CN106636615B - The mica treatment process of lithium carbonate is prepared using lepidolite - Google Patents
The mica treatment process of lithium carbonate is prepared using lepidolite Download PDFInfo
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- CN106636615B CN106636615B CN201611248243.2A CN201611248243A CN106636615B CN 106636615 B CN106636615 B CN 106636615B CN 201611248243 A CN201611248243 A CN 201611248243A CN 106636615 B CN106636615 B CN 106636615B
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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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- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a kind of mica treatment process preparing lithium carbonate using lepidolite, lepidolite is put under high-temperature pressure in reaction kettle by a certain percentage with dilute sulfuric acid to react；The silica sand byproduct that slurry after reaction is added after the drying of workshop carries out spice；Powder after spice enters kiln and roasting is dried；Material after roasting directly adds water to carry out leaching reaction at a certain temperature；Slurry after leaching prepares battery-level lithium carbonate and industrial level lithium carbonate by crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology.It is an advantage of the invention that：The technique can reduce 35% or more than prior art gypsum by-product, and the quality of the larger raising of lithium carbonate overall recovery, lithium carbonate is slightly promoted than existing product quality, and each index can be up to state standards；Solves the problems, such as kiln knot wall after the white residue spice that slurry after acidleach is added after the drying of workshop.
Description
Technical field
The present invention relates to a kind of processing methods of mineral raw material, are prepared at the mica of lithium carbonate in particular with lepidolite
Science and engineering skill.
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, the common issue that new energy is the world is developed and used, lithium electricity new energy is as new energy
One of important industry of development is increasingly paid attention to by various countries；Therefore the comprehensive exploitation of lepidolite raw material is become with application and is worked as
Modern heat subject.
Chinese Yichuan Ta Nb tailings are tantalum niobium lithium mine albite granite mineral deposit and the China YouSe of current Fia
Multi-metallic minerals belonging to metal industry parent company pick up one of mine resources base, and Yichuan Ta Nb tailings contain abundant rare
Metal material, such as tantalum, niobium, lithium, rubidium, caesium, potassium, sodium.Lepidolite is the obtained byproduct of Ta Nb tailings flotation, and annual output can
Reach 200,000 tons or more.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 value and strategic importance.
Wherein：Lithium and its esters are the basic materials of lithium electricity new energy, be described as by scientist " industrial monosodium glutamate, the energy it
Star " is the preferred materials for producing lithium ion battery, is the important meals for developing new energy, 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
Small, safe and reliable feature, price are only the 1/5 of now lithium ion battery, will be used for electric vehicle.
In the existing lithium carbonate production technology of company higher, the by-product that with respect to spodumene and salt lake bittern carries lithium technology production cost
Product are more, lack industry competition advantage.This technology is intended to develop a kind of front end pretreating process of lepidolite, lithium cloud is not being influenced
In mother under the premise of the leaching rate of valuable metal, reduces the by-product volume of subsequent handling and improve the rate of recovery of lithium carbonate, reduce
The production cost of lithium carbonate.
Invention content
The purpose of the present invention is to provide the mica treatment process for preparing lithium carbonate using lepidolite, before a kind of lepidolite
End pretreating process reduces the by-product volume of subsequent handling under the premise of the leaching rate of valuable metal in not influencing lepidolite
And the rate of recovery of lithium carbonate is improved, reduce the production cost of lithium carbonate.
The technical solution adopted by the present invention is as follows：The mica treatment process of lithium carbonate is prepared using lepidolite, feature exists
In：
（1）Lepidolite is put under high-temperature pressure in reaction kettle by a certain percentage with dilute sulfuric acid to react；
（2）The silica sand byproduct that slurry after reaction is added after the drying of workshop carries out spice；
（3）Powder after spice enters kiln and roasting is dried；
（3）Material after roasting directly adds water to carry out leaching reaction at a certain temperature；
（4）Slurry after leaching is by crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology system
Standby battery-level lithium carbonate and industrial level lithium carbonate.
Step of the present invention（1）A concentration of 35wt%~55wt% of dilute sulfuric acid.
Step of the present invention（1）It is 1 that lepidolite, which is by solid-liquid mass ratio with dilute sulfuric acid certain proportion,: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）Calcination 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）A certain proportion of gypsum wash water is first mended in neutralization reaction kettle to the slurry centrifuged out；
（2）First add calcium carbonate to adjust pH value to 3-4 in neutralization reaction kettle, then lime is added to adjust pH value to 8-9；
（3）The flow of control blanking flow and wash water after adjusting pH value；
（3）The filtered gypsum of band filter enters vertical type squeezer after being starched again by certain solid-to-liquid ratio and carries out latter step journey
Sequence.
Its advantage is that：Neutralization step together with will being with program integration in two before, reduces one section of neutralization step；2、
L i2O contents are reduced to 0.2-0.4% by 0.7-1.0% before in gypsum, and produce control and relatively stablize, and workshop lithium carbonate returns
Yield improves 5% or more.
Step of the present invention（4）The wash water after wash water and neutralization removal of impurities after middle centrifugation is all to enter dirt after handling
Water factory does not carry out recycling to lithium therein, causes larger lithium loss and economic loss；Recycling cycle profit is carried out to wash water
It is with, the step of improving the rate of recovery of lithium carbonate, creating additional economic benefit：
（1）The wash water centralized collection after wash water and neutralization removal of impurities after centrifugation；
（2）Wash water after centralized collection is first passed through to squeeze into plate and frame filter press again after settling and be 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 improves the lithium rate of recovery.
Step of the present invention（4）3 countercurrent washings are carried out to the solid slag isolated after middle centrifugation, it is solid after washing
State slag is discharged, and experiment shows that 170kg butt solid slags can about be generated by often producing one ton of lithium carbonate, detected in the solid slag through chemical examination and contained
Li20 is 0.3%, the main contents of CaCO3 90% or more.Solid slag is used in neutralization removal of impurities process by the present invention, is reduced raw material and is thrown
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 the carbon steel surge tank of a 6m3, press filtration first to be sent to surge tank with belt capsule；
（3）Water stirring is added to size mixing by certain solid-to-liquid ratio in surge tank；
（4）Slurry pump after sizing mixing is squeezed into neutralization removal of impurities process and is recycled.
Advantage is：The solid slag that removal of impurities generates can all be used to neutralize removal of impurities process and be used instead of part calcium carbonate raw material；In
It is all recycled with the lithium in removal of impurities, improves the rate of recovery of lithium carbonate.
Step of the present invention（1）In to ensure the extraction rate of acidleach workshop section 95% or more, acid-leaching reaction kettle need to close pressure one
It fixes time, closes after pressure due to there is the generation of HF gases in reaction kettle, can seal and stir generation corrosion to the machine of reaction kettle, lead to equipment
Service life is short, need to repair at regular intervals；Main reaction process is changed to synthesis under normal pressure, reduces the repair frequency of reaction kettle
Rate improves safe operating factor, improves production efficiency.Advantage：1, operating procedure is less, suitably reduces the workload of employee,
Synthesis under normal pressure can carry out workshop volume production；2, reaction condition milder, safer after being changed to synthesis under normal pressure；3, reduce reaction
Corrosion of the HF of generation to reaction kettle, extends service life of equipment.Accordingly reduce maintenance of equipment expense, that improves equipment has
The working time is imitated, reaction kettle frequency of maintenance is greatly lowered；4, reduce sulfuric acid 110-130kg per kettle material；5, rate of water make-up after reacting
It increases, reduces the sour water treating capacity for the white residue filter cloth wash water that need to be handled；6, the extraction rate of mica is improved；The extraction rate of mica
1-2% is improved, 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, the fluorine gas separated from lepidolite raw material is collected, stopping heating no longer being escaped to control the fluorine gas in lepidolite raw material
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, the 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 when the calcining of lepidolite, lithium
The bulkiness of mica material increases, and temperature is rapidly reached 1500 DEG C or more by this technology, until lepidolite lamellar structure is opened
The high temperature that one times or so of required temperature can make the lamellar structure of lepidolite be opened rapidly.Since lithium exists at high operating temperatures
Easily separate out, the leaching for the lithium that is highly advantageous under weakly acidic condition, significantly shortens the reaction time, in lepidolite raw material
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 for improving rare metal raw material in lepidolite raw material, reduces energy consumption, when shortening reaction
Between and acid-base raw materials consumption dosage.The technique can reduce 35% or more than prior art gypsum by-product, and lithium carbonate always recycles
The quality of the larger raising of rate, lithium carbonate is slightly promoted than existing product quality, and each index can be up to state standards；After acidleach
Solves the problems, such as kiln knot wall after the white residue spice that slurry is added after the drying of workshop.
Specific implementation mode
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 roasting → material adds water extraction → crystallisation by cooling → centrifugation → neutralization removal of impurities → evaporation and concentration → sinker.
Specific method is：The mica treatment process of lithium carbonate is prepared using lepidolite, it is characterised in that：
（1）Lepidolite is put under high-temperature pressure in reaction kettle by a certain percentage with dilute sulfuric acid to react；Dilute sulfuric acid it is dense
Degree is 35wt%~55wt%, and it is 1 that lepidolite, which is by solid-liquid mass ratio with dilute sulfuric acid certain proportion,:3-4；The temperature of high temperature is
1600-1900℃；Reaction a period of time is 45-75 minutes；
（2）The silica sand byproduct that slurry after reaction is added after the drying of workshop carries out spice；Slurry and silica sand byproduct are mixed
Material is than being 5-10:1；
（3）Powder after spice enters kiln and roasting is dried；Calcination temperature is 150-300 DEG C in kiln, and the time is
30-50 minutes；
（3）Material after roasting directly adds water to carry out leaching reaction at a certain temperature；
（4）Slurry after leaching is by crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology system
Standby battery-level lithium carbonate and industrial level lithium carbonate.
Crystallisation by cooling：Slurry obtained by upper step is injected in refrigerated cylinder, under ceaselessly stirring condition, temperature is down to 0~
- 50 DEG C are isolated solid arcanite and washing lotion, and washing lotion returns in mother liquor tank, to washing lotion plus water, heat temperature raising, crystallized preparation, and
It is separated off rubidium, caesium, arcanite, it is mother liquor 1 to separate the filtrate after solid rubidium, caesium, arcanite.
It centrifuges；Mother liquor 1 after leaching is detached, 3 countercurrent washings, washing are carried out to the solid slag isolated
Solid slag is discharged afterwards, and makes in the reaction kettle that wash water returns to pressure leaching process, and remaining slurry carries out neutralizing removal of impurities reaction in next step.
Neutralize removal of impurities：（1）A certain proportion of gypsum wash water is first mended in neutralization reaction kettle to the slurry centrifuged out；
（2）First add calcium carbonate to adjust pH value to 3-4 in neutralization reaction kettle, then lime is added to adjust pH value to 8-9；（3）After adjusting pH value
Control the flow of blanking flow and wash water；（3）The filtered gypsum of band filter enters vertical after being starched again by certain solid-to-liquid ratio
Squeezer carries out latter step program.
Sinker；Removal of impurities is neutralized after evaporation and concentration, obtains the solution containing Li+；Sinker is passed through to the solution containing Li+
Carbon dioxide gas or carbonate can prepare lithium carbonate；Sulfate i.e. preparation is added and carries lithium sulfate product.Using present invention side
Method improves up to 50% or more the recovery rate of lithium in lepidolite raw material.Also improve the resource utilization to lepidolite raw material.
It is of the present invention neutralize removal of impurities principle be：Existing neutralization workshop section is divided into neutralization 1, neutralizes 2, neutralizes 3 works
Sequence, flow it is longer and neutralize generate gypsum in Li2O contents it is higher.Experiment finds that the workshop section can be by three processes before
Parameters, the Li2O that can be reduced in gypsum such as two processes, and moisturizing, pH value, leaching requirement by controlling reaction is adjusted to contain
Amount.This project be intended to neutralize workshop section carry out technology Modification, for existing workshop technological transformation design provide more optimized process conditions,
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 facilitate the understanding of the method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvement and modification are also fallen within the protection scope of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to 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, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (5)
1. preparing the mica treatment process of lithium carbonate using lepidolite, it is characterised in that：
（1）Lepidolite is put under high-temperature pressure in reaction kettle by a certain percentage with dilute sulfuric acid to react；
（2）The silica sand byproduct that slurry after reaction is added after the drying of workshop carries out spice；
（3）Powder after spice enters kiln and roasting is dried；
（4）Material after roasting directly adds water to carry out leaching reaction at a certain temperature；
（5）Slurry after leaching prepares electricity by crystallisation by cooling, centrifugation, neutralization removal of impurities, evaporation and concentration, sinker production technology
Pond level lithium carbonate or industrial level lithium carbonate；
The step（1）A concentration of 35wt%~55wt% of dilute sulfuric acid；
The step（1）It is 1 that lepidolite, which is by solid-liquid mass ratio with dilute sulfuric acid certain proportion,:3-4；
The step（1）The temperature of high temperature is 1600-1900 DEG C；
The step（1）Reaction a period of time is 45-75 minutes；
The step（5）Neutralizing removal step is：
（1）A certain proportion of gypsum wash water is first mended in neutralization reaction kettle to the slurry centrifuged out；
（2）First add calcium carbonate to adjust pH value to 3-4 in neutralization reaction kettle, then lime is added to adjust pH value to 8-9；
（3）The flow of control blanking flow and wash water after adjusting pH value；
（4）The filtered gypsum of band filter enters vertical type squeezer after being starched again by certain solid-to-liquid ratio and carries out latter step program.
2. the mica treatment process of lithium carbonate is prepared using lepidolite according to claim 1, it is characterised in that：The step
（2）Middle slurry and silica sand byproduct spice ratio are 5-10:1.
3. the mica treatment process of lithium carbonate is prepared using lepidolite according to claim 1, it is characterised in that：The step
（3）Calcination temperature is 150-300 DEG C in kiln, and the time is 30-50 minutes.
4. the mica treatment process of lithium carbonate is prepared using lepidolite according to claim 1, it is characterised in that：The step
（5）Wash water after middle centrifugation and the step of neutralizing the wash water recycling after removal of impurities be：
（1）The wash water centralized collection after wash water and neutralization removal of impurities after centrifugation；
（2）Wash water after centralized collection is first passed through to squeeze into plate and frame filter press again after settling and be squeezed；
（3）Clear liquid after squeezing is used as band machine gypsum wash water；
（4）Reduce the discharge of filter cloth wash water and improves the lithium rate of recovery.
5. the mica treatment process of lithium carbonate is prepared using lepidolite according to claim 1, it is characterised in that：The step
（5）The solid slag isolated is used in neutralization removal of impurities process after middle centrifugation, raw material input cost is reduced and improves carbon
The sour lithium rate of recovery, step are：
（1）Plate compression is first passed through after removal of impurities bucket removal of impurities；
（2）Increase a 6m3Carbon steel surge tank, the solid slag after press filtration first sent with belt capsule to surge tank；
（3）Water stirring is added to size mixing by certain solid-to-liquid ratio in surge tank；
（4）Slurry pump after sizing mixing is squeezed into neutralization removal of impurities process and is recycled.
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| 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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| CN102295303B (en) * | 2011-08-08 | 2013-09-04 | 江西本源新材料科技有限公司 | Extraction method of lithium carbonate |
| CN103014317B (en) * | 2012-12-04 | 2015-02-11 | 宜春银锂新能源有限责任公司 | Method for extracting lithium salt from lepidolite |
| CN103145158B (en) * | 2013-02-28 | 2014-11-05 | 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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