CN107619956A - A kind of Rare Earth Mine precipitation roasting extraction process - Google Patents
A kind of Rare Earth Mine precipitation roasting extraction process Download PDFInfo
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- CN107619956A CN107619956A CN201710933115.XA CN201710933115A CN107619956A CN 107619956 A CN107619956 A CN 107619956A CN 201710933115 A CN201710933115 A CN 201710933115A CN 107619956 A CN107619956 A CN 107619956A
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- leachate
- rare earth
- precipitation
- cleaning solution
- earth mine
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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
Abstract
The invention discloses a kind of Rare Earth Mine to precipitate roasting extraction process, comprises the following steps：Leachate is collected；Leachate pre-processes；PH of leaching solution is adjusted：The pH value for adjusting leachate is 5.1 5.2；Leachate filtering and impurity removing：Leachate after regulation pH value is subjected to vacuum filtration washing, obtains cleaning solution and removal of impurities slag；The temperature for adjusting cleaning solution is 30 40 DEG C；Flocculant is added in cleaning solution, is stirred；Adjust cleaning solution pH value dynamic precipitation：The pH value for adjusting cleaning solution is 9 11, and the speed that control ph rises is 1 2/h, carries out dynamic precipitation, and then vacuum filtration washing, obtains precipitation slag and supernatant；Precipitation slag is calcined：Obtained precipitation slag is put into roaster and is calcined, the material obtained after roasting is rare earth oxide.The present invention carries out cross-linking reaction, accelerates settling velocity, improve deposition efficiency, what it is due to addition is organic flocculant, volatilization of being burnt in roasting process, does not influence the extraction of rare earth by adding flocculant in precipitation process.
Description
Technical field
The invention belongs to Extraction of rare eart technology, specifically, is related to a kind of Rare Earth Mine precipitation roasting extraction 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 two closely related with 15 elements of group of the lanthanides
Element -- scandium (Sc) and yttrium (Y) totally 17 kinds of elements, referred to as rare earth element (RareEarth), abbreviation rare earth (RE or R).
Chemical precipitation is the important process of Extraction of rare eart, but often occurs that precipitation is not thorough in precipitation process, precipitation
The problems such as process is long, cross-linking reaction are often used in precipitation process as a kind of technology by the poly- figure of molecule.
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 precipitation roasting carries
Taking 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 precipitation roasting extraction 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：PH of leaching solution is adjusted：Sodium hydroxide calcium or carbonic acid are added into the obtained Rare Earth Mine leachate without solid
Calcium either one kind in calcium bicarbonate or oxalic acid, the pH value for adjusting leachate is 5.1-5.2；
S4：Leachate filtering and impurity removing：Leachate after regulation pH value is subjected to vacuum filtration washing, obtains cleaning solution and removal of impurities
Slag；
S5：Cleaning solution temperature adjustment：The temperature for adjusting cleaning solution is 30-40 DEG C；
S6：Flocculant is adjusted：Flocculant is added in cleaning solution, is stirred；
S7：Adjust cleaning solution pH value dynamic precipitation：Sodium hydroxide calcium either calcium carbonate or carbon are added into obtained leachate
One kind in sour hydrogen calcium or oxalic acid, the pH value for adjusting cleaning solution are 9-11, and the speed that control ph rises is 1-2/h, is carried out
Dynamic precipitation, then vacuum filtration washing, obtains precipitation slag and supernatant；
S8：Precipitation slag is calcined：Obtained precipitation slag is put into roaster and is calcined, sintering temperature is controlled in 900-1000
DEG C, the material that roasting time control obtains after 1-2 hours, roasting is rare earth oxide.
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 vacuum degree control being filtered by vacuum in S4 is less than -0.1MPa.
In the present invention, the method for cleaning solution temperature adjustment is heating water bath in S5.
In the present invention, flocculant is organic polymer coargulator in S6.
In the present invention, organic polymer coargulator is starch, cellulose, chitosan etc. and one kind in acrylamide.
In the present invention, the time control of dynamic precipitation is in 3-5 hours in S7.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art.
The present invention carries out cross-linking reaction, accelerates settling velocity, improve precipitation effect by adding flocculant in precipitation process
Rate, what it is due to addition is organic flocculant, volatilization of being burnt in roasting process, does not influence the extraction of rare earth.
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
In embodiment, the technical scheme in embodiment is clearly and completely described, following examples be used for illustrate the present invention,
But it is not limited to the scope of the present invention.
It is term " on ", " under ", "front", "rear", "left", "right", " perpendicular in the description of the invention, it is necessary to explanation
Directly ", the orientation of the instruction such as " interior ", " outer " or position relationship be based on the orientation or position relationship shown in embodiment, merely to
Be easy to the description present invention and simplify description, rather than instruction or imply signified device or element must have specific orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the 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
Leachate containing La is collected in the mineral deposit downstream leached from Stope leaching mineral deposit downstream or diafiltration, and obtained Rare Earth Mine is leached
Liquid carries out separation of solid and liquid by dusting cover；The sieve aperture of dusting cover is 325 mesh, obtains the Rare Earth Mine leachate without solid；To what is obtained
Sodium hydroxide calcium is added in Rare Earth Mine leachate without solid, the pH value for adjusting leachate is 5.1；By the leaching after regulation pH value
Go out liquid and carry out vacuum filtration washing, the vacuum degree control of vacuum filtration obtains cleaning solution and removal of impurities slag in -0.1MPa；Regulation is washed
The temperature for washing liquid is 35 DEG C；The method of cleaning solution temperature adjustment is heating water bath, and starch is added in cleaning solution, is stirred；
Sodium hydroxide calcium is added into obtained leachate, the pH value for adjusting cleaning solution is 10, and the speed that control ph rises is 1.5/
H, carries out dynamic precipitation, and the time control of dynamic precipitation at 3.5 hours and then is filtered by vacuum washing, obtains precipitation slag and supernatant
Liquid；Obtained precipitation slag is put into roaster and is calcined, at 950 DEG C, roasting time control is small 1.5 for sintering temperature control
When, the material obtained after roasting is rare earth oxide.
Embodiment 2
Collect the mixing of leachate containing Y and the leachate containing Er 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；The sieve aperture of dusting cover is 400 mesh, is obtained without solid
Rare Earth Mine leachate；Calcium carbonate is added into the obtained Rare Earth Mine leachate without solid, the pH value for adjusting leachate is
5.2；The leachate after pH value will be adjusted and carry out vacuum filtration washing, the vacuum degree control of vacuum filtration is washed in -0.2MPa
Wash liquid and removal of impurities slag；The temperature for adjusting cleaning solution is 40 DEG C；The method of cleaning solution temperature adjustment is heating water bath, in cleaning solution
Flocculant is added, flocculant is cellulose, is stirred；Calcium carbonate is added into obtained leachate, adjusts the pH of cleaning solution
It is worth for 9, the speed that control ph rises be 1.2/h, carries out dynamic precipitation, and the time control of dynamic precipitation is at 4 hours and then very
Empty filtering and washing, obtains precipitation slag and supernatant；Obtained precipitation slag is put into roaster and is calcined, sintering temperature control
At 1000 DEG C, roasting time was controlled at 1 hour, and the material obtained after roasting is rare earth oxide.
Embodiment 3
Collect leachate containing Sc 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；The sieve aperture of dusting cover is 325 mesh, obtains the Rare Earth Mine leachate without solid；To what is obtained
Oxalic acid is added in Rare Earth Mine leachate without solid, the pH value for adjusting leachate is 5.2；Leachate after regulation pH value is entered
Row vacuum filtration washing, the vacuum degree control of vacuum filtration obtain cleaning solution and removal of impurities slag in -0.3MPa；Adjust cleaning solution
Temperature is 30 DEG C；The method of cleaning solution temperature adjustment is heating water bath, and chitosan is added in cleaning solution, is stirred；Xiang get
Oxalic acid is added in the leachate arrived, the pH value for adjusting cleaning solution is 11, and the speed that control ph rises is 2/h, enters Mobile state and sinks
Form sediment, the time control of dynamic precipitation at 3 hours and then is filtered by vacuum washing, obtains precipitation slag and supernatant；The precipitation that will be obtained
Slag is put into roaster and is calcined, and sintering temperature control is at 900 DEG C, and roasting time control was at 2 hours, the thing obtained after roasting
Material is rare earth oxide.
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 (8)
1. a kind of Rare Earth Mine precipitation roasting extraction 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：PH of leaching solution is adjusted：Sodium hydroxide calcium or carbonic acid are added into the obtained Rare Earth Mine leachate without solid
Calcium either one kind in calcium bicarbonate or oxalic acid, the pH value for adjusting leachate is 5.1-5.2；
S4：Leachate filtering and impurity removing：Leachate after regulation pH value is subjected to vacuum filtration washing, obtains cleaning solution and removal of impurities
Slag；
S5：Cleaning solution temperature adjustment：The temperature for adjusting cleaning solution is 30-40 DEG C；
S6：Flocculant is adjusted：Flocculant is added in cleaning solution, is stirred；
S7：Adjust cleaning solution pH value dynamic precipitation：Sodium hydroxide calcium either calcium carbonate or carbon are added into obtained leachate
One kind in sour hydrogen calcium or oxalic acid, the pH value for adjusting cleaning solution are 9-11, and the speed that control ph rises is 1-2/h, is carried out
Dynamic precipitation, then vacuum filtration washing, obtains precipitation slag and supernatant；
S8：Precipitation slag is calcined：Obtained precipitation slag is put into roaster and is calcined, sintering temperature is controlled in 900-1000
DEG C, the material that roasting time control obtains after 1-2 hours, roasting is rare earth oxide.
2. a kind of Rare Earth Mine precipitation roasting extraction process according to claim 1, it is characterised in that S1 middle rare earth ore deposit leaches
Liquid is one or several kinds of mixing of the leachate containing Y either in leachate containing Er or leachate containing Sc or leachate containing La
Thing.
A kind of 3. Rare Earth Mine precipitation roasting extraction process according to claim 1, it is characterised in that the sieve aperture of dusting cover in S2
For the mesh of 325 mesh -400.
4. a kind of Rare Earth Mine precipitation roasting extraction process according to claim 1, it is characterised in that be filtered by vacuum in S4
Vacuum degree control is less than -0.1MPa.
A kind of 5. Rare Earth Mine precipitation roasting extraction process according to claim 1, it is characterised in that cleaning solution temperature in S5
The method of regulation is heating water bath.
6. a kind of Rare Earth Mine precipitation roasting extraction process according to claim 1, it is characterised in that flocculant is to have in S6
Machine high polymer coagulant.
7. a kind of Rare Earth Mine precipitation roasting extraction process according to claim 6, it is characterised in that organic polymer flocculates
Agent is starch, cellulose, chitosan etc. and one kind in acrylamide.
A kind of 8. Rare Earth Mine precipitation roasting extraction process according to claim 1, it is characterised in that dynamic precipitation in S7
Time control is in 3-5 hours.
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| CN201710933115.XA CN107619956A (en) | 2017-10-10 | 2017-10-10 | A kind of Rare Earth Mine precipitation roasting extraction process |
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| CN201710933115.XA CN107619956A (en) | 2017-10-10 | 2017-10-10 | A kind of Rare Earth Mine precipitation roasting extraction process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735708A (en) * | 2019-03-21 | 2019-05-10 | 江西理工大学 | A kind of weathered superficial leaching rare-earth ore leaching agent and leaching method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033976A (en) * | 1988-01-08 | 1989-07-19 | 赣州有色冶金研究所 | Use the mixed precipitant precipitating rare earth |
| CN101476033A (en) * | 2008-10-28 | 2009-07-08 | 黄日平 | Novel method for leaching, impurity removing and precipitating ion type rare earth ore |
| WO2014021119A1 (en) * | 2012-08-02 | 2014-02-06 | 株式会社 日立製作所 | Method and apparatus for separating and recovering rare earth elements |
| CN104711424A (en) * | 2015-03-31 | 2015-06-17 | 武汉工程大学 | Method for recovering rare earth and aluminum from weathered crust ion-adsorption type rare earth ore lixivium impurity-removal slags |
| CN105803226A (en) * | 2016-03-25 | 2016-07-27 | 长沙矿冶研究院有限责任公司 | Method for extracting rare earth and aluminum from ion adsorption type rare earth ores |
| CN106967881A (en) * | 2017-05-26 | 2017-07-21 | 江西理工大学 | A kind of method of the Extraction of rare earth from weathered superficial leaching rare-earth ore |
-
2017
- 2017-10-10 CN CN201710933115.XA patent/CN107619956A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033976A (en) * | 1988-01-08 | 1989-07-19 | 赣州有色冶金研究所 | Use the mixed precipitant precipitating rare earth |
| CN101476033A (en) * | 2008-10-28 | 2009-07-08 | 黄日平 | Novel method for leaching, impurity removing and precipitating ion type rare earth ore |
| WO2014021119A1 (en) * | 2012-08-02 | 2014-02-06 | 株式会社 日立製作所 | Method and apparatus for separating and recovering rare earth elements |
| CN104711424A (en) * | 2015-03-31 | 2015-06-17 | 武汉工程大学 | Method for recovering rare earth and aluminum from weathered crust ion-adsorption type rare earth ore lixivium impurity-removal slags |
| CN105803226A (en) * | 2016-03-25 | 2016-07-27 | 长沙矿冶研究院有限责任公司 | Method for extracting rare earth and aluminum from ion adsorption type rare earth ores |
| CN106967881A (en) * | 2017-05-26 | 2017-07-21 | 江西理工大学 | A kind of method of the Extraction of rare earth from weathered superficial leaching rare-earth ore |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735708A (en) * | 2019-03-21 | 2019-05-10 | 江西理工大学 | A kind of weathered superficial leaching rare-earth ore leaching agent and leaching method |
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Application publication date: 20180123 |