CN108070726A - A kind of method that lithium salts is extracted from lepidolite raw material - Google Patents
A kind of method that lithium salts is extracted from lepidolite raw material Download PDFInfo
- Publication number
- CN108070726A CN108070726A CN201711415937.5A CN201711415937A CN108070726A CN 108070726 A CN108070726 A CN 108070726A CN 201711415937 A CN201711415937 A CN 201711415937A CN 108070726 A CN108070726 A CN 108070726A
- Authority
- CN
- China
- Prior art keywords
- lepidolite
- raw material
- lithium salts
- extracted
- roasting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Geochemistry & Mineralogy (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention discloses a kind of method that lithium salts is extracted from lepidolite raw material, uses lepidolite as raw material, and lepidolite ore is pre-processed, is roasted, mechanical activation is handled, is leached, separation and Extraction process.The generation of raw material firing stage fluorine gas is reduced to the damage of equipment and the pollution of environment, the high temperature difference thermal response that thermal decomposition and ion generator generate opens lepidolite layer structure, size of microcrystal reduces, the extraction and application rate of rare metal raw material in lepidolite raw material is improved, the addition of buffer solution can reduce energy consumption, shorten the reaction time, and the consumption dosage of acid-base raw materials, practical performance is excellent, novel in design, is a kind of good innovation scheme.
Description
Technical field
The present invention relates to the technical method of extraction lithium salts, more particularly to a kind of side that lithium salts is extracted from lepidolite raw material
Method.
Background technology
Lepidolite is a kind of important mineral resources, contains abundant Rare Metals Materials, lithium, sodium, potassium, rubidium, caesium, aluminium
Deng.With the growing tension of world energy sources, utilization new energy is the common issue in the world, and lithium electricity new energy is as new energy
One of important industry of development is increasingly paid attention to by various countries, and lithium and the salt such as its esters lithium carbonate, lithium sulfate are lithium electricity new energy
The basic raw produce of industry, and the basic material lithium metal containing lithium electricity New Energy Industry in lepidolite, therefore to lithium cloud
Female development and application become current heat subject.
At present processing lepidolite ore method, the method industrially applied predominantly calcine or roasting method, the acid-hatching of young eggs or
It is the method that calcining is combined with acidleach.In the existing calcining production to lepidolite, it is common to use be the kiln mode of production
It carries out, such as vertical coal pit stove, the layer structure quilt of lepidolite when to the calcining of lepidolite being at 800-950 DEG C
It opens, the bulkiness of lepidolite material increases.At this temperature using current calciner plant and method, it is necessary at least 60 minutes
The time of left and right, it is that maintenance high temperature heating time is long so to result in one, and energy consumption is excessive, second is that since lepidolite ore is former
The prolonged dissolving at high temperature of material and calcining so that the Rare Metals Materials burn tinctuer in lepidolite raw material improves, and reduces
The recovery utilization rate of rare metal, pollution is also big, and there is deficiencies, it is impossible to the actual demand of society.
In conclusion the defects of for the prior art, it is accordingly required in particular to a kind of method that lithium salts is extracted from lepidolite raw material,
To solve the deficiencies in the prior art.
The content of the invention
For existing existing deficiency, actual use is influenced, the present invention proposes that one kind is extracted from lepidolite raw material
The method of lithium salts, it is novel in design, the extraction and application rate of rare metal raw material in lepidolite raw material is improved, the energy is reduced and disappears
Consumption improves the economic benefit of lepidolite.
To achieve these goals, technical scheme is as follows：
A kind of method that lithium salts is extracted from lepidolite raw material, uses lepidolite as raw material, lepidolite ore is located in advance
Reason, roasting, mechanical activation processing, leaching, separation and Extraction process, first will be with CaO and Ca (CH3COO)2Through plasma generator
High-temperature roasting and fluorine removal, CaO：Ca(CH3COO)2=1：0.5, it is 1500-2000 that plasma generator is controlled, which to carry out calcining heat,
DEG C, by the mixture ball milling 3 of pretreatment it is small when, roasting additive include sodium humate, sodium hydroxide, sodium sulphate, calcium compound
Mixing, by calcination for activation powder and dilute sulfuric acid and ammonium sulfate, mixed by the mass ratio of solid-to-liquid ratio, add water, be heated to
Autoclaving reaction 60-90min is carried out at a temperature of 120 DEG C, and under pressurized state, residued in reaction fluorine in lepidolite miberal powder by into
One step removes, and obtains the solid-liquid mixed solution of containing sulfate, filtrate of removing the gred to obtain, solution are filtered to gained solid-liquid mixed solution
In be passed through carbon dioxide, add in carbonate or sulfate lithium salts is made, obtained lithium salts is lithium carbonate or lithium sulfate.
Further, filter residue of the present invention with concentration be 80-95wt% concentrated sulfuric acid solution or dilute sulfuric acid and ammonium sulfate, press
Liquid-solid ratio is 2：1 than mixing, be heated at a temperature of 150 DEG C, be stirred continuously reaction 2-4 it is small when, be separated by filtration, wash, will filter
Slag removes.
It is to control its pressure as 3 atmospheric pressure in pressurized state of the present invention.
Lepidolite after the present invention calcines fluorine removal is reacted under pressurised conditions with sulfuric acid solution, controls acidleach temperature
For 90 DEG C, solid, liquid mixture, cooling freezing are obtained, separating potassium rubidium cesium alum filters, adds alkali, cleans, sinker lithium salts.
Further, plasma generator of the present invention carries out roasting to obtain roasting material, and roasting material being crushed again must roast afterwards
Powder is burnt, calcination temperature is 1500 DEG C, roasting time 20min.
It is lithium cloud in mechanical activation of the present invention processing by lepidolite calcining through mechanical ball mill activation process to 200-350 mesh
Female calcining mixture, by lepidolite calcining mixture first through low temperature presintering fluorine removal, then through plasma generator high-temperature roasting fluorine removal,
For calcination for activation powder.
The beneficial effects of the invention are as follows：Raw material firing stage fluorine gas is reduced to generate to the damage of equipment and the pollution of environment,
The high temperature difference thermal response that thermal decomposition and ion generator generate opens lepidolite layer structure, and size of microcrystal reduces, and improves lithium
The extraction and application rate of rare metal raw material in mica raw material, the addition of buffer solution can reduce energy consumption, shorten the reaction time,
And the consumption dosage of acid-base raw materials, practical performance is excellent, novel in design, is a kind of good innovation scheme.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
A kind of method that lithium salts is extracted from lepidolite raw material, uses lepidolite as raw material, lepidolite ore is located in advance
Reason, roasting, mechanical activation processing, leaching, separation and Extraction process, first will be with CaO and Ca (CH3COO)2Through plasma generator
High-temperature roasting and fluorine removal, CaO：Ca(CH3COO)2=1：0.5, it is 1500-2000 that plasma generator is controlled, which to carry out calcining heat,
DEG C, by the mixture ball milling 3 of pretreatment it is small when, roasting additive include sodium humate, sodium hydroxide, sodium sulphate, calcium compound
Mixing, by calcination for activation powder and dilute sulfuric acid and ammonium sulfate, mixed by the mass ratio of solid-to-liquid ratio, add water, be heated to
Autoclaving reaction 60-90min is carried out at a temperature of 120 DEG C, and under pressurized state, residued in reaction fluorine in lepidolite miberal powder by into
One step removes, and obtains the solid-liquid mixed solution of containing sulfate, filtrate of removing the gred to obtain, solution are filtered to gained solid-liquid mixed solution
In be passed through carbon dioxide, add in carbonate or sulfate lithium salts is made, obtained lithium salts is lithium carbonate or lithium sulfate.
Filter residue with concentration be 80-95wt% concentrated sulfuric acid solution or dilute sulfuric acid and ammonium sulfate, be 2 by liquid-solid ratio：1 ratio
Mixing, be heated at a temperature of 150 DEG C, be stirred continuously reaction 2-4 it is small when, be separated by filtration, wash, filter residue is removed.Pressurize shape
State is to control its pressure as 3 atmospheric pressure.Lepidolite after calcining fluorine removal is reacted under pressurised conditions with sulfuric acid solution, is controlled
Relieving haperacidity leaching temperature is 90 DEG C, obtains solid, liquid mixture, cooling freezing, and separating potassium rubidium cesium alum filters, adds alkali, cleans, sinker lithium
Salt.Plasma generator carries out roasting to obtain roasting material, and powder must be roasted afterwards by roasting material being crushed again, and calcination temperature is
1500 DEG C, roasting time 20min.Mechanical activation processing by lepidolite calcining through mechanical ball mill activation process to 200-350 mesh,
For lepidolite calcining mixture, by lepidolite calcining mixture first through low temperature presintering fluorine removal, then roast through plasma generator high temperature
Burn off fluorine is calcination for activation powder.
Using by lepidolite and Ca (CH3COO)2The high temperature difference thermal response generated by plasma generator, makes lepidolite knot
Structure changes, and the operation principle of plasma generator is that low-voltage is risen to positive high voltage and negative high voltage by booster circuit, profit
Negative ions are generated with positive high voltage and negative high voltage ionized air.The high temperature of formation calcines lepidolite raw material, by wait from
The temperature of electronic generator is rapidly reached 1500 DEG C or more, the Ca under TRANSIENT HIGH TEMPERATURE2+Ion and F-Ion, which directly generates, is insoluble in water
CaF2, the generation of HF gases is avoided, reduces the pollution to environment, CH3COO- ions present in lepidolite structure exist
The high temperature that the effusion gas and plasma generator that thermal decomposition under high temperature generates generate makes the lamellar structure of lepidolite fast
Speed is opened；Due to lithium at high operating temperatures and its each yttrium under weakly acidic condition easily separate out, extremely favorably
It is leached in yttrium, significantly shortens the reaction time.
The beneficial effects of the invention are as follows：Raw material firing stage fluorine gas is reduced to generate to the damage of equipment and the pollution of environment,
The high temperature difference thermal response that thermal decomposition and ion generator generate opens lepidolite layer structure, and size of microcrystal reduces, and improves lithium
The extraction and application rate of rare metal raw material in mica raw material, the addition of buffer solution can reduce energy consumption, shorten the reaction time,
And the consumption dosage of acid-base raw materials, practical performance is excellent, novel in design, is a kind of good innovation scheme.
It should be understood by those skilled in the art that the present invention is not limited to the above embodiments, above-described embodiment and explanation
Merely illustrating the principles of the invention described in book, it is of the invention without departing from the spirit and scope of the present invention also to have respectively
Kind changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by
Appended claims and its equivalent define.
Claims (6)
1. a kind of method that lithium salts is extracted from lepidolite raw material, uses lepidolite as raw material, it is characterised in that：To lepidolite ore
Pre-processed, roasted, mechanical activation processing, leach, separation and Extraction process, first will be with CaO and Ca (CH3COO)2Through wait from
Electronic generator high-temperature roasting and fluorine removal, CaO：Ca(CH3COO)2=1：0.5, control plasma generator carry out calcining heat be
1500-2000 DEG C, by the mixture ball milling 3 of pretreatment it is small when, roasting additive include sodium humate, sodium hydroxide, sodium sulphate,
The mixing of calcium compound by calcination for activation powder and dilute sulfuric acid and ammonium sulfate, is mixed by the mass ratio of solid-to-liquid ratio, add water,
It is heated at a temperature of 120 DEG C, and autoclaving reaction 60-90min is carried out under pressurized state, residued in reaction in lepidolite miberal powder
Fluorine is further removed, and obtains the solid-liquid mixed solution of containing sulfate, and gained solid-liquid mixed solution is filtered and removes the gred and must filter
Liquid is passed through carbon dioxide in solution, adds in carbonate or lithium salts is made in sulfate, and obtained lithium salts is lithium carbonate or sulphur
Sour lithium.
2. a kind of method that lithium salts is extracted from lepidolite raw material according to claim 1, it is characterised in that：Filter residue concentration
It is 2 by liquid-solid ratio for the concentrated sulfuric acid solution or dilute sulfuric acid and ammonium sulfate of 80-95wt%：1, than mixing, is heated to 150 DEG C of temperature
Under degree, be stirred continuously reaction 2-4 it is small when, be separated by filtration, wash, filter residue is removed.
3. a kind of method that lithium salts is extracted from lepidolite raw material according to claim 1, it is characterised in that：Pressurized state is
It is 3 atmospheric pressure to control its pressure.
4. a kind of method that lithium salts is extracted from lepidolite raw material according to claim 1, it is characterised in that：After calcining fluorine removal
Lepidolite reacted under pressurised conditions with sulfuric acid solution, acidleach temperature is controlled to obtain solid, liquid mixture for 90 DEG C, is cooled down
Freezing, separating potassium rubidium cesium alum, filtering add alkali, clean, sinker lithium salts.
5. a kind of method that lithium salts is extracted from lepidolite raw material according to claim 1, it is characterised in that：Plasma occurs
Device carries out roasting to obtain roasting material, and powder must be roasted afterwards by roasting material being crushed again, and calcination temperature is 1500 DEG C, during roasting
Between be 20min.
6. a kind of method that lithium salts is extracted from lepidolite raw material according to claim 1, it is characterised in that：At mechanical activation
Lepidolite calcining through mechanical ball mill activation process to 200-350 mesh, is lepidolite calcining mixture, lepidolite calcining is mixed by reason
Material is closed first through low temperature presintering fluorine removal, then is calcination for activation powder through plasma generator high-temperature roasting fluorine removal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711415937.5A CN108070726A (en) | 2017-12-25 | 2017-12-25 | A kind of method that lithium salts is extracted from lepidolite raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711415937.5A CN108070726A (en) | 2017-12-25 | 2017-12-25 | A kind of method that lithium salts is extracted from lepidolite raw material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108070726A true CN108070726A (en) | 2018-05-25 |
Family
ID=62155650
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711415937.5A Pending CN108070726A (en) | 2017-12-25 | 2017-12-25 | A kind of method that lithium salts is extracted from lepidolite raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108070726A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010991A (en) * | 2010-10-29 | 2011-04-13 | 江西本源新材料科技有限公司 | Method for extracting lithium salt and removing potassium from lithium mica raw material |
| CN102718234A (en) * | 2012-07-12 | 2012-10-10 | 张勇 | Method for extracting lithium carbonate from lepidolite |
| CN103014316A (en) * | 2012-12-04 | 2013-04-03 | 宜春银锂新能源有限责任公司 | Novel method for processing lepidolite material |
| CN103014317A (en) * | 2012-12-04 | 2013-04-03 | 宜春银锂新能源有限责任公司 | Method for extracting lithium salt from lepidolite |
| CN104313349A (en) * | 2014-10-10 | 2015-01-28 | 李宇龙 | Method of extracting lithium salt from lepidolite |
| CN105039699A (en) * | 2015-06-03 | 2015-11-11 | 江西合纵锂业科技有限公司 | Method for treatment and resource utilization of alkali metal slag extracted through lepidolite solid fluorine reconstruction |
| CN107475537A (en) * | 2017-07-17 | 2017-12-15 | 江西南氏锂电新材料有限公司 | Lithium, rubidium, the method for cesium salt are extracted from lepidolite raw material |
-
2017
- 2017-12-25 CN CN201711415937.5A patent/CN108070726A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010991A (en) * | 2010-10-29 | 2011-04-13 | 江西本源新材料科技有限公司 | Method for extracting lithium salt and removing potassium from lithium mica raw material |
| CN102718234A (en) * | 2012-07-12 | 2012-10-10 | 张勇 | Method for extracting lithium carbonate from lepidolite |
| CN103014316A (en) * | 2012-12-04 | 2013-04-03 | 宜春银锂新能源有限责任公司 | Novel method for processing lepidolite material |
| CN103014317A (en) * | 2012-12-04 | 2013-04-03 | 宜春银锂新能源有限责任公司 | Method for extracting lithium salt from lepidolite |
| CN104313349A (en) * | 2014-10-10 | 2015-01-28 | 李宇龙 | Method of extracting lithium salt from lepidolite |
| CN105039699A (en) * | 2015-06-03 | 2015-11-11 | 江西合纵锂业科技有限公司 | Method for treatment and resource utilization of alkali metal slag extracted through lepidolite solid fluorine reconstruction |
| CN107475537A (en) * | 2017-07-17 | 2017-12-15 | 江西南氏锂电新材料有限公司 | Lithium, rubidium, the method for cesium salt are extracted from lepidolite raw material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107475537B (en) | The method of lithium, rubidium, cesium salt is extracted from lepidolite raw material | |
| CN104313349A (en) | Method of extracting lithium salt from lepidolite | |
| CN103145158B (en) | Method for preparing lithium carbonate from lepidolite through sulfuric acid roasting method | |
| JP4332591B2 (en) | Method for recovering silica and then alumina from coal ash | |
| KR102278372B1 (en) | Method for recoering lithium from lithium compound | |
| CN101775505B (en) | Method and device for extracting lithium from lapidolite by chloridizing roasting method | |
| CN103014317B (en) | Method for extracting lithium salt from lepidolite | |
| CN107089674A (en) | A kind of spodumene sodium sulphate pressure leaching puies forward lithium technique | |
| CN104876250B (en) | Method for extracting lithium and removing aluminum by treating lepidolite with sulfuric acid | |
| CN108584994A (en) | A kind of method of lepidolite calcined by rotary kiln lithium carbonate | |
| CN102897810B (en) | Method for producing aluminum oxide by using fly ash | |
| CN101811712A (en) | Method for preparing metallurgical-grade aluminum oxide by using fluid-bed fly ash | |
| CN108330298B (en) | Method for extracting rubidium, cesium, lithium and potassium from polymetallic mica ore | |
| CN108517423B (en) | Method for extracting lithium and lithium salt by roasting lepidolite in rotary kiln | |
| CN105039699A (en) | Method for treatment and resource utilization of alkali metal slag extracted through lepidolite solid fluorine reconstruction | |
| CN115216645B (en) | Method for extracting lithium from electrolytic aluminum waste residue by mixed salt calcination | |
| CN108570566A (en) | The technique that lepidolite raw material Roasting And Leaching extracts lithium | |
| CN109911922A (en) | A kind of method that lepidolite ore prepares battery-level lithium carbonate | |
| CN104140117A (en) | Process for extracting lithium salt by adopting method for autoclaving lepidolite with sulfuric acid | |
| CN112624161B (en) | Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite | |
| CN114318008A (en) | Method for extracting lithium by secondary reverse leaching of spodumene with nitric acid | |
| CN103014316B (en) | Novel method for processing lepidolite material | |
| CN106629803B (en) | The method for producing calcium chloride and aluminium polychloride using high-calcium fly ass | |
| CN108383140A (en) | A kind of clearer production technology and method of lithium sulfate | |
| CN105948084A (en) | Method for producing magnesium sulfate monohydrate with copper tailings taken as raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180525 |
|
| RJ01 | Rejection of invention patent application after publication |