CN110182831A - The technology of salt lake extraction lithium carbonate - Google Patents
The technology of salt lake extraction lithium carbonate Download PDFInfo
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- CN110182831A CN110182831A CN201910453127.1A CN201910453127A CN110182831A CN 110182831 A CN110182831 A CN 110182831A CN 201910453127 A CN201910453127 A CN 201910453127A CN 110182831 A CN110182831 A CN 110182831A
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- filtered fluid
- lithium carbonate
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- salt lake
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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
Abstract
The embodiment of the invention discloses the technologies that lithium carbonate is extracted in salt lake, comprising the following steps: brine launches flocculant, is centrifuged after standing, retains supernatant；Supernatant is subjected to sunning evaporation and concentration, collection obtains filtered fluid one；Filtered fluid one is imported into heating container, and is vacuumized, crosses and filters out sediment, obtain filtered fluid two；Filtered fluid two is imported into cooling vessel, and is vacuumized, crosses and filters out sediment, obtain filtered fluid three；Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, filtering removal sediment obtains filtered fluid four；Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, after hot water washing, calcination, obtains pure Lithium Carbonate.In the invention application, the chemical reagent that processing step uses is only flocculant, carbon dioxide, ammonium hydroxide, reduces reagent to influence caused by lithium carbonate purification, ensure that the degree of purity of lithium carbonate.
Description
Technical field
The present embodiments relate to technical field of chemical purification, and in particular to the technology of salt lake extraction lithium carbonate.
Background technique
Production lithium salts raw material is divided into two class of solid mineral and liquid mine in the world at present, and mineral mention lithium due to high energy consumption and pollution
The reasons such as big, have gradually reduced, and extract lithium salts since pollution is lower using salt lake bittern as raw material, and share increases year by year.
The method for extracting lithium salts from salt lake bittern mainly has the precipitation method, extraction, electrolysis method, ion-exchange etc..It is heavy
Shallow lake method alkali consumption is big, the lithium rate of recovery is low, is not suitable for brine and low lithium brine of the processing containing a large amount of alkaline-earth metal.Lithium is mentioned from brine
Studying more method is solvent extraction, and this method lithium extraction yield is high, but the use of a large amount of ordinary organic solvents, can be made
Equipment seriously corroded, and serious environmental pollution can be brought.It is straight that ionic adsorption method is suitable for the low salt lake bittern of ion concentration
It connects and mentions lithium, but since processing brine amount is big, water consume, resin consumption, power consumption are increased accordingly, especially in freshwater resources ratio
Poorer area is somewhat limited, while being led to resin poison in process of production and broken also being needed to solve
Certainly.
The above method is in the prevalence of technical process poor operability, long flow path, and product cost is higher, it is difficult to produce height
The problem of lithium carbonate of purity.Therefore, the technical problem for solving continuously to extract pure Lithium Carbonate from salt lake bittern seems to pass
It is important.
Summary of the invention
For this purpose, the embodiment of the present invention provides the technology that lithium carbonate is extracted in salt lake, to solve high-purity carbon in the prior art
Sour lithium production stage is cumbersome, and poor operability is at high cost, and is easy the problem of being polluted by organic reagent.
To achieve the goals above, the embodiment of the present invention provides the following technical solutions:
According to a first aspect of the embodiments of the present invention, the technology of lithium carbonate is extracted in salt lake, comprising the following steps:
Salt lake bittern is weighed, flocculant is launched into brine, is centrifuged after standing, retains supernatant；
Supernatant is subjected to sunning evaporation, concentration ratio 50%, filtration from sodium chloride solid is collected and obtains filtered fluid
One；
Filtered fluid one is imported into heating container, and is vacuumized, heating is rapidly heated to 75-85 DEG C, and constant temperature maintains 10-
15 minutes, it is then filtered to remove the sediment of iron and aluminium, obtains filtered fluid two；
Filtered fluid two is imported into cooling vessel, and is vacuumized, by water cooling fast cooling to 10-15 DEG C, constant temperature is tieed up
It holds 15-30 minutes, then filters off the sediment of deliming, zinc and lead, obtain filtered fluid three；
Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, when measurement pH value reaches 12, is stopped
It is only added dropwise, and continues stirring 20 minutes, then filter off the sediment of demagging and calcium, obtain filtered fluid four；
Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, warp
After hot water washing, calcination, pure Lithium Carbonate is obtained.
Further, the flocculant launched into brine is aluminium chloride.
Further, after putting into flocculant, time of repose is 1-1.5 hours, and centrifugal rotational speed is 250-300 revs/min, from
The heart time is 15-20 minutes.
Further, the strong base solution being added dropwise into filtered fluid three is the ammonium hydroxide that concentration is 25%.
Further, the heating temperature of filtered fluid one in the heating container is 85 DEG C, and holding time is 10 minutes.
Further, cooling temperature of the filtered fluid two in cooling vessel is 15 DEG C, and holding time is 15 minutes.
The embodiment of the present invention has the advantages that
By physical step, and it is aided with the process of cooling and heating, accelerates the precipitation of silt, calcium, zinc, magnesium etc. in brine heavy
Shallow lake process also improves the purification purity of lithium carbonate, purity is 99.95% or more to improve lithium carbonate purification efficiency；This
In patent application, the chemical reagent that processing step uses is only flocculant, carbon dioxide, ammonium hydroxide, reduces reagent to lithium carbonate
It is influenced caused by purification, ensure that the degree of purity of lithium carbonate.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily, it is clear that described embodiment is the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
According to a first aspect of the embodiments of the present invention, the technology of lithium carbonate is extracted in salt lake, comprising the following steps:
Salt lake bittern is weighed, flocculant is launched into brine, is centrifuged after standing, retains supernatant；This step is mainly wadded a quilt with cotton
Silt, boron radical ion, iron etc. in solidifying salt lake bittern, accelerate precipitation process by flocculation, establish base for the purification of lithium ion
Plinth.In this embodiment, the flocculant launched into brine is aluminium chloride.After putting into flocculant, time of repose is 1-1.5 hours,
Centrifugal rotational speed is 250-300 revs/min, and centrifugation time is 15-20 minutes.
Supernatant is subjected to sunning evaporation, concentration ratio 50%, sodium chloride is precipitated, and filtration from sodium chloride solid is received
Collection obtains filtered fluid one；
Filtered fluid one is imported into heating container, and is vacuumized, heating is rapidly heated to 75-85 DEG C, and constant temperature maintains 10-
15 minutes, it is then filtered to remove the sediment of iron and aluminium, obtains filtered fluid two.
Filtered fluid two is imported into cooling vessel, and is vacuumized, by water cooling fast cooling to 10-15 DEG C, constant temperature is tieed up
It holds 15-30 minutes, then filters off the sediment of deliming, zinc and lead, obtain filtered fluid three.
Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, when measurement pH value reaches 12, is stopped
It is only added dropwise, and continues stirring 20 minutes, then filter off the sediment of demagging and calcium, obtain filtered fluid four；Into filtered fluid three
The strong base solution of dropwise addition is the ammonium hydroxide that concentration is 25%.
Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, warp
After hot water washing, calcination, pure Lithium Carbonate is obtained.
Further, the heating temperature of filtered fluid one in the heating container is 85 DEG C, and holding time is 10 minutes.
Further, cooling temperature of the filtered fluid two in cooling vessel is 15 DEG C, and holding time is 15 minutes.
Embodiment 1
According to a first aspect of the embodiments of the present invention, the technology of lithium carbonate is extracted in salt lake, specifically extracts Qinghai
Lithium ion in Cha Er Han Salt Lake, for manufacturing lithium carbonate, comprising the following steps:
Salt lake bittern is weighed, flocculant is launched into brine, flocculant and brine ratio are 1:10, are centrifuged, stay after standing
Deposit supernatant；This step is mainly silt, boron radical ion, iron etc. in flocculation salt lake bittern, is accelerated and was precipitated by flocculation
Journey lays the foundation for the purification of lithium ion.In this embodiment, the flocculant launched into brine is aluminium chloride.Put into flocculant
Afterwards, time of repose is 1.5 hours, and centrifugal rotational speed is 250 revs/min, and centrifugation time is 20 minutes.
Supernatant is subjected to sunning evaporation, concentration ratio 50%, sodium chloride is precipitated, and filtration from sodium chloride solid is received
Collection obtains filtered fluid one；
Filtered fluid one is imported into heating container, and is vacuumized, heating is rapidly heated to 85 DEG C, and constant temperature maintains 10 points
Then clock is filtered to remove the sediment of iron and aluminium, obtain filtered fluid two.
Filtered fluid two is imported into cooling vessel, and is vacuumized, by water cooling fast cooling to 15 DEG C, constant temperature maintains 15
Minute, the sediment of deliming, zinc and lead is then filtered off, filtered fluid three is obtained.
Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, when measurement pH value reaches 12, is stopped
It is only added dropwise, and continues stirring 20 minutes, then filter off the sediment of demagging and calcium, obtain filtered fluid four；Into filtered fluid three
The strong base solution of dropwise addition is the ammonium hydroxide that concentration is 25%.
Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, warp
After hot water washing, calcination, pure Lithium Carbonate is obtained.
By producing and purifying, the purity of lithium carbonate reaches 99.954%.
Embodiment 2
According to a first aspect of the embodiments of the present invention, the technology of lithium carbonate is extracted in salt lake, specifically extracts Qinghai
Lithium ion in Cha Er Han Salt Lake, for manufacturing lithium carbonate, comprising the following steps:
Salt lake bittern is weighed, flocculant is launched into brine, is centrifuged after standing, retains supernatant；This step is mainly wadded a quilt with cotton
Silt, boron radical ion, iron etc. in solidifying salt lake bittern, accelerate precipitation process by flocculation, establish base for the purification of lithium ion
Plinth.In this embodiment, the flocculant launched into brine is aluminium chloride.After putting into flocculant, time of repose is 1 hour, centrifugation
Revolving speed is 300 revs/min, and centrifugation time is 20 minutes.
Supernatant is subjected to sunning evaporation, concentration ratio 50%, sodium chloride is precipitated, and filtration from sodium chloride solid is received
Collection obtains filtered fluid one；
Filtered fluid one is imported into heating container, and is vacuumized, heating is rapidly heated to 75 DEG C, and constant temperature maintains 15 points
Then clock is filtered to remove the sediment of iron and aluminium, obtain filtered fluid two.
Filtered fluid two is imported into cooling vessel, and is vacuumized, by water cooling fast cooling to 15 DEG C, constant temperature maintains 15
Minute, the sediment of deliming, zinc and lead is then filtered off, filtered fluid three is obtained.
Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, when measurement pH value reaches 12, is stopped
It is only added dropwise, and continues stirring 20 minutes, then filter off the sediment of demagging and calcium, obtain filtered fluid four；Into filtered fluid three
The strong base solution of dropwise addition is the ammonium hydroxide that concentration is 25%.
Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, warp
After hot water washing, calcination, pure Lithium Carbonate is obtained.
By producing and purifying, the purity of lithium carbonate reaches 99.95%.
Embodiment 3
According to a first aspect of the embodiments of the present invention, the technology of lithium carbonate is extracted in salt lake, specifically extracts Qinghai
Lithium ion in Cha Er Han Salt Lake, for manufacturing lithium carbonate, comprising the following steps:
Salt lake bittern is weighed, flocculant is launched into brine, is centrifuged after standing, retains supernatant；This step is mainly wadded a quilt with cotton
Silt, boron radical ion, iron etc. in solidifying salt lake bittern, accelerate precipitation process by flocculation, establish base for the purification of lithium ion
Plinth.In this embodiment, the flocculant launched into brine is aluminium chloride.After putting into flocculant, time of repose is 1.5 hours, from
Heart revolving speed is 300 revs/min, and centrifugation time is 15 minutes.
Supernatant is subjected to sunning evaporation, concentration ratio 50%, sodium chloride is precipitated, and filtration from sodium chloride solid is received
Collection obtains filtered fluid one；
Filtered fluid one is imported into heating container, and is vacuumized, heating is rapidly heated to 75 DEG C, and constant temperature maintains 10 points
Then clock is filtered to remove the sediment of iron and aluminium, obtain filtered fluid two.
Filtered fluid two is imported into cooling vessel, and is vacuumized, by water cooling fast cooling to 10 DEG C, constant temperature maintains 30
Minute, the sediment of deliming, zinc and lead is then filtered off, filtered fluid three is obtained.
Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, when measurement pH value reaches 12, is stopped
It is only added dropwise, and continues stirring 20 minutes, then filter off the sediment of demagging and calcium, obtain filtered fluid four；Into filtered fluid three
The strong base solution of dropwise addition is the ammonium hydroxide that concentration is 25%.
Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, warp
After hot water washing, calcination, pure Lithium Carbonate is obtained.
By producing and purifying, the purity of lithium carbonate reaches 99.96%.
The embodiment of the present invention has the advantages that
By physical step, and it is aided with the process of cooling and heating, accelerates the precipitation of silt, calcium, zinc, magnesium etc. in brine heavy
Shallow lake process also improves the purification purity of lithium carbonate, purity is 99.98% or more to improve lithium carbonate purification efficiency；This
In patent application, the chemical reagent that processing step uses is only flocculant, carbon dioxide, ammonium hydroxide, reduces reagent to lithium carbonate
It is influenced caused by purification, ensure that the degree of purity of lithium carbonate.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (6)
1. the technology of salt lake extraction lithium carbonate, which comprises the following steps:
Salt lake bittern is weighed, flocculant is launched into brine, is centrifuged after standing, retains supernatant；
Supernatant is subjected to sunning evaporation, concentration ratio 50%, filtration from sodium chloride solid is collected and obtains filtered fluid one；
Filtered fluid one is imported into heating container, and is vacuumized, heating is rapidly heated to 75-85 DEG C, and constant temperature maintains 10-15 points
Then clock is filtered to remove the sediment of iron and aluminium, obtain filtered fluid two；
Filtered fluid two is imported into cooling vessel, and is vacuumized, by water cooling fast cooling to 10-15 DEG C, constant temperature maintains 15-
30 minutes, the sediment of deliming, zinc and lead is then filtered off, obtains filtered fluid three；
Filtered fluid three is imported into and is adjusted in container, and strong base solution is added dropwise while stirring, when measurement pH value reaches 12, stops drop
Add, and continue stirring 20 minutes, then filters off the sediment of demagging and calcium, obtain filtered fluid four；
Filtered fluid four is imported into crystallisation vessel, and is passed through the carbon dioxide of saturation, reaction obtains precipitating lithium carbonate, through hot water
After washing, calcination, pure Lithium Carbonate is obtained.
2. the technology that lithium carbonate is extracted in salt lake as described in claim 1, which is characterized in that the flocculation launched into brine
Agent is aluminium chloride.
3. the technology that lithium carbonate is extracted in salt lake as claimed in claim 2, which is characterized in that after investment flocculant, stand
Time is 1-1.5 hours, and centrifugal rotational speed is 250-300 revs/min, and centrifugation time is 15-20 minutes.
4. the technology that lithium carbonate is extracted in salt lake as described in claim 1, which is characterized in that be added dropwise into filtered fluid three
Strong base solution is the ammonium hydroxide that concentration is 25%.
5. the technology that lithium carbonate is extracted in salt lake as described in claim 1, which is characterized in that filtered fluid one is in heating container
In heating temperature be 85 DEG C, holding time is 10 minutes.
6. the technology that lithium carbonate is extracted in salt lake as described in claim 1, which is characterized in that filtered fluid two is in cooling vessel
In cooling temperature be 15 DEG C, holding time is 15 minutes.
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| CN201910453127.1A CN110182831A (en) | 2019-05-28 | 2019-05-28 | The technology of salt lake extraction lithium carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112299454A (en) * | 2020-11-12 | 2021-02-02 | 萍乡市拓源实业有限公司 | Method for improving direct yield of battery-grade lithium carbonate prepared from brine |
| RU2795224C1 (en) * | 2019-12-11 | 2023-05-02 | Дзе Юниверсити Оф Бритиш Коламбиа | Process and method for lithium carbonate purification based on a lithium chloride solution with impurities |
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Application publication date: 20190830 |