CN105668650A - Method for preparing low-sodium cobaltosic oxide - Google Patents
Method for preparing low-sodium cobaltosic oxide Download PDFInfo
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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Abstract
The invention discloses a method for preparing low-sodium cobaltosic oxide. The method includes a preparation step, to be more specific, mixing cobalt salt and complex agents with one another to obtain mixtures and carrying out complex reaction on the mixtures to obtain cobalt salt complex compound solution; a reaction step, to be more specific, filling a reaction device with the cobalt salt complex compound solution, sodium hydroxide solution and air under a stirring condition, carrying out sufficient reaction on the cobalt salt complex compound solution, the sodium hydroxide solution and the air under the conditions of the reaction temperature of 85-95 DEG C and the pH (potential of hydrogen) of 9.0-9.8 to obtain precipitates, centrifugally washing the precipitates after reaction is completed and drying the precipitates to obtain the low-sodium cobaltosic oxide. The method has the advantages that precursors for cobaltosic oxide battery materials are prepared by the aid of the high-temperature and low-pH method, primary particles of the formed precursors are large, accordingly, inclusion of Na+ among the particles can be effectively reduced, and the content of the Na+ can be effectively decreased; the content of the Na+ which remains on the surfaces of the particles further can be reduced if the method is matched with intensified washing; the precursors for the cobaltosic oxide battery materials have regular morphology and are high in yield, and accordingly problems of excessively high content of Na+ in existing cobaltosic oxide battery materials and high cost of the existing cobaltosic oxide battery materials can be solved.
Description
Technical field
The present invention relates to technical field of lithium ion, the preparation method particularly relating to a kind of low sodium Cobalto-cobaltic oxide.
Background technology
Lithium ion battery enjoys favor because of advantages such as its voltage are high, energy density is high, have extended cycle life, environmental pollution is little, in recent years, along with the further growth of small movable battery requirements, creates good opportunity for lithium ion battery industrial expansion. Positive electrode is core and the key of lithium ion battery. Wherein LiCoO2Stability Analysis of Structures, specific capacity are high, combination property highlights, and have good chemical property, are the commonly used positive electrodes of current commercial Li-ion battery.
Take the Na in the Cobalto-cobaltic oxide battery material presoma that precipitation of hydroxide method produces at present+Content is typically in about 100-300ppm. Na+Too high levels, it is easy to cause cobaltosic oxide precursor poor fluidity, for increasing the internal resistance of battery after cell positive material. Although ammonia or the ammonium salt sedimentation method produce Na in Cobalto-cobaltic oxide product+Content is low, and product quality is better, but produces substantial amounts of ammonia nitrogen waste water, and production cost is high, and seriously polluted to environment.
Summary of the invention
The preparation method that the technical problem to be solved in the present invention is to provide a kind of low sodium Cobalto-cobaltic oxide, to reduce Na between granule+Be mingled with, it is thus achieved that even particle distribution, good fluidity and Na+The low sodium Cobalto-cobaltic oxide material that mass concentration is low.
The technical problem to be solved is achieved by the following technical programs: the preparation method of a kind of low sodium Cobalto-cobaltic oxide, comprises the following steps:
Preparation process, mixes cobalt salt with chelating agent and carries out complex reaction and obtain cobalt salt complex solution;
Reactions steps, cobalt salt complex solution, sodium hydroxide solution and air are passed in reaction unit under agitation and fully reacts, reaction temperature is 85 ~ 95 DEG C, and pH is 9.0 ~ 9.8, reacts and the precipitate of acquisition washs after terminating and dries acquisition low sodium Cobalto-cobaltic oxide by centrifugation.
Further, in preparation process, described cobalt salt is cobaltous chloride or cobaltous sulfate, described chelating agent at least one in EDTA, diethanolamine, triethanolamine and DTPA.
Further, in reactions steps, reaction temperature is 85 ~ 95 DEG C, and pH is 9.0 ~ 9.8, and the response time is 5 ~ 20h, and mixing speed is 180 ~ 215r/min.
Further, described preparation process also includes sodium hydroxide being dissolved in water and obtaining sodium hydroxide solution, and the mass percent controlling sodium hydroxide is 25-32%.
Further, in preparation process, cobalt salt concentration is 30 ~ 150g/L, and the addition of chelating agent is the 1 ~ 6% of cobalt ion gross mass.
Further, in reactions steps, described centrifuge washing is the hot water centrifuge washing more than 5 times with more than 90 DEG C.
Further, in reactions steps, described dry temperature is 70 ~ 100 DEG C, and drying time is 2 ~ 8h.
Further, in described low sodium Cobalto-cobaltic oxide sodium ion mass concentration lower than 100ppm.
Further, in reactions steps, the uninterrupted of described cobalt salt complex solution is 120 ~ 200L/h; Air intake is 15 ~ 35m3/h。
Further, in reactions steps, in reaction unit, first add pure water and EDTA mixing, and be warming up to 85 ~ 95 DEG C.
There is advantages that the present invention adopts high temperature, the method for low pH prepares Cobalto-cobaltic oxide battery material presoma, the primary particle of the presoma of formation is bigger, it is possible to effectively reduce Na between granule+Be mingled with, effectively reduce Na+Content; As coordinated strengthening washing, the Na remaining in particle surface also can be reduced further+Content. Additionally, the Cobalto-cobaltic oxide battery material presoma regular appearance that the method for the invention obtains, productivity is high.
Accompanying drawing explanation
Fig. 1 is the flow chart of the low sodium Cobalto-cobaltic oxide preparation method of the present invention.
Fig. 2 is the surface topography schematic diagram of the Cobalto-cobaltic oxide that embodiment 1 prepares.
Detailed description of the invention
It should be noted that when not conflicting, the embodiment in the application and the feature in embodiment can be combined with each other, and below in conjunction with the drawings and specific embodiments, the present invention are described in further detail.
As it is shown in figure 1, the preparation method that the present invention provides a kind of low sodium Cobalto-cobaltic oxide, comprise the following steps:
A) preparation cobalt salt-chelating agent cobalt salt complex solution: cobalt salt and chelating agent are mixed to get the cobalt salt complex solution that cobalt salt concentration is 30 ~ 150g/L, and the addition of its complexing agent is preferably the 1 ~ 6% of cobalt ion gross mass; Described cobalt salt can adopt cobaltous chloride or cobaltous sulfate, it is preferred to use cobaltous chloride; Namely described chelating agent can be selected for EDTA(: tetraacethyl diaminoethanes), diethanolamine, triethanolamine, DTPA(diethylenetriamine pentacarboxylic acid salt) at least one, it is preferred to use EDTA.
B) preparation sodium hydroxide solution: sodium hydroxide is formulated as the sodium hydroxide solution that mass percent is 25 ~ 32%.
C) Cobalto-cobaltic oxide is prepared: hydroxide solution that the cobalt salt complex solution that prepared by preparation process, step b) prepare and air is taked under agitation and stream mode is passed in reaction unit and reacts, reaction temperature is 85 ~ 95 DEG C, pH is 9.0 ~ 9.8, reaction terminate after by hot water centrifuge washing at least 5 times through more than 90 DEG C of the precipitate that obtains, preferably washing 8 times, and at 70 ~ 100 DEG C of drying and processing 2 ~ 8h, prepare Na+Mass concentration is at the battery-grade cobaltosic oxide battery material presoma of below 100ppm and regular appearance.
In step c), described reaction unit is preferably reactor, and controlling cobalt salt complex solution uninterrupted is 120 ~ 200L/h, and air intake is 15 ~ 35m3/ h;Controlling stirring paddle mixing speed in reaction unit in course of reaction is 180 ~ 215r/rpm, and the response time is 5 ~ 20h.
Above step a) and step b) are all parts for preparation process, there is no strict tandem and distinguish, even, it is also possible to adopt the hydroxide solution that directly commercially concentration is suitable to carry out step of replacing b).
Preferably, in step c), in reaction unit, first add pure water to its internal stirring paddle, be subsequently adding chelating agent mixing, and be warming up to 85 ~ 95 DEG C, then carry out follow-up operation. The chelating agent added when the chelating agent added in this step is with preparation cobalt salt solution is consistent.
The present invention adopts high temperature, the method for low pH prepares Cobalto-cobaltic oxide battery material presoma, and the primary particle of the presoma of formation is bigger, it is possible to effectively reduce Na between granule+Be mingled with, effectively reduce Na+Content; As coordinated strengthening washing, the Na remaining in particle surface also can be reduced further+Content. Additionally, the Cobalto-cobaltic oxide battery material presoma regular appearance that the method for the invention obtains, productivity is high, overcomes Na in existing Cobalto-cobaltic oxide battery material+Too high levels and the problem of high cost.
Specific embodiment of the invention process is further illustrated below by way of several embodiments.
Embodiment 1:
A) compound concentration is the cobaltous chloride-EDTA solution of 30g/L, and EDTA addition is the 1.27% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 32%;
C) in reactor, add pure water to stirring paddle, and add 600gEDTA, be warmed up to 85 DEG C. Temperature herein refers to reaction temperature, should first be warming up to reaction temperature before starting the reaction, maintain constant reaction temperature, adds the cobaltous chloride-EDTA of preparation, liquid caustic soda etc. and reacts. The sodium hydroxide solution of the cobaltous chloride-EDTA solution prepared by above-mentioned steps a) under agitation, step b) preparation and air also circulate in reactor, control cobalt liquid-EDTA liquid inventory and are sized to 120L/h, air mass flow 15m3/ h, speed of agitator is 180 turns/min, and the temperature maintaining course of reaction is 85 DEG C, and pH is 9.5, reacts 5h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 70 DEG C dry, obtain the spherical Co of black3O4Powder body, its surface topography as in figure 2 it is shown, the weight/mass percentage composition of its cobalt is 72.5%, Na+Mass concentration is sized to 78ppm.
Embodiment 2:
A) compound concentration is the cobaltous chloride-diethanolamine solution of 60g/L, and diethanolamine addition is the 1.0% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 25%;
C) in reactor, add pure water to stirring paddle, and add 600g diethanolamine, be warmed up to 90 DEG C. The sodium hydroxide solution of cobaltous chloride-diethanolamine solution of being prepared by above-mentioned steps a) under agitation, step b) preparation and air also circulate in reactor, control cobalt liquid-EDTA liquid inventory and are sized to 150L/h, air mass flow 15m3/ h, speed of agitator is 190 turns/min, and the temperature maintaining course of reaction is 90 DEG C, and pH is 9.0, reacts 8h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 80 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 72.8%, Na+Mass concentration is sized to 102ppm, and its surface topography is similar with Fig. 2.
Embodiment 3:
A) compound concentration is the cobaltous chloride-triethanolamine solution of 90g/L, and triethanolamine addition is the 2% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 30%;
C) in reactor, add pure water to stirring paddle, and add 600g triethanolamine, be warmed up to 95 DEG C. The sodium hydroxide solution of cobaltous chloride-triethanolamine solution of being prepared by above-mentioned steps a) under agitation, step b) preparation and air also circulate in reactor, control cobalt liquid-EDTA liquid inventory and are sized to 150L/h, air mass flow 25m3/ h, speed of agitator is 215 turns/min, and the temperature maintaining course of reaction is 95 DEG C, and pH is 9.2, reacts 15h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 100 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 72.6%, Na+Mass concentration is sized to 82ppm, and its surface topography is similar with Fig. 2.
Embodiment 4:
A) compound concentration is the cobaltous sulfate-DTPA solution of 120g/L, and DTPA addition is the 6% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 28%;
C) in reactor, add pure water to stirring paddle, and add 600gDTPA, be warmed up to 90 DEG C. The sodium hydroxide solution of the cobaltous sulfate-DTPA solution prepared by above-mentioned steps a) under agitation, step b) preparation and air also circulate in reactor, control cobaltous sulfate-DTPA liquid inventory and are sized to 180L/h, air mass flow 30m3/ h, speed of agitator is 200 turns/min, and the temperature maintaining course of reaction is 90 DEG C, and pH is 9.8, reacts 20h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 85 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 72.1%, Na+Mass concentration is sized to 110ppm, and its surface topography is similar with Fig. 2.
Embodiment 5
A) compound concentration is the cobaltous chloride-EDTA solution of 150g/L, and EDTA addition is the 4% of cobalt ion gross mass;
C) in reactor, add pure water to stirring paddle, and add 600gEDTA, be warmed up to 85 DEG C. Cobaltous chloride-EDTA the solution prepared by above-mentioned steps a) under agitation, the sodium hydroxide solution that mass fraction is 32% directly buied from the market and air also circulate in reactor, control cobalt liquid-EDTA liquid inventory and be sized to 200L/h, air mass flow 35m3/ h, speed of agitator is 200 turns/min, and the temperature maintaining course of reaction is 85 DEG C, and pH is 9.6, reacts 12h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 80 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 72.6%, Na+Mass concentration is sized to 95ppm, and its surface topography is similar with Fig. 2.
Comparative example 1:
A) compound concentration is the cobaltous chloride-EDTA solution of 60g/L, and EDTA addition is the 3.5% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 25%;
C) in reactor, add pure water to stirring paddle, and add 600gEDTA, be warmed up to 40 DEG C. Under agitation by the cobaltous chloride-EDTA solution of above-mentioned steps a), the sodium hydroxide solution of step b) preparation and air circulate in reactor, control cobalt liquid-EDTA liquid inventory and be sized to 150L/h, air mass flow 15m3/ h, speed of agitator is 190 turns/min, and the temperature maintaining course of reaction is 40 DEG C, and pH is 9.0, reacts 8h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 80 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 72.1%, Na+Mass concentration is sized to 395ppm.
Comparative example 2:
A) compound concentration is the cobaltous chloride-EDTA solution of 150g/L, and EDTA addition is the 4% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 32%;
C) in reactor, add pure water to stirring paddle, and add 600gEDTA, be warmed up to 70 DEG C. Under agitation by the cobaltous chloride-EDTA solution of above-mentioned preparation process, the sodium hydroxide solution of step b) preparation and air circulate in reactor, control cobalt liquid-EDTA liquid inventory and be sized to 200L/h, air mass flow 35m3/ h, speed of agitator is 200 turns/min, and the temperature maintaining course of reaction is 70 DEG C, and pH is 9.6, reacts 12h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 80 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 71.8%, Na+Mass concentration is sized to 257ppm.
Comparative example 3:
A) compound concentration is the cobaltous chloride-EDTA solution of 90g/L, and EDTA addition is the 2.5% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 28%;
C) in reactor, add pure water to stirring paddle, and add 600gEDTA, be warmed up to 60 DEG C. Under agitation by the cobaltous chloride-EDTA solution of above-mentioned preparation process, the sodium hydroxide solution of step b) preparation and air circulate in reactor, control cobalt liquid-EDTA liquid inventory and be sized to 150L/h, air mass flow 25m3/ h, speed of agitator is 215 turns/min, and the temperature maintaining course of reaction is 60 DEG C, and pH is 9.2, reacts 15h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 100 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 72.3%, Na+Mass concentration is sized to 289ppm.
Comparative example 4:
A) compound concentration is the cobaltous chloride-EDTA solution of 60g/L, and EDTA addition is the 3.5% of cobalt ion gross mass;
B) preparation mass fraction is the sodium hydroxide solution of 32%;
C) in reactor, add pure water to stirring paddle, and add 600gEDTA, be warmed up to 50 DEG C. Under agitation by the cobaltous chloride-EDTA solution of above-mentioned preparation process, the sodium hydroxide solution of step b) preparation and air circulate in reactor, control cobalt liquid-EDTA liquid inventory and be sized to 150L/h, air mass flow 15m3/ h, speed of agitator is 190 turns/min, and the temperature maintaining course of reaction is 50 DEG C, and pH is 9.0, reacts 8h, obtains finely dispersed black precipitate, and through 95 DEG C of hot water centrifuge washings, 80 DEG C dry, obtain the spherical Co of black3O4Powder body, the weight/mass percentage composition of its cobalt is 71.6%, Na+Mass concentration is sized to 325ppm.
The experiment in 85 ~ 95 DEG C of high temperature ranges that embodiment 1 ~ 5 is mainly concerned with for the present invention, the experiment that comparative example 1 ~ 4 is early stage to be carried out the temperature of 40-70 DEG C. Na in the Cobalto-cobaltic oxide obtained under cryogenic+Content is of a relatively high, it is impossible to meet the requirement in market, and therefore, the present invention improves reaction temperature on the basis of early stage, adopts high temperature, Na in cobaltosic oxide precursor that the condition of low pH obtains+Mass concentration substantially reduce, even up to below 100ppm, improve the mobility of presoma well, the internal resistance of battery after being simultaneously used for positive electrode, can be effectively reduced.
Embodiment described above only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (10)
1. a preparation method for low sodium Cobalto-cobaltic oxide, comprises the following steps:
Preparation process, mixes cobalt salt with chelating agent and carries out complex reaction and obtain cobalt salt complex solution;
Reactions steps, cobalt salt complex solution, sodium hydroxide solution and air are passed in reaction unit under agitation and fully reacts, reaction temperature is 85 ~ 95 DEG C, and pH is 9.0 ~ 9.8, reacts and the precipitate of acquisition washs after terminating and dries acquisition low sodium Cobalto-cobaltic oxide by centrifugation.
2. low sodium Cobalto-cobaltic oxide preparation method according to claim 1, it is characterised in that in preparation process, described cobalt salt is cobaltous chloride or cobaltous sulfate, described chelating agent at least one in EDTA, diethanolamine, triethanolamine and DTPA.
3. low sodium Cobalto-cobaltic oxide preparation method according to claim 1 and 2, it is characterised in that in reactions steps, the response time is 5 ~ 20h, and mixing speed is 180 ~ 215r/min.
4. low sodium Cobalto-cobaltic oxide preparation method according to claim 1, it is characterised in that described preparation process also includes sodium hydroxide being dissolved in water and obtaining sodium hydroxide solution, and the mass percent controlling sodium hydroxide is 25-32%.
5. low sodium Cobalto-cobaltic oxide preparation method according to claim 1 and 2, it is characterised in that in preparation process, cobalt salt concentration is 30 ~ 150g/L, and the addition of chelating agent is the 1 ~ 6% of cobalt ion gross mass.
6. low sodium Cobalto-cobaltic oxide preparation method according to claim 1, it is characterised in that in reactions steps, described centrifuge washing is the hot water centrifuge washing at least 5 times with more than 90 DEG C.
7. low sodium Cobalto-cobaltic oxide preparation method according to claim 1, it is characterised in that in reactions steps, described dry temperature is 70 ~ 100 DEG C, and drying time is 2 ~ 8h.
8. low sodium Cobalto-cobaltic oxide preparation method according to claim 1, it is characterised in that in described low sodium Cobalto-cobaltic oxide, the mass concentration of sodium ion is lower than 100ppm.
9. low sodium Cobalto-cobaltic oxide preparation method according to claim 1, it is characterised in that in reactions steps, the uninterrupted of described cobalt salt complex solution is 120 ~ 200L/h; Air intake is 15 ~ 35m3/h。
10. low sodium Cobalto-cobaltic oxide preparation method according to claim 1 and 2, it is characterised in that in reactions steps, first adds pure water and chelating agent mixing in reaction unit, and is warming up to 85 ~ 95 DEG C.
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| CN108172782A (en) * | 2017-12-13 | 2018-06-15 | 郑州大学 | A kind of preparation method and application with shell-core structure carbon package porous oxidation Asia cobalt nano material |
| 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 |
| 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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| 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 |
| CN108172782A (en) * | 2017-12-13 | 2018-06-15 | 郑州大学 | A kind of preparation method and application with shell-core structure carbon package porous oxidation Asia cobalt nano material |
| 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 |
| 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 |
| CN112850801A (en) * | 2019-11-28 | 2021-05-28 | 荆门市格林美新材料有限公司 | Preparation method of large-particle cobaltosic oxide |
| 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 |
| 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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