CN108584994A - A kind of method of lepidolite calcined by rotary kiln lithium carbonate - Google Patents
A kind of method of lepidolite calcined by rotary kiln lithium carbonate Download PDFInfo
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- CN108584994A CN108584994A CN201810488067.2A CN201810488067A CN108584994A CN 108584994 A CN108584994 A CN 108584994A CN 201810488067 A CN201810488067 A CN 201810488067A CN 108584994 A CN108584994 A CN 108584994A
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- lepidolite
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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
- C01D15/08—Carbonates; Bicarbonates
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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
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention seeks to provide a kind of method of lepidolite calcined by rotary kiln lithium carbonate, using lepidolite as raw material, using calcining and water soaking method, including calcining, water logging, filtering, separation, freezing sinker lithium carbonate, the calcining is calcined together to lepidolite raw material and auxiliary material using calcined by rotary kiln device, it comprises the technical steps that, 1）Lepidolite is crushed to 200 300 mesh, is lepidolite powder；2）Lepidolite powder is uniformly mixed to roast raw material together with auxiliary material, controls the mass ratio of lepidolite powder and auxiliary material；3）Roasting raw material are placed in calcined by rotary kiln device, carry out calcining as calcining material, control calcined by rotary kiln time, temperature.Operating process of the present invention is stablized, with short production cycle, and utilization rate of equipment and installations is high, and production cost is low, and three waste discharge is few, the small production method of effect on environment.
Description
Technical field：The present invention relates to a kind of extracting method of lithium carbonate, especially a kind of lepidolite calcined by rotary kiln system
The method of lithium carbonate.
Background technology：
With national new energy development plan, lithium electricity new energy supports one of development energy industry as state key；Lithium carbonate
Develop important foundation raw material as lithium electricity new energy, production and demand are increasing, and price is also higher and higher.
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, the common issue that new energy is the world is developed and used, is increasingly paid attention to by various countries；
Lithium and its esters lithium carbonate, the salt such as lithium sulfate are the basic raw produce of lithium electricity New Energy Industry, and contain lithium in lepidolite
The basic material lithium metal of electric New Energy Industry, therefore current heat subject is become to the development and application of lepidolite.
Yichuan city tantalum niobium lithium mine is the tantalum niobium lithium mine of current Fia, and tantalum niobium lithium resource is abundant, two in lepidolite
Lithium content is aoxidized up to 4.5%, there is extraction lithium carbonate resources advantage condition.Therefore lithium carbonate is extracted by raw material of lepidolite
With broader market prospects and preferable economic benefit.
From the point of view of current existing production technology, the production yield of lithium carbonate is not satisfactory, and comprehensive productivity effect is not high, throws
Enter and output ratio deficiency, it is difficult to realize industrialized production.The preparation of lithium carbonate extracts method by raw material of lepidolite at present,
Mainly there are sulfuric acid process or potassium sulfate calcining connection, because of potassium sulfate calcination method, its potassium sulfate consumption is excessive, and energy consumption is high,
Material circulation is big, and the lithium rate of recovery is low, thus causes to prepare that lithium carbonate, the product cost of lithium sulfate are excessively high, and sulfuric acid process is using dense
Sulfuric acid and lepidolite ore high-temperature roasting, carbonate sinker, same high energy consumption, and environmental pollution influence greatly, especially the row of exhaust gas
It puts larger, larger pressure is caused to environment.
Invention content：The present invention seeks to provide a kind of method of lepidolite calcined by rotary kiln lithium carbonate, with lepidolite
It is with natural gas using calcining and water soaking method, including calcining, water logging, filtering, separation, freezing sinker lithium carbonate for raw material
Fuel, utilization rate of equipment and installations is high, and environmentally friendly three waste discharge is small, the low method for preparing lithium carbonate of production cost.
The present invention discloses a kind of method of lepidolite calcined by rotary kiln lithium carbonate, using lepidolite as raw material, using calcining
And water soaking method, including calcining, water logging, filtering, separation, freezing sinker lithium carbonate, it includes following method and step to be：
The calcining is to be calcined together to lepidolite raw material and auxiliary material using calcined by rotary kiln device, including following technique walks
Suddenly, 1）Lepidolite is crushed to 200-300 mesh, is lepidolite powder,
2）Lepidolite powder is uniformly mixed together with auxiliary material to roast raw material, the mass ratio for controlling lepidolite powder and auxiliary material is
60-70：40-30；
3）Roasting raw material are placed in calcined by rotary kiln device, carry out calcining as calcining material, the control calcined by rotary kiln time is 40-
60 minutes, control calcination temperature was 820-920 DEG C.
The auxiliary material is the mixing of potassium sulfate, calcium sulfate, lime stone three；Control lepidolite and auxiliary material each component quality hundred
Divide than being lepidolite 65-68 wt%, potassium sulfate 12-15wt%, calcium sulfate 16-18 wt%, lime stone 2-4 wt%.
The calcining uses natural gas for the energy, and it is 230-280 cubic metres of natural gases that lepidolite energy consumption per ton is calcined in control；
It controls calcined by rotary kiln and absorbs again discharge outward by cyclone dust collection, bag collection, scrubbing tower into generated flue gas.
Preferably, be the water logging be will calcine material and water using wet ball-milling leach, control water extraction time for 2-3 it is small
When, it is separated by filtration removing filter residue, to contain Li+Water-leach liquor, control calcining material and water solid-liquid mass ratio are 0.8-1：1.
Further, it is that the freezing sinker includes the following steps：（1）Freezing, is that will contain Li+Water-leach liquor is stirring
Under, -30~40 DEG C are cooled to, after isolating solid rubidium, caesium, arcanite, is separated by filtration, filter residue is washed, filtrate is recovered as mother liquor；
（2）It neutralizes, is that calcium hydroxide emulsion is added into mother liquor, obtains the solid, liquid mixed solution of neutralization reaction, filter, filter must be recycled
Liquid；（3）Concentration, is that will recycle filtrate to be evaporated concentration, obtains Li+The concentrate solution of a concentration of 15-30g/l；（4）Sinker carbon
Sour lithium, carbon dioxide gas is filled with into concentrate solution, and sinker reacts 60-80 minutes at a temperature of 80-95 DEG C, then filter,
It is mechanically decoupled to obtain lithium carbonate crude product, then be rinsed with water, drying prepares lithium carbonate product, and filtrate recycles through processing.
The calcining is to control the draw ratio of kiln as 15-18, and the slewing rate for controlling rotary kiln is 0.27-2.75
Rev/min.
Preferably, be the freezing it is secondary freezing, it is primary to freeze, it is that will contain Li+Water-leach liquor under stiring, cools down
To -5~40 DEG C, after isolating solid rubidium, caesium, arcanite, it is separated by filtration, obtains separating filtrate；Separating filtrate is carried out again secondary cold
Freeze, is that separating filtrate is cooled to -8~-30 DEG C under stiring, isolates solid potassium, rubidium, cesium alum, filtrate is recovered as mother liquor.
A kind of method of lepidolite calcined by rotary kiln lithium carbonate of the present invention, using lepidolite as raw material, using calcining and water
Leaching method, including calcining, water logging, filtering, separation, freezing sinker lithium carbonate, using net gas as energy in calcination process
Source, to the method that existing kiln calcines lithium processed, though that is, sulfate rotary kiln baking lepidolite extraction lithium technique is industrial at present
There is application, but yield is smaller, only thousands of tons of, chief reason are exactly that stove cannot steady and sustained life to annual output
Production, frequent occurrence raw material and knot kiln the phenomenon that.Sulfuric acid potassium application rate is larger, and cost is accordingly also high.Calcined by rotary kiln carbon of the present invention
The method of sour lithium by controlling the quality proportioning of lepidolite raw material and auxiliary material potassium sulfate, calcium sulfate and lime stone, while using day
Right gas not will produce knot kiln as the energy, when so as to effectively prevent lepidolite raw material from being calcined in rotary kiln with auxiliary material and go out
The case where existing raw material, occurs.The material after calcined by rotary kiln is with water extract technology simultaneously, is to be leached with water, and show
Roasting material usually only has 1-1.1% or so containing lithium caused by some lepidolite rotary kiln bakings, routinely liquid-solid ratio 3:1 soaks
The leachate gone out only has 3 grams per liters or so containing lithium, thus the amount containing lithium in leachate is too low, comes to subsequent production lithium carbonate
It says that concentration is too low, thus liquid-solid ratio must be reduced, be desirable to reach 12 grams per liters or more, that is to say, that liquid can be only achieved admittedly
It is more than 12 grams per liters.The present invention uses wet ball-milling extract technology, to increase substantially the content of the lithium in leachate, and
Its leached mud can be used as the raw material of construction material because being water logging being general solid slag, and lepidolite energy consumption per ton is
230-280 cubic metres of natural gases, have saved combustion gas resource, and rotary kiln flue gas is inhaled by cyclone dust collection, bag collection, scrubbing tower
It receives, it can qualified discharge.Operating process simultaneously is stablized, with short production cycle, and utilization rate of equipment and installations is high, and production cost is low, and three waste discharge is few,
The small production method of effect on environment.
A kind of method of lepidolite calcined by rotary kiln lithium carbonate of the present invention is using calcining and water soaking method, leached mud
General solid slag, the raw material that can be used as construction material use, and considerably reduce its production cost.
Purity is up to 99.0% or more after testing for the lithium carbonate prepared using the method for the present invention, product each the relevant technologies after testing
Index such as table 1
| Li2CO3 | 99.2% |
| Na+ | 0.028% |
| K+ | 0.002% |
| Fe3+ | 0.0018% |
| Ca2+ | 0.006% |
| Mg2+ | 0.003% |
| SO4 2- | 0.06% |
| Cl- | 0.007% |
| Cu2+ | 0.002% |
| Si | 0.007% |
In production process of the present invention, the main chemical reactions equation that is related to：
Li2O+H2SO4→Li2SO4+H2O
K2O+H2SO4→K2SO4+H2O
Na2O+H2SO4→Na2SO4+H2O
Li2SO4+Ca(OH)2→2LiOH+CaSO4
2LiOH+CO3+H2O→LiCO3 。
Specific implementation mode：
With reference to specific embodiment, the present invention is described in further detail.
Concentration involved in 1 embodiment of embodiment is mass concentration
（1）Lepidolite lepidolite powder is crushed, lepidolite is crushed to 200-300 mesh, is placed in reaction unit, raw material lithium cloud
Main chemical compositions such as following table in female powder, surplus is fluorine（wt%）
| Li2O | K2O+ Na2O | Al2O3 | SiO2 | Fe2O3 | Rb2O | Cs2O |
| 4.3% | 10.56% | 24.10% | 54.34% | 0.29% | 1.63% | 0.28% |
(2) system roasting raw material：Lepidolite powder and auxiliary material that above-mentioned mass component forms are mixed into roasting by certain mass ratio
Raw material.
（3）Raw material calcined by rotary kiln system calcining material is roasted,
Calcining is 15-18 using the draw ratio of kiln, that is, uses 4 × 60 meters and 4 × 72 meters of rotary kilns productions, and control
The slewing rate of rotary kiln is 0.27-2.75 revs/min.Slewing rate by controlling rotary kiln can reach when identical
The interior calcining increased to calcining material keeps the calcining of calcining material more abundant, and the slewing rate of rotary kiln is 0.27-2.75 revs/min
Within its rotate it is more existing it is slow more than half.
The process conditions that the present embodiment this step uses are：
67 wt% of raw material lepidolite,
It is potassium sulfate 13wt%, 17 wt% of calcium sulfate, 3 wt% of lime stone with auxiliary material；
The calcined by rotary kiln time is 40-60 minutes,
Calcination temperature is 820-920 DEG C；The calcining material obtained after being calcined is gone out with water logging,
It is 0.8 that control water logging, which goes out solid, liquid mass ratio,:1；
Calcining uses natural gas for the energy, and it is 230-280 cubic metres of natural gases that lepidolite energy consumption per ton is calcined in control；Control revolution
Kiln is calcined into generated flue gas absorbs again discharge outward by cyclone dust collection, bag collection, scrubbing tower；
4) water logging, filtering, separation, freezing sinker lithium carbonate,
Water logging is by 3）Step calcining material and water are leached using wet ball-milling, and control water extraction time is 2-3 hours, is separated by filtration
Filter residue is removed, to contain Li+Water-leach liquor, control calcining material and water solid-liquid mass ratio are 0.8：1；Control contains Li simultaneously+Water-leach liquor
In Li+Concentration is in 12g/l or more；
Separation：Separation can carry out separating treatment by existing method, and separation can be also carried out by following technique will contain Li+Water
Leachate washs the solid isolated with the hot water that temperature is 80 DEG C in separation process, and cleaning solution enters mother liquor tank, for mother
Liquid；
Freezing sinker includes the following steps：（1）Freezing, it is primary to freeze using secondary freezing, it is that will contain Li+Water-leach liquor is stirring
It mixes down, is cooled to -5~40 DEG C, after isolating solid rubidium, caesium, arcanite, be separated by filtration, obtain separating filtrate；Again to separating filtrate into
The secondary freezing of row, is that separating filtrate is cooled to -8~-30 DEG C under stiring, isolates solid potassium, rubidium, cesium alum, filtrate recycling
For mother liquor；
（2）It neutralizes, is that calcium hydroxide emulsion is added into mother liquor, obtains the solid, liquid mixed solution of neutralization reaction, filter, must recycle
Filtrate；（3）Concentration, is that will recycle filtrate to be evaporated concentration, obtains Li+The concentrate solution of a concentration of 15-30g/l；（4）Sinker system
Lithium carbonate is filled with carbon dioxide gas into concentrate solution, and sinker reacts 70 minutes at a temperature of 80-95 DEG C, then filters, machine
Tool detaches to obtain lithium carbonate crude product, then is rinsed with water, and drying prepares lithium carbonate product, and flushing water is recycled through processing.
It should be noted that：The above above-mentioned technical solution disclosed in this invention, it is non-that it is limited；Although with reference to aforementioned
Invention is explained in detail for each embodiment, it will be understood by those of ordinary skill in the art that：It still can be to preceding
It states the technical solution recorded in each embodiment to modify, either which part or all technical features is equally replaced
It changes；And these modifications or replacements, the model for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution
It encloses, should all cover in the claim of the present invention and the range of specification.
Claims (7)
1. a kind of method of lepidolite calcined by rotary kiln lithium carbonate, using lepidolite as raw material, using calcining and water soaking method, packet
Calcining, water logging, filtering, separation, freezing sinker lithium carbonate are included, it is characterized in that：
The calcining is to be calcined together to lepidolite raw material and auxiliary material using calcined by rotary kiln device, including following technique walks
Suddenly, 1）Lepidolite is crushed to 200-300 mesh, is lepidolite powder,
2）Lepidolite powder is uniformly mixed together with auxiliary material to roast raw material, the mass ratio for controlling lepidolite powder and auxiliary material is
60-70：40-30；
3）Roasting raw material are placed in calcined by rotary kiln device, carry out calcining as calcining material, the control calcined by rotary kiln time is 40-
60 minutes, control calcination temperature was 820-920 DEG C.
2. a kind of method of lepidolite calcined by rotary kiln lithium carbonate according to claim 1, it is characterized in that the auxiliary material is
The mixing of potassium sulfate, calcium sulfate, lime stone three；It is lepidolite 65-68 to control lepidolite and auxiliary material each component mass percent
Wt%, potassium sulfate 12-14wt%, calcium sulfate 16-18 wt%, lime stone 2-4 wt%.
3. a kind of method of lepidolite calcined by rotary kiln lithium carbonate according to claim 1, it is characterized in that the calcining is adopted
It is the energy with natural gas, it is 230-280 cubic metres of natural gases that lepidolite energy consumption per ton is calcined in control；Calcined by rotary kiln is controlled into institute
The flue gas of generation absorbs again discharge outward by cyclone dust collection, bag collection, scrubbing tower.
4. a kind of method of lepidolite calcined by rotary kiln lithium carbonate according to claim 1, it is characterized in that the water logging is
Calcining material and water are leached using wet ball-milling, control water extraction time is 2-3 hours, removing filter residue is separated by filtration, to contain
Li+The solid-liquid mass ratio of water-leach liquor, control calcining material and water is 0.8-1：1.
5. a kind of method of lepidolite calcined by rotary kiln lithium carbonate according to claim 1, it is characterized in that the freezing is heavy
Lithium includes the following steps：（1）Freezing, is that will contain Li+Water-leach liquor under stiring, is cooled to -30~40 DEG C, isolates solid
It after rubidium, caesium, arcanite, is separated by filtration, washs filter residue, filtrate is recovered as mother liquor；（2）It neutralizes, is that calcium hydroxide is added into mother liquor
Lotion obtains the solid, liquid mixed solution of neutralization reaction, and filtering must recycle filtrate；（3）Concentration, is that will recycle filtrate to be evaporated
Concentration, obtains Li+The concentrate solution of a concentration of 15-30g/l；（4）Sinker lithium carbonate, carbon dioxide gas is filled with into concentrate solution
Body, sinker reacts 60-80 minute at a temperature of 80-95 DEG C, then filtering, it is mechanically decoupled obtain lithium carbonate crude product, then be rinsed with water,
Drying prepares lithium carbonate product, and filtrate recycles through processing.
6. according to a kind of method of lepidolite calcined by rotary kiln lithium carbonate of claim 1 or 3, it is characterized in that the calcining
It is to control the draw ratio of kiln as 15-18, the slewing rate for controlling rotary kiln is 0.27-2.75 revs/min.
7. according to a kind of method of lepidolite calcined by rotary kiln lithium carbonate of claim 1 or 5, it is characterized in that the freezing
It is primary to freeze for secondary freezing, it is that will contain Li+Water-leach liquor under stiring, is cooled to -5~40 DEG C, isolate solid rubidium, caesium,
It after arcanite, is separated by filtration, obtains separating filtrate；Secondary freezing is carried out to separating filtrate again, is that separating filtrate cools down under stiring
To -8~-30 DEG C, solid potassium, rubidium, cesium alum are isolated, filtrate is recovered as mother liquor.
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Cited By (8)
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|---|---|---|---|---|
| CN109019643A (en) * | 2018-10-11 | 2018-12-18 | 江西安德力高新科技有限公司 | A kind of technique that montebrasite extracts lithium salts |
| CN109896539A (en) * | 2018-10-19 | 2019-06-18 | 辽宁旭日新能源科技有限公司 | A kind of preparation method of lithium carbonate |
| CN110342551A (en) * | 2019-08-27 | 2019-10-18 | 江西安德力高新科技有限公司 | It is a kind of using lepidolite as the lithium carbonate production system of raw material |
| CN110885090A (en) * | 2019-12-31 | 2020-03-17 | 江西南氏锂电新材料有限公司 | Method for preparing battery-grade lithium carbonate by using lepidolite as raw material through one-step method |
| CN110923452A (en) * | 2019-11-11 | 2020-03-27 | 中南大学 | Process for recovering potassium and sodium salts from lithium-precipitated liquid of lepidolite by using ethanol |
| CN112374512A (en) * | 2020-11-12 | 2021-02-19 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by removing impurities from lepidolite clinker |
| CN113636579A (en) * | 2021-09-10 | 2021-11-12 | 宜春银锂新能源有限责任公司 | Process for preparing lithium carbonate by novel lepidolite sulfate roasting method |
| CN116119691A (en) * | 2023-02-20 | 2023-05-16 | 国发新能源科技(江门)有限公司 | Method for preparing lithium carbonate by lepidolite roller kiln calcination |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019643A (en) * | 2018-10-11 | 2018-12-18 | 江西安德力高新科技有限公司 | A kind of technique that montebrasite extracts lithium salts |
| CN109896539A (en) * | 2018-10-19 | 2019-06-18 | 辽宁旭日新能源科技有限公司 | A kind of preparation method of lithium carbonate |
| CN110342551A (en) * | 2019-08-27 | 2019-10-18 | 江西安德力高新科技有限公司 | It is a kind of using lepidolite as the lithium carbonate production system of raw material |
| CN110342551B (en) * | 2019-08-27 | 2022-02-18 | 江西金德锂新能源科技有限公司 | Lithium carbonate production system using lepidolite as raw material |
| CN110923452A (en) * | 2019-11-11 | 2020-03-27 | 中南大学 | Process for recovering potassium and sodium salts from lithium-precipitated liquid of lepidolite by using ethanol |
| CN110885090A (en) * | 2019-12-31 | 2020-03-17 | 江西南氏锂电新材料有限公司 | Method for preparing battery-grade lithium carbonate by using lepidolite as raw material through one-step method |
| CN112374512A (en) * | 2020-11-12 | 2021-02-19 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by removing impurities from lepidolite clinker |
| CN113636579A (en) * | 2021-09-10 | 2021-11-12 | 宜春银锂新能源有限责任公司 | Process for preparing lithium carbonate by novel lepidolite sulfate roasting method |
| CN116119691A (en) * | 2023-02-20 | 2023-05-16 | 国发新能源科技(江门)有限公司 | Method for preparing lithium carbonate by lepidolite roller kiln calcination |
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