions gross mass；
b）Prepare the sodium hydroxide solution that mass fraction is 28%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g EDTA, 60 DEG C are warming up to.In stirring bar
By cobalt chloride-EDTA solution, the step b of above-mentioned preparation process under part）The sodium hydroxide solution and air cocurrent of preparation are passed through instead
Answer in kettle, it is 150L/h, air mass flow 25m to control cobalt liquid-EDTA liquid inventories size3/ h, speed of agitator is 215 turns/min,
The temperature of maintenance reaction process be 60 DEG C, pH is 9.2, react 15h, obtain finely dispersed black precipitate, through 95 DEG C of hot water from
The heart is washed, and 100 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 72.3%, Na+Mass concentration
Size is 289ppm.
Comparative example 4：
a）Compound concentration is 60g/L cobalt chloride-EDTA solution, and EDTA additions are the 3.5% of cobalt ions gross mass；
b）Prepare the sodium hydroxide solution that mass fraction is 32%；
c）Pure water is added into reactor to agitating paddle bottom, and adds 600g EDTA, 50 DEG C are warming up to.In stirring bar
By cobalt chloride-EDTA solution, the step b of above-mentioned preparation process under part）The sodium hydroxide solution and air cocurrent of preparation are passed through instead
Answer in kettle, it is 150L/h, air mass flow 15m to control cobalt liquid-EDTA liquid inventories size3/ h, speed of agitator is 190 turns/min,
The temperature of maintenance reaction process is 50 DEG C, and pH is 9.0, reacts 8h, obtains finely dispersed black precipitate, is centrifuged through 95 DEG C of hot water
Washing, 80 DEG C of dryings obtain the spherical Co of black3O4Powder, the weight/mass percentage composition of its cobalt is 71.6%, Na+Mass concentration is big
Small is 325ppm.
Embodiment 1 ~ 5 is the experiment in 85 ~ 95 DEG C of high temperature ranges of the invention being mainly concerned with, and comparative example 1 ~ 4 is
Experiment of the early stage in 40-70 DEG C of temperature progress.Na in the cobaltosic oxide obtained under cryogenic+ Content is relatively
High, it is impossible to meet the requirement in market, therefore, the present invention improves reaction temperature on the basis of early stage, using high temperature, low pH
Na in the cobaltosic oxide precursor that condition is obtained+Mass concentration substantially reduce, be even up to below 100ppm, well
The mobility of presoma is improved, while for the internal resistance of battery can be effectively reduced after positive electrode.
Embodiment described above only expresses embodiments of the present invention, and it describes more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent substitution or equivalent transformation
Art scheme, all should fall within the scope and spirit of the invention.
Claims (10)
1. a kind of preparation method of low sodium cobaltosic oxide, comprises the following steps：
Preparation process, mixes progress complex reaction with complexing agent by cobalt salt and obtains cobalt salt complex solution；
Reactions steps, cobalt salt complex solution, sodium hydroxide solution and air are passed through in reaction unit under agitation
Fully reacted, reaction temperature is 85 ~ 95 DEG C, pH is the .8 of 9 .2 ~ 9, reaction washes the sediment of acquisition through centrifugation after terminating
Wash and dry the low sodium cobaltosic oxide of acquisition.
2. low sodium cobaltosic oxide preparation method according to claim 1, it is characterised in that in preparation process, the cobalt
Salt is cobalt chloride or cobaltous sulfate, and the complexing agent is selected from least one of EDTA, diethanol amine, triethanolamine and DTPA.
3. low sodium cobaltosic oxide preparation method according to claim 1 or 2, it is characterised in that in reactions steps, instead
It is 5 ~ 20h between seasonable, mixing speed is 180 ~ 215r/min.
4. low sodium cobaltosic oxide preparation method according to claim 1, it is characterised in that the preparation process also includes
Sodium hydroxide is dissolved in water and sodium hydroxide solution is obtained, and controls the mass percent of sodium hydroxide for 25-32%.
5. low sodium cobaltosic oxide preparation method according to claim 1 or 2, it is characterised in that in preparation process, cobalt
Salinity is 30 ~ 150g/L, and the addition of complexing agent is the 1 ~ 6% of cobalt ions gross mass.
6. low sodium cobaltosic oxide preparation method according to claim 1, it is characterised in that described in reactions steps
Centrifuge washing is the hot water centrifuge washing at least 5 times with more than 90 DEG C.
7. low sodium cobaltosic oxide preparation method according to claim 1, it is characterised in that described in reactions steps
Dry temperature is 70 ~ 100 DEG C, and drying time is 2 ~ 8h.
8. low sodium cobaltosic oxide preparation method according to claim 1, it is characterised in that the low sodium cobaltosic oxide
The mass concentration of middle sodium ion is less than 100ppm.
9. low sodium cobaltosic oxide preparation method according to claim 1, it is characterised in that described in reactions steps
The uninterrupted of cobalt salt complex solution is 120 ~ 200L/h；Air intake is 15 ~ 35 m3/h。
10. low sodium cobaltosic oxide preparation method according to claim 1 or 2, it is characterised in that in reactions steps,
Pure water is added first into reaction unit and complexing agent is mixed, and is warming up to 85 ~ 95 DEG C.
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| CN106082358A (en) * | 2016-06-22 | 2016-11-09 | 荆门市格林美新材料有限公司 | The preparation method of Cobalto-cobaltic oxide |
| CN108862405A (en) * | 2017-05-15 | 2018-11-23 | 江苏凯力克钴业股份有限公司 | A kind of preparation method and device of low sodium cobaltosic oxide |
| CN107188243A (en) * | 2017-06-27 | 2017-09-22 | 荆门市格林美新材料有限公司 | The method of the ultra-fine battery-grade cobaltosic oxide of Hydrothermal Synthesiss |
| CN108172782B (en) * | 2017-12-13 | 2021-06-04 | 郑州大学 | Preparation method and application of carbon-coated porous cobaltous oxide nano material with shell-core structure |
| CN112850801B (en) * | 2019-11-28 | 2023-10-31 | 荆门市格林美新材料有限公司 | Preparation method of large-particle cobaltosic oxide |
| CN112850803A (en) * | 2019-11-28 | 2021-05-28 | 荆门市格林美新材料有限公司 | Synthesis method of high-tap-density superfine cobaltosic oxide |
| CN112645393A (en) * | 2020-12-21 | 2021-04-13 | 格林美（江苏）钴业股份有限公司 | Preparation method of cobaltosic oxide |
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| CN101585559B (en) * | 2009-06-14 | 2011-02-16 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
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