CN106636615A - Mica treatment process for preparing lithium carbonate by utilizing lepidolite - Google Patents
Mica treatment process for preparing lithium carbonate by utilizing lepidolite Download PDFInfo
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- CN106636615A CN106636615A CN201611248243.2A CN201611248243A CN106636615A CN 106636615 A CN106636615 A CN 106636615A CN 201611248243 A CN201611248243 A CN 201611248243A CN 106636615 A CN106636615 A CN 106636615A
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- 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
- C22B1/06—Sulfating roasting
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- 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
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- 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
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- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- 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
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Abstract
The invention discloses a mica treatment process for preparing lithium carbonate by utilizing lepidolite. The process comprises the following steps: putting lepidolite and diluted sulfuric acid into a reaction kettle in a certain ratio at high temperature and normal pressure to react; adding the reacted slurry into a silica sand byproduct which is dried in workshop, and mixing the materials; drying and roasting the mixed powder in a kiln; directly adding water into the roasted material to perform a leaching reaction at a certain temperature; performing cooling crystallization, centrifugal separation, neutralized impurity removal, evaporation concentration and lithium depositing production processes on the leached slurry to prepare battery grade lithium carbonate and industrial lithium carbonate. The process has the advantages that gypsum byproduct in the process can be reduced by more than or equal to 35 percent in comparison with that in the prior art, the overall recovery of lithium carbonate is greatly increased, the quality of lithium carbonate is slightly improved in comparison with that of existing products, and each index can reach the national standard; and the problem of material attachment of a kiln can be solved after the acid leached slurry is added into and mixed with the workshop dried silica slag.
Description
Technical field
The present invention relates to a kind of processing method of mineral raw material, in particular with lepidolite science and engineering at the mica of lithium carbonate is prepared
Skill.
Background technology
Lepidolite is a kind of important mineral resources, and it contains abundant Rare Metals Materials, lithium, sodium, potassium, rubidium, caesium, aluminium etc..
With the growing tension of world energy sources, common issue of the new forms of energy for the world is developed, lithium electricity new forms of energy are sent out as new forms of energy
One of important industry of exhibition, is increasingly paid attention to by various countries；Therefore the comprehensive exploitation and application to lepidolite raw material becomes current
Heat subject.
Chinese Yichuan Ta Nb tailings are the tantalum niobium lithium ore deposit albite granite mineral deposits of current Fia, are also China YouSe
One of multi-metallic minerals selecting and purchasing mine resources base belonging to metal industry parent company, Yichuan Ta Nb tailings contain abundant rare
Metal material, such as tantalum, niobium, lithium, rubidium, caesium, potassium, sodium.Lepidolite is the byproduct obtained by Ta Nb tailings flotation, and annual production can
Reach more than 200,000 tons.Its concentrate contains Li2O4.4%；Rb2O1.3%；Cs2O0.243%；Be carry lithium, rubidium, caesium it is important
The raw material of industry, it is developed and utilized with particularly significant economic worth and strategic importance.
Wherein：Lithium and its esters are the basic materials of lithium electricity new forms of energy, be described as by scientist " industrial monosodium glutamate, the energy it
Star ", is the preferred materials for producing lithium ion battery, is development new forms of energy, the important meals of new material.Lithium ion secondary in recent years
Battery is increased with average annual 20% development speed.The novel polymer lithium ion battery that the U.S. succeeds in developing recently has volume
Little, safe and reliable the characteristics of, its price only shows the 1/5 of lithium ion battery, will be used for electric automobile.
Higher, the by-product that carries lithium technology production cost in the relative spodumene of the existing lithium carbonate production technology of company and salt lake bittern
Product are more, lack industry competition advantage.This technology is intended to develop a kind of front end pretreating process of lepidolite, is not affecting lithium cloud
In mother on the premise of the leaching rate of valuable metal, the by-product volume of subsequent handling and the rate of recovery of raising lithium carbonate are reduced, reduced
The production cost of lithium carbonate.
The content of the invention
It is an object of the invention to provide preparing the mica handling process of lithium carbonate using lepidolite, a kind of front end of lepidolite is pre-
Handling process, in lepidolite is not affected on the premise of the leaching rate of valuable metal, reduces the by-product volume of subsequent handling and carries
The rate of recovery of high carbon acid lithium, reduces the production cost of lithium carbonate.
The technical solution used in the present invention is as follows：The mica handling process of lithium carbonate is prepared using lepidolite, its feature exists
In：
（1）Lepidolite puts into reaction kettle for reaction under high-temperature pressure by a certain percentage with dilute sulfuric acid；
（2）Reacted slurry adds the silica sand byproduct after the drying of workshop to carry out spice；
（3）Powder after spice is dried roasting into kiln；
（3）Material after roasting directly adds water the leaching reaction that carry out at a certain temperature；
（4）Slurry after leaching prepares electricity through crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology
Pond level lithium carbonate and industrial level lithium carbonate.
Step of the present invention（1）The concentration of dilute sulfuric acid is 35wt%～55wt%.
Step of the present invention（1）It by solid-liquid mass ratio is 1 that lepidolite and dilute sulfuric acid certain proportion are:3-4.
Step of the present invention（1）The temperature of high temperature is 1600-1900 DEG C.
Step of the present invention（1）Reaction a period of time is 45-75 minutes.
Step of the present invention（2）Middle slurry and silica sand byproduct spice ratio are 5-10:1.
Step of the present invention（3）Sintering temperature is 150-300 DEG C in kiln, and the time is 30-50 minutes.
Step of the present invention（4）Neutralizing removal step is：
（1）The slurry gone out to centrifugation first mends a certain proportion of gypsum wash water in neutralization reaction kettle；
（2）First add calcium carbonate to adjust pH value to 3-4 in neutralization reaction kettle, then add lime to adjust pH value to 8-9；
（3）Adjust the flow that blanking flow and wash water are controlled after pH value；
（3）Gypsum after band filter filtration carries out latter step program after starching again by certain solid-to-liquid ratio into vertical type squeezer.
Its advantage is：By in two roads before with program integration for together with neutralization step, reduce one section of neutralization step；2nd, gypsum
Middle L i2O contents are reduced to 0.2-0.4% by 0.7-1.0% before, and produce more stable, the rate of recovery of workshop lithium carbonate of control
Improve more than 5%.
Step of the present invention（4）The wash water after wash water and neutralization removal of impurities after middle centrifugation is all that dirt is entered after process
Water factory, does not carry out recycling to lithium therein, causes larger lithium and loses and economic loss；Wash water is carried out to reclaim circulation profit
With, the rate of recovery of lithium carbonate is improved, be the step of create extra economic benefit：
（1）The wash water centralized collection after wash water and neutralization removal of impurities after centrifugation；
（2）Wash water after centralized collection, first passes through to be squeezed in plate and frame filter press again after sedimentation and is squeezed；
（3）The stillness of night after squeezing is used as band machine gypsum wash water；
（4）Reduce the discharge of filter cloth wash water and improve the lithium rate of recovery.
Step of the present invention（4）Solid slag after middle centrifugation to isolating carries out 3 countercurrent washings, solid after washing
State slag is discharged, and experiment shows, often producing one ton of lithium carbonate can about produce 170kg butt solid slags, and Jing chemical examinations are detected and contained in the solid slag
Li20 is 0.3%, the main contents of CaCO3 more than 90%.The present invention is used in solid slag in neutralization removal of impurities operation, reduces raw material and throws
Enter cost and improve the lithium carbonate rate of recovery, step is：
（1）Plate compression is first passed through after removal of impurities bucket removal of impurities；
（2）Increase the solid slag after carbon steel surge tank, the press filtration of a 6m3 and first deliver to surge tank with belt capsule；
（3）Size mixing by the stirring that adds water of certain solid-to-liquid ratio in surge tank；
（4）Slurry pump after sizing mixing is squeezed into neutralization removal of impurities operation and is recycled.
Advantage is：The solid slag that removal of impurities is produced can all be used to neutralizing removal of impurities operation and replace part calcium carbonate raw material to use；In
All reclaimed with the lithium in removal of impurities, improve the rate of recovery of lithium carbonate.
Step of the present invention（1）In to ensure the extraction rate of acidleach workshop section more than 95%, acid-leaching reaction kettle need to close pressure one
Fix time, close due to there are HF gases to produce in reactor after pressure, generation corrosion can be sealed and stirred to the machine of reactor, cause equipment
Service life is short, need to be keeped in repair at set intervals；Main reaction process is changed to into synthesis under normal pressure, the maintenance frequency of reactor is reduced
Rate, improves APF, improve production efficiency.Advantage：1st, operating procedure is less, suitably reduces the workload of employee,
Synthesis under normal pressure can carry out workshop volume production；2nd, it is changed to after synthesis under normal pressure, it is reaction condition milder, safer；3rd, reaction is reduced
Corrosion of the HF of generation to reactor, extends service life of equipment.Maintenance of equipment expense is accordingly reduced, having for equipment is improved
The effect working time, reactor frequency of maintenance is greatly lowered；4th, sulfuric acid 110-130kg is reduced per kettle material；5th, rate of water make-up after reacting
Increase, reduce the sour water treating capacity of the white residue filter cloth wash water that need to be processed；6th, improve the extraction rate of mica；The extraction rate of mica
1-2% is improve, the output capacity of lithium carbonate has been correspondingly improved.
The present invention operation principle be：Lepidolite reacts in reaction unit, controlling reaction temperature be 1600-1900 DEG C it
Between, collect the fluorine gas separated from lepidolite raw material, to control lepidolite raw material in fluorine gas no longer escape stopping heating
Reaction, typical time is within 3 minutes；The lamellar structure of lepidolite raw material is opened, lithium separate out under acid environment；
Again by strong sulfuric acid response therein, its time is 20-60 minutes；Stirring is allowed to fully react to obtain slurry.
It is an advantage of the invention that：It is that the layer structure of the lepidolite at 800-950 DEG C is opened during the calcining of lepidolite, lithium
The bulkiness of mica material is increased, and temperature is rapidly reached more than 1500 DEG C, is opened to lepidolite lamellar structure by this technology
Temperature required one times or so of high temperature, the lamellar structure that can make lepidolite is opened rapidly.Because at high operating temperatures lithium exists
Easily separate out, the leaching of the lithium that is highly advantageous to, significantly shortens the reaction time, in lepidolite raw material under weakly acidic condition
Fluorine evaporates to form a weakly acidic environment, the extraction being highly advantageous in lepidolite raw material under the plasma condition of high temperature
Process.The extraction and application rate of rare metal raw material in lepidolite raw material is improve, energy resource consumption is reduced, when shortening reaction
Between, and the consumption consumption of acid-base raw materials.The technique can reduce more than 35% than existing process gypsum by-product, and lithium carbonate is always reclaimed
The larger raising of rate, the quality of lithium carbonate is slightly lifted than existing product quality, and each index can be up to state standards；After acidleach
Slurry to be added and solve the problems, such as that kiln ties wall after the white residue spice after the drying of workshop.
Specific embodiment
The technological process of production of the present invention is sketched：Lepidolite and concentrated sulfuric acid high-temperature calcination and fluorine removal → slurry → slurry drying → slurry
Material roasting → material adds water extraction → crystallisation by cooling → centrifugation → neutralization removal of impurities → evaporation and concentration → sinker.
Concrete grammar is：The mica handling process of lithium carbonate is prepared using lepidolite, it is characterised in that：
（1）Lepidolite puts into reaction kettle for reaction under high-temperature pressure by a certain percentage with dilute sulfuric acid；The concentration of dilute sulfuric acid is
35wt%～55wt%, it by solid-liquid mass ratio is 1 that lepidolite and dilute sulfuric acid certain proportion are:3-4；The temperature of high temperature is
1600-1900℃；Reaction a period of time is 45-75 minutes；
（2）Reacted slurry adds the silica sand byproduct after the drying of workshop to carry out spice；Slurry and silica sand byproduct spice ratio
For 5-10:1；
（3）Powder after spice is dried roasting into kiln；Sintering temperature is 150-300 DEG C in kiln, and the time is 30-50
Minute；
（3）Material after roasting directly adds water the leaching reaction that carry out at a certain temperature；
（4）Slurry after leaching prepares electricity through crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology
Pond level lithium carbonate and industrial level lithium carbonate.
Crystallisation by cooling：By upper step gained slurry, in injection refrigerated cylinder, under ceaselessly stirring condition, temperature is down to 0～
- 50 DEG C are isolated solid arcanite and washing lotion, and washing lotion is returned in mother liquor tank, washing lotion are added water, heat temperature raising, crystallized preparation, and
Rubidium, caesium, arcanite are separated off, the filtrate after solid rubidium, caesium, arcanite is separated for mother liquor 1.
Centrifugation；Mother liquor 1 after leaching is separated, the solid slag to isolating carries out 3 countercurrent washings, washed
Afterwards solid slag is discharged, and wash water is returned in the reactor of pressure leaching operation, and remaining slurry is carried out in next step and removal of impurities is reacted.
Neutralization removal of impurities：（1）The slurry gone out to centrifugation first mends a certain proportion of gypsum wash water in neutralization reaction kettle；
（2）First add calcium carbonate to adjust pH value to 3-4 in neutralization reaction kettle, then add lime to adjust pH value to 8-9；（3）After adjusting pH value
The flow of control blanking flow and wash water；（3）Gypsum after band filter filtration enters vertical after starching again by certain solid-to-liquid ratio
Squeezer carries out latter step program.
Sinker；Neutralization removal of impurities obtains the solution containing Li+ Jing after being concentrated by evaporation；Sinker, is passed through to the solution containing Li+
Lithium carbonate is prepared by carbon dioxide, or carbonate；Add sulfate to prepare and carry lithium sulfate product.Using present invention side
Method is improved up to more than 50% to the recovery rate of lithium in lepidolite raw material.Also improve the resource utilization to lepidolite raw material.
It is of the present invention neutralization removal of impurities principle be：Existing neutralization workshop section is divided into neutralization 1, neutralization 2,3 works of neutralization
Sequence, flow process it is longer and neutralize produce gypsum in Li2O contents it is higher.Experiment finds that the workshop section can be by three operations before
It is adjusted to two operations, and the parameter such as moisturizing, pH value, the leaching requirement by control reaction, the Li2O that can be reduced in gypsum contains
Amount.This project be intended to neutralize workshop section carry out technology Modification, for existing workshop technological transformation design provide the process conditions for more optimizing,
The equipment investment of reduction company project construction, reduces the production cost of lithium carbonate, improves the rate of recovery of lithium carbonate.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that right
For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out
Some improvement and modification, these are improved and modification is also fallen in the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
Various modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope for causing.
Claims (10)
1. the mica handling process of lithium carbonate is prepared using lepidolite, it is characterised in that：
（1）Lepidolite puts into reaction kettle for reaction under high-temperature pressure by a certain percentage with dilute sulfuric acid；
（2）Reacted slurry adds the silica sand byproduct after the drying of workshop to carry out spice；
（3）Powder after spice is dried roasting into kiln；
（3）Material after roasting directly adds water the leaching reaction that carry out at a certain temperature；
（4）Slurry after leaching prepares electricity through crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology
Pond level lithium carbonate and industrial level lithium carbonate.
2. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（1）The concentration of dilute sulfuric acid is 35wt%～55wt%.
3. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（1）It by solid-liquid mass ratio is 1 that lepidolite and dilute sulfuric acid certain proportion are:3-4.
4. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（1）The temperature of high temperature is 1600-1900 DEG C.
5. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（1）Reaction a period of time is 45-75 minutes.
6. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（2）Middle slurry and silica sand byproduct spice ratio are 5-10:1.
7. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（3）Sintering temperature is 150-300 DEG C in kiln, and the time is 30-50 minutes.
8. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（4）Neutralizing removal step is：
（1）The slurry gone out to centrifugation first mends a certain proportion of gypsum wash water in neutralization reaction kettle；
（2）First add calcium carbonate to adjust pH value to 3-4 in neutralization reaction kettle, then add lime to adjust pH value to 8-9；
（3）Adjust the flow that blanking flow and wash water are controlled after pH value；
（3）Gypsum after band filter filtration carries out latter step program after starching again by certain solid-to-liquid ratio into vertical type squeezer.
9. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
（4）The step of wash water after middle centrifugation and the wash water recycle and reuse after neutralization removal of impurities is：
（1）The wash water centralized collection after wash water and neutralization removal of impurities after centrifugation；
（2）Wash water after centralized collection, first passes through to be squeezed in plate and frame filter press again after sedimentation and is squeezed；
（3）The stillness of night after squeezing is used as band machine gypsum wash water；
（4）Reduce the discharge of filter cloth wash water and improve the lithium rate of recovery.
10. using lepidolite the mica handling process of lithium carbonate is prepared according to claim 1, it is characterised in that：The step
Suddenly（4）Solid slag after middle centrifugation to isolating is used in neutralization removal of impurities operation, is reduced raw material input cost and is improved
The lithium carbonate rate of recovery, step is：
（1）Plate compression is first passed through after removal of impurities bucket removal of impurities；
（2）Increase a 6m3Carbon steel surge tank, press filtration after solid slag first deliver to surge tank with belt capsule；
（3）Size mixing by the stirring that adds water of certain solid-to-liquid ratio in surge tank；
（4）Slurry pump after sizing mixing is squeezed into neutralization removal of impurities operation and is recycled.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106915754A (en) * | 2017-05-11 | 2017-07-04 | 江西南氏锂电新材料有限公司 | A kind of lithium carbonate extraction process based on lepidolite ore |
| CN108728671A (en) * | 2018-08-31 | 2018-11-02 | 江西海汇龙洲锂业有限公司 | It is a kind of to stir cleaning device convenient for lepidolite extracted lithium leaching solid material |
| CN110550644A (en) * | 2019-10-08 | 2019-12-10 | 河北铸合集团兴隆县矿业有限公司 | method for separating and extracting battery-grade lithium carbonate, rubidium and cesium salts from lepidolite |
| CN108728671B (en) * | 2018-08-31 | 2024-05-31 | 江西海汇龙洲锂业有限公司 | Stirring and washing device convenient for lepidolite lithium extraction and leaching of solid materials |
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| CN103145158A (en) * | 2013-02-28 | 2013-06-12 | 江西赣锋锂业股份有限公司 | Method for preparing lithium carbonate from lepidolite through sulfuric acid roasting method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106915754A (en) * | 2017-05-11 | 2017-07-04 | 江西南氏锂电新材料有限公司 | A kind of lithium carbonate extraction process based on lepidolite ore |
| CN106915754B (en) * | 2017-05-11 | 2018-03-09 | 江西南氏锂电新材料有限公司 | A kind of lithium carbonate extraction process based on lepidolite ore |
| CN108728671A (en) * | 2018-08-31 | 2018-11-02 | 江西海汇龙洲锂业有限公司 | It is a kind of to stir cleaning device convenient for lepidolite extracted lithium leaching solid material |
| CN108728671B (en) * | 2018-08-31 | 2024-05-31 | 江西海汇龙洲锂业有限公司 | Stirring and washing device convenient for lepidolite lithium extraction and leaching of solid materials |
| CN110550644A (en) * | 2019-10-08 | 2019-12-10 | 河北铸合集团兴隆县矿业有限公司 | method for separating and extracting battery-grade lithium carbonate, rubidium and cesium salts from lepidolite |
| CN110550644B (en) * | 2019-10-08 | 2021-10-12 | 河北铸合集团兴隆县矿业有限公司 | Method for separating and extracting battery-grade lithium carbonate, rubidium and cesium salts from lepidolite |
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|---|---|
| CN106636615B (en) | 2018-08-10 |
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