CN107699719A - A kind of Rare Earth Mine leachate impurity removal process - Google Patents
A kind of Rare Earth Mine leachate impurity removal process Download PDFInfo
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- CN107699719A CN107699719A CN201710933009.1A CN201710933009A CN107699719A CN 107699719 A CN107699719 A CN 107699719A CN 201710933009 A CN201710933009 A CN 201710933009A CN 107699719 A CN107699719 A CN 107699719A
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- rare earth
- leachate
- earth mine
- crystal seed
- removal process
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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
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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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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- General Life Sciences & Earth Sciences (AREA)
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- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of Rare Earth Mine leachate impurity removal process, comprise the following steps：Leachate is collected：Collect Rare Earth Mine leachate in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration；Leachate pre-processes：Obtained Rare Earth Mine leachate is subjected to separation of solid and liquid by dusting cover；Obtain the Rare Earth Mine leachate without solid；Add miscellaneous dose of suppression：Tartaric acid is added into the obtained Rare Earth Mine leachate without solid；Add crystal seed：Crystal seed is added by adding in the solution after pressing down miscellaneous dose, regulation pH value is 56, and control temperature treats that crystal seed is grown up at 30 40 DEG C；Filtering and impurity removing：After crystal seed is grown up, obtained material is subjected to vacuum filtration washing, obtains cleaning solution and removal of impurities slag；Wash liquor rare earth element：By cleaning solution by the way that rare-earth compound is obtained by extraction.The present invention is cleaned by adding miscellaneous dose of suppression and adding crystal seed, and dedoping step is simply rapid, does not bring impurity, does not produce waste, is brought great convenience to production.
Description
Technical field
The invention belongs to Rare Earth Mine extract technology, specifically, is related to a kind of Rare Earth Mine leachate impurity removal process.
Background technology
Rare earth is increasingly subject to extensive concern both domestic and external, rare earth is exactly Periodic as important strategic resource
Lanthanide series in table -- lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium
(Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), and it is closely related with 15 elements of group of the lanthanides
Two elements -- scandium (Sc) and yttrium (Y) totally 17 kinds of elements, referred to as rare earth element (RareEarth), abbreviation rare earth (RE or R).
From China ion adsorption type rare earth ore be found, name and maceration method extraction process invention after, ion type is dilute
Tu Kuang deposit impregnating technology is successively using sodium chloride and ammonium sulfate as leaching ore deposit agent, and depositing technology is successively using oxalic acid, ammonium hydrogen carbonate
Ammoniacal liquor, sodium carbonate etc. are used as precipitating reagent precipitating rare earth from rare earth feed liquid.Current production technology one is no impurity removal process, production
Product impurity is higher；Second, deposit impregnating technology and depositing technology use ammonium sulfate, oxalic acid and ammonium hydrogen carbonate, ammonium, nitrogen content discharge are exceeded,
Wastewater treatment difficulty is big, and in general manufacturer is all utilized without Sewage treatment, and environment is polluted, and indivedual producers are to portion
The waste water of split system is reclaimed, but cost recovery is very high.
In view of this it is special to propose the present invention.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided a kind of Rare Earth Mine leachate removal of impurities
Technique,
In order to solve the above technical problems, the present invention is using the basic conception of technical scheme：
A kind of Rare Earth Mine leachate impurity removal process, comprises the following steps：
S1：Leachate is collected：Collect Rare Earth Mine leachate in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration；
S2：Leachate pre-processes：Obtained Rare Earth Mine leachate is subjected to separation of solid and liquid by dusting cover；Obtain dilute without solid
Native ore deposit leachate；
S3：Add miscellaneous dose of suppression：Tartaric acid is added into the obtained Rare Earth Mine leachate without solid；
S4：Add crystal seed：Crystal seed is added by adding in the solution after pressing down miscellaneous dose, regulation pH value is 5-6, and control temperature is in 30-40
DEG C, treat that crystal seed is grown up；
S5：Filtering and impurity removing：After crystal seed is grown up, obtained material is subjected to vacuum filtration washing, obtains cleaning solution and removal of impurities slag；
S6：Wash liquor rare earth element：By cleaning solution by the way that rare-earth compound is obtained by extraction.
In the present invention, S1 middle rare earth ore deposits leachate be leachate containing Y either leachate containing Er or leachate containing Sc or
One or several kinds of mixtures in leachate containing La.
In the present invention, the sieve aperture of dusting cover is the mesh of 325 mesh -400 in S2.
In the present invention, the mass percent concentration that tartaric acid is added in S3 is 1.5%-2.5%.
In the present invention, the mass ratio of S3 mesotartaric acid and Rare Earth Mine leachate is 1:400-1:500.
In the present invention, crystal seed is one kind in crystal formation rare-earth oxalate, crystal formation rare earth carbonate in S4.
In the present invention, the mass ratio of crystal seed and Rare Earth Mine leachate is 1 in S4:100-1:200.
In the present invention, the granularity after crystal seed is grown up in S5 is the mesh of 30 mesh -100.
In the present invention, the vacuum degree control being filtered by vacuum in S5 is less than -0.1MPa.
In the present invention, cleaning solution is passed through to the technique of extraction in cross current solvent extraction, counter-current extraction and fractional extraction in S6
It is a kind of.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art.
The present invention is cleaned by adding miscellaneous dose of suppression and adding crystal seed, and dedoping step is simply rapid, does not bring impurity, no
Waste is produced, is brought great convenience to production.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in embodiment is clearly and completely described, following examples are used to illustrate the present invention, but are not limited to
The scope of the present invention.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；Can
To be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary.For this
For the those of ordinary skill in field, the concrete meaning of above-mentioned term in the present invention can be understood with concrete condition.
Embodiment 1
Collect the mixing of leachate containing Y and the leachate containing La in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration
Thing；Obtained Rare Earth Mine leachate is subjected to separation of solid and liquid by dusting cover；Sieve aperture is 400 mesh, obtains the Rare Earth Mine without solid
Leachate；Tartaric acid is added into the obtained Rare Earth Mine leachate without solid；The mass percent concentration of tartaric acid is
2.5%, the mass ratio of tartaric acid and Rare Earth Mine leachate is 1:500, add crystal seed, crystal seed by adding in the solution after pressing down miscellaneous dose
For crystal formation rare earth carbonate, the mass ratio of crystal seed and Rare Earth Mine leachate is 1:200, regulation pH value is 5.5, and control temperature is 40
DEG C, treat that crystal seed is grown up；After crystal seed is grown up, the granularity after crystal seed is grown up is 100 mesh, and obtained material is carried out into vacuum filtration washes
Wash, the vacuum degree control of vacuum filtration obtains cleaning solution and removal of impurities slag in -0.1MPa；By cleaning solution by the way that rare earth is obtained by extraction
Element compound, the technique of extraction is cross current solvent extraction.
Embodiment 2
Collect the mixing of leachate containing Er and the leachate containing Sc in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration
Thing；Obtained Rare Earth Mine leachate is subjected to separation of solid and liquid by dusting cover；Sieve aperture is 325 mesh, obtains the Rare Earth Mine without solid
Leachate；Tartaric acid is added into the obtained Rare Earth Mine leachate without solid；The mass percent concentration of tartaric acid is
1.5%, the mass ratio of tartaric acid and Rare Earth Mine leachate is 1:400, add crystal seed, crystal seed by adding in the solution after pressing down miscellaneous dose
For crystal formation rare-earth oxalate, the mass ratio of crystal seed and Rare Earth Mine leachate is 1:100, regulation pH value is 6, and control temperature is 40
DEG C, treat that crystal seed is grown up；After crystal seed is grown up, the granularity after crystal seed is grown up is 30 mesh, and obtained material is carried out into vacuum filtration washes
Wash, the vacuum degree control of vacuum filtration obtains cleaning solution and removal of impurities slag in -0.2MPa；By cleaning solution by the way that rare earth is obtained by extraction
Element compound, the technique of extraction is counter-current extraction.
Embodiment 3
Collect leachate containing Er in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration；Obtained Rare Earth Mine is leached
Liquid carries out separation of solid and liquid by dusting cover；Sieve aperture is 350 mesh, obtains the Rare Earth Mine leachate without solid；Be free of admittedly to what is obtained
Tartaric acid is added in the Rare Earth Mine leachate of body；The mass percent concentration of tartaric acid is 2%, tartaric acid and Rare Earth Mine leachate
Mass ratio be 1:450, add crystal seed by adding in the solution after miscellaneous dose of suppression, crystal seed is crystal formation rare-earth oxalate, crystal seed with it is dilute
The mass ratio of native ore deposit leachate is 1:150, regulation pH value is 5, and control temperature treats that crystal seed is grown up at 35 DEG C；After crystal seed is grown up,
Granularity after crystal seed is grown up is 50 mesh, and obtained material carried out into vacuum filtration washing, the vacuum degree control of vacuum filtration-
0.3MPa, obtain cleaning solution and removal of impurities slag；By cleaning solution by the way that rare-earth compound is obtained by extraction, the technique of extraction is fractionation
Extraction.
Described above is only presently preferred embodiments of the present invention, not makees any formal limitation to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any technology people for being familiar with this patent
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompting make it is a little change or be modified to
The equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit pair according to the present invention
Any simple modification, equivalent change and modification that above example is made, in the range of still falling within the present invention program.
Claims (10)
1. a kind of Rare Earth Mine leachate impurity removal process, it is characterised in that comprise the following steps：
S1：Leachate is collected：Collect Rare Earth Mine leachate in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration；
S2：Leachate pre-processes：Obtained Rare Earth Mine leachate is subjected to separation of solid and liquid by dusting cover；Obtain dilute without solid
Native ore deposit leachate；
S3：Add miscellaneous dose of suppression：Tartaric acid is added into the obtained Rare Earth Mine leachate without solid；
S4：Add crystal seed：Crystal seed is added by adding in the solution after pressing down miscellaneous dose, regulation pH value is 5-6, and control temperature is in 30-40
DEG C, treat that crystal seed is grown up；
S5：Filtering and impurity removing：After crystal seed is grown up, obtained material is subjected to vacuum filtration washing, obtains cleaning solution and removal of impurities slag；
S6：Wash liquor rare earth element：By cleaning solution by the way that rare-earth compound is obtained by extraction.
A kind of 2. Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that S1 middle rare earth ore deposit leachates
For one or several kinds of mixtures in leachate containing Y either leachate containing Er or leachate containing Sc or leachate containing La.
3. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that the sieve aperture of dusting cover is in S2
The mesh of 325 mesh -400.
4. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that tartaric acid is added in S3
Mass percent concentration is 1.5%-2.5%.
5. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that S3 mesotartaric acid and rare earth
The mass ratio of ore deposit leachate is 1:400-1:500.
6. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that crystal seed is that crystal formation is dilute in S4
One kind in native oxalates, crystal formation rare earth carbonate.
7. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that crystal seed and Rare Earth Mine in S4
The mass ratio of leachate is 1:100-1:200.
8. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that after crystal seed is grown up in S5
Granularity is the mesh of 30 mesh -100.
9. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that what is be filtered by vacuum in S5 is true
Reciprocal of duty cycle is controlled less than -0.1MPa.
10. a kind of Rare Earth Mine leachate impurity removal process according to claim 1, it is characterised in that lead to cleaning solution in S6
The technique for crossing extraction is one kind in cross current solvent extraction, counter-current extraction and fractional extraction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710933009.1A CN107699719A (en) | 2017-10-10 | 2017-10-10 | A kind of Rare Earth Mine leachate impurity removal process |
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| CN201710933009.1A CN107699719A (en) | 2017-10-10 | 2017-10-10 | A kind of Rare Earth Mine leachate impurity removal process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418506A (en) * | 2022-08-27 | 2022-12-02 | 萍乡鑫森新材料有限责任公司 | Impurity removal method for rare earth ore extraction |
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| CN101186968A (en) * | 2006-11-24 | 2008-05-28 | 江西赣锋锂业有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115418506A (en) * | 2022-08-27 | 2022-12-02 | 萍乡鑫森新材料有限责任公司 | Impurity removal method for rare earth ore extraction |
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Application publication date: 20180216 |