CN108570566A - The technique that lepidolite raw material Roasting And Leaching extracts lithium - Google Patents
The technique that lepidolite raw material Roasting And Leaching extracts lithium Download PDFInfo
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- CN108570566A CN108570566A CN201810488098.8A CN201810488098A CN108570566A CN 108570566 A CN108570566 A CN 108570566A CN 201810488098 A CN201810488098 A CN 201810488098A CN 108570566 A CN108570566 A CN 108570566A
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- lepidolite
- raw material
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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
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
-
- 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
Abstract
A kind of technique of lepidolite raw material Roasting And Leaching extraction lithium disclosed by the invention, acidleach processing is first carried out using lepidolite is used, then the process calcined again, before this by eliminating most of pernicious gas object fluorine in lepidolite raw material after acidleach, that is fluorine removal, then activation process is carried out to the material after calcining simultaneously using by secondary clacining or roasting, the lithium yield extracted from lepidolite is set to be greatly enhanced, and it is convenient using mechanical ball mill activation act, simply, environmental protection, improve the extraction and application rate of rare metal raw material in lepidolite raw material, reduce energy consumption, shorten the reaction time, and the consumption dosage of acid-base raw materials.
Description
Technical field：Lithium method is put forward the present invention relates to a kind of lepidolite, lepidolite is former especially from lepidolite raw material
The technique for expecting Roasting And Leaching extraction lithium.
Background technology：
Lepidolite is a kind of important mineral resources, contains abundant Rare Metals Materials, lithium, sodium, potassium, rubidium, caesium, aluminium etc..
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 sent out as new energy
One of important industry of exhibition is increasingly paid attention to by various countries；Lithium and its esters lithium carbonate, the salt such as lithium sulfate are the productions of 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 lepidolite
Development and application become current heat subject.It is rich due to containing in lepidolite raw material during development and application lithium and its salt
Rich other metallic elements, and only extract lithium metal and its salt do not make development and application to remaining metal, such significant wastage preciousness
Mineral resources, and certain pollution will also result in environment, and the production cost of lithium carbonate is greatly reduced.
The main lime burning method of processing lepidolite ore method, sulfuric acid process, sulfate process, autoclaving method at present.Lime stone roasts
Burning method is by lepidolite ore and lime stone by 1:3 mixing are milled, and are roasted at 875 ~ 911 DEG C.Roasting material chilling water quenching, it is levigate laggard
Row leaches；Lithium resolution ratio is 81% or so.This method raw material sources are extensive, cheap.However existence stream flux is big, if
The disadvantages such as standby efficiency is low, high energy consumption, and the lithium metal rate of recovery is low.Sulfuric acid process is by lepidolite ore at 900 DEG C or so, the roasting of water flowing steam
The concentrated sulfuric acid after burning defluorinate again with 98% roasts 2 hours at 300 DEG C or so, and the leaching rate of this method lithium can be more than 90%.But sulfuric acid
Method processing lepidolite can make ferrimanganic, calcium, magnesium and aluminium therein sulfate corresponding with sulfuric acid reaction generation, especially aluminium, it
Content in mineral is up to 20% or more, consumes a large amount of sulfuric acid；And these metals enter leachate, make the purge amount of solution
Increase, this is the impassable environment of sulfuric acid process.
Simultaneously in the existing calcination process to lepidolite, it is common to use be that the kiln mode of production carries out, important is
It is calcined with vertical coal pit stove etc., the layer structure of lepidolite when to the calcining of lepidolite being at 800-950 DEG C
It is opened, the bulkiness of lepidolite material increases.Current calciner plant and method are used at this temperature, result in one in this way
It is to maintain high temperature heating time long, energy consumption is excessive；Second is that since lepidolite ore raw material dissolves at high temperature for a long time
With calcining so that the Rare Metals Materials burn tinctuer in lepidolite raw material improves, and reduces the recycling of rare metal especially lithium
Utilization rate.
Therefore, people begin to use the preparation method that rotary kiln type is calcined, rotary kiln baking lepidolite to extract lithium technique, but
It is that existing roasting material leaching liquid-solid ratio is all smaller, generally only 1:1, often the content of lithium ion is relatively low general in leachate
Only several grams per liters, concentration are relatively low.Roasting material leachate is solid than smaller, and corresponding stirring intensity requires big, but conventional stirring
Machine is difficult to reach requirement, results in putting forward lithium yield so low.On the other hand single calcining manners and mixed to the stirring of extract
Conjunction method, the influence that lithium yield is put forward to the preparation of lepidolite is also larger, thus how come provide a kind of synthesis to lepidolite into
The method of row calcining and processing, so as to which the yield for carrying lithium from lepidolite is greatly improved.
Invention content：The present invention seeks to provide a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium, is with lithium cloud
Mother is raw material, and method, including acidleach, calcining, activation, filtering, freezing, concentration, sinker are combined using acidleach and calcining, is used
The first acidleach method that calcining machine activates again, to improve the comprehensive development and utilization rate of lepidolite.
The present invention provides a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium, is adopted using lepidolite as raw material
It is combined method, including acidleach, calcining, activation, filtering, freezing, concentration, sinker with acidleach and calcining, is to use first acidleach again
The method of calcining carries out as follows：
1）, the acidleach be that lepidolite is crushed to 50-100 mesh and dilution heat of sulfuric acid mixes, acidleach hybrid reaction 0.5-1 is small
When, fluorine removal is acidleach roasting material；
2）, the calcining, using secondary clacining method, primary calcining is using kiln roast and fluorine removal,
It is by 1）The acidleach roasting material of step is placed in kiln, in 220 DEG C of -300 DEG C of temperature lower calcinations 30-60 minutes, once
Fluorine removal obtains roasting material of lepidolite；
Secondary clacining is calcined using ion generator, be by roasting material of lepidolite send into plasma generator into
Row high-temperature calcination simultaneously continues fluorine removal, and the temperature for controlling secondary clacining is 1000-1600 DEG C, time 10-30 minute, plasma calcining
After fluorine removal, lepidolite secondary clacining material is obtained；
3), mechanical ball mill activates, and lepidolite secondary clacining material is added water, heats, and ball milling activation Solid-liquid mixture is made as, by ball milling
Activation Solid-liquid mixture is placed in ball-milling device, carries out mechanical activation ball-milling treatment, and filtering obtains ball milling leachate and ball milling filter
Slag is after reaction filtered reaction solution, freezing and crystallizing, neutralizes removal of impurities, concentration, and lithium salts is made in sinker.
Preferably, it is step 1）The acidleach is to control a concentration of 50wt%-65wt% of dilution heat of sulfuric acid and control acid
The pH of solution is 1-2 when soaking hybrid reaction.
Further, it is step 1）The acidleach is to control the liquid of dilute sulfuric acid and lepidolite consolidate mass ratio as 2-3：1.
Preferably, it is step 2）The primary calcining is to control the draw ratio of kiln as 15-18, controls rotary kiln
Slewing rate is 0.50-3.85 revs/min.
Preferably, it is step 2）It is 1500 DEG C to control the secondary clacining temperature.
Preferably, it is step 3）It is 0.8-1 that the liquid of control ball milling activation Solid-liquid mixture, which consolidates mass ratio,:1.
Preferably, it is step 3）Control the Li in the ball milling leachate+Concentration reaches 12g/l.
Preferably, it is step 3）The temperature for controlling ball milling activation Solid-liquid mixture is 40-60 DEG C.
Preferably, it when being fluorine removal, is recycled using pumping, and gas recovery calcium hydroxide or sodium hydroxide solution is inhaled
It receives.
Further, it is that the filtering is filtered using bag type filtering machine.
A kind of technique of lepidolite raw material Roasting And Leaching extraction lithium disclosed by the invention, is first carried out using lepidolite is used
Acidleach is handled, and the process then calcined again had by eliminating the major part in lepidolite raw material after acidleach before this
Then evil gas object fluorine, i.e. fluorine removal carry out activation process to the material after calcining simultaneously using by secondary clacining or roasting, make
The lithium yield extracted from lepidolite is greatly enhanced, and convenient using mechanical ball mill activation act, simply, ring
It protects.When carrying out secondary clacining to lepidolite especially by ion generator, because of the generation of ion generator instant transient high fever,
The high temperature difference thermal response for making lepidolite be generated in calcining, makes lepidolite structure change, mainly monolithic lepidolite stratiform
Its opening dissociation of chip architecture is fluffy.So that the various yttriums in lepidolite raw material easily leach.Pass through ion generator
Temperature be rapidly reached 1000 DEG C or more, the lamellar structure of lepidolite can be made to be opened rapidly.Due to lithium at high operating temperatures
And its easily separate out, the yttrium that is highly advantageous to are leached each yttrium under weakly acidic condition, significantly
Shorten the reaction time, the fluorine in lepidolite raw material evaporates to form a weakly acidic ring under the plasma condition of high temperature
Border, the extraction process being highly advantageous in lepidolite raw material.The extraction and application rate of rare metal raw material in lepidolite raw material is improved,
Energy consumption is reduced, the consumption dosage of reaction time and acid-base raw materials is shortened.On the other hand, since lepidolite raw material is
Stratiform chip architecture is detrimental to ball milling before not opening, therefore works as and use plasma generator by the layer structure of lepidolite
After opening, it is conducive to filter the subsequent extracted of lepidolite with regard to pole when carrying out ball milling.Therefore using the method for the present invention to lepidolite original
When material carries out calcination process, the recovery rate of lithium and other yttriums in lepidolite raw material greatly improves, after testing
Lithium extraction rate reached is to 97% or more.
Specific implementation mode：The specific technical solution of the present invention is described in further detail with reference to embodiment,
Each group involved in embodiment is divided into mass parts or mass ratio, and the concentration being related to is mass concentration.
Embodiment 1：
A kind of technique of lepidolite raw material Roasting And Leaching extraction lithium of the present invention, using acidleach and is forged using lepidolite as raw material
Burning is combined method, and the raw material that the present embodiment uses is the lepidolite raw material of Yichuan tantalum niobium lithium mine production, primary chemical composition
Composition such as following table（wt%）Surplus is fluorine,
| Li2O | K2O | Na2O | AL2O3 | SiO2 | Fe2O3 | Rb2O | Cs2O |
| 5.23 | 10.78 | 0.64 | 24.21 | 51.68 | 0.43 | 1.62 | 0.41 |
Including acidleach, calcining, activation, filtering, freezing, concentration, sinker, the method that the acidleach is calcined again, as follows into
Row：
1）, acidleach be that above-mentioned lepidolite, which is crushed to 50-100 mesh and a concentration of 50-65wt% dilution heat of sulfuric acid, to be mixed, and control is dilute
It is 2-3 that the liquid of sulfuric acid and lepidolite, which consolidates mass ratio,：1；Acidleach hybrid reaction 0.5-1 hours, fluorine removal, when fluorine removal, generation it is fluorine-containing
Gas is recycled using pumping, and gas recovery calcium hydroxide or sodium hydroxide solution are absorbed（Similarly hereinafter）.It is that will use sulfuric acid
The gas given off in the lepidolite mixed material of solution dipping is mainly fluoro-gas, is aspirated, is used in combination with air extractor is unified
It in lye and recycles, similarly hereinafter, is made as acidleach roasting material；
2）, calcining, using secondary clacining method, primary calcining is using kiln roast and fluorine removal,
It is by 1）The acidleach roasting material of step is placed in kiln, and the draw ratio for controlling kiln is 15-18, i.e. kiln
Specifications and models be 4 × 60 meters etc. different size kiln, control rotary kiln slewing rate be 0.50-3.85 turn/
Minute；And at a temperature of 220 DEG C -300 DEG C, calcine 30-60 minutes, a fluorine removal obtains roasting material of lepidolite；
Secondary clacining is calcined using ion generator, be by roasting material of lepidolite send into plasma generator into
Row high-temperature calcination continues fluorine removal, and the temperature for controlling secondary clacining is 1000-1600 DEG C, and preferably 1500 DEG C, time 10-30 divides
Clock, preferably 15 minutes obtain lepidolite secondary clacining material after plasma calcines fluorine removal；Laminar structured quilt in this way in lepidolite
It thoroughly opens, each metal ion such as lithium in lepidolite is easily leached；
3), mechanical ball mill activates, and lepidolite secondary clacining material is added water, heats, and is made as ball milling activation Solid-liquid mixture, being can
Warm water is added to lepidolite secondary clacining material, usually 40-50 DEG C of the temperature control of warm water, solid-liquid is activated by ball milling
Mixture is placed in ball-milling device, carries out mechanical activation ball-milling treatment, and the liquid of control ball milling activation Solid-liquid mixture consolidates mass ratio
For 0.8-1:1, filtering obtains ball milling leachate, the Li in ball milling leachate+Concentration can reach 12g/l and ball milling filter residue, reaction knot
Reaction solution is filtered after beam, reaction solution designated herein is ball milling leachate, i.e., by ball milling leachate through filtering, freezing knot
Crystalline substance neutralizes removal of impurities, concentration, and lithium salts is made in sinker, and it can be lithium sulfate, lithium carbonate etc. to prepare lithium salts as needed.It neutralizes, divide
Prior art can be used from, sinker to carry out, also following proposal can be used to carry out sinker and be added into ball milling leachate
Alkali such as potassium hydroxide or sodium hydroxide, it is 14 that pH value is adjusted under conditions of keeping stirring；And thickening, impurity elimination is detached, is obtained
To containing Li+Solution；Sinker is to containing Li+Solution be passed through carbon dioxide gas, or add carbonate that can prepare lithium carbonate；Add
Enter sulfate and prepare to carry lithium sulfate product；The recovery rate of each rare metal is shown in Table 2.
It calculates after testing, the lithium using the method for the present invention acidleach and after calcining in lepidolite raw material is extracted to be obtained with leaching rate
It greatly improves and is shown in Table 2 using the leaching rate of each rare element of this example.
Table 2
| Li extracts leaching rate/% | K extracts leaching rate/% | Rb extracts leaching rate/% | Cs extracts leaching rate/% | |
| 1 | 97. 14 | 89.21 | 86.95 | 81.98 |
| 2 | 86.23 | 72.81 | 74.24 | 70.06 |
Explanation：Table 2, the technique to use lepidolite raw material Roasting And Leaching of the present invention to extract lithium extract lithium cloud with using the prior art
Lithium and the comparison to each yttrium extraction and leaching rate in female raw material.
In table 2,1 be using lepidolite raw material Roasting And Leaching of the present invention extraction lithium technique to lithium in lepidolite raw material and respectively
The leaching rate of rare element extraction；
2 be reference examples, is the extraction using existing calcining extractive technique to lithium and the extraction of each rare element in lepidolite raw material
Leaching rate.
The technical characteristic without description can realize that details are not described herein by or using the prior art in the present invention.When
So, above description is not limitation of the present invention, and the present invention is also not limited to the above embodiment, the common skill of this field
The variations, modifications, additions or substitutions that art personnel are made in the essential scope of the present invention should also belong to the protection model of the present invention
It encloses.
Claims (10)
1. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium is mutually tied with calcining using acidleach using lepidolite as raw material
Conjunction method, including acidleach, calcining, activation, filtering, freezing, concentration, sinker, it is characterized in that the method calcined again using first acidleach,
It carries out as follows：
1）, the acidleach be that lepidolite is crushed to 50-100 mesh and dilution heat of sulfuric acid mixes, acidleach hybrid reaction 0.5-1 is small
When, fluorine removal is acidleach roasting material；
2), the calcining, using secondary clacining method, primary calcining is roast simultaneously fluorine removal using kiln,
It is by 1）The acidleach roasting material of step is placed in kiln, in 220 DEG C of -300 DEG C of temperature lower calcinations 30-60 minutes, once
Fluorine removal obtains roasting material of lepidolite；
Secondary clacining is calcined using ion generator, be by roasting material of lepidolite send into plasma generator into
Row high-temperature calcination simultaneously continues fluorine removal, and the temperature for controlling secondary clacining is 1000-1600 DEG C, time 10-30 minute, plasma calcining
After fluorine removal, lepidolite secondary clacining material is obtained；
3), mechanical ball mill activates, and lepidolite secondary clacining material is added water, heats, and ball milling activation Solid-liquid mixture is made as, by ball milling
Activation Solid-liquid mixture is placed in ball-milling device, carries out mechanical activation ball-milling treatment, and filtering obtains ball milling leachate and ball milling filter
Slag is after reaction filtered reaction solution, freezing and crystallizing, neutralizes removal of impurities, concentration, and lithium salts is made in sinker.
2. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 1）It is described
Acidleach is to control a concentration of 50wt%-65wt% of dilution heat of sulfuric acid, and the pH of solution is 1-2 when controlling acidleach hybrid reaction.
3. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 1）It is described
Acidleach is to control the liquid of dilute sulfuric acid and lepidolite consolidate mass ratio as 2-3：1.
4. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 2）It is described
Calcining is to control the draw ratio of kiln as 15-18, and the slewing rate for controlling rotary kiln is 0.50-3.85 revs/min.
5. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 2）Control
The secondary clacining temperature is 1500 DEG C.
6. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 3）Control
It is 0.8-1 that the liquid of ball milling activation Solid-liquid mixture, which consolidates mass ratio,:1.
7. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 3）Control
Li in the ball milling leachate+Concentration reaches 12g/l.
8. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that step 3）Control
The temperature that ball milling activates Solid-liquid mixture is 40-60 DEG C.
9. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium uses it is characterized in that when fluorine removal according to claim 1
Pumping recycling, and gas recovery calcium hydroxide or sodium hydroxide solution are absorbed.
10. a kind of technique of lepidolite raw material Roasting And Leaching extraction lithium according to claim 1, it is characterized in that the filtering is adopted
It is filtered with bag type filtering machine.
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Cited By (6)
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| CN110904343A (en) * | 2019-12-31 | 2020-03-24 | 江西南氏锂电新材料有限公司 | Method for extracting lithium by drying lepidolite by utilizing waste heat |
| CN112176185A (en) * | 2020-09-28 | 2021-01-05 | 江西永兴特钢新能源科技有限公司 | Method for removing fluorine from lepidolite roasting leaching solution |
| CN112342371A (en) * | 2020-11-12 | 2021-02-09 | 萍乡市拓源实业有限公司 | Low-temperature roasting process for lepidolite |
| CN112575204A (en) * | 2020-12-09 | 2021-03-30 | 四川卡森科技有限公司 | Lithium extraction method based on rotary kiln |
| CN112624161A (en) * | 2020-12-31 | 2021-04-09 | 江西南氏锂电新材料有限公司 | Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite |
| CN112877548A (en) * | 2021-01-12 | 2021-06-01 | 中国科学院过程工程研究所 | Method for recovering valuable metals from waste lithium ion battery anode powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110904343A (en) * | 2019-12-31 | 2020-03-24 | 江西南氏锂电新材料有限公司 | Method for extracting lithium by drying lepidolite by utilizing waste heat |
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| CN112575204A (en) * | 2020-12-09 | 2021-03-30 | 四川卡森科技有限公司 | Lithium extraction method based on rotary kiln |
| CN112624161A (en) * | 2020-12-31 | 2021-04-09 | 江西南氏锂电新材料有限公司 | Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite |
| CN112877548A (en) * | 2021-01-12 | 2021-06-01 | 中国科学院过程工程研究所 | Method for recovering valuable metals from waste lithium ion battery anode powder |
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