CN108893623A - The method of lithium is stripped from the load organic phases extracted of brine containing lithium - Google Patents
The method of lithium is stripped from the load organic phases extracted of brine containing lithium Download PDFInfo
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- CN108893623A CN108893623A CN201810750237.XA CN201810750237A CN108893623A CN 108893623 A CN108893623 A CN 108893623A CN 201810750237 A CN201810750237 A CN 201810750237A CN 108893623 A CN108893623 A CN 108893623A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
A method of it being stripped lithium from the load organic phases extracted of brine containing lithium, strip liquor is water or Low acid solution in the method for the back extraction lithium；Stripping process uses multi-stage countercurrent mode；And stripping process includes the following steps：In the first stage, the load organic phases extracted of brine containing lithium are added, are contacted with first order strip liquor, back extraction obtains the strip liquor of load lithium；In the second level into penultimate stage, the load organic phases after back extraction carry out next stage, and the strip liquor of the load lithium after back extraction enters upper level；In afterbody, fresh strip liquor is added, the organic phase recycling utilization being stripped.The method of back extraction lithium of the invention is using water or the strip liquor of Low acid, utilize the back extraction of chlorine ion concentration control lithium and co-extraction iron ion in multistage, lithium is efficiently stripped, iron is retained in organic phase simultaneously, increased costs caused by avoiding corrosion and additional lye of the reverse-extraction of high acid equipment, simplify removal process of the lithium in strip liquor.
Description
Technical field
The invention belongs to extraction chemistries, chemical technology field, and in particular to a kind of to have from the load extracted of brine containing lithium
The method of lithium is stripped in machine phase.
Background technique
Lithium is the important source material of secondary clean energy, and the extensive use of lithium ion battery has pushed the rapid increasing of lithium demand
Long, the consumption figure of lithium was all increased with the speed for being more than 10% in recent years.The consumption figure of Chinese lithium in 2016 reaches 8.4 ten thousand tons,
2017 estimated more than 90,000 tons.China is the consumption big country of lithium, and in the past few years total lithium consumption figure accounts for about world's aggregate consumption
40%.Chinese lithium resource is abundant, and gross reserves is 3,500,000 tons, accounts for about the 20% of global reserves, is only second to Chile and occupies the second in the world.
The lithium resource in China 85% is present in salt lake, and ore resource only accounts for 15%.It is very high due to containing in the salt lake of China Qinghai Area
The ratio of the magnesium of concentration, magnesium and lithium is between 50-2000, significantly larger than Chilean, Bolivia area salt lake, the extraction cost of lithium
Height, difficulty are big, therefore a large amount of lithium ore of the annual import in China and brine containing lithium.
For lithium is extracted in high Mg/Li ratio brine, China has researched and developed multiple technologies, including precipitating calcining technology,
Membrane separation technique, adsorption technology, ion exchange technique and solvent extraction technology.Wherein solvent extraction technology treating capacity is big, behaviour
Make simply, pollution is small, to obtain extensive research and development.United States Patent (USP) US3537813 discloses a kind of solvent within 1970
Extract the method that lithium is extracted in high magnesium solution, method preferably uses 20%TBP (tributyl phosphate) and 80%DIBK (two fourths
Base ketone) it is extractant, with Fe (III) for co-extraction ion extractuin lithium, lithium and iron are stripped with water after load organic phases washing.Strip liquor
In add NaCl, extract iron with TBP and diethylhexyl phosphoric acid (D2EHPA), realize the separation of iron lithium.Process uses two extractions
Extraction circulation process is negated, operating process iron is difficult to control, and DIBK is water-soluble big, and loss is serious, and this method does not obtain quotient
Industry application.For the disadvantage for overcoming DIBK solubility big, patent CN87103431 provides one kind and extracts chlorine from brine containing lithium
Change the method for lithium, method does diluent extraction lithium using the solvent kerosene of the TBP and 30%-50% of 70%-50%, with 0.5~
Lithium is stripped using the hydrochloric acid of 6.0~9.0mol/L after the inorganic acid elution co-extraction impurity of 2.0mol/L.Lithium by back extraction to water phase and
Iron stays in the separation that organic phase realizes lithium and iron.After the hydrochloric acid in film dialysis recycling strip liquor, lithium is further purified, evaporates dense
The purity that pure lithium chloride is obtained after contracting reaches 99%, and the total recovery of lithium reaches 90.8%.Method is stripped using concentrated hydrochloric acid, if
Standby seriously corroded, and strip liquor middle and high concentration HCl recovery is difficult, and lithium purification and recovery step is complicated.
Patent CN107502741A discloses a kind of compound extracting system that lithium is extracted from brine containing lithium, is put forward for the first time
The back extraction of lithium in compound extracting system is realized using aqueous slkali, this method avoids corrosion of the peracid to equipment in strip stages,
But need to consume a large amount of aqueous slkali.
Currently, to obtain the strip liquor of pure lithium, Li-Fe coextraction load organic phases (1) use (the > 2mol/ containing high concentration
L) HCl solution is stripped；(2) it is stripped using aqueous slkali；(3) Li and Fe is stripped using water, then extracts Fe again, realize Li's and Fe
Separation.Three kinds of stripping methods are difficult to obtain high-purity lithium product, and at high cost, enforcement difficulty is big.
Summary of the invention
In view of the deficiencies of the prior art, it is organic from the load extracted of brine containing lithium that the purpose of the present invention is to provide one kind
The method that lithium is stripped in phase, at least one of to solve the above problems.
The present invention is achieved through the following technical solutions：
The present invention provide it is a kind of from the load organic phases extracted of brine containing lithium be stripped lithium method, strip liquor be water or
Low acid solution；Stripping process uses multi-stage countercurrent mode；And stripping process includes the following steps：(1) in multi-stage countercurrent device
The first order in, the load organic phases extracted of brine containing lithium, the brine containing lithium load organic phases extracted and the are added
The contact of level-one strip liquor, obtains the strip liquor of load lithium after back extraction, the load organic phases after back extraction enter the second level；(2) more
The second level of stage countercurrent device is into penultimate stage, and the load organic phases after upper level back extraction are contacted with this grade of strip liquor, instead
Load organic phases after extraction enter next stage, and the strip liquor of the load lithium after back extraction enters upper level；(3) in multi-stage countercurrent device
Afterbody in, be added fresh strip liquor, the load organic phases after upper level back extraction are contacted with the new strip liquor, instead
It obtains regeneration organic phase after extraction to recycle, load water phase enters upper level.
Preferably, the Low acid solution includes the solution of LiCl, NaCl or KCl；H in the Low acid solution+It is dense
Spend < 1mol/L.
Preferably, in step (1), in the organic phase of the load lithium containing extractant TBP, co-extraction ion Fe, Cl and
Li。
Preferably, in step (1), the ratio of the organic phase and water phase is 10: 1~100: 1, preferably 30: 1~50: 1.
Preferably, in step (1), Cl in the first order strip liquor-Concentration be 1~6mol/L, preferably 2~
4mol/L。
Preferably, Li concentration is 5~30g/L, free acid concentration < in the strip liquor for the load lithium that every level-one obtains
0.5mol/L。
Preferably, in step (2), in the second level of multi-stage countercurrent device into penultimate stage, Cl in strip liquor-It is dense
Degree is 0.5~5mol/L, preferably 2~3mol/L.
Preferably, the back extraction series of the stripping process is preferably 2~5 grades.
It can be seen from the above technical proposal that of the invention be stripped lithium from the load organic phases extracted of brine containing lithium
Method has the advantages that：
The organic phase for extracting back loading lithium is stripped using water and Low acid solution, avoids corrosion of the reverse-extraction of high acid to equipment
With increased costs caused by additional lye, the removal process that removal process of the lithium in strip liquor simplifies lithium is simplified, substantially
Degree reduces process costs.
Detailed description of the invention
Fig. 1 is the flow chart of multi-stage countercurrent stripping process in the embodiment of the present invention.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this hair
It is bright to be described in further detail.
A method of it being stripped lithium from the load organic phases extracted of brine containing lithium, is stripped in the method for the back extraction lithium
Liquid is water or Low acid solution；Stripping process uses multi-stage countercurrent mode；And stripping process includes the following steps：In the first order
In, the load organic phases extracted of brine containing lithium are added, are contacted with first order strip liquor, back extraction obtains the strip liquor of load lithium；
In the second level into penultimate stage, load organic phases after back extraction carry out next stage, the strip liquor of the load lithium after back extraction into
Enter upper level；In afterbody, fresh strip liquor is added, the organic phase recycling utilization being stripped.Of the invention
The method of lithium is stripped using the strip liquor of water or Low acid, utilizes the anti-of chlorine ion concentration control lithium in multistage and co-extraction iron ion
Extraction, lithium is efficiently stripped, while iron is retained in organic phase, caused by avoiding corrosion and additional lye of the reverse-extraction of high acid equipment
Increased costs simplify removal process of the lithium in strip liquor.
Specifically, the present invention provides a kind of method that lithium is stripped from the load organic phases extracted of brine containing lithium, back extraction
Liquid is water or Low acid solution；Stripping process uses multi-stage countercurrent mode.Fig. 1 is that multi-stage countercurrent was stripped in the embodiment of the present invention
The flow chart of journey.As shown in Figure 1, stripping process includes the following steps：(1) in the first order of multi-stage countercurrent device, addition contains
Lithium brine load organic phases extracted, the brine containing lithium load organic phases extracted are contacted with first order strip liquor, instead
The strip liquor of load lithium is obtained after extraction, the load organic phases after back extraction enter the second level；(2) in the second level of multi-stage countercurrent device
Into penultimate stage, upper level back extraction after load organic phases contacted with this grade of strip liquor, the load organic phases after back extraction into
Enter next stage, the strip liquor of the load lithium after back extraction enters upper level；(3) it in the afterbody of multi-stage countercurrent device, is added
Fresh strip liquor, the load organic phases after upper level back extraction contact with the new strip liquor, obtain regenerating after back extraction organic
It mutually recycles, load water phase enters upper level.
Preferably, the Low acid solution includes the solution of LiCl, NaCl or KCl；H in the Low acid solution+It is dense
Spend < 1mol/L.
Preferably, in step (1), in the organic phase of the load lithium containing extractant TBP, co-extraction ion Fe, Cl and
Li。
Preferably, in step (1), the ratio of the organic phase and water phase is 10: 1~100: 1, preferably 30: 1~50: 1.
Preferably, in step (1), Cl in the first order strip liquor-Concentration be 1~6mol/L, preferably 2~
4mol/L。
Preferably, Li concentration is 5~30g/L, free acid concentration < in the strip liquor for the load lithium that every level-one obtains
0.5mol/L。
Preferably, in step (2), in the second level of multi-stage countercurrent device into penultimate stage, Cl in strip liquor-It is dense
Degree is 0.5~5mol/L, preferably 2~3mol/L.
Preferably, the back extraction series of the stripping process is preferably 2~5 grades.
Below in conjunction with specific embodiment, lithium is stripped from the load organic phases extracted of brine containing lithium to provided by the invention
Method be described in further detail.
Embodiment 1
Extractant is done using 40%TBP+20%P507, kerosene makees diluent, and the concentration that Li is loaded in extraction system is
The concentration of 0.3g/L, Fe are 5.2g/L.Using water as stripping agent, O/A=50: 1 is being compared, two-stage countercurrent back extraction；In the second level plus
Enter stripping agent, first order Cl-Concentration is 2.1mol/L, second level Cl-Concentration is 1.8mol/L；The back extraction ratio of lithium is 99%, water phase
The concentration of middle lithium is 14.8g/L, and the back extraction ratio of iron is ignored.The lithium carbonate of purity 98% is obtained after sodium carbonate precipitating.
Embodiment 2
Extractant is done using 40%TBP+20%P204, kerosene makees diluent, and the concentration that Li is loaded in extraction system is
The concentration of 0.35g/L, Fe are 5.2g/L.Using water as stripping agent, O/A=100: 1 is being compared, Pyatyi countercurrent reextraction；In level V
Stripping agent, first order Cl is added-Concentration is 4.6mol/L, the second level to level V Cl-Concentration is 3.8~0.5mol/L；Lithium it is anti-
Extraction rate is 93%, and the concentration of lithium is 32.6g/L in water phase, and the back extraction ratio of iron is ignored.Purity is obtained after sodium carbonate precipitating
98.5% lithium carbonate.
Embodiment 3
Extractant is done using 40%TBP+20%N503, kerosene makees diluent, and the concentration that Li is loaded in extraction system is
The concentration of 0.28g/L, Fe are 4.7g/L.Using 1mol/L LiCl+0.4mol/L HCl as stripping agent, O/A=20: 1 is being compared,
Three-level countercurrent reextraction；Stripping agent, first order Cl is added in the third level-Concentration is 1.9mol/L, the second level to third level Cl-Concentration
For 1.8~1.2mol/L；The back extraction ratio of lithium is 85%, and the concentration of lithium is 11.8g/L in water phase, and the back extraction ratio of iron is ignored.
The lithium carbonate of purity 99% is obtained after sodium carbonate precipitating.
Embodiment 4
Extractant is done using 40%TBP+30%DIBK, kerosene makees diluent, and the concentration that Li is loaded in extraction system is
The concentration of 0.4g/L, Fe are 5.4g/L.Using 3.5mol/LNaCl as stripping agent, O/A=40: 1 is being compared, Pyatyi countercurrent reextraction；
Stripping agent, first order Cl is added in level V-Concentration is 5.6mol/L, the second level to level V Cl-Concentration is 5.2~4.2mol/
L；The back extraction ratio of lithium is 92%, and the concentration of lithium is 14.7g/L in water phase, and the back extraction ratio of iron is ignored.After sodium carbonate precipitating
To the lithium carbonate of purity 98%.
In conclusion the method for the invention for being stripped lithium from the load organic phases extracted of brine containing lithium avoids peracid
Increased costs caused by being stripped corrosion and the additional lye equipment, simplify removal process of the lithium in strip liquor, meanwhile,
It is easy to improve the concentration of lithium in strip liquor, Direct precipitation obtains lithium carbonate product, simplifies the recycling of lithium.After the water-soluble liquid precipitate lithium of lithium
Mother liquor can be returned directly to the stripping section of lithium, entire extraction process does not discharge waste liquid, realizes clean manufacturing.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (8)
1. it is a kind of from the load organic phases extracted of brine containing lithium be stripped lithium method, which is characterized in that strip liquor be water or
Low acid solution；Stripping process uses multi-stage countercurrent mode；And stripping process includes the following steps：
(1) in the first order of multi-stage countercurrent device, the load organic phases extracted of brine containing lithium, the extraction of brine containing lithium is added
Load organic phases after taking are contacted with first order strip liquor, and the strip liquor of load lithium is obtained after back extraction, and the load after back extraction is organic
Mutually enter the second level；
(2) in the second level of multi-stage countercurrent device into penultimate stage, the load organic phases and the grade after upper level back extraction are anti-
Extract liquid contact, the load organic phases after back extraction enter next stage, and the strip liquor of the load lithium after back extraction enters upper level；
(3) in the afterbody of multi-stage countercurrent device, be added fresh strip liquor, the load organic phases after upper level back extraction with
The new strip liquor contact, obtains regeneration organic phase and recycles, load water phase enters upper level after back extraction.
2. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
The Low acid solution includes the solution of LiCl, NaCl or KCl；H in the Low acid solution+Concentration < 1mol/L.
3. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
In step (1), contain extractant TBP, co-extraction ion Fe, Cl and Li in the organic phase of the load lithium.
4. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
In step (1), the ratio of the organic phase and water phase is 10: 1~100: 1, preferably 30: 1~50: 1.
5. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
In step (1), the concentration of C1- is 1~6mol/L, preferably 2~4mol/L in the first order strip liquor.
6. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
Li concentration is 5~30g/L, free acid concentration < 0.5mol/L in the strip liquor for the load lithium that every level-one obtains.
7. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
In step (2), in the second level of multi-stage countercurrent device into penultimate stage, in strip liquor the concentration of Gl- be 0.5~
5mol/L, preferably 2~3mol/L.
8. the method according to claim 1 for being stripped lithium from the load organic phases extracted of brine containing lithium, feature exist
In,
The back extraction series of the stripping process is preferably 2~5 grades.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558799A (en) * | 2021-07-02 | 2023-01-03 | 浙江新化化工股份有限公司 | Method for extracting lithium |
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| CN115558799B (en) * | 2021-07-02 | 2023-12-01 | 浙江新化化工股份有限公司 | Method for extracting lithium |
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