CN110042262A - Method for selectively leaching low-grade deposition type lithium ore - Google Patents
Method for selectively leaching low-grade deposition type lithium ore Download PDFInfo
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- CN110042262A CN110042262A CN201910445903.3A CN201910445903A CN110042262A CN 110042262 A CN110042262 A CN 110042262A CN 201910445903 A CN201910445903 A CN 201910445903A CN 110042262 A CN110042262 A CN 110042262A
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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
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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
- 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
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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 method for selectively leaching low-grade deposition type lithium ore, which relates to the technical field of comprehensive smelting of the lithium ore by a pyrogenic process and a wet process and comprises the following steps: a. crushing the deposition type lithium raw ore into ore powder; b. roasting the mineral powder at 500-750 ℃ for 0.5-4.0 hours; c. cooling the roasted mineral powder for 1-24 hours at normal temperature to obtain cooled cooked mineral powder; d. putting the cooked ore powder into 0.5-4.0 mol/L inorganic acid to react for 0.5-4.0 hours, wherein the liquid-solid ratio is 2-20L/kg, the leaching temperature is 20-60 ℃, so as to obtain a lithium-rich material liquid, washing the residues to be neutral, and recycling the acid washing liquid; in the deposition type lithium raw ore, the content of lithium oxide is not more than 1%, and lithium element is mainly existed in the clay mineral in the form of lithium chlorite. Aiming at the specific technical difficulty of the Guizhou deposit type lithium ore, the method ensures that the leaching rate of the lithium element is higher than 95 percent, and can effectively inhibit the leaching of impurity elements; has the characteristics of low processing energy consumption and convenient and controllable operation.
Description
Technical field
The present invention relates to lithium mine pyrogenic process wet process integrated smelting technical field, a kind of low product of Selectively leaching are specifically related to
The method of position appositional pattern lithium mine.
Background technique
The enrichment of the Guizhou area Liu Panshui Lang Dai appositional pattern lithium ore resources, originates in Permian System dragon cry of certain animals group, has found in area at present
Many places lithium mine point, average Li2O grade 0.51%；Orebody thickness 0.49-7.77 m, average 2.96 m；Lithium mine metal according to a preliminary estimate
12318.12 tons of amount reaches medium-sized deposit scale.The appositional pattern lithium mine forms based on clay mineral, predominantly dickite, quartz
With chlorite etc., elemental lithium mainly in the form of cookeite preservation in clay mineral.Lithium clay disseminated grain size is very thin, is grinding
It is difficult to monomer dissociation during mine, the enriching and recovering of lithium cannot achieve using conventional physical upgrading method, therefore can only use
Elemental lithium in the metallurgical method enriching and recovering appositional pattern lithium mine.
Chinese lithium resource is mainly distributed on the provinces such as Qinghai, Tibet, Sichuan, Xinjiang, Jiangxi, Inner Mongol, lithium ore resources type
It is varied, but about 70% or more lithium resource preservation contains a large amount of major element ion such as in salt lake bittern: K in salt lake+、Ca2+、Na+、Mg2+Deng and minor elements Li+The salt of equal formation.Currently, carbonate precipitation method, solvent extraction, absorption method
Deng the extraction for being widely used in Lithium from Salt Lake Brine.Ore lithium resource concentrates on the provinces such as Sichuan, Jiangxi, Hunan, Xinjiang,
Most of lithium deposite is granitic pegmatite-type mineral deposit and alkali feldspar granite type mineral deposit, ore lithium oneself find out that resource reserve accounts for entirely
20% or so of state's lithium resource gross reserves.Natural spodumene is roasted at 950-1100 DEG C, turns it by α-spodumene of monoclinic system
Become β-spodumene of tetragonal crystal system, chemical activity increases, can occur with soda acid it is various react, then by sulfuric acid and β-spodumene
It is blended at 250-300 DEG C and roasts, displacement reaction is occurred by sulfating roasting, that is, produce soluble lithium sulfate and insoluble
Gangue.(Li Jun, Zhu Qingshan, Li Hongzhong typical case mention lithium progress [J] Chinese science containing lithium minerals roasting: chemistry, and 2017,
47(11): 1273-1283.)
Guizhou appositional pattern lithium mine, head grade is not high, average Li2O grade 0.51%, mineral composition is based on clay mineral, lithium member
Plain main preservation is expected to using specific temperature roasting-Selectively leaching method from the appositional pattern lithium in cookeite mineral
Selective enrichment recycles elemental lithium in mine.
The method that directly selecting property leaches elemental lithium from the appositional pattern lithium mine at present is not reported.Although passing through sulfate
Or the modified roasting-leaching with sulfuric acid technique of the villiaumite method of extracting elemental lithium from low-grade clay pit containing lithium has a small amount of document, special
Benefit report.Such as: high will etc. develops the technique that the low-grade clay pit containing lithium of one kind proposes lithium method, Publication No. CN
The patented method of 103849761 B is mixed using sulfate, villiaumite with raw ore for the low-grade clay pit containing lithium of north Henan
It is modified roasting at 800 DEG C, the technique for being granulated dump leaching then is carried out to the raw material after modified roasting, the leaching rate of lithium reaches
91%.The technique carries out high-temperature roasting by the method for adding a large amount of roasting auxiliary agents in raw ore, the requirement to equipment and cost
It is all higher.
Summary of the invention
The present invention is directed to it is low-grade to provide a kind of Selectively leaching for defect and deficiency present in the above-mentioned prior art
The method of appositional pattern lithium mine, this method are directed to the particular technology difficult point of similar this kind of lithium mine of Guizhou appositional pattern, soak its elemental lithium
Extracting rate is higher than 95%, while can effectively inhibit the leaching of impurity element；With processing, low energy consumption, operates convenient controllable feature.
The present invention is realized by using following technical proposals:
A kind of method of the low-grade appositional pattern lithium mine of Selectively leaching, it is characterised in that steps are as follows:
A, appositional pattern lithium crushing raw ore at miberal powder；
B, the miberal powder is roasted 0.5 ~ 4.0 hour at 500 ~ 750 DEG C；
C, the miberal powder after roasting is cooled down 1 ~ 24 hour at normal temperature, obtains ripe miberal powder after cooling；
D, the ripe miberal powder is put into and is reacted in the inorganic acid of 0.5 ~ 4.0mol/L 0.5 ~ 4.0 hour, liquid-solid ratio 2-20L/kg,
20 ~ 60 DEG C of extraction temperature, rich lithium feed liquid is obtained, recrement is washed to neutrality, acid wash liquid is recycled；
In the appositional pattern lithium raw ore, oxidate for lithium content is not more than 1%, the main preservation in the form of cookeite of elemental lithium
In clay mineral.
Further, it is 20% ~ 90% that miberal powder, which is can the be sieved particle accounting of 200 mesh mesh sizes, in the step a.
Further, the inorganic acid in the step b is one of sulfuric acid, hydrochloric acid or nitric acid.
Compared with prior art, the beneficial effects obtained by the present invention are as follows it is as follows:
1, the present invention is relative to applicant in " a kind of side of Selectively leaching appositional pattern Rare Earth Mine filed in November, 2018 day
The patent of invention of method ", Publication No. " 109266839A ", publication date are " on January 25th, 2019 ".Although its processing step is substantially
Identical, still, the present invention most importantly, specifically carries out Selectively leaching, needle for the appositional pattern lithium mine on the ground such as Guizhou
To oxidate for lithium content in appositional pattern lithium raw ore be not more than 1%, elemental lithium mainly in the form of cookeite preservation in clay mineral
Special circumstances, filter out specific processing step referring in particular to comparative example 1 and comparative example 2 by experiment several times, it is special
It is not that the miberal powder is roasted to process conditions as 0.5 ~ 4.0 hour at 500 ~ 750 DEG C, has reached in compared with the existing technology
For the entirely different technical effect of the low-grade lithium mine of appositional pattern: the cookeite in appositional pattern lithium mine is a kind of close to two octahedrals
The layer aluminosilicate clay mineral of body can be sloughed completely in its layer structure by control maturing temperature and calcining time
Hydroxyl, improves the activity of mineral, and the distribution of major impurity silicon atom is also able to maintain original state.Maturing temperature is lower than 500 DEG C, lithium
Hydroxyl in chlorite layer structure does not remove completely, and the amorphous structure of high activity is not yet formed, and elemental lithium just can not be effective
It leaches, maturing temperature is higher than 750 DEG C, and cookeite mineral structure is totally disrupted, and can gradually form mullite, major impurity silicon
Crystal form can also change, elemental lithium is wrapped up again, causes elemental lithium also can not effectively leach, in roasting process not
It avoids generating additional harmful exhaust emissions using additive.
2, in the present invention, by the way that miberal powder is roasted 0.5 ~ 4.0 hour at 500 ~ 750 DEG C；By the miberal powder after roasting normal
Temperature is lower 1 ~ 24 hour cooling, obtains ripe miberal powder after cooling；And the ripe miberal powder is put into the inorganic acid of 0.5 ~ 4.0mol/L
Middle reaction 0.5 ~ 4.0 hour, liquid-solid ratio 2-20L/kg, obtains rich lithium feed liquid by 20 ~ 60 DEG C of extraction temperature.Through the above steps
Leaching condition is controlled, is sufficiently proved by comparative example 1 and 2 and embodiment, this method not exclusively destroys the mineral of cookeite
Structure, the elemental lithium in Selectively leaching amorphous li green mud stone structure, elemental lithium leaching rate is higher than 95%, while can effectively press down
The leaching of impurity elemental silicon processed, silicon leaching rate < 5% avoid the impurity such as silicon from largely entering rich lithium feed liquid.
Specific embodiment
Comparative example 1
By taking certain pegmatite is containing lithium minerals as an example, main component is spodumene, and oxidation lithium content is 5.96%, roasting transition temperature 700
DEG C when, α-spodumene of monoclinic system is only 0.83% to tetragonal crystal system β-spodumene conversion ratio, almost can not in subsequent technique
Leach elemental lithium.Because α-spodumene just starts largely to be transformed into tetragonal crystal system β-spodumene, and process is subsequent when being greater than 900 DEG C
After sulfuric acid curing, water logging technique, elemental lithium could be leached largely, and roasting transition temperature is lower than 900 DEG C, the lithium member in spodumene mine
Plain leaching rate is less than 40%.(the research [J] with reference to such as Li Zhong to spodumene yield in roasting acidification leaching process.Jiangxi
Work, 2016,6:84-85)
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 40% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 700 DEG C
It burns 2.5 hours, is being placed at room temperature for 8 hours after the completion of roasting, it is small to be added to reaction 2.5 in the hydrochloric acid solution of 2.5mol/L later
When, liquid-solid ratio=10L/kg, 40 DEG C of extraction temperature, elemental lithium leaching rate is 97.51%, silicon leaching rate < 5%.
Comparative example 2
It is mainly cookeite containing lithium minerals using the low-grade clay pit containing lithium in Henan somewhere as research object, oxidation lithium content is
0.50%, Best experimental condition are as follows: 800 DEG C of maturing temperature, 2 h of calcining time, calcium sulfate/raw ore is than 0.7, calcirm-fluoride/raw ore ratio
0.2, sodium sulphate/raw ore is than 0.2, extraction time 1h, and 20 DEG C of extraction temperature, liquid-solid ratio 3:1, sulfuric acid concentration 50%, with this condition
Lithium leaching rate is 95.32%.When maturing temperature is 500 DEG C, the leaching rate of lithium is only 40% or so.(with reference to rivers such as Li Ronggai
The southern low-grade clay pit containing lithium in somewhere proposes lithium new process research [J].Mining metallurgical engineering, 2014,34(6): 81-84)
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 60% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 500 DEG C
It burns 2.0 hours, is being placed at room temperature for 24 hours after the completion of roasting, it is small to be added to reaction 1.0 in the sulfuric acid solution of 3.0mol/L later
When, liquid-solid ratio=18L/kg, 30 DEG C of extraction temperature, elemental lithium leaching rate is 96.43%, silicon leaching rate < 5%.
Embodiment 1
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 35% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 450 DEG C
It burns 2.0 hours, is being placed at room temperature for 6.0 hours after the completion of roasting, it is small to be added to reaction 2.0 in the nitric acid solution of 2.0mol/L later
When, liquid-solid ratio=8L/kg, 35 DEG C of extraction temperature, elemental lithium leaching rate is 40.3%, silicon leaching rate < 5%.
Embodiment 2
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 40% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 500 DEG C
It burns 2.5 hours, is being placed at room temperature for 8.0 hours after the completion of roasting, it is small to be added to reaction 2.5 in the hydrochloric acid solution of 2.5mol/L later
When, liquid-solid ratio=10L/kg, 40 DEG C of extraction temperature, elemental lithium leaching rate is 95.43%, silicon leaching rate < 5%.
Embodiment 3
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 45% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 550 DEG C
It burns 3.0 hours, is being placed at room temperature for 10 hours after the completion of roasting, it is small to be added to reaction 3.0 in the nitric acid solution of 3.0mol/L later
When, liquid-solid ratio=12L/kg, 45 DEG C of extraction temperature, elemental lithium leaching rate is 96.67%, silicon leaching rate < 5%.
Embodiment 4
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 50% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 600 DEG C
It burns 3.5 hours, is being placed at room temperature for 12 hours after the completion of roasting, it is small to be added to reaction 3.5 in the sulfuric acid solution of 3.5mol/L later
When, liquid-solid ratio=14L/kg, 50 DEG C of extraction temperature, elemental lithium leaching rate is 97.26%, silicon leaching rate < 5%.
Embodiment 5
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 55% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 650 DEG C
It burns 4.0 hours, is being placed at room temperature for 18 hours after the completion of roasting, it is small to be added to reaction 4.0 in the hydrochloric acid solution of 4.0mol/L later
When, liquid-solid ratio=16L/kg, 55 DEG C of extraction temperature, elemental lithium leaching rate is 97.89%, silicon leaching rate < 5%.
Embodiment 6
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 60% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 700 DEG C
It burns 2.0 hours, is being placed at room temperature for 24 hours after the completion of roasting, it is small to be added to reaction 0.5 in the nitric acid solution of 2.0mol/L later
When, liquid-solid ratio=18L/kg, 60 DEG C of extraction temperature, elemental lithium leaching rate is 97.79%, silicon leaching rate < 5%.
Embodiment 7
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 65% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 750 DEG C
It burns 0.5 hour, is being placed at room temperature for 2 hours after the completion of roasting, it is small to be added to reaction 1.0 in the sulfuric acid solution of 2.5mol/L later
When, liquid-solid ratio=20L/kg, 20 DEG C of extraction temperature, elemental lithium leaching rate is 95.33%, silicon leaching rate < 5%.
Embodiment 8
The particle for weighing the 200 mesh mesh sizes that can be sieved accounts for 70% or more Guizhou appositional pattern lithium raw ore 200g, roasts at 900 DEG C
It burns 2.0 hours, is being placed at room temperature for 24 hours after the completion of roasting, is being added in the hydrochloric acid solution of 3mol/L and reacts 2 hours later, liquid
Gu ratio=16L/kg, 45 DEG C of extraction temperature, elemental lithium leaching rate is 26.82%, silicon leaching rate < 5%.
Claims (3)
1. a kind of method of the low-grade appositional pattern lithium mine of Selectively leaching, it is characterised in that steps are as follows:
A, appositional pattern lithium crushing raw ore at miberal powder；
B, the miberal powder is roasted 0.5 ~ 4.0 hour at 500 ~ 750 DEG C；
C, the miberal powder after roasting is cooled down 1 ~ 24 hour at normal temperature, obtains ripe miberal powder after cooling；
D, the ripe miberal powder is put into and is reacted in the inorganic acid of 0.5 ~ 4.0mol/L 0.5 ~ 4.0 hour, liquid-solid ratio 2-20L/kg,
20 ~ 60 DEG C of extraction temperature, rich lithium feed liquid is obtained, recrement is washed to neutrality, acid wash liquid is recycled；
In the appositional pattern lithium raw ore, oxidate for lithium content is not more than 1%, the main preservation in the form of cookeite of elemental lithium
In clay mineral.
2. a kind of method of the low-grade appositional pattern lithium mine of Selectively leaching according to claim 1, it is characterised in that: described
It is 20% ~ 90% that miberal powder, which is can the be sieved particle accounting of 200 mesh mesh sizes, in step a.
3. a kind of method of the low-grade appositional pattern lithium mine of Selectively leaching according to claim 1, it is characterised in that: described
Inorganic acid in step b is one of sulfuric acid, hydrochloric acid or nitric acid.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358934A (en) * | 2019-08-26 | 2019-10-22 | 中国科学院地球化学研究所 | The method that ion-exchange extracts lithium in carbonate clay type lithium mine |
| CN111575504A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for efficiently leaching lithium from lithium-containing claystone |
| CN113528860A (en) * | 2021-07-13 | 2021-10-22 | 中南大学 | Method for efficiently extracting lithium from clay type lithium ore by using pulse voltage |
| CN114757306A (en) * | 2022-06-14 | 2022-07-15 | 中国煤炭地质总局勘查研究总院 | Method, device and equipment for classifying coal-based sedimentary lithium resources and storage medium |
| CN114891998A (en) * | 2022-05-27 | 2022-08-12 | 广东邦普循环科技有限公司 | Method for recycling lithium from lithium clay |
| CN114959253A (en) * | 2022-06-30 | 2022-08-30 | 广东邦普循环科技有限公司 | Method for extracting lithium from lithium clay |
| CN114959305A (en) * | 2022-05-30 | 2022-08-30 | 玉溪师范学院 | Method for leaching lithium from clay ionic lithium resource in organic acid |
| CN115350806A (en) * | 2022-08-17 | 2022-11-18 | 广东邦普循环科技有限公司 | Method for enriching lithium from lithium clay ore |
| CZ309557B6 (en) * | 2020-12-14 | 2023-04-12 | Česká Geologická Služba | Method of treating lithium raw material |
| CN116829745A (en) * | 2023-04-19 | 2023-09-29 | 广东邦普循环科技有限公司 | Method for selectively extracting lithium from sedimentary type lean lithium clay and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358934A (en) * | 2019-08-26 | 2019-10-22 | 中国科学院地球化学研究所 | The method that ion-exchange extracts lithium in carbonate clay type lithium mine |
| CN110358934B (en) * | 2019-08-26 | 2020-05-12 | 中国科学院地球化学研究所 | Method for extracting lithium from carbonate clay type lithium ore by ion exchange method |
| WO2021036263A1 (en) * | 2019-08-26 | 2021-03-04 | 中国科学院地球化学研究所 | Method for extracting lithium from carbonate clay type lithium ore by ion exchange method |
| CN111575504A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for efficiently leaching lithium from lithium-containing claystone |
| CZ309557B6 (en) * | 2020-12-14 | 2023-04-12 | Česká Geologická Služba | Method of treating lithium raw material |
| CN113528860A (en) * | 2021-07-13 | 2021-10-22 | 中南大学 | Method for efficiently extracting lithium from clay type lithium ore by using pulse voltage |
| CN113528860B (en) * | 2021-07-13 | 2022-05-27 | 中南大学 | Method for efficiently extracting lithium from clay type lithium ore by using pulse voltage |
| CN114891998A (en) * | 2022-05-27 | 2022-08-12 | 广东邦普循环科技有限公司 | Method for recycling lithium from lithium clay |
| CN114959305A (en) * | 2022-05-30 | 2022-08-30 | 玉溪师范学院 | Method for leaching lithium from clay ionic lithium resource in organic acid |
| CN114757306A (en) * | 2022-06-14 | 2022-07-15 | 中国煤炭地质总局勘查研究总院 | Method, device and equipment for classifying coal-based sedimentary lithium resources and storage medium |
| CN114959253A (en) * | 2022-06-30 | 2022-08-30 | 广东邦普循环科技有限公司 | Method for extracting lithium from lithium clay |
| CN115350806A (en) * | 2022-08-17 | 2022-11-18 | 广东邦普循环科技有限公司 | Method for enriching lithium from lithium clay ore |
| CN115350806B (en) * | 2022-08-17 | 2023-10-17 | 广东邦普循环科技有限公司 | Method for enriching lithium from lithium clay ore |
| CN116829745A (en) * | 2023-04-19 | 2023-09-29 | 广东邦普循环科技有限公司 | Method for selectively extracting lithium from sedimentary type lean lithium clay and application thereof |
| CN116829745B (en) * | 2023-04-19 | 2024-04-09 | 广东邦普循环科技有限公司 | Method for selectively extracting lithium from sedimentary type lean lithium clay and application thereof |
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