CN109929993A - A kind of pretreatment of lepidolite ore and leaching method - Google Patents
A kind of pretreatment of lepidolite ore and leaching method Download PDFInfo
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- CN109929993A CN109929993A CN201910341938.2A CN201910341938A CN109929993A CN 109929993 A CN109929993 A CN 109929993A CN 201910341938 A CN201910341938 A CN 201910341938A CN 109929993 A CN109929993 A CN 109929993A
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Abstract
The present invention relates to ores to mention lithium technology field, specifically discloses pretreatment and the leaching method of a kind of lepidolite ore, comprising the following steps: 1. levigate reagent；2. mixing；3. roasting；4. pulverizing and jevigating；5. one section of leaching；6. two sections of leachings；7. slurrying is washed.The method of the present invention economy, has industrial application value at strong operability, and calcium oxide and calcium carbonate, which is added, in roasting can play the role of solid fluorine, while can improve calcining sintering character, and calcining is loose frangible.
Description
Technical field
The invention belongs to ores to mention lithium technology field, and in particular to a kind of pretreatment of lepidolite ore and leaching method.
Background technique
Lithium has characteristics, lithium and its compounds such as density is low, chemical activity is strong in chargeable electricity as most light metal
The fields such as pond, atomic energy, ultra-light alloy, electronic device, ceramics, glass, electrolytic aluminium, refrigerant and medical sedative have can not
The effect of substitution.
Due to the development of electric car, demand of the lithium battery in world market is constantly soaring and causes the demand to lithium
It is quickly soaring, how to develop and use various lithium resources and prepare lithium carbonate, meet the needs of market is to lithium carbonate, is pendulum in our faces
Preceding urgent task.
Lithium mainly exists in the form of solid mineral resource and two kinds of liquid Mineral resource in nature, solid mineral resource
It is broadly divided into spodumene mineral and lepidolite mineral again.Chinese spodumene mineral resources compare shortage, and lepidolite is very abundant,
Yichun Prefecture, Jiangxi Province lepidolite reserves are huge, and the reserves of lithium are calculated as 257.8 ten thousand tons with lithia.In lepidolite also containing potassium,
A variety of valuable elements such as rubidium, caesium, fluorine, therefore lithium carbonate, and synthetical recovery valuable element are extracted by raw material of lepidolite, have wide
Wealthy market prospects and good economic benefit.
Lepidolite extracted lithium method mainly has acid system, alkaline process, salt method three categories at present.Acid system mainly using sulfuric acid as leaching agent,
It generally needs preparatory high temperature defluorinate roasting to destroy micaceous structure, or adds sulfuric acid baking, then leach again.In the presence of calcining defluorinate energy consumption
Height, environmental pollution is big, sulfuric acid dosage is larger, and leachate spent acid is high, neutralizes the disadvantages of slag yield is big.
Alkaline process has traditional limestone sintering process, roasting defluorinate lime autoclaving method, the direct autoclaving method of milk of lime etc..Wherein stone
Lime stone sintering process lepidolite ore per ton needs to admix 3.5 tons of lime stones, roasts at 950~1050 DEG C, throughput is big, energy consumption
Height, leachate lithium concentration is low, and the leaching rate of lithium is not high；Lime autoclaving method liquid-solid ratio is big, and filtering is difficult with washing, and leachate lithium is dense
Spend low, the leaching rate of lithium is not high.
Salt method mixed with sulfate, chloride etc. and lepidolite after at high temperature calcination reaction mention lithium.Wherein chlorate method
Roasting generate chlorine, environmental pollution is big, equipment seriously corroded, and in lithium carbonate product chlorine root be easy it is exceeded.Traditional sulfuric acid
Salt method generally uses potassium sulfate, expensive, and reagent cost is high.
Patent CN101885496A discloses a kind of process for extracting lithium from lithionite by fluorine chemistry, and lepidolite adds sulfuric acid and fluosilicic acid,
First in 50~150 DEG C of pre-reaction 1h, rotary kiln is entered back into 150~350 DEG C of 1~4h of reaction, is then gone out with water logging.The patent does not have
The conversion ratio and leaching rate and overall recovery of open lithium, and add sodium carbonate precipitating after concentrated removal of impurities, have to 80% or more
Lithium salts crude product.
Patent CN102337399A discloses a kind of method of extracting lithium by processing lepidolite through alkali dissolution process, by lepidolite and aqueous alkali
Mixing, reacts 6 hours or more, leached mud carries out secondary leaching under similarity condition again, the patent at 8 kilograms of pressure, 150 DEG C
The leaching rate of lithium is not disclosed.
Patent CN102586587A discloses a kind of new method for handling lepidolite ore, and lepidolite ore passes through 900 DEG C of high temperature
Defluorinate is calcined, then levigate rear and lime and alkali metal salt mixing carry out autoclaving leaching, low pressure boils leaching 2 hours or so at 150 DEG C,
Leaching rate Li90%, K80%, Rb70%.
Patent CN101736169A discloses a kind of method that defluorinate roasting villaumite autoclaving mentions lithium from lepidolite, exists first
900 DEG C of main calcining defluorinates, are added calcium oxide and the sodium chloride autoclaving in autoclave after levigate, which does not disclose lithium and rubidium
The leaching rate of potassium.
Patent CN103145158A discloses a kind of method that sulfuric acid roasting method lepidolite prepares lithium carbonate, first 900
DEG C main calcining defluorinate, it is then levigate to mix sour roasting, it is leached by two sections, the leaching rate of lithium is 96% or more.
Patent disclosed above is required to high-temperature calcination defluorinate and combines low temperature sulfuric acid baking or high pressure leaching, technique stream again
Journey is long, and equipment investment is big, energy consumption is high, complicated for operation.
Patent CN1827527A discloses the method for a kind of lepidolite and sodium sulphate and calcium salt Roasting And Leaching lithium, specially lithium
Mica and CaSO4、CaF2、Na2SO4Mixing is roasted at 900~1100 DEG C, uses diluted acid leaching after calcining is levigate, this patent is best
Under the conditions of the leaching rate of lithium be 90.1%, in slag also containing 0.3% lithium, the leaching of rubidium caesium is in confused situation.
Patent CN85101989A discloses the method for a kind of lepidolite and potassium sulfate Roasting And Leaching lithium, specially 1 part of lithium cloud
Female and 0.5 part of K2SO4Mixing roasts at 950 DEG C, is gone out after calcining is levigate with water logging, lithium leaching rate 85.3~89.4%.
Traditional sulfating roasting method generally uses single potassium sulfate, or a small amount of sodium sulphate is mixed based on potassium sulfate,
Potassium sulfate is expensive, and reagent cost is high, thus industrial application value is not high.Sulfating roasting proposes lithium technique and seeks to the greatest extent at present
The dosage that amount reduces potassium sulfate increases the dosage of sodium sulphate, under the premise of guaranteeing lithium leaching rate, reduces the examination of potassium sulfate as far as possible
Agent cost, but after the dosage of increase sodium sulphate, calcining occurs sintering and even melts, and leads to not progress industrial operation, and rubidium
The leaching rate of caesium is very low.
Summary of the invention
The purpose of the present invention is to provide a kind of pretreatment of lepidolite ore and leaching methods, and not only the leaching rate of lithium is high,
The leaching rate of rubidium caesium is also substantially improved.
Technical scheme is as follows:
A kind of pretreatment of lepidolite ore and leaching method, comprising the following steps:
1. levigate reagent
By potassium sulfate, sodium sulphate, fluorine fixing material, calcining raising agent, rubidium caesium displacer is levigate；
2. mixing
Lepidolite concentrate powder is mixed with levigate potassium sulfate, sodium sulphate, fluorine fixing material, calcining raising agent, rubidium caesium displacer
Uniformly；
3. roasting
After 2. mixed material calcining that step is obtained, obtains roasting clinker and be known as calcining；
4. pulverizing and jevigating
By calcining pulverizing and jevigating；
5. one section of leaching
Levigate calcining is transferred in batch extractor and carries out one section of leaching, one section of leaching agent used is 10~100g/L
H2SO4Solution, the dosage of one section of leaching agent are 1.2~1.5 times of lepidolite ore amount；One section of extraction temperature is 60~80 DEG C, one section
Leaching mixing time is 30~240min；
6. two sections of leachings
One section of leached mud and two sections of leaching agents are mixed, two sections of leaching agents used are 10~100g/L H2SO4It is molten
Liquid, the dosage of two sections of leaching agents are 1.2~1.5 times of lepidolite ore amount；Two sections of extraction temperatures are 60~80 DEG C, and two sections of leachings are stirred
Mixing the time is 60~90min；
5. two sections of leachate return steps are used as one section of leaching agent to participate in one section of leaching；
7. slurrying is washed
30min is mixed in two sections of leached muds and water at 50 DEG C, leaching requirement is 1.2~1.5 times of lepidolite ore amount；
6. filtered washing water return step, by the way that sulfuric acid is added, is configured to containing 10~100g/L H2SO4It is molten
Then liquid participates in two sections of leachings as two sections of leaching agents；
Leached mud drying weighing, analyzes lithium, rubidium content, calculates lithium, rubidium leaching rate, can be used as building materials original after final recycling
Material.
Step 1. in, it is ensured that each reagent is milled down to 90% less than 60 mesh, and 50% less than 200 mesh.
Step 2. in, fluorine fixing material CaO, CaCO3、CaSO4、CaCl2One of or a variety of mixtures, can play
Gu the effect of fluorine；
Calcining raising agent is CaO, CaCO3One of or a variety of mixtures, calcining can be made loose；
Rubidium caesium displacer is strontium sulfate.
Step 2. in, sulfuric acid potassium application rate be lepidolite ore amount 5~40%, sodium sulphate dosage be lepidolite ore amount 10~
50%, fluorine fixing material dosage is the 5~15% of lepidolite ore amount, and calcining raising agent dosage is the 5~15% of lepidolite ore amount, rubidium caesium
Displacer dosage is the 2~10% of lepidolite ore amount.
Step 3. in, mixed material is calcined into 60~120min at 875~975 DEG C.
Step 4. in, it is ensured that calcining pulverizing and jevigating to 85% be less than -100 mesh.
Step 5. obtained in one section of leachate for recycling lithium rubidium caesium, byproduct potassium sulfate obtained in removal process,
1. sodium sulphate return step recycles.
Step 2. in, sulfuric acid potassium application rate be lepidolite ore amount 10~20%, sodium sulphate dosage be lepidolite ore amount 25
~35%.
Step 5. in, one section of leaching mixing time is 60~90min.
In 6. solution that step is prepared, H2SO4Content is 50~80g/L.
Remarkable result of the invention is:
(1) tailings amount is few；
1 ton of lepidolite is handled using the method for the present invention and only generates 1.2 tons of tailings, and tailings ingredient be kaliophilite, leucite,
CaF2, essentially identical with the chemical component of lepidolite raw ore, leached tailings are easy to handle.
(2) fluorine evolution is less when roasting and calcining is loose；
Calcium oxide and calcium carbonate, which is added, in roasting in the method for the present invention can play the role of solid fluorine, only about 0.7% fluorine
It is escaped in the form of HF, while calcining sintering character can be improved, calcining is loose frangible.
(3) ore grinding energy consumption is lower；
The method of the present invention can directly be employed without levigate to the lepidolite concentrate of hardly possible mill, and ore grinding energy can be greatly reduced
Consumption.
(4) leachate lithium concentration is high, and impurity is few；
For the method for the present invention due to being leached using the small liquid-solid ratio of dilute sulfuric acid, leachate lithium concentration is up to 10~15g/L, can
Lithium concentration energy consumption is greatly decreased.And by leaching acid leaching solution return again, final pH of leaching solution is leached 4~5 or so
Liquid impurity is few, subsequent easy to handle.
(5) lithium leaching rate is high, and has leached part rubidium caesium；
It can reach 95.2% using the method for the present invention lithium leaching rate, rubidium caesium leaching rate is up to 66.4%.It simultaneously can be with
Demand according to market to rubidium caesium targetedly changes the additional amount of rubidium caesium displacer, controls the output capacity of rubidium caesium.
(6) reagent consumption is few, and production cost is low；
The method of the present invention economy, has industrial application value at strong operability, using the sulfuric acid of the high sodium sulphate of low potassium sulfate
The usage amount of potassium sulfate is greatly reduced in salt roasting technique, the K in roasting process2SO4Actual consumption about 10%, Na2SO4Actually disappear
Consumption about 12%.And in lithium carbonate preparation process output byproduct Na2SO4It can be all returned to calcining process use, solved
Byproduct Na2SO4Handling problems save reagent cost of material again.
Detailed description of the invention
Fig. 1 is lepidolite of the present invention pretreatment and extract technology flow diagram.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
As shown in Figure 1, pretreatment and the leaching method of a kind of lepidolite ore, comprising the following steps:
1. levigate reagent
Potassium sulfate, sodium sulphate, fluorine fixing material, calcining raising agent, rubidium caesium displacer are milled down to 90% less than 60 mesh, and
Ensure 50% less than 200 mesh.
2. mixing
Lepidolite concentrate powder is mixed with levigate potassium sulfate, sodium sulphate, fluorine fixing material, calcining raising agent, rubidium caesium displacer
Uniformly；
Wherein, sulfuric acid potassium application rate is 5~40%, preferably the 10~20% of lepidolite ore amount；Sodium sulphate dosage is lithium cloud
The 10~50% of female mine amount, preferably 25~35%；Fluorine fixing material is CaO, CaCO3、CaSO4、CaCl2One of or it is a variety of
Mixture, can play the role of solid fluorine, and dosage is the 5~15% of lepidolite ore amount；Calcining raising agent is CaO, CaCO3In
One or more mixtures, dosage are the 5~15% of lepidolite ore amount, and calcining can be made loose；Rubidium caesium displacer is sulfuric acid
Strontium, dosage are the 2~10% of lepidolite ore amount.
3. roasting
2. mixed material that step is obtained calcines 60~120min at 875~975 DEG C, obtains roasting clinker and is known as roasting
Sand；
4. pulverizing and jevigating
Calcining pulverizing and jevigating to 85% is less than -100 mesh.
5. one section of leaching
Levigate calcining is transferred in batch extractor and carries out one section of leaching, one section of leaching agent used is 10~100g/L
H2SO4Solution, the dosage of one section of leaching agent are 1.2~1.5 times of lepidolite ore amount；One section of extraction temperature is 60~80 DEG C, one section
Leaching mixing time is 30~240min, preferably 60~90min；
One section of leachate is for recycling lithium rubidium caesium, byproduct potassium sulfate obtained in removal process, sodium sulphate return step
1. recycling.
6. two sections of leachings
One section of leached mud and two sections of leaching agents are mixed, two sections of leaching agents used are 10~100g/L H2SO4It is molten
Liquid, H2SO4Content is preferably 50~80g/L, and the dosage of two sections of leaching agents is 1.2~1.5 times of lepidolite ore amount；Two sections of leachings
Temperature is 60~80 DEG C, and two sections of leaching mixings time are 60~90min；
H in two sections of leachates2SO45. concentration range directly return step can be used as one section of leaching agent ginseng in 10~100g/L
It is leached with one section.
7. slurrying is washed
30min is mixed in two sections of leached muds and water at 50 DEG C, leaching requirement is 1.2~1.5 times of lepidolite ore amount；
6. filtered washing water return step, by the way that sulfuric acid is added, is configured to containing 10~100g/L H2SO4It is molten
Then liquid participates in two sections of leachings as two sections of leaching agents；
Leached mud drying weighing, analyzes lithium, rubidium content, calculates lithium, rubidium leaching rate, can be used as building materials original after final recycling
Material.
Embodiment
Six embodiments have selected the lepidolite ore of four kinds of different grades to carry out, and one of lepidolite ore composition is shown in Table 1,
For other three kinds of lepidolite ores other than lithium rubidium caesium changes of contents, other are miscellaneous essentially identical.
1 lepidolite ore composition of table
| Ingredient | Li2O | SiO2 | Al2O3 | K2O | Fe2O3 | MnO | F | Rb2O | Na2O | Cs2O |
| Content % | 3.05 | 50.1 | 3.5 | 7.6 | 2.2 | 0.40 | 4.2 | 1.03 | 1.68 | 0.065 |
Embodiment 1
It is operated as follows:
1. taking 100g lepidolite concentrate, following reagent: 10g K is weighed2SO4、30g Na2SO4、5g CaO、5g CaCO3、3g
Rubidium caesium displacer, reagent is mixed and finely ground to 50% less than 200 mesh；
2. lepidolite concentrate is uniformly mixed with levigate reagent；
3. the material of mixing is placed in crucible in 1050 DEG C of roasting 60min；
4. calcining pulverizing and jevigating to 85% is less than -100 mesh；
One section of leaching is carried out 5. levigate calcining is transferred in batch extractor, leaching agent used is to grasp under previous equal conditions
Make two sections of obtained leachates, dosage 120ml, temperature is 50 DEG C, stirs 60min；
6. two sections of leachings, the washing water and sulfuric acid operated under previous equal conditions are added in one section of leached mud are used
Amount is 120mL, is made into H2SO4Concentration is the leaching agent of 20g/L, opens and stirs, 50 DEG C of reaction temperature, reaction time 60min；
5. two sections of leachate return steps participate in one section of leaching；
7. slurrying is washed, 30min is mixed in two sections of leached muds and 120mL water, then temperature 50 C filters, wash
6. water return step carries out two sections of leachings；
Leached mud drying weighing, analyzes lithium, rubidium content, calculates lithium, rubidium leaching rate.
Other five embodiment operating procedures are identical with embodiment 1, only change reagent addition with when certain
The operating condition of six embodiments and parameter and result are listed in table 2, in table 3 by a little operating parameters.
2 embodiment roasting condition of table
3 embodiment leaching condition of table and result
The present invention due to taking two sections of leachings, and wherein one section take sulfuric acid leaching, therefore the leaching rate of lithium is very high, most
Good has reached 95.2%；Rubidium caesium displacer has crucial effect to the leaching of rubidium, and when rubidium caesium displacer is not added, the leaching rate of rubidium is most
There was only 4.6% well, after having added 10% rubidium caesium displacer, the leaching rate of rubidium reaches 66.4%.Since the market of rubidium is very small, because
This can adjust the dosage of rubidium caesium displacer according to the market situation of rubidium, and not have to make any change to technique, can adjust at any time
The yield of whole rubidium caesium.
The above is presently preferred embodiments of the present invention, is not made any form of restriction to invention, of the invention
Technical spirit is to convert lepidolite ore phase using sulfating roasting, and additive improvement calcining sintering character is added, and improves rubidium
Leaching rate keeps lepidolite sulfating roasting technique economical and commercial operability.All technical spirits pair under this invention
Above embodiments make any simple modification, equivalent change and modification, belong to the protection scope of technical solution of the present invention.
Claims (10)
1. pretreatment and the leaching method of a kind of lepidolite ore, it is characterised in that: the following steps are included:
1. levigate reagent
By potassium sulfate, sodium sulphate, fluorine fixing material, calcining raising agent, rubidium caesium displacer is levigate；
2. mixing
Lepidolite concentrate powder is uniformly mixed with levigate potassium sulfate, sodium sulphate, fluorine fixing material, calcining raising agent, rubidium caesium displacer；
3. roasting
After 2. mixed material calcining that step is obtained, obtains roasting clinker and be known as calcining；
4. pulverizing and jevigating
By calcining pulverizing and jevigating；
5. one section of leaching
Levigate calcining is transferred in batch extractor and carries out one section of leaching, one section of leaching agent used is 10~100g/L H2SO4
Solution, the dosage of one section of leaching agent are 1.2~1.5 times of lepidolite ore amount；One section of extraction temperature is 60~80 DEG C, one section of leaching
Mixing time is 30~240min；
6. two sections of leachings
One section of leached mud and two sections of leaching agents are mixed, two sections of leaching agents used are 10~100g/L H2SO4Solution, two
The dosage of section leaching agent is 1.2~1.5 times of lepidolite ore amount；Two sections of extraction temperatures are 60~80 DEG C, when two sections of leachings are stirred
Between be 60~90min；
5. two sections of leachate return steps are used as one section of leaching agent to participate in one section of leaching；
7. slurrying is washed
30min is mixed in two sections of leached muds and water at 50 DEG C, leaching requirement is 1.2~1.5 times of lepidolite ore amount；
6. filtered washing water return step, by the way that sulfuric acid is added, is configured to containing 10~100g/L H2SO4Solution, so
Two sections of leachings are participated in as two sections of leaching agents afterwards；
Leached mud drying weighing, analyzes lithium, rubidium content, calculates lithium, rubidium leaching rate, can be used as building materials raw material after final recycling.
2. pretreatment and the leaching method of a kind of lepidolite ore as described in claim 1, it is characterised in that: step 1. in, really
It protects each reagent and is milled down to 90% less than 60 mesh, and 50% less than 200 mesh.
3. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 2, it is characterised in that: step 2. in, Gu
Fluorine agent is CaO, CaCO3、CaSO4、CaCl2One of or a variety of mixtures, solid fluorine can be played the role of；
Calcining raising agent is CaO, CaCO3One of or a variety of mixtures, calcining can be made loose；
Rubidium caesium displacer is strontium sulfate.
4. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 3, it is characterised in that: step 2. in, sulphur
Sour potassium application rate is the 5~40% of lepidolite ore amount, and sodium sulphate dosage is the 10~50% of lepidolite ore amount, and fluorine fixing material dosage is lithium
The 5~15% of Mica Mine amount, calcining raising agent dosage are the 5~15% of lepidolite ore amount, and rubidium caesium displacer dosage is lepidolite
The 2~10% of mine amount.
5. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 4, it is characterised in that: step 3. in, will
Mixed material calcines 60~120min at 875~975 DEG C.
6. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 5, it is characterised in that: step 4. in, really
It protects calcining pulverizing and jevigating and is less than -100 mesh to 85%.
7. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 6, it is characterised in that: step 5. in obtain
One section of leachate for recycling lithium rubidium caesium, byproduct potassium sulfate obtained in removal process, sodium sulphate return step are 1. sharp again
With.
8. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 7, it is characterised in that: step 2. in, sulphur
Sour potassium application rate is the 10~20% of lepidolite ore amount, and sodium sulphate dosage is the 25~35% of lepidolite ore amount.
9. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 8, it is characterised in that: step 5. in, one
It is 60~90min that section, which leaches mixing time,.
10. pretreatment and the leaching method of a kind of lepidolite ore as claimed in claim 9, it is characterised in that: 6. step is prepared
Solution in, H2SO4Content is 50~80g/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498873A (en) * | 2020-04-21 | 2020-08-07 | 华南理工大学 | Carbonate roasting method and system for extracting lithium carbonate from lepidolite |
| CN114318008A (en) * | 2021-12-27 | 2022-04-12 | 四川顺应锂材料科技有限公司 | Method for extracting lithium by secondary reverse leaching of spodumene with nitric acid |
| CN115821060A (en) * | 2022-11-18 | 2023-03-21 | 宜丰国轩锂业有限公司 | Method for extracting lithium from lepidolite through composite salt method sectional roasting |
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