CN105645443A - Method for lithium salts from high-magnesium lithium-containing brine - Google Patents
Method for lithium salts from high-magnesium lithium-containing brine 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for lithium salts from high-magnesium lithium-containing brine. The method comprises the following steps: extraction: mixing a tributyl phosphate extraction system with high-magnesium lithium-containing brine and an alkaline solution, and carrying out lithium extraction to obtain a lithium-carried extraction system and an extracted water phase; exchange: mixing a lithium salt water solution with the lithium-carried extraction system to remove impurities in the lithium-carried extraction system, thereby obtaining a high-purity-lithium-carried extraction system and an exchanged water phase: and back extraction: carrying out back extraction on the high-purity-lithium-carried extraction system with an acid solution to obtain a lithium-salt-containing water phase, and drying the water phase by distillation to obtain the lithium salts. The alkaline solution can be mixed with the extraction phase in the back extraction step and the extracted water phase in the extraction step, and the obtained regenerated extraction system can be recycled. The alkali solution is added in the extraction technique, thereby solving the problem of uncontrollable extraction process and unstable regeneration of the extraction system in the prior art.
Description
Technical field
The invention belongs to technical field of chemical separation, be specifically related to a kind of method extracting lithium salts from high-Mg Li-contained bittern.
Background technology
The pollution of environment and the minimizing of petroleum reserves; energy crisis threatens the stable sustainable development of society day by day; lithium is as the electric energy carrier of a kind of high-energy-density; become minimizing environmental pollution; the strategy metal restructured the use of energy; being referred to as " energy metal of 21st century ", industry monosodium glutamate, strategic position is notable. Current high-purity lithium salts constantly expands in the application of the high-technology fields such as electronics new material and new forms of energy, and at lithium battery, the industry such as medicine is widely used, the rise of lithium power vehicle so that the demand of pure lithium salts is more urgent. Saline lake lithium resource accounts for more than the 60% of whole world lithium reserves, and the utilization of Lithium from Salt Lake Brine resource is the exploitation focus of countries in the world, and China's saline lake lithium resource enriches, and China is had important strategic importance by the exploitation of saline lake lithium resource. In salt lake bittern, the exploitation of high-purity lithium salts is more effective utilizes saline lake lithium resource.
Current extraction is the effective ways that salt lake bittern lithium extracts, and current extraction mentions the Technology Patents of lithium from salt lake bittern to be had: within 1963, RobertD just adopts carbamide ketone extractant to extract lithium (US3306712A) from sulphate lake; Qinghai Yanhu Inst., Chinese Academy of Sciences Huang Shi Qiang in 1987 et al. extracts lithium (CN1005145B) with tributyl phosphate for extraction system from salt lake bittern; Southern Yangtze University Lee is all adopting TBP-ion liquid abstraction system separation Lithium from Salt Lake Brine (CN10176780A); Yanhu Inst., Chinese Academy of Sciences's Lee's hamming is with the lithium ion (CN101698488A) in TBP-CON-KS extraction system separation salt; Chinese Academy of Sciences's organic chemistry institute also has the research (CN201210164159) separating lithium ion in salt with TBP with amide-type extraction system.Research for above patent, the extraction of lithium resource in the salt of China's height lithium magnesium ratio, extraction is to efficiently separate method, wherein in extraction, its extracting process of extraction system of tributyl phosphate (TBP) is comparatively effective, the method substantially adopts extracting-back extraction technical process, its Patent CN87103431 reports extraction-washing-back extraction-wash acid technique separation salt lithium resource, and patent CN201210055323 adds alkali metal chloride or the technique of alkaline-earth metal phase inversion on the basis of patent CN87103431.
But above-mentioned extraction process, control point is more complicated, after extractant regeneration, extraction ability is unstable, cause that the response rate fluctuation of salt lithium is bigger, and then reduce the response rate, simultaneously because the instability of extraction efficiency and affect washing and the back extraction in technique later stage, cause product design and purity be unstable; Yet with the technology controlling and process of fuzzy uncertain, whole technological process exists from flow to product and the problem demanding prompt solution such as the response rate of lithium is unstable, still has substantial amounts of job demand to carry out in the process realizing scale application.
Summary of the invention
It is an object of the present invention to provide a kind of method extracting lithium salts from high-Mg Li-contained bittern, solve to control process in prior art complicated, regeneration extraction ability is unstable, the technical problem that handicraft product is unstable.
The present invention solves that the technical scheme that above-mentioned technical problem adopts is as follows:
A kind of method extracting lithium salts from high-Mg Li-contained bittern, the method comprises the steps:
Extraction step, mixes calcium phosphate+ forage system with high-Mg Li-contained bittern and alkaline solution, carries out the extraction of lithium, obtain load lithium extraction system and extract after aqueous phase;
Exchange step, adopts Aqueous Lithium Salts mix with the extraction system of aforementioned load lithium, to remove the impurity in the extraction system of load lithium, and aqueous phase after obtaining the extraction system of load high purity lithium and exchanging;
Stripping steps, carries out back extraction by the extraction system of aforementioned load high purity lithium and acid solution, obtains the aqueous phase containing lithium salts, and aqueous phase obtains lithium salts after being evaporated.
Further, also include after described stripping steps:
Extraction system regeneration step, mixes alkaline solution with aqueous phase after the extraction obtained in the extraction phase obtained in described stripping steps and described extraction step, it is thus achieved that the extraction system after regeneration and aqueous phase after regeneration; Extraction system after described regeneration can be cycled to used in extraction step.
Preferably, described diluent is sulfonated kerosene, aviation gasoline or aromatic hydrocarbon.
Preferably, the preparation method of described calcium phosphate+ forage system is: mixed with the hydrochloric acid solution of iron chloride by the mixed solution of tributyl phosphate and diluent, obtain organic facies and aqueous phase after static, separate described organic facies and namely prepare described calcium phosphate+ forage system.
Preferably, in the mixed solution of described tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 30%��100%; Iron chloride concentration in hydrochloric acid solution is 0.5��4mol/L; When the mixed solution of tributyl phosphate and diluent mixes with the hydrochloric acid solution of iron chloride, volume ratio is 0.1��10, and incorporation time is 1-30min.
Preferably, described extraction step and the alkaline solution adopted in extraction system regeneration step are sodium hydroxide or potassium hydroxide solution, and concentration is 2mol/L��10mol/L.
Preferably, in described extraction step, by controlling the addition of alkaline solution, controlling the hydrogen ion concentration of aqueous phase after extracting is 0.001��0.2mol/L.
Preferably, in described extraction system regeneration step, by controlling the addition of alkaline solution, controlling the hydrogen ion concentration of aqueous phase after regenerating is 0.001��0.5mol/L.
Preferably, in the Aqueous Lithium Salts in described exchange step, lithium concentration is 0.1-5mol/L, and the lithium salts of employing is one or more in lithium chloride, lithium sulfate or lithium nitrate.
Preferably, described extraction step, exchange step, stripping steps and extraction system regeneration step adopt extraction tower equipment or membrane contactor to realize extracting, exchange, and back extraction and extraction system regenerate.
Compared with prior art, beneficial effects of the present invention is as follows:
1, improve for prior art adopts the process that high-Mg Li-contained bittern is extracted by TBP extractant, the present invention adopts the amount controlling to add aqueous slkali in extraction step and extraction system regeneration step, control the acidity of aqueous phase after extracting and the acidity of aqueous phase after extraction system regeneration, thus realizing the cycle applications of the stable and extraction system of extraction process and extraction system regenerative process, ensure to carry out containing stablizing of lithium salt extraction process process, the response rate of the lithium obtained by the process of the present invention is stable between 70-99%, final products purity can be controlled between 80-99.9%.
2, the present invention is the addition by controlling aqueous slkali, the aqueous phase acidity stablizing extraction step and extractant regeneration step stably extracts and the operation of extraction system regeneration step, the circulation stablizing extraction process further carries out, and this process solves extraction process in prior art and is difficult to control to the technological problems unstable with extraction system regeneration.
3, by using the aqueous phase of extraction system regeneration step and extraction step as control point, it is achieved regeneration extraction system is stable, and then extracts and obtain stable product containing the lithium in lithium salt and back extraction; Need not can realizing stable technical process by other rate-determining steps, relative to other containing the extracting method of lithium in lithium salt, control process simply effective, the response rate of lithium is stable, and product purity is stable.
Detailed description of the invention
If the high-Mg Li-contained bittern adopted in specific embodiment is containing boron ion, it is necessary to carry out boron lithium separation in advance. If containing other impurity, can first carry out pretreatment and remove partial impurities.
Embodiment 1
The preparation of calcium phosphate+ forage system: the mixed solution of tributyl phosphate and diluent, then mix with the hydrochloric acid solution of iron chloride, static organic facies and the aqueous phase of obtaining, separate organic facies and be calcium phosphate+ forage system; The calcium phosphate+ forage system obtained carries out extraction step first. In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 50%, and diluent is sulfonated kerosene; In the hydrochloric acid solution of iron chloride, the concentration of iron chloride is the volume ratio that the mixed solution of 2mol/L, tributyl phosphate and diluent mixes with the hydrochloric acid solution of iron chloride is 4, and incorporation time is 10min.
Extraction step: adopt separatory funnel to add high-Mg Li-contained bittern (Mg/Li=15 mol ratio, hydrionic concentration is 0.01) as aqueous phase; The sodium hydrate aqueous solution of calcium phosphate+ forage system and 5mol/L mixes as organic facies, biphase carries out two-stage countercurrent cascade extraction. By regulating the addition of sodium hydrate aqueous solution, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.03mol/L.
Exchange step: the extraction system of the load lithium that extraction step obtains and the lithium chloride solution of 3mol/L, compares 10:1 and carries out the mixing of two-stage tandem adverse current, it is thus achieved that the extraction system of exchange back loading high purity lithium.
Stripping steps: the extraction system of load high purity lithium carries out 2 stage countercurrent tandem back extractions again with 7M hydrochloric acid, and after back extraction, aqueous phase is as product.
Extraction system regeneration step: the aqueous phase obtained in the extraction system, the sodium hydrate aqueous solution of 5mol/L and the extraction step that are obtained by stripping steps mixes, and is layered as organic facies and aqueous phase, the extraction system after separation organic facies is namely regenerated after static. By regulating the addition of sodium hydrate aqueous solution, the aqueous phase acidity (c [H+]) controlled in this step is 0.8mol/L.
The circulation of the extraction system after regeneration is adopted to extract, exchange, back extraction. Process cycles carries out 8 times, and the extraction yield of salt lithium is stable between 80-85%, and the purity of product lithium chloride is stable between 90-94%.
Embodiment 2
The preparation of calcium phosphate+ forage system: tributyl phosphate mixes with the hydrochloric acid solution of iron chloride with mixing diluents solution, static organic facies and the aqueous phase of obtaining, separate organic facies and be calcium phosphate+ forage system; The calcium phosphate+ forage system obtained carries out extraction step first. In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 80%, and diluent is sulfonated kerosene; In the hydrochloric acid solution of iron chloride, the concentration of iron chloride is 2.2mol/L, and the volume ratio that tributyl phosphate mixes with the hydrochloric acid solution of iron chloride with mixing diluents solution is 4, and incorporation time is 3min.
Extraction step: adopt separatory funnel to add high-Mg Li-contained bittern (Mg/Li=15 mol ratio, hydrionic concentration is 0.01) as aqueous phase; The sodium hydrate aqueous solution of calcium phosphate+ forage system and 5mol/L mixes as organic facies, biphase carries out two-stage countercurrent cascade extraction. By regulating the addition of sodium hydrate aqueous solution, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.01mol/L.
Exchange step: the extraction system of the load lithium that extraction step obtains and the lithium chloride solution of 4mol/L, compares 10:1 and carries out the mixing of two-stage tandem adverse current, it is thus achieved that the extraction system of exchange back loading high purity lithium.
Stripping steps: the extraction system of load high purity lithium carries out 2 stage countercurrent tandem back extractions again with 7M hydrochloric acid, and after back extraction, aqueous phase is as product.
Extraction system regeneration step: the aqueous phase that extraction system, the sodium hydrate aqueous solution of 5mol/L and the extraction step obtained by stripping steps obtains mixes, and is layered as organic facies and aqueous phase, the extraction system after separation organic facies is namely regenerated after static. By regulating the addition of sodium hydrate aqueous solution, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.1mol/L.
The circulation of the extraction system after regeneration is adopted to carry out extracting, exchanging (aqueous phase then adopts the lithium chloride aqueous phase solution produced in a circulation exchange step), back extraction. Process cycles carries out 25 times, and the extraction yield of salt lithium is stable between 85-90%, and the purity of product lithium chloride is stable between 92-95%.
Embodiment 3
The preparation of extraction system: tributyl phosphate mixes with the hydrochloric acid solution of iron chloride with mixing diluents solution, static organic facies and the aqueous phase of obtaining, separate organic facies and be calcium phosphate+ forage system; The calcium phosphate+ forage system obtained carries out extraction step first. In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 50%, and diluent is sulfonated kerosene; In the hydrochloric acid solution of iron chloride, the concentration of iron chloride is 2mol/L, and tributyl phosphate and mixing diluents solution mix with the hydrochloric acid solution of iron chloride and is in a ratio of 4, and incorporation time is 10min.
Extraction step: adopt mixer-settler technique to carry out, add certain high-Mg Li-contained bittern (Mg/Li=12 mol ratio, hydrionic concentration is 0.01) as aqueous phase; The sodium hydrate aqueous solution of calcium phosphate+ forage system and 8mol/L mixes as organic facies, biphase carries out two-stage countercurrent extraction. By regulating the addition of sodium hydrate aqueous solution, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.02mol/L.
Exchange step: the extraction system of the load lithium that extraction step obtains and the lithium chloride solution of 4mol/L, compares 10:1 and carries out two-stage countercurrent mixing, it is thus achieved that the extraction system of exchange back loading high purity lithium.
Stripping steps: the extraction system of load high purity lithium carries out 2 stage countercurrent back extractions again with 7M hydrochloric acid, and after back extraction, aqueous phase is as product.
Extraction system regeneration step: the aqueous phase that extraction system, the sodium hydrate aqueous solution of 8mol/L and the extraction step obtained by stripping steps obtains mixes, and is layered as organic facies and aqueous phase, the extraction system after separation organic facies is namely regenerated after static. By regulating the addition of sodium hydroxide, after control extracts, aqueous phase acidity (c [H+]) is 0.1mol/L.
Adopting the extraction system after regeneration to control parameter according to each section, circulation carries out extracting, exchanging (aqueous phase then adopts the lithium chloride aqueous phase solution produced in a circulation exchange step, and volume ratio is 10%), back extraction. Process cycles carries out 100 hours, and the extraction yield of salt lithium is stable between 85-89%, and the purity of product lithium chloride is stable between 95-97%.
Embodiment 4
The preparation of extraction system: tributyl phosphate mixes with the hydrochloric acid solution of iron chloride with mixing diluents solution, static organic facies and the aqueous phase of obtaining, separate organic facies and be calcium phosphate+ forage system; The calcium phosphate+ forage system obtained carries out extraction step first. In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 80%, and diluent is sulfonated kerosene; In the hydrochloric acid solution of iron chloride, the concentration of iron chloride is 3mol/L, and tributyl phosphate and mixing diluents solution mix with the hydrochloric acid solution of iron chloride and is in a ratio of 4, and incorporation time is 5min.
Extraction step: adopt vibrating sieve plate extraction tower technique to carry out, add certain (Mg/Li=12 mol ratio, hydrionic concentration is 0.01) containing lithium salt as aqueous phase; The sodium hydrate aqueous solution of calcium phosphate+ forage system and 8mol/L mixes as organic facies, biphase carries out two-stage countercurrent extraction. By regulating the addition of sodium hydroxide, after control extracts, aqueous phase acidity (c [H+]) is 0.01mol/L.
Exchange step: the extraction system of the load lithium that extraction step obtains and the lithium chloride solution of 4mol/L, compares 10:1 and carries out 2 stage countercurrent mixing, it is thus achieved that the extraction system of exchange back loading high purity lithium.
Stripping steps: the extraction system of load high purity lithium carries out 2 stage countercurrent back extractions again with 7M hydrochloric acid, and after back extraction, aqueous phase is as product.
Extraction system regeneration step: the aqueous phase that extraction system, the sodium hydrate aqueous solution of 8mol/L and the extraction step obtained by stripping steps obtains mixes, and is layered as organic facies and aqueous phase, the extraction system after separation organic facies is namely regenerated after static. By regulating the addition of sodium hydroxide, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.03mol/L.
Adopting the extraction system after regeneration to control parameter according to each section, circulation carries out extracting, exchanging (aqueous phase then adopts the lithium chloride aqueous phase solution produced in a circulation exchange step, and volume ratio is 25%), back extraction.Process cycles carries out 220 hours, and the extraction yield of salt lithium is stable between 86-89%, and the purity of product lithium chloride is stable between 95-99%.
Embodiment 5
The preparation of extraction system: tributyl phosphate mixes with the hydrochloric acid solution of iron chloride with mixing diluents solution, static organic facies and the aqueous phase of obtaining, separate organic facies and be calcium phosphate+ forage system; The calcium phosphate+ forage system obtained carries out extraction step first. In the mixed solution of tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 80%, and diluent is sulfonated kerosene; In the hydrochloric acid solution of iron chloride, the concentration of iron chloride is 3mol/L, and tributyl phosphate and mixing diluents solution mix with the hydrochloric acid solution of iron chloride and is in a ratio of 4, and incorporation time is 2min.
Extraction step: adopt vibrating sieve plate extraction tower technique to carry out, add certain high-Mg Li-contained bittern (Mg/Li=10 mol ratio) as aqueous phase; The sodium hydrate aqueous solution of calcium phosphate+ forage system and 8mol/L mixes as organic facies, biphase carries out two-stage countercurrent extraction. By regulating the addition of sodium hydroxide, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.03mol/L.
Exchange step: the extraction system of the load lithium that extraction step obtains and the lithium chloride solution of 4mol/L, compares 10:1 and carries out 2 stage countercurrent mixing, it is thus achieved that the extraction system of exchange back loading high purity lithium.
Stripping steps: the extraction system of load high purity lithium carries out 4 stage countercurrent back extractions again with 7M hydrochloric acid, and after back extraction, aqueous phase is as product.
Extraction system regeneration step: the aqueous phase that extraction system, the sodium hydrate aqueous solution of 8mol/L and the extraction step obtained by stripping steps obtains mixes, and is layered as organic facies and aqueous phase, the extraction system after separation organic facies is namely regenerated after static. By regulating the addition of sodium hydroxide, controlling the acidity (c [H+]) of aqueous phase after extracting is 0.03mol/L.
Adopting the extraction system after regeneration to control parameter according to each section, circulation carries out extracting, exchanging (aqueous phase then adopts the lithium chloride aqueous phase solution produced in a circulation exchange step, and volume ratio is 30%), back extraction.
Process cycles carries out 200 hours, and the extraction yield of salt lithium is stable between 88-92%, and the purity of product lithium chloride is stable between 99-99.5%.
Above are only the part preferred embodiment of the present invention, the present invention is not limited in the content of embodiment. To those skilled in the art, can there be various change and change, any change made and change in the concept of technical solution of the present invention, all within scope.
Claims (10)
1. the method extracting lithium salts from high-Mg Li-contained bittern, the method comprises the steps:
Extraction step, mixes calcium phosphate+ forage system with high-Mg Li-contained bittern and alkaline solution, carries out the extraction of lithium, obtain load lithium extraction system and extract after aqueous phase;
Exchange step, adopts Aqueous Lithium Salts mix with the extraction system of aforementioned load lithium, to remove the impurity in the extraction system of load lithium, and aqueous phase after obtaining the extraction system of load high purity lithium and exchanging;
Stripping steps, carries out back extraction by the extraction system of aforementioned load high purity lithium and acid solution, obtains the aqueous phase containing lithium salts, and aqueous phase obtains lithium salts after being evaporated.
2. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that also include after described stripping steps:
Extraction system regeneration step, mixes alkaline solution with aqueous phase after the extraction obtained in the extraction phase obtained in described stripping steps and described extraction step, it is thus achieved that the extraction system after regeneration and aqueous phase after regeneration; Extraction system after described regeneration can be cycled to used in extraction step.
3. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that: described diluent is sulfonated kerosene, aviation gasoline or aromatic hydrocarbon.
4. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1, it is characterized in that, the preparation method of described calcium phosphate+ forage system is: mixed with the hydrochloric acid solution of iron chloride by the mixed solution of tributyl phosphate and diluent, obtain organic facies and aqueous phase after static, separate described organic facies and namely prepare described calcium phosphate+ forage system.
5. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 4, it is characterised in that: in the mixed solution of described tributyl phosphate and diluent, the volumetric concentration of tributyl phosphate is 30%��100%; Iron chloride concentration in hydrochloric acid solution is 0.5��4mol/L; When the mixed solution of tributyl phosphate and diluent mixes with the hydrochloric acid solution of iron chloride, volume ratio is 0.1��10.
6. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1 or 2, it is characterized in that: described extraction step and the aqueous solution that alkaline solution is sodium hydroxide or potassium hydroxide adopted in extraction system regeneration step, concentration is 2mol/L��10mol/L.
7. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that: in described extraction step, by controlling the addition of alkaline solution, controlling the hydrogen ion concentration of aqueous phase after extracting is 0.001��0.2mol/L.
8. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1, it is characterised in that: in described extraction system regeneration step, by controlling the addition of alkaline solution, controlling the hydrogen ion concentration of aqueous phase after regeneration is 0.001��0.5mol/L.
9. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1, it is characterized in that: in the Aqueous Lithium Salts in described exchange step, lithium concentration is 0.1-5mol/L, the lithium salts of employing is one or more in lithium chloride, lithium sulfate or lithium nitrate.
10. a kind of method extracting lithium salts from high-Mg Li-contained bittern as claimed in claim 1 or 2, it is characterized in that: described extraction step, exchange step, stripping steps and extraction system regeneration step adopt extraction tower equipment or membrane contactor to realize extracting, exchange, back extraction and extraction system regeneration.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521159A (en) * | 2016-10-11 | 2017-03-22 | 天津科技大学 | Method for extracting lithium in brine based on extraction system containing Fe (III) and 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 |
| CN107779612A (en) * | 2017-12-08 | 2018-03-09 | 中国科学院青海盐湖研究所 | A kind of technique that lithium is extracted from alkaline bittern |
| 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 |
| CN115679121A (en) * | 2021-07-26 | 2023-02-03 | 浙江新化化工股份有限公司 | Method for extracting lithium |
Citations (4)
| 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 |
| 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 |
-
2016
- 2016-01-07 CN CN201610008780.3A patent/CN105645443B/en not_active Expired - Fee Related
Patent Citations (4)
| 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 |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 徐宝荣等: "《分析化学》", 28 February 2003, 中国农业出版社 * |
| 贾旭宏等: ""磷酸三丁酯萃取体系从盐湖卤水提取锂"", 《无机盐工业》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106521159A (en) * | 2016-10-11 | 2017-03-22 | 天津科技大学 | Method for extracting lithium in brine based on extraction system containing Fe (III) and 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 |
| CN107779612A (en) * | 2017-12-08 | 2018-03-09 | 中国科学院青海盐湖研究所 | A kind of technique that lithium is extracted from alkaline bittern |
| 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 |
| CN115679121A (en) * | 2021-07-26 | 2023-02-03 | 浙江新化化工股份有限公司 | Method for extracting lithium |
| CN115679121B (en) * | 2021-07-26 | 2024-01-23 | 浙江新化化工股份有限公司 | Method for extracting lithium |
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