CN109574047A - The method of high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium - Google Patents
The method of high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium 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
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D265/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom and one oxygen atom as the only ring hetero atoms
- C07D265/04—1,3-Oxazines; Hydrogenated 1,3-oxazines
- C07D265/12—1,3-Oxazines; Hydrogenated 1,3-oxazines condensed with carbocyclic rings or ring systems
- C07D265/14—1,3-Oxazines; Hydrogenated 1,3-oxazines condensed with carbocyclic rings or ring systems condensed with one six-membered ring
- C07D265/18—1,3-Oxazines; Hydrogenated 1,3-oxazines condensed with carbocyclic rings or ring systems condensed with one six-membered ring with hetero atoms directly attached in position 2
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The method of high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium, it is characterised in that: extractant is added into medical waste liquid containing lithium, collects water phase and organic phase；Heated aqueous is concentrated；Extractant extraction liquid separation is added, water phase and organic phase are collected；Resin is added, collects water phase as mother liquor；Alkali and Na are added into mother liquor2CO3, pH is adjusted, obtains clear liquid after separation of solid and liquid；Clear liquid pH is adjusted back with hydrochloric acid, is boiled；Again with the pH to 6.0 ~ 8.0 of LiOH tune clear liquid, scavenging solution is obtained；Scavenging solution is concentrated by evaporation, LiCl saturated solution is obtained, organic solvent is added, crystal obtains LiCl crude product after being precipitated；Crude product is dissolved with organic solvent, is separated by solid-liquid separation, is spray-dried to obtain LiCl product；It will be evaporated after organic mix, thin layer chromatography separates various organic matters, obtains Sustiva.The present invention realizes the recycling of high-purity lithium chloride and Sustiva, method simple possible by multi-step removal of impurities recovery process.
Description
Technical field
The present invention relates to the recyclings of the waste liquid containing lithium, and in particular to it is a kind of recycled from medical waste liquid containing lithium high-purity according to
The method of Fa Weilun and lithium chloride.
Background technique
Lithium, silvery white non-ferrous metal, symbol of element Li, atomic number 3, atomic weight 6.941.0.534 g/cm3 of density, is density
The smallest metal.180 DEG C of fusing point, 1340 DEG C of boiling point.Dew empties gradual change yellow or black in gas.It meets water vigorous reaction and generates hydrogen
Lithia and hydrogen react rapidly with dilute hydrochloric acid and dilute sulfuric acid and release hydrogen, slower with cold effect of sulfuric acid, violent with nitric acid effect
It is strong.It is not reacted with oxygen under room temperature, is reacted with nitrogen and generate protective nitridation lithium layer.It is heated to generating oxygen at 100 DEG C or more
Change lithium, the effect of red heat Shi Nengyu hydrogen.It can be with halogen and the direct chemical combination of sulphur under certain condition.
Lithium compound has the effects that calm, analgesia, diuresis can treat mental disease, wind in terms of having been used for medicine for many years
The diseases such as wet arthritis.During producing medicine intermediate containing lithium, a large amount of waste liquids containing lithium can be generated.The prior art is to containing lithium
The recovery method of lithium is mainly as follows in waste liquid:
Patent CN1072190C is mainly to provide a kind of recovery method for producing lithium in lithium alkylide waste liquid.Its under nitrogen protection,
Na is used after adjusting pH with HCl after waste liquid is hydrolyzed2CO3Precipitating obtains lithium carbonate product, and mother liquor is centrifuged to obtain chlorine
Change lithium.Patent WO2017181759A1 mainly uses H2O2Oxidation removal is carried out to the organic Colors in waste liquid, then is carried out inorganic
Sodium refining agent is added after the removal of impurity, obtains lithium chloride products after spray drying.Patent CN102815680A is mainly concerned with
To addition phosphoric acid in waste liquid containing lithium to prepare lithium phosphate.Patent CN105129826B is mainly concerned with medicine and synthetic plastic waste liquid
Middle recycling lithium, major way are to be concentrated by evaporation, roast clean after crude product, carbonization, thermally decompose to obtain product.Patent
CN1781847A main technique is while to add BaCl2 and oxalic acid thereto with hydrochloric acid alkali tune, after filtering again plus during hydrochloric acid adjusts
Property, it is spray-dried to obtain LiCl product.
Above-mentioned most of prior art is not directed to the removal of organic matter in waste liquid, even if relating to organic matter removal
Patent, organic removal rate is not high, and the liquid after removal of impurities still has remaining organic matter, and solution colour is partially yellow, needs to use dioxygen
Water decoloring, but do not completely remove organic matter fundamentally, and process is longer, the rate of recovery is low, and introducing other impurity leads to product matter
It is poor to measure；If the organic matter not exclusively in removal waste liquid, it will seriously affect product quality, product whiteness and purity are difficult to control.
On the other hand, it is not directed to the method that certain drug is extracted in recycling from medicine waste liquid containing lithium in the prior art.
Summary of the invention
The rate of recovery is lower when recycling lithium from medical waste liquid containing lithium, has a secondary pollution in order to overcome in the past, cost recovery compared with
Height, complex procedures and the defect for not completely removing organic matter, and the technological gap that drug ingedient is collected not from waste liquid is filled up,
The method that the present invention provides a kind of to recycle high-purity Sustiva and lithium chloride from medicine waste liquid containing lithium.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: it is a kind of to recycle high-purity from medical waste liquid containing lithium
The method of Sustiva and lithium chloride, successively includes the following steps:
Step (1) extracts liquid separation: extractant is added into medical waste liquid containing lithium, at least extraction is primary, collection water phase and organic
Phase；
Step (2) is concentrated by evaporation: it will be concentrated through the heated aqueous that the step (1) extracted, it is cooling, and saturation is closed on until reaching
State is without being precipitated salt；
Step (3) extracts liquid separation: the extractant extraction liquid separation being added in the water phase after Xiang Suoshu step (2) concentration, at least extracts
Take primary, collection water phase and organic phase；
Step (4), absorption: being added resin in water phase obtained by Xiang Suoshu step (4), stirs, filtering, regathers water phase as female
Liquid；
Step (5), removal of impurities: the mother liquid obtained middle addition alkali of Xiang Suoshu step (4) and Na2CO3, pH to 6 ~ 12 is adjusted, is separated by solid-liquid separation
After obtain clear liquid；The pH to 3 ~ 8 that the clear liquid is adjusted with hydrochloric acid, boils；Adjusted again with lithium hydroxide boil the pH of rear clear liquid to
6.0 ~ 8.0, it is purified liquid；
Step (6), solventing-out process purification: gained scavenging solution in the step (5) is concentrated by evaporation, until obtaining LiCl saturation
Solution, then the first organic solvent is added into the LiCl saturated solution, after LiCl crystal structure is precipitated, obtain LiCl crude product；
Step (7) dissolves, and spray drying: the second organic solvent of LiCl crude product obtained in the step (6) is dissolved, molten
Xie Hou, separation of solid and liquid obtain solution, and solution obtains high-purity technical level-one LiCl by spray drying；
Step (8), is evaporated: by the gained of the step (1) and step (3) is organic mix after be evaporated with Rotary Evaporators, obtain
It is dissolved in extractant to viscous brown shape mixture, then by the viscous brown shape mixture, using thin layer chromatography, separation is each
Kind organic matter, various organic matters are placed in container and are dissolved in dehydrated alcohol, are sealed, and are stood volatilization, are obtained Sustiva crystal.
Related content in above-mentioned technical proposal is explained as follows:
1, in above scheme, it is described medicine waste liquid containing lithium contain lithium ion, sulfate ion, chloride ion, calcium ion, iron ion,
Magnesium ion, sodium ion, potassium ion and Sustiva.
2, in above scheme, in the step (1), it is described medicine waste liquid containing lithium and extractant volume ratio be 1:10 ~
10:1。
3, in above scheme, in the step (1), step (3) and step (8), the extractant is acetic acid second
Ester.
4, in above scheme, in the step (2), heating thickening temperature is 80 ~ 120 DEG C.
5, in above scheme, in the step (4), the alkali is NaOH.
6, in above scheme, in the step (6), first organic solvent is ethyl alcohol, methanol, ether, ethylene glycol
And any one or a few the mixture in tetrahydrofuran.
7, in above scheme, in the step (7), second organic solvent is ethyl alcohol, methanol, ether and second two
Any one in alcohol.
8, in above scheme, the resin is macroreticular ion exchange resin, trade mark D231, DK251,731 and 290
In any one.
Design concept of the present invention: the present invention includes that organic matter is kept completely separate technique, impurity removal process and recovery process, is adopted
With extraction, concentration, again extract, resins exchange, removal of impurities, evaporation, dissolved, dehydrated alcohol dissolution, spray drying, rotation be evaporated to obtain
Industrial level-one lithium chloride products and Sustiva monocrystalline.That is, the present invention can carry out adequately medical waste liquid containing lithium
Recycling and utilization, can not only be recovered to the lithium chloride of high-purity, moreover it is possible to high-purity is recovered to from organic phase from water phase
Sustiva, recovery process is simple, and can guarantee that recycled product impurities content is very low on this basis.It is specific as follows:
Step (1) be in order to tentatively remove the organic matter in waste liquid, meanwhile, Sustiva is retained in organic phase.
Step (2) is the preparation done for step (3), evaporation-concentration step (1) resulting water phase.
Step (3) is the organic matter in order to contain in secondary removal water phase, at this point, contain lithium chloride in water phase, organic phase
In contain Sustiva, for recycling Sustiva for, have collected organic phase to greatest extent.
Step (4) is to be purified to the water sample for eliminating organic matter by resin, be can remove by the step most of
Metal cation impurity, such as iron ion, calcium ion magnesium ion and potassium ion etc..
Step (5) is further to eliminate the metal ions such as iron ion and calcium ion for deep impurity-removing.
Step (6) is that LiCl crystal structure is precipitated, obtains LiCl crude product, goes at this time using dilution crystallization principle
In addition to impurity most in lithium chloride.
The quality of step (7) resulting lithium chloride is high, reaches industrial primary standard, purity is up to 99% or more.
Step (8) is to separate Sustiva from various organic matters.Step first is evaporated with Rotary Evaporators
Suddenly the gained organic phase of (1) and step (3) obtains viscous brown shape mixture, then uses thin layer chromatography, separates various organic
Various organic matters are placed in container and are dissolved in dehydrated alcohol by object, sealing, after standing volatilization a period of time, obtain Sustiva crystalline substance
Body.
Compared with prior art, the beneficial effects of the present invention are:
(1) recovery process of the invention is simple, and operation is simple, and can recycle industrial level-one lithium chloride and Sustiva simultaneously.
(2) present invention can recycle lithium from the medical waste liquid containing large amount of organic, and the rate of recovery is high, and the rate of recovery reaches
96% or more, separation thoroughly, does not introduce other impurity, without the whiteness and purity that hydrogen peroxide is controllable lithium chloride products is added,
It recycles obtained lithium chloride and reaches industrial primary standard and whiteness qualification, purity is up to 99% or more.
(3) present invention has carried out abundant recycling to organic phase, and Sustiva monocrystalline is extracted from organic phase, is not added
Enter other precipitating reagents, does not influence product quality, the purity is high of Sustiva.
In short, the present invention is using waste liquid caused by pharmaceutical industry as raw material sources, cleaned recovery process by multi-step, both
It realizes the recycling of lithium chloride and realizes the recycling of Sustiva, and the purity of two kinds of products is very high, realizes to waste liquid
It is effectively treated, method simple possible, energy consumption is lower, is added without other precipitating reagents.
Detailed description of the invention
Attached drawing 1 is the nuclear magnetic spectrum of efavirenz.
Specific embodiment
The present invention will be further described below with reference to examples:
Raw material involved in embodiment 1 ~ 3 is the liquid such as generated intermediate waste liquid in medicine production, mainly group
At as shown in the table:
Embodiment 1: the method for high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium
Successively include the following steps:
Step (1) takes 500mL waste water to pour into 1L separatory funnel with graduated cylinder, and 100mL ethyl acetate is added and extracts liquid separation, respectively
Extraction is three times.Collect water phase 500mL and organic phase 260mL.
Step (2) is concentrated by evaporation: the water sample for taking 500mL to extract is in 500mL beaker, and heating temperature is 100 DEG C, concentration
It is cooling to 220mL or so stopping heating, saturation state is closed on so that reaching, without salt is precipitated.
Step (3) extracts liquid separation: 40mL ethyl acetate is added in the water phase after Xiang Suoshu step (2) concentration and extracts liquid separation,
Extraction three times, collects water phase and organic phase；
Step (4), absorption: being added 30g resin in water phase obtained by Xiang Suoshu step (4), stirring is reacted 3 hours, filtering, then is received
Collect water phase as mother liquor；
Mother liquor obtained in step (4) removal of impurities: is first used the NaOH solution of 10 mol/L or so to adjust pH to 12, together by step (5)
When Na is added2CO3It is separated by solid-liquid separation after being stirred 30 min；Gained clear liquid industry HCl is adjusted into pH to 2.0, boils 30
min；Liquid is purified with the pH to 7.0 that rear clear liquid is boiled in saturation LiOH solution adjusting；
Step (6), solventing-out process purification: gained scavenging solution in the step (5) is concentrated by evaporation, until obtaining LiCl saturation
Solution, then dehydrated alcohol is added into LiCl saturated solution, until obtaining LiCl crude product after LiCl crystal structure is precipitated；
Step (7), dissolve, spray drying: by LiCl crude product obtained in the step (6) according to 170 g LiCl be dissolved in 1L without
Dehydrated alcohol, stirring and dissolving 30min or so is added in the ratio of water-ethanol, and separation of solid and liquid obtains the ethanol solution of LiCl, directly sprays
Mist is dried to obtain industrial level-one lithium chloride products；
Step (8), is evaporated: by the gained of the step (1) and step (3) is organic mix after be evaporated with Rotary Evaporators, obtain
It is dissolved in ethyl acetate to viscous brown shape mixture, then by the viscous brown shape mixture, using thin layer chromatography, separation
Various organic matters are placed in container and are dissolved in dehydrated alcohol by various organic matters, sealing, stand volatilization a period of time after, obtain according to
Fa Weilun crystal.
The rate of recovery of lithium is 97%, purity 99.2%.The HPLC purity of Sustiva is 99.8%.Such as the nuclear-magnetism figure of Fig. 1
Spectrum proves that gained crystal is Sustiva.
Embodiment 2: the method for high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium
Successively include the following steps:
Step (1) takes 500mL waste water to pour into 10L separatory funnel with graduated cylinder, and 5000mL ethyl acetate is added and extracts liquid separation, point
It does not extract three times.Collect water phase 500mL and organic phase 1300mL.
Step (2) is concentrated by evaporation: for the water sample for taking 500mL to extract in 500mL beaker, heating temperature is 90 DEG C, is concentrated into
220mL or so stops heating, cooling, saturation state is closed on so that reaching, without salt is precipitated.
Step (3) extracts liquid separation: 40mL ethyl acetate is added in the water phase after Xiang Suoshu step (2) concentration and extracts liquid separation,
Extraction three times, collects water phase and organic phase；
Step (4), absorption: being added 30g resin in water phase obtained by Xiang Suoshu step (4), stirring is reacted 3 hours, filtering, then is received
Collect water phase as mother liquor；
Mother liquor obtained in step (4) removal of impurities: is first used the NaOH solution of 10 mol/L or so to adjust pH to 12, together by step (5)
When Na is added2CO3It is separated by solid-liquid separation after being stirred 30 min；Gained clear liquid industry HCl is adjusted into pH to 2.0, boils 30
min；Liquid is purified with the pH to 7.0 that rear clear liquid is boiled in saturation LiOH solution adjusting；
Step (6), solventing-out process purification: gained scavenging solution in the step (5) is concentrated by evaporation, until obtaining LiCl saturation
Solution, then ethylene glycol is added into LiCl saturated solution, until obtaining LiCl crude product after LiCl crystal structure is precipitated；
Step (7), dissolve, spray drying: by LiCl crude product obtained in the step (6) according to 170 g LiCl be dissolved in 1L without
Dehydrated alcohol, stirring and dissolving 30min or so is added in the ratio of water-ethanol, and separation of solid and liquid obtains the ethanol solution of LiCl, directly sprays
Mist is dried to obtain industrial level-one lithium chloride products；
Step (8), is evaporated: by the gained of the step (1) and step (3) is organic mix after be evaporated with Rotary Evaporators, obtain
It is dissolved in ethyl acetate to viscous brown shape mixture, then by the viscous brown shape mixture, using thin layer chromatography, separation
Various organic matters are placed in container and are dissolved in dehydrated alcohol by various organic matters, sealing, stand volatilization a period of time after, obtain according to
Fa Weilun crystal.
The rate of recovery of lithium is 97.5%, purity 99.4%.The HPLC purity of Sustiva is 99.7%.
Embodiment 3: the method for high-purity Sustiva and lithium chloride is recycled from medicine waste liquid containing lithium
Successively include the following steps:
Step (1) takes 500mL waste water to pour into 1L separatory funnel with graduated cylinder, and 50mL ethyl acetate is added and extracts liquid separation, extracts respectively
It takes three times.Collect water phase 500mL and organic phase 130mL.
Step (2) is concentrated by evaporation: the water sample for taking 500mL to extract is in 500mL beaker, and heating temperature is 110 DEG C, concentration
It is cooling to 220mL or so stopping heating, saturation state is closed on so that reaching, without salt is precipitated.
Step (3) extracts liquid separation: 40mL ethyl acetate is added in the water phase after Xiang Suoshu step (2) concentration and extracts liquid separation,
Extraction three times, collects water phase and organic phase；
Step (4), absorption: being added 30g resin in water phase obtained by Xiang Suoshu step (4), stirring is reacted 3 hours, filtering, then is received
Collect water phase as mother liquor；
Mother liquor obtained in step (4) removal of impurities: is first used the NaOH solution of 10 mol/L or so to adjust pH to 12, together by step (5)
When be added Na2CO3 be stirred 30 min after be separated by solid-liquid separation；Gained clear liquid industry HCl is adjusted into pH to 2.0, boils 30
min；Liquid is purified with the pH to 7.0 that rear clear liquid is boiled in saturation LiOH solution adjusting；
Step (6), solventing-out process purification: gained scavenging solution in the step (5) is concentrated by evaporation, until obtaining LiCl saturation
Solution, then ether is added into LiCl saturated solution, until obtaining LiCl crude product after LiCl crystal structure is precipitated；
Step (7), dissolve, spray drying: by LiCl crude product obtained in the step (6) according to 170 g LiCl be dissolved in 1L without
Dehydrated alcohol, stirring and dissolving 30min or so is added in the ratio of water-ethanol, and separation of solid and liquid obtains the ethanol solution of LiCl, directly sprays
Mist is dried to obtain industrial level-one lithium chloride products；
Step (8), is evaporated: by the gained of the step (1) and step (3) is organic mix after be evaporated with Rotary Evaporators, obtain
It is dissolved in ethyl acetate to viscous brown shape mixture, then by the viscous brown shape mixture, using thin layer chromatography, separation
Various organic matters are placed in container and are dissolved in dehydrated alcohol by various organic matters, sealing, stand volatilization a period of time after, obtain according to
Fa Weilun crystal.
The rate of recovery of lithium is 98%, purity 99.5%.The HPLC purity of Sustiva is 99.6%.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method for recycling high-purity Sustiva and lithium chloride from medicine waste liquid containing lithium, it is characterised in that: successively wrap
Include the following steps:
Step (1) extracts liquid separation: extractant is added into medical waste liquid containing lithium, collects water phase and organic phase；
Step (2) is concentrated by evaporation: it will be concentrated through the heated aqueous that the step (1) extracted, it is cooling, and saturation is closed on until reaching
State is without being precipitated salt；
Step (3) extracts liquid separation: the extractant extraction liquid separation being added in the water phase after Xiang Suoshu step (2) concentration, collects water
Phase and organic phase；
Step (4), absorption: being added resin in water phase obtained by Xiang Suoshu step (4), stirs, filtering, regathers water phase as female
Liquid；
Step (5), removal of impurities: the mother liquid obtained middle addition alkali of Xiang Suoshu step (4) and Na2CO3, pH to 6 ~ 12 is adjusted, after separation of solid and liquid
Obtain clear liquid；The pH to 3 ~ 8 that the clear liquid is adjusted with hydrochloric acid, boils；The pH to 6.0 for boiling rear clear liquid is adjusted with lithium hydroxide again
~ 8.0, it is purified liquid；
Step (6), solventing-out process purification: gained scavenging solution in the step (5) is concentrated by evaporation, until obtaining LiCl saturation
Solution, then the first organic solvent is added into the LiCl saturated solution, reduce the solubility of LiCl in the solution to fast
Speed crystallization is precipitated, and after the precipitation of LiCl crystal structure, obtains LiCl crude product；
Step (7) dissolves, and spray drying: the second organic solvent of LiCl crude product obtained in the step (6) is dissolved, molten
Xie Hou, separation of solid and liquid obtain solution, and solution obtains high-purity LiCl by spray drying；
Step (8), is evaporated: by the gained of the step (1) and step (3) is organic mix after be evaporated, obtain viscous brown shape
Mixture, then the viscous brown shape mixture is dissolved in extractant, using thin layer chromatography, various organic matters are separated, it is close
Envelope stands volatilization, obtains Sustiva crystal.
2. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: the medicine waste liquid containing lithium contains lithium ion, sulfate ion, chloride ion, calcium ion, iron ion, magnesium ion, sodium
Ion and Sustiva.
3. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: in the step (1), the volume ratio of the medicine waste liquid containing lithium and extractant is 1:10 ~ 10:1.
4. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: in the step (1), step (3) and step (8), the extractant is ethyl acetate.
5. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: in the step (2), heating thickening temperature is 80 ~ 120 DEG C.
6. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: in the step (4), the alkali is NaOH.
7. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: in the step (6), first organic solvent is ethyl alcohol, methanol, ether, ethylene glycol and tetrahydrofuran
In any one or a few mixture.
8. the method according to claim 1 that high-purity Sustiva and lithium chloride are recycled from medicine waste liquid containing lithium,
Be characterized in that: in the step (7), second organic solvent is any one in ethyl alcohol, methanol, ether and ethylene glycol
Kind.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112850756A (en) * | 2020-10-30 | 2021-05-28 | 江西理工大学 | Method for extracting and preparing high-purity anhydrous lithium sulfate solid from byproduct mirabilite of lithium smelting enterprise |
| WO2021228936A1 (en) * | 2020-05-13 | 2021-11-18 | Katholieke Universiteit Leuven | Method for producing battery grade lithium hydroxide monohydrate |
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| CN106337138A (en) * | 2016-11-03 | 2017-01-18 | 深圳市捷鑫资产管理有限公司 | Technology for preparing high-purity anhydrous lithium chloride through centrifugal extraction of salt lake brine |
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| WO2021228936A1 (en) * | 2020-05-13 | 2021-11-18 | Katholieke Universiteit Leuven | Method for producing battery grade lithium hydroxide monohydrate |
| CN112850756A (en) * | 2020-10-30 | 2021-05-28 | 江西理工大学 | Method for extracting and preparing high-purity anhydrous lithium sulfate solid from byproduct mirabilite of lithium smelting enterprise |
| CN112850756B (en) * | 2020-10-30 | 2022-11-25 | 江西理工大学 | Method for extracting and preparing high-purity anhydrous lithium sulfate solid from byproduct mirabilite of lithium smelting enterprise |
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