CN105600839A - Preparation method of battery-grade cobalt carbonate - Google Patents
Preparation method of battery-grade cobalt carbonate Download PDFInfo
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- CN105600839A CN105600839A CN201410670437.6A CN201410670437A CN105600839A CN 105600839 A CN105600839 A CN 105600839A CN 201410670437 A CN201410670437 A CN 201410670437A CN 105600839 A CN105600839 A CN 105600839A
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Abstract
The invention relates to a preparation method of battery-grade cobalt carbonate, which belongs to the field of electrochemistry. The method comprises the following steps: 1) preparing 60-120 g/L of a cobalt salt aqueous solution and 100-400 g/L of an ammonium bicarbonate aqueous solution; 2) adding the ammonium bicarbonate aqueous solution in a reaction vessel, heating the material to the temperature of 40-60 DEG C; 3) under a stirring state, adding the cobalt salt aqueous solution in the reaction vessel; 4) controlling a pH value of a reaction terminal point at 7-7.5; 5) standing and aging the material for more than 1 hour, precipitating an upper layer and extracting mother liquor, keeping a precipitate in the reaction vessel; adding the ammonium bicarbonate aqueous solution in the reaction vessel, heating the material to the temperature of 40-60 DEG C; 6) repeating steps of 3)-5), performing secondary precipitation; and 7) then repeating the steps of 2)-5) until the required granularity is achieved. The method has the advantages of simple operation and easy control, can be widely used for producing battery materials such as cobaltosic oxide and powder metallurgy materials such as cobaltpowder having conventional granularity and large granularity.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of preparation method of LITHIUM BATTERY cobalt carbonate, the coarsegrain spherical cobaltous carbonate that the method is produced can be used for producing the battery material such as cobaltosic oxide, cobalt powder and the metal material of regular particle size and coarsegrain.
Background technology
Cobalt carbonate is as cobaltosic oxide, the presoma of the battery materials such as cobalt acid lithium, determine to a great extent the performance of battery material, use now more cobaltosic oxide particle size mostly to be D50=5-10 micron, it is by being to be that D50 is that the cobalt carbonate calcining of 10-12 micron forms by granularity, this part is used for middle-end battery material, and the research of battery material direction is in recent years found, the battery material performance that the cobaltosic oxide of coarsegrain is produced is better, have higher voltage platform and compacted density, the battery material more application of being produced by the cobaltosic oxide of coarsegrain is in high-end field. and the cobaltosic oxide of coarsegrain is mainly formed by the cobalt carbonate calcining of coarsegrain, therefore the cobalt carbonate of coarsegrain plays conclusive effect to the performance of cobaltosic oxide and battery material.
Production granularity is more in the cobalt carbonate technique of D50=10-12 micron now, there are cobalt liquid and ammonium bicarbonate aqueous solution stream to add the method (and addition) of reactor, cobalt liquid adds the method (positive addition) in ammonium bicarbonate aqueous solution, ammonium bicarbonate aqueous solution adds the method (anti-addition) in cobalt liquid and repeats and addition, but just in the process of producing cobalt carbonate, also addition is poor with the positive prepared cobalt carbonate granularity of addition and sphericity for these methods, ram-jolt density is on the low side, can make epigranular and the good cobalt carbonate of sphericity although repeat also addition, ram-jolt density is also better, but repeat to precipitate number of times nearly more than 20 time, production time is long, requirement equipment is many.
And these methods are just suitable for when the cobalt carbonate in D50=10 micron left and right in production granularity, and if production granularity at D50=15-20 micron even more when the cobalt carbonate of coarsegrain, said method just cannot reach, and product granularity, pattern are all poor. Therefore how overcoming the deficiencies in the prior art is problems that current technical field of electrochemistry is needed solution badly.
Summary of the invention
The object of the invention is in order to solve the deficiencies in the prior art, a kind of preparation method of LITHIUM BATTERY cobalt carbonate is provided, the method production technology, simple to operate, be easy to control, can be widely used in the battery material such as cobaltosic oxide, cobalt powder of producing regular particle size and coarsegrain.
The present invention is by cobalt liquid and the repeatedly anti-method adding of ammonium bicarbonate aqueous solution, by controlling the Parameter Conditions such as reaction end PH, temperature, flow, mixing speed, concentration, produces the spherical cobaltous carbonate of regular particle size and coarsegrain.
The technical solution used in the present invention is as follows:
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), preparation cobalt saline solution 60-120g/L, ammonium bicarbonate aqueous solution 100-400g/L;
Step (2), joins ammonium bicarbonate aqueous solution in reactor by reactor volume 1/3, is heated to 40-60 DEG C;
Step (3), under stirring, joins cobalt saline solution in the ammonium bicarbonate aqueous solution in reactor by the flow of 1-5L/h;
Step (4), controlling reaction end PH is 7-7.5,, when in cobalt saline solution adition process, when pH value reaches 7-7.5 in reactor, stops adding cobalt saline solution;
Step (5), still aging 1 hour above after, by the liquor abstraction after the precipitation of upper strata, sediment is stayed in reactor;
Step (6) adds reactor volume 1/3 ammonium bicarbonate aqueous solution again in reactor, is warming up to 40-60 DEG C;
Step (7), repeating step (3)-(5), precipitate for the second time;
Step (8), repeating step (2)-(5) again after precipitation for the second time, until reach needed granularity.
Cobalt saline solution described in technique scheme is cobalt chloride or cobalt sulfate solution.
In technique scheme, further preferably described carbonic hydroammonium is 1.3:1 with the amount of substance ratio of cobalt chloride addition.
When being deposited to cobalt carbonate granularity in technique scheme and being D50=8-10 micron, carry out 2-4 precipitation process and can reach requirement granularity.
In technical solution of the present invention, when after precipitation 3-5 time, in reactor, sediment is more, and by a part of sediment in reactor is transferred in another reactor, two reactors can circulate precipitation to accelerate granularity speed of production simultaneously.
The described speed that reduces by half of step in technical solution of the present invention (3) is 150-200 rev/min.
In technique scheme, further preferably the preparation method of described LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), preparation cobalt chloride solution 60-120g/L, ammonium bicarbonate aqueous solution 100-400g/L;
Step (2), joins ammonium bicarbonate aqueous solution in reactor by 20L, is heated to 40-60 DEG C;
Step (3), under stirring, joins cobalt chloride solution in the ammonium bicarbonate aqueous solution in reactor by the flow of 3L/h;
Step (4), in the time that the cobalt chloride adding and carbonic hydroammonium mass ratio are 1:1.3, stops adding cobalt chloride solution;
Step (5), still aging 1 hour above after, by the liquor abstraction after the precipitation of upper strata, sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 40-60 DEG C;
Step (7), repeating step (3)-(5), precipitate for the second time;
Step (8), repeating step (2)-(5) again after precipitation for the second time, until reach needed granularity.
Compared with prior art, its beneficial effect is in the present invention:(1) preparation method of LITHIUM BATTERY cobalt carbonate of the present invention, simple to operate, is easy to control, and just can make at short notice epigranular, pattern is good, ram-jolt density is high cobalt carbonate; (2) the present invention not only can produce the cobaltosic oxide of regular particle size, can also produce granularity at the even more spherical cobaltous carbonate of coarsegrain of 15-20 micron, and product good sphericity, epigranular; (3) the product scope of application of the present invention is wider, can be widely used in producing the battery material such as cobaltosic oxide, cobalt acid lithium of coarsegrain.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the obtained LITHIUM BATTERY cobalt carbonate of embodiment 3;
Fig. 2 is the scanning electron microscope (SEM) photograph of the obtained LITHIUM BATTERY cobalt carbonate of embodiment 8.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 100g/L, ammonium bicarbonate aqueous solution concentration is 300g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 40 DEG C;
Step (3), opens and stirs, and speed of agitator is 200 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.0, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 8.7 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 40 DEG C;
Step (7), opens and stirs, repeat to precipitate for the second time, operation and precipitated phase for the first time with, for the second time after precipitation granularity be D50 at 10.2 microns, after precipitation, granularity is that D50 is 12 microns for the third time, ram-jolt density 1.9g/cm3。
Embodiment 2
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt sulfate solution compound concentration is 100g/L, ammonium bicarbonate aqueous solution concentration is 400g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 50 DEG C;
Step (3), opens and stirs, and speed of agitator is 150 revs/min, in reactor, adds cobalt sulfate solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.2, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 9.2 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 50 DEG C;
Step (7), opens and stirs, repeat to precipitate for the second time, operation and precipitated phase for the first time with, for the second time after precipitation granularity be D50 at 11.7 microns, ram-jolt density 1.9g/cm3。
Embodiment 3
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 80g/L, ammonium bicarbonate aqueous solution concentration is 250g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 60 DEG C;
Step (3), opens and stirs, and speed of agitator is 180 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.3, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 8.3 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 60 DEG C;
Step (7), opens and stirs, and repeats to precipitate for the second time, and operation is with precipitated phase is same for the first time, and after precipitation, granularity is that D50 is at 10.5 microns for the second time. After precipitation, granularity is that D50 is 12 microns for the third time, ram-jolt density 1.9g/cm3. Its scanning electron microscope (SEM) photograph as shown in Figure 1.
Embodiment 4
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 60g/L, ammonium bicarbonate aqueous solution concentration is 100g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 60 DEG C;
Step (3), opens and stirs, and speed of agitator is 180 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), in the time that the carbonic hydroammonium adding is 1.3:1 with the amount of substance ratio of cobalt chloride addition, stops adding cobalt chloride solution; This is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 8.3 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 60 DEG C;
Step (7), opens and stirs, and repeats to precipitate for the second time, and operation is with precipitated phase is same for the first time, and after precipitation, granularity is that D50 is at 10.5 microns for the second time. After precipitation, granularity is that D50 is 12 microns for the third time, ram-jolt density 1.9g/cm3。
Embodiment 5
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 120g/L, ammonium bicarbonate aqueous solution concentration is 400g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 60 DEG C;
Step (3), opens and stirs, and speed of agitator is 180 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.5, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 8.3 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 60 DEG C;
Step (7), opens and stirs, and repeats to precipitate for the second time, and operation is with precipitated phase is same for the first time, and after precipitation, granularity is that D50 is at 10.5 microns for the second time. After precipitation, granularity is that D50 is 12 microns for the third time, ram-jolt density 1.9g/cm3。
Embodiment 6
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 100g/L, ammonium bicarbonate aqueous solution concentration is 300g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 40 DEG C;
Step (3), opens and stirs, and speed of agitator is 200 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.0, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 8.7 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 40 DEG C;
Step (7), open and stir, repeat to precipitate for the second time, operation is with precipitated phase is same for the first time, after precipitation, granularity is that D50 is at 12.5 microns for the second time, after repeating to precipitate for the third time, D50 is at 14.3 microns, repeat above step, when having carried out, after the 4th precipitation, precipitation in reactor being migrated out to 1/3 to another reactor, after respectively adding 20L ammonium bicarbonate aqueous solution in two reactors, proceed precipitation, when proceeding to after 5 precipitations, granularity reaches D50 at 19.2 microns, ram-jolt density 2.0g/cm3。
Embodiment 7
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 100g/L, ammonium bicarbonate aqueous solution concentration is 400g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 50 DEG C;
Step (3), opens and stirs, and speed of agitator is 150 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.2, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 9.2 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) again adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 50 DEG C;
Step (7), open and stir, repeat to precipitate for the second time, operation is with precipitated phase is same for the first time, after precipitation, granularity is that D50 is at 11.7 microns for the second time, after repeating to precipitate for the third time, D50 is at 13.5 microns, repeat above step, when having carried out, after the 4th precipitation, precipitation in reactor being migrated out to 1/3 to another reactor, after respectively adding 20L ammonium bicarbonate aqueous solution in two reactors, proceed precipitation, when proceeding to after 6 precipitations, granularity reaches D50 at 18.8 microns, ram-jolt density 2.0g/cm3。
Embodiment 8
A preparation method for LITHIUM BATTERY cobalt carbonate, comprises the steps:
Step (1), cobalt chloride solution compound concentration is 80g/L, ammonium bicarbonate aqueous solution concentration is 250g/L;
Step (2) first adds 20L ammonium bicarbonate aqueous solution in reactor, is warming up to 60 DEG C;
Step (3), opens and stirs, and speed of agitator is 180 revs/min, in reactor, adds cobalt chloride solution with the flow of 3L/h;
Step (4), controlling reaction end PH is 7.3, and this is for precipitating for the first time, and now the cobalt carbonate granularity of precipitation is that D50 is at 8.3 microns;
Step (5), after still aging 1 hour extracts upper strata clarified mother liquor out, and sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 60 DEG C;
Step (7), open and stir, repeat to precipitate for the second time, operation is with precipitated phase is same for the first time, after precipitation, granularity is that D50 is at 10.5 microns for the second time, after repeating to precipitate for the third time, D50 is at 13 microns, repeat above step, when having carried out, after the 5th precipitation, precipitation in reactor being migrated out out to 1/3 to another reactor, after respectively adding 20L ammonium bicarbonate aqueous solution in two reactors, proceed precipitation, when proceeding to after seven precipitations, granularity reaches D50 at 20.3 microns, ram-jolt density 2.0g/cm3. Its scanning electron microscope (SEM) photograph as shown in Figure 2.
Claims (7)
1. a preparation method for LITHIUM BATTERY cobalt carbonate, is characterized in that comprising the steps:
Step (1), preparation cobalt saline solution 60-120g/L, ammonium bicarbonate aqueous solution 100-400g/L;
Step (2), joins ammonium bicarbonate aqueous solution in reactor by reactor volume 1/3, is heated to 40-60 DEG C;
Step (3), under stirring, joins cobalt saline solution in the ammonium bicarbonate aqueous solution in reactor by the flow of 1-5L/h;
Step (4), controlling reaction end PH is 7-7.5,, when in cobalt saline solution adition process, when pH value reaches 7-7.5 in reactor, stops adding cobalt saline solution;
Step (5), still aging 1 hour above after, by the liquor abstraction after the precipitation of upper strata, sediment is stayed in reactor;
Step (6) adds reactor volume 1/3 ammonium bicarbonate aqueous solution again in reactor, is warming up to 40-60 DEG C;
Step (7), repeating step (3)-(5), precipitate for the second time;
Step (8), repeating step (2)-(5) again after precipitation for the second time, until reach needed granularity.
2. the preparation method of LITHIUM BATTERY cobalt carbonate according to claim 1, is characterized in that described cobalt saline solution is cobalt chloride or cobalt sulfate solution.
3. the preparation method of LITHIUM BATTERY cobalt carbonate according to claim 2, is characterized in that described carbonic hydroammonium and the amount of substance ratio of cobalt chloride addition are 1.3:1.
4. the preparation method of LITHIUM BATTERY cobalt carbonate according to claim 1, when it is characterized in that being deposited to cobalt carbonate granularity and being D50=8-10 micron, carries out 2-4 precipitation process and reaches requirement granularity.
5. the preparation method of LITHIUM BATTERY cobalt carbonate according to claim 1, it is characterized in that when after precipitation 4-5 time, in reactor, sediment is more, by a part of sediment in reactor is transferred in another reactor, two reactors can circulate precipitation to accelerate granularity speed of production simultaneously.
6. the preparation method of LITHIUM BATTERY cobalt carbonate according to claim 1, is characterized in that the described speed that reduces by half of step (3) is 150-200 rev/min.
7. the preparation method of LITHIUM BATTERY cobalt carbonate according to claim 1, is characterized in that comprising the steps:
Step (1), preparation cobalt chloride solution 60-120g/L, ammonium bicarbonate aqueous solution 100-400g/L;
Step (2), joins ammonium bicarbonate aqueous solution in reactor by 20L, is heated to 40-60 DEG C;
Step (3), under stirring, joins cobalt chloride solution in the ammonium bicarbonate aqueous solution in reactor by the flow of 3L/h;
Step (4), in the time that the cobalt chloride adding and carbonic hydroammonium mass ratio are 1:1.3, stops adding cobalt chloride solution;
Step (5), still aging 1 hour above after, by the liquor abstraction after the precipitation of upper strata, sediment is stayed in reactor;
Step (6) adds 20L ammonium bicarbonate aqueous solution again in reactor, is warming up to 40-60 DEG C;
Step (7), repeating step (3)-(5), precipitate for the second time;
Step (8), repeating step (2)-(5) again after precipitation for the second time, until reach needed granularity.
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| CN106673073A (en) * | 2016-12-23 | 2017-05-17 | 荆门市格林美新材料有限公司 | Method for preparing small-particle size large-bulk cobalt carbonate |
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| CN106673073A (en) * | 2016-12-23 | 2017-05-17 | 荆门市格林美新材料有限公司 | Method for preparing small-particle size large-bulk cobalt carbonate |
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| CN109467135A (en) * | 2018-10-31 | 2019-03-15 | 眉山顺应动力电池材料有限公司 | A kind of LITHIUM BATTERY cobalt carbonate preparation method and the cobalt carbonate of preparation |
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| CN109354076A (en) * | 2018-12-14 | 2019-02-19 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation preparation dimensional Co CO3Method |
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