CN105645443B - A method of extracting lithium salts from high-Mg Li-contained bittern - Google Patents
A method of extracting lithium salts from high-Mg Li-contained bittern Download PDFInfo
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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
- C01D15/04—Halides
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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
- C01D15/06—Sulfates; Sulfites
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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
- C01D15/10—Nitrates
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Abstract
The method that the invention discloses a kind of to extract lithium salts from high-Mg Li-contained bittern.This method comprises the following steps：Calcium phosphate+ forage system is mixed with high-Mg Li-contained bittern and alkaline solution, carries out the extraction of lithium by extraction step, obtains water phase after the extraction system for loading lithium and extraction；Exchange step is mixed with the extraction system of aforementioned load lithium using Aqueous Lithium Salts, with the impurity in the extraction system of removal load lithium, obtains water phase after the extraction system for loading high purity lithium and exchange；The extraction system of aforementioned load high purity lithium is stripped with acid solution, obtains water phase containing lithium salt, water phase obtains lithium salts after being evaporated by stripping steps.Alkaline solution can also be mixed with water phase after the extraction phase in stripping steps and the extraction in institute's extraction step, obtains regenerated extraction system and recycled.The present invention by the way that aqueous slkali is added in extraction process, solve the problems, such as in the prior art extraction process be difficult to control and extraction system regenerate it is unstable.
Description
Technical field
The invention belongs to technical field of chemical separation, and in particular to a kind of side extracting lithium salts from high-Mg Li-contained bittern
Method.
Background technology
The pollution of environment and the reduction of petroleum reserves, energy crisis have increasingly threatened the stabilization sustainable development of society,
Electric energy carrier of the lithium as a kind of high-energy density, it has also become reduce environmental pollution, the strategy metal restructured the use of energy is claimed
For " energy metal of 21st century ", industrial monosodium glutamate, strategic position is notable.Current high-purity lithium salts is in electronics new material and new energy
The application of the high-technology fields such as source constantly expands, and in lithium battery, the industries such as medicine are widely used, lithium power vehicle it is emerging
It rises so that the demand to pure lithium salts is more urgent.Saline lake lithium resource accounts for 60% or more of global lithium reserves, Lithium from Salt Lake Brine money
The utilization in source is the exploitation hot spot of countries in the world, and China's saline lake lithium resource is abundant, and the utilization of saline lake lithium resource have China
There is important strategic importance.The exploitation of high-purity lithium salts more effectively utilizes saline lake lithium resource in salt lake bittern.
Extraction is the effective ways of salt lake bittern lithium extraction at present, and extraction lifts the work of lithium from salt lake bittern at present
Skill technology related patents have：Robert D in 1963 just extract lithium using urea ketone extractant from sulphate lake
(US3306712A)；Qinghai Yanhu Inst., Chinese Academy of Sciences Huang Shi Qiang in 1987 et al. using tributyl phosphate as extraction system from
Lithium (CN1005145B) is extracted in salt lake bittern；Southern Yangtze University Lee is being all made of TBP- ion liquid abstraction systems separation salt lake halogen
Lithium (CN1017678 0A) in water；Yanhu Inst., Chinese Academy of Sciences's Lee's hamming is detached with TBP-CON-KS extraction systems in brine
Lithium ion (CN101698488A)；Organic chemistry research institute of the Chinese Academy of Sciences also has to be detached with TBP and amides extraction system
The research (CN201210164159) of lithium ion in brine.For the research of the above patent, the high lithium magnesium in China than brine in lithium
The extraction of resource, extraction are to efficiently separate method, its extraction of the extraction system of tributyl phosphate (TBP) wherein in extraction
Method is more effective, and this method substantially uses extracting-back extraction technical process, and Patent CN87103431, which is reported, to be extracted-wash
It washs-back extraction-and washes sour technique separation brine lithium resource, patent CN201210055323 increases on the basis of patent CN87103431
The technique of alkali metal chloride or alkaline-earth metal phase inversion.
But above-mentioned extraction process, control point is more complex, and extraction ability is unstable after extractant regeneration, leads to brine lithium
Rate of recovery fluctuation is larger, the rate of recovery is thereby reduced, simultaneously because the washing that is unstable and influencing the technique later stage of extraction efficiency
And back extraction, it causes product design and purity is unstable；However due to the technology controlling and process of fuzzy uncertain, entire technological process is deposited
From flow to product and the urgent problems to be solved such as the rate of recovery of lithium is unstable, during realizing scale application still
There is a large amount of need of work to carry out.
Invention content
The method that it is an object of the present invention to provide a kind of to extract lithium salts from high-Mg Li-contained bittern, solves in the prior art
Control process is complicated, and regeneration extraction ability is unstable, the unstable technical problem of handicraft product.
Used technical solution is as follows to solve above-mentioned technical problem by the present invention：
A method of extracting lithium salts from high-Mg Li-contained bittern, this method comprises the following steps：
Calcium phosphate+ forage system is mixed with high-Mg Li-contained bittern and alkaline solution, carries out lithium by extraction step
Extraction obtains water phase after the extraction system for loading lithium and extraction；
Exchange step is mixed using Aqueous Lithium Salts with the extraction system of aforementioned load lithium, with the extraction of removal load lithium
Impurity in system obtains water phase after the extraction system for loading high purity lithium and exchange；
The extraction system of aforementioned load high purity lithium is stripped with acid solution, obtains water phase containing lithium salt by stripping steps,
Water phase obtains lithium salts after being evaporated.
Further, further include after the stripping steps：
Extraction system regeneration step walks the extraction phase obtained in alkaline solution and the stripping steps and the extraction
Water phase mixes after the extraction obtained in rapid, water phase after the extraction system and regeneration after being regenerated；Extractor body after the regeneration
System can recycle for extraction step.
Preferably, the diluent is sulfonated kerosene, aviation gasoline or aromatic hydrocarbon.
Preferably, the preparation method of the calcium phosphate+ forage system is：By the mixing of tributyl phosphate and diluent
Solution is mixed with the hydrochloric acid solution of iron chloride, and organic phase and water phase are obtained after static, is detached the organic phase and is obtained institute
State calcium phosphate+ forage system.
Preferably, in the mixed solution of the tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 30%
~100%；A concentration of 0.5~4mol/L of the iron chloride in hydrochloric acid solution；The mixed solution of tributyl phosphate and diluent with
Volume ratio is 0.1~10 when the hydrochloric acid solution mixing of iron chloride, incorporation time 1-30min.
Preferably, the alkaline solution used in the extraction step and extraction system regeneration step is sodium hydroxide or hydrogen-oxygen
Change potassium solution, a concentration of 2mol/L~10mol/L.
Preferably, in the extraction step, by controlling the addition of alkaline solution, the hydrogen ion of water phase is dense after control extraction
Degree is 0.001~0.2mol/L.
Preferably, in the extraction system regeneration step, by controlling the addition of alkaline solution, water phase after control regeneration
Hydrogen ion concentration is 0.001~0.5mol/L.
Preferably, lithium concentration is 0.1-5mol/L in the Aqueous Lithium Salts in the exchange step, and the lithium salts used is chlorine
Change one or more of lithium, lithium sulfate or lithium nitrate.
Preferably, the extraction step, exchange step, stripping steps and extraction system regeneration step are using extraction tower
Or membrane contactor realizes extraction, exchanges, back extraction and extraction system regeneration.
Compared with prior art, beneficial effects of the present invention are as follows：
1, change for the process for using TBP extractants to extract high-Mg Li-contained bittern in the prior art
Into the present invention is using the amount for adding aqueous slkali in control extraction step and extraction system regeneration step, water phase after control extraction
Acidity and extraction system regeneration after water phase acidity, to realize extraction process and extraction system regenerative process stabilization and
The cycle applications of extraction system ensure that stablizing for the extraction process process of brine containing lithium carries out, and process through the invention obtains
The rate of recovery of the lithium obtained is stablized between 70-99%, and final products purity is can be controlled between 80-99.9%.
2, the present invention is the addition by controlling aqueous slkali, stablizes the water phase acid of extraction step and extractant regeneration step
Spend the cycle progress for further stablizing extraction process to stablize the operation of extraction and extraction system regeneration step, this technique side
Method solves extraction process in the prior art and is difficult to control regenerates unstable technological problems with extraction system.
3, by regarding the water phase of extraction system regeneration step and extraction step as control point, realize that regeneration extraction system is steady
It is fixed, and then extract the lithium in brine containing lithium and the product of back extraction acquisition stabilization；It does not need other rate-determining steps and work can be realized
Skill process is stablized, and relative to the extracting method of lithium in other brine containing lithium, control process is simple and effective, and the rate of recovery of lithium is stablized,
Product purity is stablized.
Specific implementation mode
If the high-Mg Li-contained bittern used in specific embodiment contains boron ion, need to carry out boron lithium separation in advance.Such as
Fruit contains other impurities, can first carry out pretreatment removal partial impurities.
Embodiment 1
The preparation of calcium phosphate+ forage system：The mixed solution of tributyl phosphate and diluent, then the salt with iron chloride
Acid solution is mixed, and static to obtain organic phase and water phase, separation organic phase is calcium phosphate+ forage system；Obtained phosphorus
Sour tributyl extraction system carries out extraction step for the first time.In the mixed solution of tributyl phosphate and diluent, tributyl phosphate
Volumetric concentration be 50%, diluent is sulfonated kerosene；In the hydrochloric acid solution of iron chloride, a concentration of 2mol/L of iron chloride, phosphorus
The volume ratio that the mixed solution of sour tributyl and diluent is mixed with the hydrochloric acid solution of iron chloride is 4, incorporation time 10min.
Extraction step：Using separatory funnel be added high-Mg Li-contained bittern (Mg/Li=15 molar ratios, it is hydrionic a concentration of
0.01) it is used as water phase；The sodium hydrate aqueous solution of calcium phosphate+ forage system and 5mol/L mixing be used as organic phase, two-phase into
Row two-stage countercurrent cascade extraction.By adjusting the addition of sodium hydrate aqueous solution, the acidity (c [H+]) of water phase after control extraction
For 0.03mol/L.
Exchange step：The lithium chloride solution of the extraction system and 3mol/L of the load lithium that extraction step obtains, compares 10:1
It carries out two-stage tandem adverse current to mix, obtains the extraction system for exchanging back loading high purity lithium.
Stripping steps：The extraction system for loading high purity lithium carries out the back extraction of 2 stage countercurrent tandems, water phase after back extraction with 7M hydrochloric acid again
As product.
Extraction system regeneration step：By stripping steps obtain extraction system, 5mol/L sodium hydrate aqueous solution and
The water phase obtained in extraction step is mixed, and organic phase and water phase is layered as after static, after separation organic phase is namely regenerated
Extraction system.By adjusting the addition of sodium hydrate aqueous solution, the aqueous phase acidity (c [H+]) controlled in the step is
0.8mol/L。
It is extracted, is exchanged, back extraction using the extraction system cycle after regeneration.Process cycles carry out 8 times, the extraction of brine lithium
Rate is taken to stablize between 80-85%, the purity of product lithium chloride is stablized between 90-94%.
Embodiment 2
The preparation of calcium phosphate+ forage system：The hydrochloric acid solution of tributyl phosphate and diluent mixed solution and iron chloride
It is mixed, static to obtain organic phase and water phase, separation organic phase is calcium phosphate+ forage system；Obtained tricresyl phosphate fourth
Ester extraction system carries out extraction step for the first time.In the mixed solution of tributyl phosphate and diluent, the volume of tributyl phosphate
A concentration of 80%, diluent is sulfonated kerosene；In the hydrochloric acid solution of iron chloride, a concentration of 2.2mol/L of iron chloride, tricresyl phosphate
Butyl ester is 4 with the volume ratio that diluent mixed solution is mixed with the hydrochloric acid solution of iron chloride, incorporation time 3min.
Extraction step：Using separatory funnel be added high-Mg Li-contained bittern (Mg/Li=15 molar ratios, it is hydrionic a concentration of
0.01) it is used as water phase；The sodium hydrate aqueous solution of calcium phosphate+ forage system and 5mol/L mixing be used as organic phase, two-phase into
Row two-stage countercurrent cascade extraction.By adjusting the addition of sodium hydrate aqueous solution, the acidity (c [H+]) of water phase after control extraction
For 0.01mol/L.
Exchange step：The lithium chloride solution of the extraction system and 4mol/L of the load lithium that extraction step obtains, compares 10:1
It carries out two-stage tandem adverse current to mix, obtains the extraction system for exchanging back loading high purity lithium.
Stripping steps：The extraction system for loading high purity lithium carries out the back extraction of 2 stage countercurrent tandems, water phase after back extraction with 7M hydrochloric acid again
As product.
Extraction system regeneration step：By stripping steps obtain extraction system, 5mol/L sodium hydrate aqueous solution and
The water phase that extraction step obtains is mixed, and organic phase and water phase, the extraction after separation organic phase is namely regenerated are layered as after static
Take system.By adjusting the addition of sodium hydrate aqueous solution, the acidity (c [H+]) of water phase is 0.1mol/L after control extraction.
Extracted, exchanged that (water phase is then recycled in exchange step using upper one and produced using the extraction system cycle after regeneration
Raw lithium chloride aqueous phase solution), back extraction.Process cycles carry out 25 times, and the extraction yield of brine lithium is stablized between 85-90%, production
The purity of product lithium chloride is stablized between 92-95%.
Embodiment 3
The preparation of extraction system：Tributyl phosphate is mixed with diluent mixed solution with the hydrochloric acid solution of iron chloride,
Static to obtain organic phase and water phase, separation organic phase is calcium phosphate+ forage system；Obtained calcium phosphate+ forage body
System carries out extraction step for the first time.In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is
50%, diluent is sulfonated kerosene；In the hydrochloric acid solution of iron chloride, a concentration of 2mol/L of iron chloride, tributyl phosphate with it is dilute
It releases agent mixed solution and is mixed with the hydrochloric acid solution of iron chloride and be comparably 4, incorporation time 10min.
Extraction step：It is carried out using mixer-settler technique, certain high-Mg Li-contained bittern (Mg/Li=12 molar ratios, hydrogen is added
0.01) a concentration of of ion is used as water phase；The sodium hydrate aqueous solution mixing conduct of calcium phosphate+ forage system and 8mol/L
Organic phase, two-phase carry out two-stage countercurrent extraction.By adjusting the addition of sodium hydrate aqueous solution, the acid of water phase after control extraction
It is 0.02mol/L to spend (c [H+]).
Exchange step：The lithium chloride solution of the extraction system and 4mol/L of the load lithium that extraction step obtains, compares 10:1
Two-stage countercurrent mixing is carried out, the extraction system for exchanging back loading high purity lithium is obtained.
Stripping steps：The extraction system for loading high purity lithium carries out 2 stage countercurrent back extraction, water phase conduct after back extraction with 7M hydrochloric acid again
Product.
Extraction system regeneration step：By stripping steps obtain extraction system, 8mol/L sodium hydrate aqueous solution and
The water phase that extraction step obtains is mixed, and organic phase and water phase, the extraction after separation organic phase is namely regenerated are layered as after static
Take system.By adjusting the addition of sodium hydroxide, aqueous phase acidity (c [H+]) is 0.1mol/L after control extraction.
Using the extraction system after regeneration according to each section of control parameter, cycle extracted, exchanges that (water phase then uses upper one
The lithium chloride aqueous phase solution that generates in cycle exchange step, volume ratio 10%), back extraction.Process cycles carry out 100 hours,
The extraction yield of brine lithium is stablized between 85-89%, and the purity of product lithium chloride is stablized between 95-97%.
Embodiment 4
The preparation of extraction system：Tributyl phosphate is mixed with diluent mixed solution with the hydrochloric acid solution of iron chloride,
Static to obtain organic phase and water phase, separation organic phase is calcium phosphate+ forage system；Obtained calcium phosphate+ forage body
System carries out extraction step for the first time.In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is
80%, diluent is sulfonated kerosene；In the hydrochloric acid solution of iron chloride, a concentration of 3mol/L of iron chloride, tributyl phosphate with it is dilute
It releases agent mixed solution and is mixed with the hydrochloric acid solution of iron chloride and be comparably 4, incorporation time 5min.
Extraction step：It is carried out using vibrating sieve plate extraction tower process, certain brine containing lithium (Mg/Li=12 molar ratios, hydrogen is added
0.01) a concentration of of ion is used as water phase；The sodium hydrate aqueous solution mixing conduct of calcium phosphate+ forage system and 8mol/L
Organic phase, two-phase carry out two-stage countercurrent extraction.By adjusting the addition of sodium hydroxide, aqueous phase acidity (c [H after control extraction
+]) it is 0.01mol/L.
Exchange step：The lithium chloride solution of the extraction system and 4mol/L of the load lithium that extraction step obtains, compares 10:1
2 stage countercurrent mixing are carried out, the extraction system for exchanging back loading high purity lithium is obtained.
Stripping steps：The extraction system for loading high purity lithium carries out 2 stage countercurrent back extraction, water phase conduct after back extraction with 7M hydrochloric acid again
Product.
Extraction system regeneration step：By stripping steps obtain extraction system, 8mol/L sodium hydrate aqueous solution and
The water phase that extraction step obtains is mixed, and organic phase and water phase, the extraction after separation organic phase is namely regenerated are layered as after static
Take system.By adjusting the addition of sodium hydroxide, the acidity (c [H+]) of water phase is 0.03mol/L after control extraction.
Using the extraction system after regeneration according to each section of control parameter, cycle extracted, exchanges that (water phase then uses upper one
The lithium chloride aqueous phase solution that generates in cycle exchange step, volume ratio 25%), back extraction.Process cycles carry out 220 hours,
The extraction yield of brine lithium is stablized between 86-89%, and the purity of product lithium chloride is stablized between 95-99%.
Embodiment 5
The preparation of extraction system：Tributyl phosphate is mixed with diluent mixed solution with the hydrochloric acid solution of iron chloride,
Static to obtain organic phase and water phase, separation organic phase is calcium phosphate+ forage system；Obtained calcium phosphate+ forage body
System carries out extraction step for the first time.In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is
80%, diluent is sulfonated kerosene；In the hydrochloric acid solution of iron chloride, a concentration of 3mol/L of iron chloride, tributyl phosphate with it is dilute
It releases agent mixed solution and is mixed with the hydrochloric acid solution of iron chloride and be comparably 4, incorporation time 2min.
Extraction step：It is carried out using vibrating sieve plate extraction tower process, (Mg/Li=10 moles of certain high-Mg Li-contained bittern is added
Than) it is used as water phase；The mixing of the sodium hydrate aqueous solution of calcium phosphate+ forage system and 8mol/L is used as organic phase, two-phase to carry out
Two-stage countercurrent extracts.By adjusting the addition of sodium hydroxide, the acidity (c [H+]) of water phase is 0.03mol/L after control extraction.
Exchange step：The lithium chloride solution of the extraction system and 4mol/L of the load lithium that extraction step obtains, compares 10:1
2 stage countercurrent mixing are carried out, the extraction system for exchanging back loading high purity lithium is obtained.
Stripping steps：The extraction system for loading high purity lithium carries out 4 stage countercurrent back extraction, water phase conduct after back extraction with 7M hydrochloric acid again
Product.
Extraction system regeneration step：By stripping steps obtain extraction system, 8mol/L sodium hydrate aqueous solution and
The water phase that extraction step obtains is mixed, and organic phase and water phase, the extraction after separation organic phase is namely regenerated are layered as after static
Take system.By adjusting the addition of sodium hydroxide, the acidity (c [H+]) of water phase is 0.03mol/L after control extraction.
Using the extraction system after regeneration according to each section of control parameter, cycle extracted, exchanges that (water phase then uses upper one
The lithium chloride aqueous phase solution that generates in cycle exchange step, volume ratio 30%), back extraction.
Process cycles carry out 200 hours, and the extraction yield of brine lithium is stablized between 88-92%, the purity of product lithium chloride
Stablize between 99-99.5%.
The part preferred embodiment of the present invention is above are only, the present invention is not limited in the content of embodiment.For ability
For technical staff in domain, can there is various change and change in the conception range of technical solution of the present invention, made by appoint
What changes and change, within the scope of the present invention.
Claims (5)
1. a kind of method for extracting lithium salts from high-Mg Li-contained bittern, this method comprises the following steps：
Calcium phosphate+ forage system is mixed with high-Mg Li-contained bittern and alkaline solution, carries out the extraction of lithium by extraction step,
Obtain load lithium extraction system and extraction after water phase；
Exchange step is mixed using Aqueous Lithium Salts with the extraction system of aforementioned load lithium, with the extraction system of removal load lithium
In impurity, obtain load high purity lithium extraction system and exchange after water phase；
The extraction system of aforementioned load high purity lithium is stripped with acid solution, obtains water phase containing lithium salt, water phase by stripping steps
Lithium salts is obtained after being evaporated；
Extraction system regeneration step, will be in the extraction phase that obtained in alkaline solution and the stripping steps and the extraction step
Water phase mixes after the extraction of acquisition, water phase after the extraction system and regeneration after being regenerated；Extraction system energy after the regeneration
Enough cycles are used for extraction step；
In the extraction step, by control alkaline solution addition, control extraction after water phase hydrogen ion concentration be 0.01~
0.03mol/L；
In the extraction system regeneration step, by controlling the addition of alkaline solution, the hydrogen ion concentration of water phase after control regeneration
For 0.03~0.8mol/L；
Lithium concentration is 0.1-5mol/L in Aqueous Lithium Salts in the exchange step, and the lithium salts used is lithium chloride, lithium sulfate
Or one or more of lithium nitrate.
2. a kind of method for extracting lithium salts from high-Mg Li-contained bittern as described in claim 1, which is characterized in that the phosphoric acid
The preparation method of tributyl extraction system is：By the hydrochloric acid solution of the mixed solution and iron chloride of tributyl phosphate and diluent into
Row mixing, obtains organic phase and water phase after static, detaches the organic phase and obtain the calcium phosphate+ forage system；It is described
Diluent is sulfonated kerosene, aviation gasoline or aromatic hydrocarbon.
3. a kind of method for extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 2, it is characterised in that：The phosphoric acid
In the mixed solution of tributyl and diluent, the volumetric concentration of tributyl phosphate is 30%~100%；Iron chloride is in hydrochloric acid solution
In a concentration of 0.5~4mol/L；The body when mixed solution of tributyl phosphate and diluent is mixed with the hydrochloric acid solution of iron chloride
Product is than being 0.1~10.
4. a kind of method for extracting lithium salts from high-Mg Li-contained bittern as described in claim 1, it is characterised in that：The extraction
The alkaline solution used in step and extraction system regeneration step is a concentration of for sodium hydroxide or the aqueous solution of potassium hydroxide
2mol/L~10mol/L.
5. a kind of method for extracting lithium salts from high-Mg Li-contained bittern as described in claim 1, it is characterised in that：The extraction
Step, exchange step, stripping steps and extraction system regeneration step realize extraction using extraction tower or membrane contactor, hand over
It changes, back extraction and extraction system regeneration.
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| CN106521159B (en) * | 2016-10-11 | 2017-12-15 | 天津科技大学 | Based on lithium in the extraction system extraction bittern containing Fe (III) and the method for recycling Fe (III) |
| CN107119196A (en) * | 2017-03-21 | 2017-09-01 | 中国科学院上海高等研究院 | The method that industrial grade methanol is prepared from bittern containing lithium |
| CN108018436A (en) * | 2017-12-04 | 2018-05-11 | 青海柴达木兴华锂盐有限公司 | Extract lithium without saponification process |
| CN107779612B (en) * | 2017-12-08 | 2019-12-13 | 中国科学院青海盐湖研究所 | Process for extracting lithium from alkaline brine |
| CN115679121B (en) * | 2021-07-26 | 2024-01-23 | 浙江新化化工股份有限公司 | Method for extracting lithium |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3793433A (en) * | 1971-07-23 | 1974-02-19 | Atomic Energy Commission | Extraction of lithium from neutral brines using a beta diketone and trioctylphosphine oxide |
| CN102001692A (en) * | 2010-12-03 | 2011-04-06 | 中国科学院青海盐湖研究所 | Coordinate extracting system for extracting lithium from salt lake brine with extraction method |
| CN102275956A (en) * | 2011-07-21 | 2011-12-14 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
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| CN104388677A (en) * | 2014-12-02 | 2015-03-04 | 中国科学院青海盐湖研究所 | Regeneration method of lithium extraction system |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3793433A (en) * | 1971-07-23 | 1974-02-19 | Atomic Energy Commission | Extraction of lithium from neutral brines using a beta diketone and trioctylphosphine oxide |
| CN102001692A (en) * | 2010-12-03 | 2011-04-06 | 中国科学院青海盐湖研究所 | Coordinate extracting system for extracting lithium from salt lake brine with extraction method |
| CN102275956A (en) * | 2011-07-21 | 2011-12-14 | 清华大学 | Method for extracting lithium carbonate from salt lake brine with high magnesium/lithium ratio |
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