CN106591578A - Method for selectively leaching out lithium from lepidolite through phosphoric acid system - Google Patents

Method for selectively leaching out lithium from lepidolite through phosphoric acid system Download PDF

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Publication number
CN106591578A
CN106591578A CN201611232340.2A CN201611232340A CN106591578A CN 106591578 A CN106591578 A CN 106591578A CN 201611232340 A CN201611232340 A CN 201611232340A CN 106591578 A CN106591578 A CN 106591578A
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Prior art keywords
lithium
phosphoric acid
lepidolite
selectively leaching
acid solution
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CN201611232340.2A
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CN106591578B (en
Inventor
郭永兴
王迎春
祝宏帅
曾小毛
欧阳红勇
刘金练
樊磊
刘志成
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Yifeng Guoxuan Lithium Industry Co ltd
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Jiangxi He Zongli Industry Science And Technology Ltd
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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
    • 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
    • C22B21/00—Obtaining aluminium
    • C22B21/0015—Obtaining aluminium by wet 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
    • C22B26/12—Obtaining lithium
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a method for selectively leaching out lithium from lepidolite through a phosphoric acid system and belongs to the field of lithium resource extraction. In order to overcome the technical defects of high impurity removing cost, incomplete impurity removing and low purity of subsequent lithium products in existing processes for extracting lithium from lepidolite ore, the method for selectively leaching out the lithium from the lepidolite through the phosphoric acid system is provided. In the preparation process of the method, a phosphoric acid solution or a mixed acid solution containing phosphoric acid is adopted for acid leaching of the lepidolite, and impurity ions generated during lithium extraction can be effectively transformed to a precipitate to enter leaching residues, so that the cost of the subsequent lithium extraction process is substantially reduced and the product purity is remarkably improved. The treatment steps of the process are simple, the treatment efficiency is high, and the industrial application prospects are excellent.

Description

A kind of method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite
Technical field
The present invention relates to a kind of method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite, belongs to lithium resource extraction Field.
The content of the invention
Lepidolite is modal lithium minerals, is the important mineral for refining lithium.It is the mafic aluminosilicate of potassium and lithium, category One kind in mica mineral.It is one of primary raw material of extraction rare metal lithium.It is also containing rubidium and caesium often in lepidolite Extract the important source material of these rare metals.Wherein Yichun City stores lepidolite ore the biggest in the world, and lithium oxide is exploited Amount accounts for 31%, the 8.2% of the world of the whole nation.
With regard to extracting lithium from lepidolite with the acid-hatching of young eggs, it will usually using sulphuric acid or hydrochloric acid.But no matter with hydrochloric acid or sulphuric acid, Can all cause lithium together to leach with substantial amounts of aluminum when lepidolite is leached, bring inconvenience to leachate remove impurity sinker operation.
Chinese patent application 2011103205160 is related to a kind of Complete cycle for producing LiFePO 4 as lithium source with lithium ore deposit Preparation method, by by lithium ore deposit calcining, acidifying, leach purification separation obtain primary lithium liquid, by primary lithium liquid carry out conversion freezing, Filtration washing, evaporation and concentration obtain synthetic reaction lithium liquid, and synthetic reaction is carried out with lithium liquid with ferrous salt solution, phosphorus source solution Liquid phase synthesis react, calcining, obtain the LiFePO 4 of carbon coating.It adds phosphorus source solution in synthesis application lithium liquid, but It is not intended to lithium ore souring stage.
《The research of sulfuric acid to leach lepidolite extracted lithium method》The method that lepidolite carries lithium with sulfuric acid reaction re-leaching is have studied, This article explore granule size, sulfuric acid concentration, liquid-solid ratio, reaction temperature, the response time on lithium extraction rate affect, research show with Lepidolite particle size reduction, sulfuric acid concentration increase, liquid-solid ratio is increased, reaction temperature is raised, the response time increases, lithium extraction rate is carried It is high；M (55% sulphuric acid): m (lepidolites of 150 mesh or so)=2: 1,135 DEG C or so reaction 9h, lithium extraction rate up to 96.72%, But itself and the foreign ion problem during unresolved remove impurity sinker.
Through information retrieval, the report that Phosphoric Acid used in the acidification technique of lithium is extracted in lepidolite Ore is not yet found Road.Based on this, the present invention proposes a kind of method that selectivity from lepidolite leaches lithium.
The content of the invention
Removal of impurities cost is high and thorough in order to overcome existing lepidolite Ore extraction lithium technique, the purity of follow-up lithium product Not high technical deficiency, the present invention provides a kind of method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite, the preparation Phosphoric acid solution or the mixed acid solution including phosphoric acid carry out Acid leaching to lepidolite used in technique, and it effectively can will carry lithium During foreign ion be converted into precipitation so that the cost for subsequently putting forward lithium technique is greatly lowered, and product purity substantially rises It is high.The recipe step is simple, and treatment effeciency is high, there is good prospects for commercial application.
This is using Phosphoric Acid basic principles of chemistry of the method for Selectively leaching lithium from lepidolite：
2H3PO4+Al2O3==AlPO4+H2O；
2H3PO4+Li2O==2LiH2PO4+H2O；
2H3PO4+K2O==2KH2PO4+H2O；
2H3PO4+Rb2O==2RbH2PO4+H2O；
2H3PO4+Cs2O==2CsH2PO4+H2O.
The present invention realizes above-mentioned technique effect by following proposal：
A kind of method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite, it comprises the steps：
Lepidolite is sized mixing with Phosphoric Acid solution by liquid-solid ratio 3.0～5.0, slurry is obtained, total phosphorus is 3mol/ in solution L～5mol/L；Slurry is reacted being heated to 80 DEG C～105 DEG C；The response time is controlled for 2h～8h, filtration carries out liquid and consolidates Separate, obtain lithium leachate.
Method using Phosphoric Acid Selectively leaching lithium from lepidolite as above, described Phosphoric Acid solution For phosphoric acid solution or be to include phosphoric acid or phosphatic acid solution.Preferably, described acid solution include hydrochloric acid, nitric acid, One or more in sulphuric acid, bromic acid.
As a kind of embodiment preferred for this invention, the described utilization Phosphoric Acid Selectively leaching from lepidolite Phosphoric Acid solution of the lepidolite with total phosphorus for 3mol/L is sized mixing according to liquid-solid ratio 5.0 in the method for lithium, then in 100 DEG C of reactions 6 hours.
As another embodiment preferred for this invention, the described utilization Phosphoric Acid selective leaching from lepidolite Go out Phosphoric Acid solution of the lepidolite with total phosphorus for 4mol/L in the method for lithium to size mixing according to liquid-solid ratio 4.0, it is then anti-in 105 DEG C Answer 4 hours.
As another embodiment preferred for this invention, the described utilization Phosphoric Acid selective leaching from lepidolite Go out Phosphoric Acid solution of the lepidolite with total phosphorus for 5mol/L in the method for lithium to size mixing according to liquid-solid ratio 3.0, it is then anti-in 80 DEG C Answer 2 hours.
The present invention has compared with prior art following technical advantage：
1) method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite of the present invention is relative to prior art Disclosed technique can be greatly lowered aluminum ions content, after the completion of process below aluminium composition 3.8g/L.
2) method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite of the present invention is relative to prior art Disclosed technique can be greatly lowered the content of other impurities ion, and it can be removed by changing into precipitation, so as to So that the follow-up lithium PROCESS FOR TREATMENT cost that carries is substantially reduced, product purity is greatly improved.
3) technique bar of the utilization Phosphoric Acid of the present invention from lepidolite corresponding to the method for Selectively leaching lithium React gentle in part, technological feasibility is strong, and the requirement to equipment is low.
Specific embodiment
The present invention is further described below by way of specific embodiment, but those skilled in the art should be able to know, the enforcement Example and the never in any form scope of restriction patent protection.
Embodiment 1
Lepidolite is sized mixing with Phosphoric Acid solution by liquid-solid ratio 5.0, total phosphorus is 3mol/L in solution, and in 95 DEG C 8 are reacted Hour, filtration carries out solid-liquor separation.Now the leaching rate of lithium is 70.8%, and the aluminium content in leachate is 2.8g/L.
Embodiment 2
Phosphoric Acid solution by lepidolite with total phosphorus for 4mol/L is sized mixing according to liquid-solid ratio 4.0, then in 100 DEG C of reactions 6 hours, filtration carried out solid-liquor separation.Now the leaching rate of lithium is 85.8%, and the aluminium content in leachate is 3.4g/L.
Embodiment 3
Phosphoric Acid solution by lepidolite with total phosphorus for 5mol/L is sized mixing according to liquid-solid ratio 3.0, then in 105 DEG C of reactions 4 hours, filtration carried out solid-liquor separation.Now the leaching rate of lithium is 92.2%, and the aluminium content in leachate is 3.2g/L.

Claims (4)

1. a kind of method of utilization Phosphoric Acid Selectively leaching lithium from lepidolite, it comprises the steps：
Lepidolite is sized mixing with Phosphoric Acid solution by liquid-solid ratio 3.0～5.0, slurry is obtained, in solution total phosphorus be 3mol/L～ 5mol/L；Slurry is reacted being heated to 80 DEG C～105 DEG C；The response time is controlled for 2h～8h, filtration carries out liquid and divides admittedly From obtaining lithium leachate.
2. the method for utilization Phosphoric Acid Selectively leaching lithium from lepidolite according to claim 1, it is characterised in that Described Phosphoric Acid is phosphoric acid solution or for phosphoric acid or phosphatic acid solution.
3. the method for utilization Phosphoric Acid Selectively leaching lithium from lepidolite according to claim 2, it is characterised in that One or more in described acid solution in hydrochloric, nitric acid, sulphuric acid, bromic acid.
4. the method for utilization Phosphoric Acid Selectively leaching lithium from lepidolite according to claim 1, it is characterised in that From lepidolite in the method for Selectively leaching lithium, preferred condition is lepidolite and Phosphoric Acid to described utilization Phosphoric Acid Solution is sized mixing by liquid-solid ratio 5.0, and total phosphorus is 3mol/L in solution, is reacted 8 hours in 95 DEG C.
CN201611232340.2A 2016-12-28 2016-12-28 A method of using Phosphoric Acid from lepidolite Selectively leaching lithium Active CN106591578B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115198109A (en) * 2022-05-27 2022-10-18 安徽大学绿色产业创新研究院 Method for extracting lithium from lithium-containing clay by mixed acid
CN115747520A (en) * 2022-11-18 2023-03-07 青海启迪清源新材料有限公司 Method for extracting lithium from lithium-containing ore

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010991A (en) * 2010-10-29 2011-04-13 江西本源新材料科技有限公司 Method for extracting lithium salt and removing potassium from lithium mica raw material
WO2012042714A1 (en) * 2010-09-29 2012-04-05 株式会社日立製作所 Lithium extraction method, and metal recovery method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012042714A1 (en) * 2010-09-29 2012-04-05 株式会社日立製作所 Lithium extraction method, and metal recovery method
CN102010991A (en) * 2010-10-29 2011-04-13 江西本源新材料科技有限公司 Method for extracting lithium salt and removing potassium from lithium mica raw material

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
冯文平等: ""硫酸浸取锂云母提锂方法的研究"", 《精细化工中间体》 *
郭春平等: ""锂云母硫酸盐法提锂研究"", 《无机盐工业》 *
黄礼煌 编著: "《化学选矿》", 30 April 2012, 冶金工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115198109A (en) * 2022-05-27 2022-10-18 安徽大学绿色产业创新研究院 Method for extracting lithium from lithium-containing clay by mixed acid
CN115747520A (en) * 2022-11-18 2023-03-07 青海启迪清源新材料有限公司 Method for extracting lithium from lithium-containing ore
CN115747520B (en) * 2022-11-18 2024-05-07 青海启迪清源新材料有限公司 Method for extracting lithium from lithium-containing ore

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Address before: 336000 Chun Chao Road, Yuanzhou District, Yichun, Jiangxi 16

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Address after: No. 36, Gongxin Avenue, Industrial Park, Yifeng County, Yichun City, Jiangxi Province, 336000

Patentee after: Yifeng Guoxuan Lithium Industry Co.,Ltd.

Address before: 336000 Jiangxi Yichun Yichun economic and Technological Development Zone, Yichun economic and Technological Development Zone No. 99 Chun Yi Road.

Patentee before: Yichun Ke Feng new material Co.,Ltd.