CN106517259B - A kind of spherical Lithii carbonate and preparation method thereof - Google Patents
A kind of spherical Lithii carbonate and preparation method thereof Download PDFInfo
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- CN106517259B CN106517259B CN201611174906.0A CN201611174906A CN106517259B CN 106517259 B CN106517259 B CN 106517259B CN 201611174906 A CN201611174906 A CN 201611174906A CN 106517259 B CN106517259 B CN 106517259B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of spherical Lithii carbonates and preparation method thereof, include the following steps：Prepare sodium carbonate liquor and lithium sulfate solution；Surface conditioning agent is added in into sodium carbonate liquor or lithium sulfate solution and is stirred evenly；Under high-speed stirred state, lithium sulfate solution and sodium carbonate liquor are mixed, wherein, controlling reaction temperature is 85~100 DEG C；Heat preservation ageing is carried out under stirring at low speed state, material separation of solid and liquid is obtained into lithium carbonate wet product and sinker mother liquor；Spherical Lithii carbonate is obtained after lithium carbonate wet product is washed and dried.The present invention obtains spherical Lithii carbonate of the purity more than 99.5% by controlling process conditions and adding in surface conditioning agent, and the purity of gained spherical Lithii carbonate is higher and is not easy to reunite, and has good mobility and dispersibility, batch mixing and processing conducive to subsequent technique.
Description
Technical field
The invention belongs to lithium carbonate preparing technical fields, more particularly, are related to a kind of ball-type lithium carbonate and its preparation side
Method.
Background technology
Lithium carbonate is the important source material of fine chemistry industry production, is widely used in glass, ceramics, electronics industry, aluminium metallurgy and pharmacy
Etc. industries, be the important source material for producing other lithium compounds and lithium metal.
Carbonic acid reason or the basic material for manufacturing lithium ion battery.In recent years, it is big with power vehicle and energy-storage battery
Scale is broken out, and lithium carbonate applies the accounting in terms of battery also higher and higher.Lithium carbonate in the application of battery, granularity and point
It is very big to dissipate influence of the property to application performance.Such as prepared in LiFePO4 technical process using solid-phase synthesis, with ferric phosphate or its
Its phosphorus, source of iron are raw material, and addition lithium carbonate and other auxiliary materials are sintered to obtain LiFePO 4 material after being sufficiently mixed.Mobility
It is then possible in other supplementary material surfaces non-homogeneous dispersion with the lithium carbonate of poor dispersion, the consistency for leading to product is bad.
Document《The Study on Preparation of spherical fine carbonic acid powder for lithium》Provide a kind of system of nanoscale ball-type lithium carbonate
Preparation Method.This method is with technical grade LiOHH2O and NH4HCO3For raw material, react 20min under the conditions of 40 DEG C, obtained solid in
200 DEG C of dry 1h obtain carbonic acid powder for lithium, and granularity is 300~400nm.
But this method has the following disadvantages：1st, lithium hydroxide is used to prepare lithium carbonate for raw material, of high cost and yield is low
(market price of lithium hydroxide is higher than lithium carbonate)；2nd, there are ammonia and the water containing ammonium ion to generate in production process, ring can be endangered
Border and worker health, are unfavorable for industrialized production.
Invention content
In order to solve the problems in the existing technology, the object of the present invention is to provide one kind is at low cost, purity is high, more sharp
In industrialized production and environmental protection and effect more preferably ball-type lithium carbonate and preparation method thereof.
An aspect of of the present present invention provides the preparation method of spherical Lithii carbonate, and the preparation method includes the following steps：
A, sodium carbonate liquor and lithium sulfate solution are prepared；
B, surface conditioning agent is added in into sodium carbonate liquor or lithium sulfate solution and is stirred evenly；
C, under high-speed stirred state, lithium sulfate solution and sodium carbonate liquor are mixed, controlling reaction temperature 50
~100 DEG C；
D, heat preservation ageing is carried out under stirring at low speed state, material separation of solid and liquid is obtained into lithium carbonate wet product and sinker is female
Liquid；
E, spherical Lithii carbonate is obtained after the lithium carbonate wet product being washed and dried.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, in step, the sodium carbonate liquor
A concentration of 100~350g/L, the concentration of the lithium sulfate solution is with Li2O is calculated as 10~65g/L, sodium carbonate liquor and lithium sulfate
The amount of solution presses CO3 2-With Li2The molar ratio of O is 0.9~1.1 control.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, the surface conditioning agent for triethanolamine,
At least one of lauryl sodium sulfate and sodium carboxymethylcellulose.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, wherein, the surface conditioning agent is with water-soluble
The mode of liquid adds in and a concentration of 1~5g/L of surface conditioning agent aqueous solution, the addition of the surface conditioning agent aqueous solution
1 ‰~5 ‰ for overall solution volume.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, in step C, the high-speed stirred state
Under mixing speed for 150~2000r/min, feed time is 1.5~2.5h.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, by the carbonic acid before addition surface conditioning agent
Sodium carbonate liquor and lithium sulfate solution after sodium solution and lithium sulfate solution or addition surface conditioning agent are warming up to 50~100
DEG C to reach the reaction temperature in step C.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, in step D, the stirring at low speed state
Under mixing speed for 30~60r/min, heat preservation Aging Temperature is 50~100 DEG C, and heat preservation digestion time is 30~120min.
According to one embodiment of the preparation method of spherical Lithii carbonate of the present invention, in step E, drying temperature for 110~
220 DEG C, drying time is 2~4h.
Another aspect provides a kind of spherical Lithii carbonate, using the preparation method system of above-mentioned spherical Lithii carbonate
.
According to one embodiment of spherical Lithii carbonate of the present invention, the purity of the spherical Lithii carbonate is more than 99.5wt%
And grain shape is spherical or elliposoidal, average grain diameter D50 is 2~10 μm.
The solution that the lithium sulfate solution and technical grade sodium carbonate that the present invention is prepared using spodumene are prepared passes through control as raw material
Process conditions add in surface conditioning agent and obtain the spherical Lithii carbonate that purity is more than 99.5%, the purity of gained spherical Lithii carbonate compared with
It is high and be not easy to reunite, there is good mobility and dispersibility, be conducive to batch mixing and the processing of subsequent technique.
Description of the drawings
Fig. 1 shows the process flow chart of the preparation method of spherical Lithii carbonate according to an exemplary embodiment of the present invention.
Specific embodiment
All features or disclosed all methods disclosed in this specification or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification, unless specifically stated, can be equivalent by other or with similar purpose
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
.
First the principle and step of the preparation method of spherical Lithii carbonate of the present invention are described in detail below.The present invention is
The sodium carbonate liquor that the lithium sulfate solution and technical grade sodium carbonate prepared using spodumene is prepared is raw material, by controlling process conditions
And add in surface conditioning agent and obtain the spherical Lithii carbonate that purity is more than 99.5%, it can effectively substitute side of the prior art
Method, and the spherical Lithii carbonate of alternative currently marketed micro mist battery-level lithium carbonate is prepared.
Fig. 1 shows the process flow chart of the preparation method of spherical Lithii carbonate according to an exemplary embodiment of the present invention.Such as
Shown in Fig. 1, exemplary embodiment according to the present invention, the preparation method of the spherical Lithii carbonate includes following multiple steps.
Step A：
Prepare sodium carbonate liquor and lithium sulfate solution.
Wherein, lithium sulfate solution is prepared with spodumene, and sodium carbonate liquor is to prepare to obtain by technical grade sodium carbonate
Clear solution.Preferably, the Ca in lithium sulfate solution is controlled2+<0.01g/L and pH value are 7~12.
Specifically, a concentration of 100~350g/L of sodium carbonate liquor, the concentration of lithium sulfate solution is with Li2O is calculated as 10~
The amount of 65g/L, sodium carbonate liquor and lithium sulfate solution presses CO3 2-With Li2The molar ratio of O is 0.9~1.1 control.
Step B：
Surface conditioning agent is added in into sodium carbonate liquor or lithium sulfate solution and is stirred evenly.
Preferably, the surface conditioning agent that the present invention selects is triethanolamine, lauryl sodium sulfate and carboxymethyl cellulose
At least one of sodium, the addition of surface conditioning agent crystal grain can be prevented to grow up and make lithium carbonate particle uniformly and narrow particle size distribution.
Wherein, surface conditioning agent, which can be added in into sodium carbonate liquor, is uniformly mixed, and can also add in lithium sulfate solution
In be uniformly mixed, but be preferably added in sodium carbonate liquor.
Specifically, surface conditioning agent can be added in a manner of aqueous solution and surface conditioning agent aqueous solution a concentration of 1
~5g/L, the addition of the surface conditioning agent aqueous solution are 1 ‰~the 5 ‰ of overall solution volume.
Step C：
Under high-speed stirred state, lithium sulfate solution and sodium carbonate liquor are mixed, preferably by lithium sulfate solution
It is slowly added into sodium carbonate liquor up to adding, wherein, controlling reaction temperature is 50~100 DEG C.
Committed step of this step for the present invention, controlling reaction temperature are 50~100 DEG C, can maintain the work of reaction system
Property, increase extent of reaction, while reduce impurity package, have larger benefit to improving product purity.During practical operation, it can will add
Sodium carbonate liquor and lithium sulfate solution before entering surface conditioning agent are warming up to 50~100 DEG C, can also be surface-treated adding in
Sodium carbonate liquor and lithium sulfate solution after agent are warming up to 50~100 DEG C, so as to reach the reaction temperature in step C.
Preferably, it is 150~2000r/min to control the mixing speed under high-speed stirred state.It is 150 to control mixing speed
The fair speed of~2000r/min, can make after reaction that the lithium carbonate of strip pattern to be formed generated length under continuous collision originally
The close particle of wide ratio and make water chestnut by collide it is smooth, so as to obtain the higher spherical Lithii carbonate particle of quality.
It is further preferred that control feed time is 1.5~2.5h.The purpose of control feed time is suitable in order to control
Charging rate, the reaction time can be extended slowly by feeding, and reduce the yield of unit interval, increase production cost；Charging rate mistake
Fast then in reaction system degree of supersaturation is excessively high, easily wraps up impurity, reduces product purity, meanwhile, it is also easy to produce short grained production
Product and occur soft-agglomerated, influence the pattern of product and relevant physical property.
Step D：
Heat preservation ageing is carried out under stirring at low speed state, material separation of solid and liquid is obtained into lithium carbonate wet product and sinker mother liquor.
Preferably, it is 30~60r/min to control the mixing speed under stirring at low speed state.Control the stirring speed in this step
Spend for relatively low speed, can make to have in product the particle of lattice defect gradually it is long it is brilliant repair, obtain the more perfect product of crystal form.
It is further preferred that control heat preservation Aging Temperature is 50~100 DEG C and heat preservation digestion time is 30~120min.Instead
Should after the completion of, mixture kept the temperature into 30~120min of ageing, advantageously forms perfect crystal form, and obtain that shape is more regular and quality
More preferably spherical Lithii carbonate.
Step E：
Spherical Lithii carbonate is obtained after lithium carbonate wet product is washed and dried.
Wherein, control drying temperature is 110~220 DEG C and drying time is 2~4h.
Spherical Lithii carbonate provided by the invention is made using the preparation method of above-mentioned spherical Lithii carbonate.Specifically, originally
It is that spherical or elliposoidal etc. is subsphaeroidal to invent the purity of spherical Lithii carbonate being prepared to be more than 99.5wt% and grain shape, is put down
Equal grain size D50 is 2~10 μm.
The spherical Lithii carbonate that the present invention is prepared can substitute currently marketed micro mist battery-level lithium carbonate, and by
There is better mobility relative to micro mist lithium carbonate, therefore to improving powder reuniting, extending in the spherical Lithii carbonate of the present invention
Have the function of in terms of shelf-life it is positive, to reducing battery synthesis sintering energy consumption also with positive meaning, while may be to carrying
High battery performance has certain advantageous effect.In addition, in face of the equipment of booming microreactor, spherical Lithii carbonate is used
The generation of plugging phenomenon can be effectively reduced or eliminated, is had a good application prospect.
It should be understood that the above embodiment and following embodiment that the present invention is described in detail are merely to illustrate the present invention rather than limit
The scope of the present invention processed, some nonessential improvement and tune that those skilled in the art's the above according to the present invention is made
It is whole to all belong to the scope of protection of the present invention.
Spherical Lithii carbonate of the present invention and preparation method thereof is described further with reference to specific embodiment.
Embodiment 1：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 1500mL of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；
310g technical grade sodium carbonate is weighed to be dissolved in 1000mL hot water and be filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 3L to hold
In device and 50 DEG C are heated to, addition sodium carboxymethyl cellulose solution (advance compound concentration is 1g/L) 3mL controls mixing speed
For 2000r/min, lithium sulfate solution is slowly added dropwise in sodium carbonate liquor, control charging rate is 17mL/min.
After having fed, continue heat preservation at 50 DEG C, control mixing speed is 30r/min, stops stirring after heat preservation ageing 30min
It mixes, material is subjected to rapidly separation of solid and liquid, then gained lithium carbonate wet product is fully eluted and dry 4h obtains ball at 110 DEG C
Shape lithium carbonate product, the performance data of product are as shown in table 1 below.
The spherical Lithii carbonate properties of product data that 1 embodiment 1 of table is prepared
Embodiment 2：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 5000mL of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；
1033g technical grade sodium carbonate is weighed to be dissolved in 3440mL hot water and be filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 10L
In container and 100 DEG C, addition triethanolamine aqueous solution (advance compound concentration is 2g/L) 10mL are heated to, control mixing speed is
Lithium sulfate solution is slowly added dropwise in sodium carbonate liquor by 1000r/min, and control charging rate is 50mL/min.
After having fed, continue heat preservation at 100 DEG C, control mixing speed is 40r/min, stops stirring after heat preservation ageing 60min
It mixes, material is subjected to rapidly separation of solid and liquid, then fully elute gained lithium carbonate wet product and obtain spherical shape in 220 DEG C of dry 2h
Lithium carbonate product, the performance data of product are as shown in table 2 below.
The spherical Lithii carbonate properties of product data that 2 embodiment 2 of table is prepared
Embodiment 3：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 10L of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；It weighs
2065g technical grade sodium carbonate is dissolved in 6880mL hot water and is filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 20L containers
In and be heated to 95 DEG C, add in sodium carboxymethyl cellulose solution (advance compound concentration is 1g/L) 15mL, control mixing speed
For 500r/min, lithium sulfate solution is slowly added dropwise in sodium carbonate liquor, control charging rate is 91mL/min.
After having fed, continue heat preservation at 90 DEG C, control mixing speed is 50r/min, stops stirring after heat preservation ageing 90min
It mixes, material is subjected to rapidly separation of solid and liquid, then fully elute gained lithium carbonate wet product and obtain spherical shape in 110 DEG C of dry 4h
Lithium carbonate product, the performance data of product are as shown in table 3 below.
The spherical Lithii carbonate properties of product data that 3 embodiment 3 of table is prepared
Embodiment 4：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 100L of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；Claim
21Kg technical grade sodium carbonate is taken to be dissolved in 70L hot water and is filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 200L containers
In and be heated to 95 DEG C, add in sodium dodecyl sulfate aqueous solution (advance compound concentration is 1g/L) 200mL, control mixing speed
For 500r/min, lithium sulfate solution is slowly added dropwise in sodium carbonate liquor, control charging rate is 850mL/min.
After having fed, continue heat preservation at 90 DEG C, control mixing speed is 60 turns/min, stops stirring after heat preservation ageing 90min
It mixes, material is subjected to rapidly separation of solid and liquid, then fully elution., then gained lithium carbonate wet product is fully eluted and in 220 DEG C
Lower dry 2h obtains spherical Lithii carbonate product, and the performance data of product is as shown in table 4 below.
The spherical Lithii carbonate properties of product data that 4 embodiment 4 of table is prepared
Embodiment 5：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 1000L of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；Claim
21Kg technical grade sodium carbonate is taken to be dissolved in 70L hot water and is filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 2000L containers
In and be heated to 95 DEG C, add in triethanolamine aqueous solution (advance compound concentration is 2g/L) 2000mL, control mixing speed is
Lithium sulfate solution is slowly added dropwise in sodium carbonate liquor by 150r/min, and control charging rate is 7700mL/min.
After having fed, continue heat preservation at 90 DEG C, maintenance mixing speed is 60r/min, stops stirring after heat preservation ageing 60min
It mixes, material is subjected to rapidly separation of solid and liquid, then fully elute gained lithium carbonate wet product and obtain spherical shape in 220 DEG C of dry 2h
Lithium carbonate product, the performance data of product are as shown in table 5 below.
The spherical Lithii carbonate properties of product data that 5 embodiment 5 of table is prepared
Embodiment 6：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 1000L of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；Claim
21Kg technical grade sodium carbonate is taken to be dissolved in 70L hot water and is filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 2000L containers
In and be heated to 95 DEG C, add in sodium dodecyl sulfate aqueous solution (advance compound concentration is 1g/L) 2000mL, control stirring speed
It spends for 300r/min, lithium sulfate solution is slowly added dropwise in sodium carbonate liquor, control charging rate is 6700mL/min.
After having fed, continue heat preservation at 90 DEG C, control mixing speed is 45r/min, stops stirring after heat preservation ageing 120min
It mixes, material is subjected to rapidly separation of solid and liquid, then fully elute gained lithium carbonate wet product and obtain spherical shape in 110 DEG C of dry 4h
Lithium carbonate product, the performance data of product are as shown in table 6 below.
The spherical Lithii carbonate properties of product data that 6 embodiment 6 of table is prepared
Embodiment 7：
Concentration is pipetted with Li2O is calculated as the lithium sulfate solution 5000mL of 55g/L, controls Ca2+<0.01g/L, pH are 7~12；
1033g technical grade sodium carbonate is weighed to be dissolved in 3440L hot water and be filtered to remove insoluble matter.Sodium carbonate liquor is transferred to 10L
In container and 95 DEG C, addition sodium dodecyl sulfate aqueous solution (advance compound concentration is 1g/L) 9mL are heated to, control stirring speed
It spends for 150r/min, lithium sulfate solution is slowly added dropwise in sodium carbonate liquor, control charging rate is 50mL/min.
After having fed, continue heat preservation at 90 DEG C, control mixing speed is 50r/min, stops stirring after heat preservation ageing 120min
It mixes, material is subjected to rapidly separation of solid and liquid, then fully elute gained lithium carbonate wet product and obtain spherical shape in 110 DEG C of dry 4h
Lithium carbonate product, the performance data of product are as shown in table 7 below.
The spherical Lithii carbonate properties of product data that 7 embodiment 7 of table is prepared
Contrasting detection data：
Micro mist refers to the lithium carbonate prepared with conventional method, passes through micro mist lithium carbonate product made from air-flow crushing.Embodiment refers to
The spherical Lithii carbonate prepared in the process of the present invention.Comparing result is as shown in table 8.
The performance comparison of 8 existing micro mist lithium carbonate of table and the spherical Lithii carbonate of the present invention
By the data of table 1 to table 8 as it can be seen that micro mist lithium carbonate prepared by airbrasive technique is nearly cuboid, the method for the present invention is used
The lithium carbonate being prepared is ball-type or nearly ball-type, influences Flow of Goods and Materials in mass velocity, the degree of compression, angle of repose, voidage etc.
Property in terms of important indicator be superior to airbrasive technique preparation micro mist lithium carbonate.The size of grain size can by adjusting technological parameter and
It is controlled, material has better mobility, therefore to improving powder reuniting, the aspect that extends the shelf life with positive work
With to reducing battery synthesis sintering energy consumption with positive meaning.
In conclusion the spherical Lithii carbonate that the present invention is prepared can substitute currently marketed micro mist LITHIUM BATTERY carbonic acid
Lithium, and since the spherical Lithii carbonate of the present invention has better mobility relative to micro mist lithium carbonate, to improving powder
Reunite, the aspect that extends the shelf life have the function of it is positive, to reducing battery synthesis sintering energy consumption also with positive meaning.This
Outside, in face of the equipment of booming microreactor, the generation of plugging phenomenon can be effectively reduced or eliminated using spherical Lithii carbonate,
It has a good application prospect.
The invention is not limited in aforementioned specific embodiments.The present invention, which expands to, any in the present specification to be disclosed
The step of new feature or any new combination and any new method or process disclosed or any new combination.
Claims (9)
1. a kind of preparation method of spherical Lithii carbonate, which is characterized in that the preparation method includes the following steps：
A, sodium carbonate liquor and lithium sulfate solution are prepared；
B, surface conditioning agent is added in into sodium carbonate liquor and is stirred evenly；
C, under high-speed stirred state, lithium sulfate solution is slowly added into sodium carbonate liquor up to adding, wherein, control is anti-
It is 95~100 DEG C to answer temperature, and the mixing speed under the high-speed stirred state is 150~2000r/min；
D, heat preservation ageing is carried out under stirring at low speed state, material separation of solid and liquid is obtained into lithium carbonate wet product and sinker mother liquor, institute
It is 30~60r/min to state the mixing speed under stirring at low speed state；
E, spherical Lithii carbonate is obtained after the lithium carbonate wet product being washed and dried.
2. the preparation method of spherical Lithii carbonate according to claim 1, which is characterized in that in step, the sodium carbonate is molten
A concentration of 100~350g/L of liquid, the concentration of the lithium sulfate solution is with Li2O is calculated as 10~65g/L, sodium carbonate liquor and sulphur
The amount of sour lithium solution presses CO3 2-With Li2The molar ratio of O is 0.9~1.1 control.
3. the preparation method of spherical Lithii carbonate according to claim 1, which is characterized in that the surface conditioning agent is three ethyl alcohol
At least one of amine, lauryl sodium sulfate and sodium carboxymethylcellulose.
4. the preparation method of spherical Lithii carbonate according to claim 3, which is characterized in that wherein, the surface conditioning agent with
The mode of aqueous solution adds in and a concentration of 1~5g/L of surface conditioning agent aqueous solution, and the surface conditioning agent aqueous solution adds
Enter 1 ‰~5 ‰ that amount is overall solution volume.
5. the preparation method of spherical Lithii carbonate according to claim 1, which is characterized in that in step C, feed time is
1.5~2.5h.
6. the preparation method of spherical Lithii carbonate according to claim 1, which is characterized in that will add in before surface conditioning agent
Sodium carbonate liquor and lithium sulfate solution after sodium carbonate liquor and lithium sulfate solution or addition surface conditioning agent are warming up to 95
~100 DEG C to reach the reaction temperature in step C.
7. the preparation method of spherical Lithii carbonate according to claim 1, which is characterized in that in step D, keep the temperature Aging Temperature
It it is 50~100 DEG C, heat preservation digestion time is 30~120min.
8. the preparation method of spherical Lithii carbonate according to claim 1, which is characterized in that in step E, drying temperature is
110~220 DEG C, drying time is 2~4h.
9. a kind of spherical Lithii carbonate, which is characterized in that using the preparation of any one of claim 1 to 8 spherical Lithii carbonate
Method is made, and the purity of the spherical Lithii carbonate is more than 99.5wt% and grain shape is spherical or elliposoidal, average grain diameter D50
It is 2~10 μm.
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| CN111453748B (en) * | 2020-06-06 | 2021-01-29 | 江西南氏锂电新材料有限公司 | Lithium precipitation crystallization method for preparing snowflake monocrystal high-purity lithium carbonate |
| CN113387376B (en) * | 2021-06-28 | 2023-03-03 | 四川能投鼎盛锂业有限公司 | Process for producing battery-grade lithium carbonate by efficiently and quickly precipitating lithium |
| CN113830800A (en) * | 2021-10-09 | 2021-12-24 | 安徽大学绿色产业创新研究院 | Method for preparing lithium carbonate with uniform particle size distribution through low-temperature homogenization |
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| CN106517259A (en) | 2017-03-22 |
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