CN110217806A - A kind of salt lake richness lithium making from brine for bulky grain lithium carbonate method - Google Patents
A kind of salt lake richness lithium making from brine for bulky grain lithium carbonate method Download PDFInfo
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- CN110217806A CN110217806A CN201910607578.6A CN201910607578A CN110217806A CN 110217806 A CN110217806 A CN 110217806A CN 201910607578 A CN201910607578 A CN 201910607578A CN 110217806 A CN110217806 A CN 110217806A
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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
- C01P2004/60—Particles characterised by their size
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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 salt lake richness lithium making from brine for the method for bulky grain lithium carbonate, comprising: step 1, salt lake richness lithium brine is heated to 70~85 DEG C, the temperature is maintained after the completion of heating and surfactant is added into the salt lake richness lithium brine；Step 2, it maintains temperature in step 1 and carbonate solution is added into the pretreated salt lake richness lithium brine, react 1~3 hour, obtain reaction product slurry；Step 3, the reaction product slurry is stood 10~20 hours, is separated by solid-liquid separation later, obtained solid particle is washed, is dried to obtain bulky grain lithium carbonate.By the way that certain surfactant is added into reaction system, make lithium carbonate particle size growth in precipitation process, obtained lithium carbonate grain d (0.9): between 300-600 microns, the foreign ion of lithium carbonate product adsorption is reduced simultaneously, improve the purity and yield of primary product, purity >=95% of primary product.
Description
Technical field
The invention belongs to technical field of inorganic, and in particular to a kind of salt lake richness lithium making from brine is for bulky grain lithium carbonate
Method.
Background technique
Salt lake bittern mentions lithium process route, and can be summarized as producing rich lithium brine, purification process (deep impurity-removing), lithium carbonate heavy
It forms sediment 3 processes；Purification process is divided into the two processes i.e. separating magnesium and lithium and deep impurity-removing of high Mg/Li ratio brine, separating magnesium and lithium one
As use ionic membrane electroosmose process.(deep impurity-removing) is that salt pan richness lithium brine is carried out Li+With the separation process of impurity element,
Li will be directly affected2CO3The quality and yield of product.Lithium carbonate precipitation process is to put into alkali into rich lithium solution after purification,
Precipitate Li2CO3The process of product, the process are to determine Li2CO3The key of product.
The prior art is to obtain the solution rich in lithium ion after preliminary purification removal of impurities, thereto using salt lake bittern as raw material
Sodium carbonate liquor is added and is settled out primary lithium carbonate product, high-purity carbonic acid is further then prepared as raw material using first level lithium carbonate
Lithium product.Purity≤95% of the primary lithium carbonate product of technology preparation at present.
Purity and the yield that lithium carbonate primary product exist in the prior art are low, cause later period purification, carbonization technique stream
The problems such as journey is long, equipment requirement and excessively high energy consumption.The lithium carbonate partial size d (0.9) of prior art production: between 10-39 microns,
Since lithium carbonate particle is small, to cause yield and purity is low, the poor fluidity of lithium carbonate product, " viscous in actual production
Wall " phenomenon is serious, and equipment loss rate is high.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of salt lake richness lithium making from brine for bulky grain carbonic acid
The method of lithium, this method make lithium carbonate particle size growth in precipitation process, the lithium carbonate particle of obtained bulky grain, thus together
When reduce lithium carbonate product adsorption foreign ion, improve the purity and yield of primary production.
The present invention is achieved by the following technical solutions:
A kind of salt lake richness lithium making from brine for bulky grain lithium carbonate method, comprising the following steps:
Step 1, salt lake richness lithium brine is heated to 70~85 DEG C, the temperature and rich to the salt lake is maintained after the completion of heating
Be added surfactant in lithium brine, the additional amount of the surfactant be the salt lake richness lithium brine quality 2%~
10%, obtain pretreated salt lake richness lithium brine；
The surfactant is the aqueous solution of PP type ammonium salt, lauryl sodium sulfate and calgon, described
The mass content of PP type ammonium salt is 0.5~2% in surfactant, the mass content of lauryl sodium sulfate is 0.5~
1%, the mass content of calgon is 0.1~0.5%；
Step 2, it maintains temperature in step 1 and carbonate solution is added into the pretreated salt lake richness lithium brine,
The additional amount of the carbonate solution is the 30%~45% of the salt lake richness lithium brine quality, is reacted 1~3 hour, is obtained anti-
Product slurry is answered, the mass concentration of the carbonate solution is 25~30%；
Step 3, the reaction product slurry is stood 10~20 hours, is separated by solid-liquid separation later, the solid that will be obtained
Particle is washed, is dried to obtain bulky grain lithium carbonate.
In above-mentioned technical proposal, the molecular weight of the PP type ammonium salt is 3~100,000 dalton.
In above-mentioned technical proposal, the carbonate solution is sodium carbonate liquor or sal volatile.
In above-mentioned technical proposal, the process of the step 1 and step 2 is stirred the salt lake richness lithium brine.
In above-mentioned technical proposal, lithium ion content is 2~3wt%, potassium content 0.1 in the salt lake richness lithium brine
~0.4 wt%, magnesium ion content are 0.08~0.1wt%, and sodium ions content is 0.2~1wt%, sulfate radical content 0.02
~0.1wt%.
In above-mentioned technical proposal, the addition quality per minute of surfactant described in step 1 is the salt lake richness lithium halogen
Water quality 0.2%~0.5%.
In above-mentioned technical proposal, the addition quality per minute of sodium carbonate liquor described in step 2 is the salt lake richness lithium halogen
Water quality 0.5%~1.5%.
In above-mentioned technical proposal, washing process described in step 3 is to wash twice, and the detergent of washing is wine for the first time
Essence, the detergent of second step are deionized water.
In above-mentioned technical proposal, step 3, the reaction product slurry is stood 10~20 hours, carries out solid-liquid point later
From by the progress first time washing of obtained solid particle, the first time washing is using alcohol as detergent, the alcohol
Additional amount be the mass of solid particles 15%~30%, for the first time wash after through once be separated by solid-liquid separation after obtain once
Solid is washed, the obtained once washing solid is carried out second and is washed, second of washing is made using deionized water
For detergent, the detergent that addition quality and the first time of the deionized water wash is identical in quality, after second is washed
Secondary washing solid is obtained through secondary separation of solid and liquid, bulky grain lithium carbonate will be obtained after secondary washing solid drying.
In above-mentioned technical proposal, the partial size of the bulky grain lithium carbonate is d (0.9): 300~600 microns.
The advantages and benefits of the present invention are:
The present invention after removing impurity, as the material liquid of precipitating lithium carbonate, is added thereto for salt lake bittern
Sodium carbonate precipitates the related work that the technical process of lithium carbonate carries out.By the way that certain surface-active is added into reaction system
Agent makes lithium carbonate particle size growth in precipitation process, obtained lithium carbonate grain d (0.9): between 300-600 microns, subtracts simultaneously
The foreign ion of few lithium carbonate product adsorption, improves the purity and yield of primary product, and the purity of primary product >=
95%.
Detailed description of the invention
Fig. 1 is lithium carbonate grain size distribution prepared by comparative example 1 of the present invention.
Fig. 2 is lithium carbonate grain size distribution prepared by comparative example 2 of the present invention.
Fig. 3 is lithium carbonate grain size distribution prepared by comparative example 3 of the present invention.
Fig. 4 is lithium carbonate grain size distribution prepared by comparative example 4 of the present invention.
Fig. 5 is bulky grain lithium carbonate grain size distribution prepared by the embodiment of the present invention 1.
Fig. 6 is the bulky grain lithium carbonate SEM image of lithium carbonate prepared by comparative example 1 of the present invention and the preparation of embodiment 1, wherein
A: lithium carbonate prepared by comparative example 1；B: bulky grain lithium carbonate prepared by embodiment 1.
It for those of ordinary skill in the art, without creative efforts, can be according to above attached
Figure obtains other relevant drawings.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, combined with specific embodiments below furtherly
Bright technical solution of the present invention.
Comparative example 1
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
2.17 wt%, potassium content 0.1wt%, magnesium ion content 0.08wt%, sodium ions content 0.22wt%, sulfuric acid
Radical content is 0.09wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 77 DEG C, maintains stirring and temperature that carbon is added after the completion of heating
Acid sodium solution 73g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 0.7%, reaction
1.5 hours, reaction product slurry is obtained, the mass concentration of the sodium carbonate liquor is 28%；
Step 2, the reaction product slurry is stood 17 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
31.1g carries out first time washing, and the first time washing uses 7g deionized water as detergent, through one after washing for the first time
Once washing solid is obtained after secondary separation of solid and liquid, and the obtained once washing solid is carried out second and is washed, described second
Secondary washing, as detergent, obtains secondary washing solid through secondary separation of solid and liquid after second of washing using 7g deionized water
30.0g will obtain lithium carbonate 25g after secondary washing solid drying.
Obtained lithium carbonate is analyzed through laser particle analyzer Mastersize 2000, test condition are as follows: particle refractive index
1.567, granule absorbance 0.1, obscurity 19.64%, dispersing agent title Ethanol, dispersing agent refractive index 1.360.
The partial size of the lithium carbonate is d (0.9): 39.234 microns, lithium ion content 13.7%；Purity 72.1% is received
Rate 87.6%.
Comparative example 2
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
2.33 wt%, potassium content 0.2wt%, magnesium ion content 0.09wt%, sodium ions content 0.35wt%, sulfuric acid
Radical content is 0.09wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 80 DEG C, stirring and temperature is maintained after the completion of heating and to institute
Addition surfactant 9g in the richness lithium brine of salt lake is stated, the addition quality per minute of the surfactant is that the salt lake is rich
Lithium brine quality 0.30% obtains pretreated salt lake richness lithium brine；
The surfactant is the aqueous solution of calgon, and the quality of calgon contains in the surfactant
Amount is 0.4%；
Step 2, stirring and temperature in step 1 are maintained and sodium carbonate is added into the pretreated salt lake richness lithium brine
Solution 75g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 0.9%, are reacted 2 hours,
Reaction product slurry is obtained, the mass concentration of the sodium carbonate liquor is 26%；
Step 3, the reaction product slurry is stood 15 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
30g carries out first time washing, and the first time washing uses 9g alcohol as detergent, through primary solid-liquid after washing for the first time
Once washing solid is obtained after separation, and the obtained once washing solid is carried out second and is washed, second of washing
Using 9g deionized water as detergent, secondary washing solid 29.1g is obtained through secondary separation of solid and liquid after second of washing, it will
Lithium carbonate 22.3g is obtained after the secondary washing solid is dry.
Obtained lithium carbonate is analyzed through laser particle analyzer Mastersize 2000, test condition are as follows: particle refractive index
1.567, granule absorbance 0.1, obscurity 13.84%, dispersing agent title Ethanol, dispersing agent refractive index 1.360.
The partial size of the lithium carbonate is d (0.9): 112.54 microns, lithium ion content 16%；Purity 84.7%, yield
85.1%.
Comparative example 3
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
2.78 wt%, potassium content 0.3wt%, magnesium ion content 0.085wt%, sodium ions content 0.82wt%, sulfuric acid
Radical content is 0.06wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 81 DEG C, stirring and temperature is maintained after the completion of heating and to institute
Addition surfactant 9.02g in the richness lithium brine of salt lake is stated, the addition quality per minute of the surfactant is the salt lake
Rich lithium brine quality 0.43% obtains pretreated salt lake richness lithium brine；
The surfactant is the aqueous solution of PP type ammonium salt (molecular weight is 3~100,000 dalton), the surface
The mass content of PP type ammonium salt is 1.2% in activating agent；
Step 2, stirring and temperature in step 1 are maintained and sodium carbonate is added into the pretreated salt lake richness lithium brine
Solution 74g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 1.1%, and reaction 2.5 is small
When, reaction product slurry is obtained, the mass concentration of the sodium carbonate liquor is 27%；
Step 3, the reaction product slurry is stood 17 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
32.1g carries out first time washing, and the first time washing uses 10g alcohol as detergent, through primary after washing for the first time
Once washing solid is obtained after separation of solid and liquid, and the obtained once washing solid is carried out second and is washed, described second
Washing, as detergent, obtains secondary washing solid through secondary separation of solid and liquid after second of washing using 10g deionized water
31.1g will obtain lithium carbonate 24.1g after secondary washing solid drying.
Obtained lithium carbonate is analyzed through laser particle analyzer Mastersize 2000, test condition are as follows: particle refractive index
1.567, granule absorbance 0.1, obscurity 15.99%, dispersing agent title Ethanol, dispersing agent refractive index 1.360.
The partial size of the grain lithium carbonate is d (0.9): 329.19 microns, lithium ion content 17.1%；Purity 90.0%,
Yield 82.4%.
Comparative example 4
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
2.90 wt%, potassium content 0.40wt%, magnesium ion content 0.10wt%, sodium ions content 0.90wt%, sulfuric acid
Radical content is 0.05wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 84 DEG C, stirring and temperature is maintained after the completion of heating and to institute
Addition surfactant 8.3g in the richness lithium brine of salt lake is stated, the addition quality per minute of the surfactant is the salt lake
Rich lithium brine quality 0.47% obtains pretreated salt lake richness lithium brine；
The surfactant is the aqueous solution of lauryl sodium sulfate, lauryl sodium sulfate in the surfactant
Mass content be 0.81%；
Step 2, stirring and temperature in step 1 are maintained and sodium carbonate is added into the pretreated salt lake richness lithium brine
Solution 76g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 1.4%, and reaction 2.9 is small
When, reaction product slurry is obtained, the mass concentration of the sodium carbonate liquor is 29%；
Step 3, the reaction product slurry is stood 19 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
27.0g carries out first time washing, and the first time washs using 8g alcohol as detergent, through once solid after washing for the first time
Once washing solid is obtained after liquid separation, the obtained once washing solid is carried out second and is washed, it is described to wash for the second time
It washs using 8g deionized water as detergent, obtains secondary washing solid 25.0g through secondary separation of solid and liquid after second of washing,
Lithium carbonate 23.7g will be obtained after secondary washing solid drying.
Obtained lithium carbonate is analyzed through laser particle analyzer Mastersize 2000, test condition are as follows: particle refractive index
1.567, granule absorbance 0.1, obscurity 16.49%, dispersing agent title Ethanol, dispersing agent refractive index 1.360.
The partial size of the lithium carbonate is d (0.9): 199.9 microns, lithium ion content 17.0%；Purity 89.5%, yield
77.2%.
Embodiment one
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
2.52 wt%, potassium content 0.25wt%, magnesium ion content 0.09wt%, sodium ions content 0.74wt%, sulfuric acid
Radical content is 0.08wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 78 DEG C, stirring and temperature is maintained after the completion of heating and to institute
Addition surfactant 7.4g in the richness lithium brine of salt lake is stated, the addition quality per minute of the surfactant is the salt lake
Rich lithium brine quality 0.35% obtains pretreated salt lake richness lithium brine；
The surfactant be PP type ammonium salt (molecular weight be 3~100,000 dalton), lauryl sodium sulfate and
The aqueous solution of calgon, the mass content of PP type ammonium salt is 2% in the surfactant, dodecyl sulphate
The mass content of sodium is 0.5%, and the mass content of calgon is 0.33%；
Step 2, stirring and temperature in step 1 are maintained and sodium carbonate is added into the pretreated salt lake richness lithium brine
Solution 77g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 1%, react 2 hours, obtain
To reaction product slurry, the mass concentration of the sodium carbonate liquor is 28%；
Step 3, the reaction product slurry is stood 15 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
30.4g carries out first time washing, and the first time washs using 6g alcohol as detergent, through once solid after washing for the first time
Once washing solid is obtained after liquid separation, the obtained once washing solid is carried out second and is washed, it is described to wash for the second time
It washs using 6g deionized water as detergent, obtains secondary washing solid 30.0g through secondary separation of solid and liquid after second of washing,
Bulky grain lithium carbonate 24.0g will be obtained after secondary washing solid drying.
Obtained bulky grain lithium carbonate is analyzed through laser particle analyzer Mastersize 2000, test condition are as follows: particle refraction
Rate 1.567, granule absorbance 0.1, obscurity 14.72%, dispersing agent title Ethanol, dispersing agent refractive index 1.360.
The partial size of the bulky grain lithium carbonate is d (0.9): 524 microns, lithium ion content 18.4%；Purity 98.9%,
Yield 97.4%.
Micro complexed surfactant solution is added in crystallizing system, system liquidity, strong surface property are increased
Increase steric hindrance, be conducive to the diffusion of lithium ion and carbanion in solution, there is good spreadability, reduce carbon
" viscous wall " phenomenon of sour lithium, mobility enhancing so that lithium carbonate partial size be made to increase, while preventing the suction of impurity particle surface again
It is attached.
Comparative example 1~4, during describing crystallization of lithium carbonate, respectively with pure system, calgon is added into system
Aqueous solution, PP type ammonium salt and lauryl sodium sulfate aqueous solution test result, embodiment 1 describes to body
The test result of complexed surfactant is added in system, the result is shown in tables 1.
1 surfactant of table compares lithium carbonate grain diameter influence
The results show that being not added with, the lithium carbonate particle that surfactant is prepared is small, purity is low, in the SEM in Fig. 6 a
Reunite serious.When adding single additive into crystallizing system, lithium carbonate partial size and purity increase, but all do not have
Have and reach the set goal, the addition of NEW TYPE OF COMPOSITE addition, the partial size and purity of lithium carbonate product greatly improves, Fig. 6 b
SEM shows that lithium carbonate is evenly distributed, and appearance is regular, and particle is larger.
The present invention reduces energy consumption to salt lake richness lithium making from brine for bulky grain lithium carbonate technique, enhances mobility, increases crystallization
The service life of device improves the comprehensive utilization degree of salt lake resources.
Embodiment two
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
2.00 wt%, potassium content 0.1wt%, magnesium ion content 0.08wt%, sodium ions content 0.20wt%, sulfuric acid
Radical content is 0.02wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 70 DEG C, stirring and temperature is maintained after the completion of heating and to institute
Addition surfactant 10g in the richness lithium brine of salt lake is stated, the addition quality per minute of the surfactant is that the salt lake is rich
Lithium brine quality 0.2% obtains pretreated salt lake richness lithium brine；
The surfactant be PP type ammonium salt (molecular weight be 3~100,000 dalton), lauryl sodium sulfate and
The aqueous solution of calgon, the mass content of PP type ammonium salt is 0.5% in the surfactant, dodecyl sulphur
The mass content of sour sodium is 1%, and the mass content of calgon is 0.1%；
Step 2, stirring and temperature in step 1 are maintained and sodium carbonate is added into the pretreated salt lake richness lithium brine
Solution 80g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 0.5%, are reacted 3 hours,
Reaction product slurry is obtained, the mass concentration of the sodium carbonate liquor is 25%；
Step 3, the reaction product slurry is stood 10 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
28.5g carries out first time washing, and the first time washing uses 10g alcohol as detergent, through primary after washing for the first time
Once washing solid is obtained after separation of solid and liquid, and the obtained once washing solid is carried out second and is washed, described second
Washing, as detergent, obtains secondary washing solid through secondary separation of solid and liquid after second of washing using 10g deionized water
25.0g will obtain bulky grain lithium carbonate 19.0g after secondary washing solid drying.
The partial size of the bulky grain lithium carbonate is d (0.9): 600 microns, lithium ion content 18.7%；Purity 99.1%,
Yield 98.7%.
Embodiment three
A kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, and lithium ion content is in the salt lake richness lithium brine
3.00 wt%, potassium content 0.4wt%, magnesium ion content 0.1wt%, sodium ions content 1.00wt%, sulfate radical
Content is 0.10wt%.
The following steps are included:
Step 1, salt lake richness lithium brine 180g is heated with stirring to 85 DEG C, stirring and temperature is maintained after the completion of heating and to institute
Addition surfactant 10g in the richness lithium brine of salt lake is stated, the addition quality per minute of the surfactant is that the salt lake is rich
Lithium brine quality 0.5% obtains pretreated salt lake richness lithium brine；
The surfactant be PP type ammonium salt (molecular weight be 3~100,000 dalton), lauryl sodium sulfate and
The aqueous solution of calgon, the mass content of PP type ammonium salt is 1.21% in the surfactant, dodecyl sulphur
The mass content of sour sodium is 0.79%, and the mass content of calgon is 0.5%；
Step 2, stirring and temperature in step 1 are maintained and sodium carbonate is added into the pretreated salt lake richness lithium brine
Solution 65g, the addition quality per minute of the sodium carbonate liquor are the salt lake richness lithium brine quality 1.5%, are reacted 1 hour,
Reaction product slurry is obtained, the mass concentration of the sodium carbonate liquor is 30%；
Step 3, the reaction product slurry is stood 20 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
32.7g carries out first time washing, and the first time washs using 5g alcohol as detergent, through once solid after washing for the first time
Once washing solid is obtained after liquid separation, the obtained once washing solid is carried out second and is washed, it is described to wash for the second time
It washs using 5g deionized water as detergent, obtains secondary washing solid 31.4g through secondary separation of solid and liquid after second of washing,
Bulky grain lithium carbonate 29.2g will be obtained after secondary washing solid drying.
The partial size of the bulky grain lithium carbonate is d (0.9): 300 microns, lithium ion content 18.0%；Purity 95.7%,
Yield 96.7%.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (10)
1. a kind of salt lake richness lithium making from brine is for the method for bulky grain lithium carbonate, which comprises the following steps:
Step 1, salt lake richness lithium brine is heated to 70~85 DEG C, the temperature is maintained after the completion of heating and to the salt lake richness lithium halogen
Surfactant is added in water, the additional amount of the surfactant is the 2%~10% of the salt lake richness lithium brine quality, is obtained
To pretreated salt lake richness lithium brine；
The surfactant is the aqueous solution of PP type ammonium salt, lauryl sodium sulfate and calgon, the surface
The mass content of PP type ammonium salt is 0.5~2% in activating agent, and the mass content of lauryl sodium sulfate is 0.5~1%,
The mass content of calgon is 0.1~0.5%；
Step 2, it maintains temperature in step 1 and carbonate solution is added into the pretreated salt lake richness lithium brine, it is described
The additional amount of carbonate solution is the 30%~45% of the salt lake richness lithium brine quality, is reacted 1~3 hour, obtains reaction and produces
Object slurry, the mass concentration of the carbonate solution are 25~30%；
Step 3, the reaction product slurry is stood 10~20 hours, is separated by solid-liquid separation later, the solid particle that will be obtained
It washed, be dried to obtain bulky grain lithium carbonate.
2. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that institute
The molecular weight for stating PP type ammonium salt is 3~100,000 dalton.
3. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that institute
Stating carbonate solution is sodium carbonate liquor or sal volatile.
4. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that institute
The process for stating step 1 and step 2 is stirred the salt lake richness lithium brine.
5. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that institute
Stating lithium ion content in the richness lithium brine of salt lake is 2~3wt%, and potassium content is 0.1~0.4wt%, and magnesium ion content is
0.08~0.1wt%, sodium ions content are 0.2~1wt%, and sulfate radical content is 0.02~0.1wt%.
6. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that step
The addition quality per minute of surfactant described in rapid 1 is the salt lake richness lithium brine quality 0.2%~0.5%.
7. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that step
The addition quality per minute of sodium carbonate liquor described in rapid 2 is the salt lake richness lithium brine quality 0.5%~1.5%.
8. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that step
Washing process described in rapid 3 is to wash twice, and the detergent of washing is alcohol for the first time, and the detergent of second step is deionization
Water.
9. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that step
Rapid 3, the reaction product slurry is stood 10~20 hours, is separated by solid-liquid separation later, obtained solid particle is carried out the
Once washing, using alcohol as detergent, the additional amount of the alcohol is the mass of solid particles for the first time washing
15%~30%, obtain once washing solid after primary be separated by solid-liquid separation after washing for the first time, described once washed what is obtained
It washs solid and carries out second of washing, second of washing is using deionized water as detergent, the addition of the deionized water
Quality and the detergent that the first time washs are identical in quality, obtain secondary washing through secondary separation of solid and liquid after second of washing and consolidate
Body will obtain bulky grain lithium carbonate after secondary washing solid drying.
10. a kind of salt lake richness lithium making from brine according to claim 1 is for the method for bulky grain lithium carbonate, which is characterized in that
The partial size of the bulky grain lithium carbonate is d (0.9): 300~600 microns.
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| CN111592019A (en) * | 2020-06-25 | 2020-08-28 | 江西九岭新能源有限公司 | Precipitation formula, process and device of large-particle lithium carbonate |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4207297A (en) * | 1978-03-27 | 1980-06-10 | Foote Mineral Company | Process for producing high purity lithium carbonate |
| JPH11310413A (en) * | 1998-04-27 | 1999-11-09 | Mitsui Chem Inc | Production of highly pure lithium carbonate |
| CN101905897A (en) * | 2010-09-01 | 2010-12-08 | 张慧媛 | Method for extracting magnesium and lithium from brine |
| CN104150519A (en) * | 2014-07-28 | 2014-11-19 | 衡阳师范学院 | Method for preparing barium sulfate and sodium carbonate from waste sodium sulfate liquid |
| CN104961143A (en) * | 2015-07-03 | 2015-10-07 | 青海恒信融锂业科技有限公司 | Method for extracting lithium from salt lake brine |
| CN106277077A (en) * | 2016-08-16 | 2017-01-04 | 北京林业大学 | A kind of hollow flower-shaped nickel hydroxide microsphere composite and preparation method and application |
| CN106365181A (en) * | 2016-08-26 | 2017-02-01 | 成都开飞高能化学工业有限公司 | Method of preparing battery-grade lithium carbonate from lithium-rich solution being high in content of impurities |
| CN107739037A (en) * | 2017-11-16 | 2018-02-27 | 中国科学院青海盐湖研究所 | A kind of method that carnallite prepares big particle diameter potassium chloride |
| CN108689422A (en) * | 2018-06-05 | 2018-10-23 | 常州市卓群纳米新材料有限公司 | A kind of large-specific surface area nano gadolinium oxide raw powder's production technology |
-
2019
- 2019-07-04 CN CN201910607578.6A patent/CN110217806B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4207297A (en) * | 1978-03-27 | 1980-06-10 | Foote Mineral Company | Process for producing high purity lithium carbonate |
| JPH11310413A (en) * | 1998-04-27 | 1999-11-09 | Mitsui Chem Inc | Production of highly pure lithium carbonate |
| CN101905897A (en) * | 2010-09-01 | 2010-12-08 | 张慧媛 | Method for extracting magnesium and lithium from brine |
| CN104150519A (en) * | 2014-07-28 | 2014-11-19 | 衡阳师范学院 | Method for preparing barium sulfate and sodium carbonate from waste sodium sulfate liquid |
| CN104961143A (en) * | 2015-07-03 | 2015-10-07 | 青海恒信融锂业科技有限公司 | Method for extracting lithium from salt lake brine |
| CN106277077A (en) * | 2016-08-16 | 2017-01-04 | 北京林业大学 | A kind of hollow flower-shaped nickel hydroxide microsphere composite and preparation method and application |
| CN106365181A (en) * | 2016-08-26 | 2017-02-01 | 成都开飞高能化学工业有限公司 | Method of preparing battery-grade lithium carbonate from lithium-rich solution being high in content of impurities |
| CN107739037A (en) * | 2017-11-16 | 2018-02-27 | 中国科学院青海盐湖研究所 | A kind of method that carnallite prepares big particle diameter potassium chloride |
| CN108689422A (en) * | 2018-06-05 | 2018-10-23 | 常州市卓群纳米新材料有限公司 | A kind of large-specific surface area nano gadolinium oxide raw powder's production technology |
Non-Patent Citations (2)
| Title |
|---|
| P. TABORGA等: "Effect of additives on size and shape of lithium carbonate crystals", 《JOURNAL OF CRYSTAL GROWTH》 * |
| 王磊鑫: ""碳酸锂反应结晶过程研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592019A (en) * | 2020-06-25 | 2020-08-28 | 江西九岭新能源有限公司 | Precipitation formula, process and device of large-particle lithium carbonate |
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