CN102936665B - Method for extracting rare earth elements - Google Patents
Method for extracting rare earth elements Download PDFInfo
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- CN102936665B CN102936665B CN2012105255845A CN201210525584A CN102936665B CN 102936665 B CN102936665 B CN 102936665B CN 2012105255845 A CN2012105255845 A CN 2012105255845A CN 201210525584 A CN201210525584 A CN 201210525584A CN 102936665 B CN102936665 B CN 102936665B
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 117
- 239000007788 liquid Substances 0.000 claims abstract description 70
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000725 suspension Substances 0.000 claims abstract description 4
- 239000012530 fluid Substances 0.000 claims description 15
- 239000000470 constituent Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 abstract 2
- 239000012071 phase Substances 0.000 description 19
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000016507 interphase Effects 0.000 description 5
- 239000012074 organic phase Substances 0.000 description 4
- -1 rare earth salts Chemical class 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 2
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- JJJOZVFVARQUJV-UHFFFAOYSA-N 2-ethylhexylphosphonic acid Chemical compound CCCCC(CC)CP(O)(O)=O JJJOZVFVARQUJV-UHFFFAOYSA-N 0.000 description 1
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical group CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241000040710 Chela Species 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- VYRDHRYMAZWQJH-UHFFFAOYSA-N [P].P Chemical compound [P].P VYRDHRYMAZWQJH-UHFFFAOYSA-N 0.000 description 1
- 150000001257 actinium Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- SRUKOJDGOUUFRB-UHFFFAOYSA-N heptylazanium;chloride Chemical compound Cl.CCCCCCCN SRUKOJDGOUUFRB-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical group 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- UXBZSSBXGPYSIL-UHFFFAOYSA-N phosphoric acid;yttrium(3+) Chemical compound [Y+3].OP(O)(O)=O UXBZSSBXGPYSIL-UHFFFAOYSA-N 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 description 1
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Classifications
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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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- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for extracting rare earth elements and a rare earth extraction system. The method comprises the following steps: inputting quantitative water solution or suspension, as heavy liquid, of rare earth elements into an extraction tank via a heavy liquid inlet at the top of the extraction tank; starting a stirring shaft; filling an extraction solvent as light liquid into the extraction tank uniformly from a liquid distributor at the bottom of the extraction tank, ensuring step-by-step mixing and mass transfer from bottom to top between the light liquid and the heavy liquid in the stirring process and enabling the light phase liquid completing mass transfer to overflow into a decanting tank from the top of the extraction tank; after the light phase liquid is decanted in the decanting tank, discharging the light components via a light liquid outlet at the top of the decanting tank; judging whether extraction is completed by detecting the concentrations of the needed rare earth elements in the light component solution discharged from the decanting tank; after extraction is completed, stopping input of the light liquid and starting an emptying valve below the decanting tank to empty the decanting tank; and discharging the heavy liquid in the extraction tank via a heavy liquid outlet at the bottom of the extraction tank.
Description
The application divides an application, the application number of original application: 201110222358.5, and invention and created name: the method for extracting rare-earth element and extracting system, the applying date: 2011-8-4.
Technical field
The present invention relates to a kind of method and rare earth extraction system of extracting rare-earth element.
Background technology
Rare earth is exactly lanthanon in the periodic table of chemical element--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 with closely-related two elements of 15 elements of group of the lanthanides--scandium (Sc) and yttrium (Y) be totally 17 kinds of elements, be called rare earth element (Rare Earth), be called for short rare earth (RE or R).
In the course of processing of the smelting of rare earth and the main primary products of rare earth, used a large amount of chemical reagent, cause annual nearly more than 200 ten thousand tons of the RE waste water that produces of China.How to reclaim these rare earth elements by extraction, be the technical problem that the field will solve.
Solvent extration is suitable for producing in batches from the lanthanum to the erbium and the higher rare earth element of abundance such as yttrium.
The solvent extraction and separation method refers in the aqueous solution of separated material, add organic solvent a kind of and that water is not miscible, by means of the effect of extraction agent, make one or more components enter organic phase, other components are still stayed aqueous phase, thereby reach the purpose of separation.
Existing a kind of rare earth element extracting system, quantitative rare earth element is suspended pours in extractor often, then sends into quantitative solvent from tank deck, then heats and opens stirring, and feed liquid is fully mixed with solvent.Then stop stirring, after static for some time, the weight component in tank is in respectively levels, and this moment is as long as the leakage fluid dram of opening on tank wall is discharged light component.The weak point of the prior art is: laminated fluid level can only pass through top visor artificial observation, is difficult to determine the tram of layering.The drain pipe position of light liquid is difficult transfers, or light liquid puts endless, or also emits together with heavy-fluid, and thoroughly or gently loss is large mutually to cause extracting and separating.
The device of the solvent extraction rare earth element that another kind is common is multi-stage countercurrent mixing-settler, two kinds of liquid phase flows in this equipment, and both entirely different objectionable interminglings, a kind of is the aqueous solution of rare earth salts, another kind is organic phase or the solvent phase of " oil ".During both counter current contact, due to the difference of each rare earth element to TBP, D2EHPA equal solvent or the existence of chela platform agent avidity in organic phase, part rare earth enters organic phase, another part is stayed in solution, multiple-contact and the reallocation of process two-phase in mixer-settlerss at different levels like this, repeat artificially, superpose, enlarge this difference, can reach the purpose that the multielement grouping separates with single-element.Ion exchange method ratio with batch-type, extraction process can be processed highly concentrated solution continuously, cost is low, is fit to batch production, and this method has developed into the effective ways of most rare earth elements (at least 11 kinds) in technical scale separation and purification hamartite, monazite and xenotime.The weak point of the prior art is: space hold is large, initial investment cost higher (for to make the purity of each single rare earth product reach 99.99%, often using the mixer-settlers device more than 1000 grades), percentage extraction are lower.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of simple in structure, percentage extraction is higher, with low cost and space hold is less extracting rare-earth element.
In order to solve the problems of the technologies described above, the extracting system that adopts in the method for extracting rare-earth element provided by the invention comprises: extraction is carried tank; The top that described extraction is carried tank is provided with heavy liquid inlet and light phase export, and the bottom that extraction is carried tank is provided with light liquid entrance and heavy out; The top that described extraction is carried tank is provided with a settling tank, and the light phase export that extraction is carried tank is connected with the bottom of this settling tank, and the top of this settling tank is provided with the light liquid outlet.Be provided with multistage rotating ring and stationary ring in tank, artificially a large extraction carried tank and be separated into a plurality of little extractions and carry tank, greatly increased the area of interphase mass transfer, reduced the mass transfer volume, saved the installing space of equipment.
During use, the heavy phase that described extraction is carried in tank is fixed, and the light liquid entrance of gently carrying pot bottom from extraction enters continuously and is spilled over to settling tank from described light phase export.
Particularly, the central axis that described extraction is carried tank is provided with stir shaft, the bottom of this stir shaft is provided with blade, described extraction carry in tank and on described stir shaft axial distribution have a plurality of stirring rings, described extraction to carry the inwall of tank and stir ring with each to be staggered and to be distributed with a plurality of stationary rings.Described extraction is carried tank for adopting the jacketed type tank body of hot steam or hot water heating, insulation, can put to regulate according to the optimum temps of different interphase mass transfers, thereby make mass transfer velocity reach the fastest.Extraction temperature should be 20-30 ℃ more suitable.
The method of described extracting rare-earth element comprises: the heavy liquid inlet that the aqueous solution of quantitative rare earth element as heavy-fluid or suspension are carried the top of tank by extraction is inputted this extraction and is carried in tank; Start stir shaft; Simultaneously, extraction is proposed the tank heating, the feed liquid that allows extraction carry in tank remains on preset temp.To enter equably extraction as the liquid distributor that the extraction solvent of light liquid is carried pot bottom from extraction and carry tank, and in whipping process, realize from bottom to top mixing step by step, mass transfer between light, heavy-fluid, the light phase liquid of completing mass transfer is proposed the tank top overflow from extraction and is entered settling tank; After light phase liquid was clarified in settling tank, light constituent was discharged by the light liquid mouth at settling tank top; By detecting the concentration of the required rare earth element from the light constituent solution that settling tank is discharged, judgement is extracted or whether extraction is completed; After extracting or extraction complete, stop the input of light liquid, open the blow-off valve of settling tank below, the emptying settling tank; Extraction is carried the heavy liquid exit that the heavy-fluid in tank carries pot bottom through extraction emits.
Further, the bottom interior wall that described extraction is carried tank is provided with the first sparger that is connected with described light liquid entrance, so that this solvent evenly enters in tank.
Further, the top inner wall that described extraction is carried tank is provided with the second sparger that is connected with described heavy liquid inlet, so that this feed liquid evenly enters in tank.
Further, each stirs ring and is evenly distributed on described stir shaft, and each stationary ring is evenly distributed on the inwall that described extraction is carried tank.Due to the distribution that is staggered of adjacent described stirring ring and stationary ring, make between light liquid and heavy-fluid realize mixing step by step from bottom to top, mass transfer, until light phase feed liquid enters settling tank from the tank top overflow when completing mass transfer.
Further, the radius sum of the width of described stirring ring and described stationary ring is carried the radius of tank less than described extraction, to form the rising passway of a solvent, makes solvent and feed liquid fully mix to realize from bottom to top stage-by-stage extraction or extraction.
Technique scheme of the present invention has the following advantages compared to existing technology: extracting system of the present invention has been broken traditional technique, extraction section is shortened, make a similar extractor that is formed by a plurality of traditional stirred pots, heavy phase is fixed in tank, can by detect settling tank output light mutually in the concentration of required Rare Earth Elements Determination, adjust at any time consumption and the working hour of light liquid, thereby improved working efficiency, saved the consumption of light liquid, also satisfy the requirement of actual production.When (2) the present invention works, by detecting the content of the Rare Earth Elements Determination in light phase fluid, judge whether feed liquid extracts complete, percentage extraction can reach 100%.(3) stir shaft in the present invention adopts speed control by frequency variation, stirs velocity of shear by adjusting, can accelerate interphase mass transfer speed, guarantees simultaneously not emulsification.A plurality of stirring rings, stationary ring that extraction is carried in tank are divided into a plurality of little extraction cells with tank body, thereby the interphase mass transfer area is strengthened, and are beneficial to the quickening mass transfer, and further make mass transfer fully, thoroughly.(4) the present invention adopt heavy phase fix, gently from tank base input and the mode of operation of overflowing from the tank body top continuously, can make interphase mass transfer fully, thoroughly, guaranteed high percentage extraction, and simple to operate, at utmost reduced the consumption of extraction agent.(5) extraction solvent of the present invention can adopt acid phosphorus (phosphine) acid esters or nitrogenous chelating extractant; The form of oxine (HQ) extraction lanthanum is LaQ3; And the form of extraction praseodymium, europium, holmium, ytterbium is LnQ32HQ, is LnQ33HQ in high HQ concentration; When adding 1,10-phenanthroline (phen) or n-heptyl ammonium chloride (R4NCl), the extraction form is LnQ32HQphen or R4NLnQ4HQ, and can improve the separation performance of rare earth; In KelexX100(7-Cl-2-thiazolinyl-3,3,6,6-tetramethyl-hexyl)-oxine or 1,10-phenanthroline has promoter action to extraction with separating.In addition, be one of good extraction agent of group of the lanthanides, actinium series and alkaline-earth metal to 1-phenyl-3-methyl-4-Benzoylpyrazols ketone [PMBP].
Description of drawings
For content of the present invention is more likely to be clearly understood, below the specific embodiment and by reference to the accompanying drawings of basis, the present invention is further detailed explanation, wherein
Fig. 1 is the structural representation of rare earth extraction of the present invention system.
Embodiment
Embodiment 1
See Fig. 1, the rare earth extraction system of the present embodiment comprises: extraction carries tank 1, be located at this extraction carry on the central axis of tank 1 and the bottom is provided with the stir shaft 2 of blade 4, described extraction is carried tank 1 in and on described stir shaft 2 axial distribution a plurality of stirring rings 3, be located at described extraction and carry the inwall of tank 1 and stir be staggered a plurality of stationary rings 5 of distribution of ring 3 with each; The top that described extraction is carried tank 1 is provided with for the heavy liquid inlet of inputting heavy-fluid with for the light phase export of exporting light feed liquid mutually, and the bottom that extraction is carried tank 1 is provided with for the light liquid entrance of input light liquid with for the heavy out of exporting heavy phase; The top that described extraction is carried tank 1 is provided with a settling tank 8, and the light phase export that extraction is carried tank 1 is connected with the bottom of this settling tank 8, and the top of this settling tank 8 is provided with the light liquid outlet.During use, the heavy phase that described extraction is carried in tank 1 is fixed, and the light liquid entrance of gently carrying tank 1 from extraction enters continuously and is spilled over to settling tank 8 from described light phase export.
Described extraction is carried tank 1 for adopting the jacketed type tank body of hot steam or hot water heating, insulation.
The bottom interior wall that described extraction is carried tank 1 is provided with the first sparger that is connected with described light liquid entrance, and this solvent sparger is ring pipe, is distributed with hydrojet perforate up on body.
The top inner wall that described extraction is carried tank 1 is provided with the second sparger that is connected with described heavy liquid inlet, and this liquid distributor is ring pipe, is distributed with hydrojet perforate down on body.
Each stirs ring 3 and is evenly distributed on described stir shaft 2, and each stationary ring 5 is evenly distributed on the inwall that described extraction is carried tank 1.The radius sum of the width of described stirring ring 3 and described stationary ring 5 is carried the radius of tank 1 less than described extraction.In Fig. 1
, control described extraction for the flow of controlling hot steam and carry the interior solution temperature of tank 1.
The method of above-mentioned rare earth extraction system extracting rare-earth element comprises:
The heavy liquid inlet that the aqueous solution of quantitative rare earth element as heavy-fluid or suspension are carried the top of tank 1 by extraction is inputted this extraction and is carried in tank 1 (when specifically implementing, can carry by this extraction the glass visor observation liquid level at tank (1) top, when liquid level arrives preset height, stop the feed liquid input; );
Start stir shaft 2; Simultaneously, extraction is proposed tank 1 heating, the feed liquid that allows extraction carry in tank 1 remains on preset temp;
To enter equably extraction as the liquid distributor that the extraction solvent of light liquid is carried tank 1 bottom from extraction carries tank 1, in whipping process, gently, realize from bottom to top mixing step by step, mass transfer between heavy-fluid, the light phase liquid of completing mass transfer is proposed tank 1 top overflow from extraction and is entered settling tank 8;
Light phase liquid is after the interior clarification of settling tank 8, and light constituent is discharged by the light liquid mouth at settling tank 8 tops;
By detecting the concentration of the required rare earth element from the light constituent solution that settling tank 8 is discharged, judgement is extracted or whether extraction is completed;
After extracting or extraction complete, stop the input of light liquid, open the blow-off valve 7 of settling tank 8 belows, emptying settling tank 8;
Extraction is carried the heavy liquid exit that the heavy-fluid in tank 1 carries tank 1 bottom through extraction emits.
Adopt extraction agent to mainly include a kind of in machine phosphoric acid, amine and carboxylic-acid, as two-(2 one ethylhexyl) phosphonic acids (P204), the own ester of 2-ethylhexyl phosphonic acid single 2-ethyl (P-507), tertiary monocarboxylic acid, quaternary amine, naphthenic acid etc.
Obviously, above-described embodiment is only for example of the present invention clearly is described, and is not to be restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And these belong to apparent variation or the change that spirit of the present invention extended out and still are among protection scope of the present invention.
Claims (1)
1. the method for an extracting rare-earth element is characterized in that:
The rare earth extraction system that adopts comprises: extraction is carried tank (1), and the top that this extraction is carried tank (1) is provided with heavy liquid inlet and light phase export, and the bottom that extraction is carried tank (1) is provided with light liquid entrance and heavy out; The top that extraction is carried tank (1) is provided with a settling tank (8), and the light phase export that extraction is carried tank (1) is connected with the bottom of this settling tank (8), and the top of this settling tank (8) is provided with the light liquid outlet; The central axis that described extraction is carried tank (1) is provided with stir shaft (2), the bottom of this stir shaft (2) is provided with blade (4), in described extraction is carried tank (1) and in the upper axial distribution of described stir shaft (2), a plurality of stirring rings (3) are arranged, described extraction is carried on the inwall of tank (1) and is stirred ring (3) and is staggered and is distributed with a plurality of stationary rings (5) with each;
The method of described extracting rare-earth element comprises:
The heavy liquid inlet that the aqueous solution of quantitative rare earth element as heavy-fluid or suspension are carried the top of tank (1) by extraction is inputted this extraction and is carried in tank (1);
Start stir shaft (2);
To enter equably extraction as the liquid distributor of extraction solvent bottom extraction is carried tank (1) of light liquid carries tank (1), in whipping process, gently, realize from bottom to top mixing step by step, mass transfer between heavy-fluid, the light phase liquid of completing mass transfer is proposed tank (1) top overflow from extraction and is entered settling tank (8);
After light phase liquid was clarified in settling tank (8), light constituent was discharged by the light liquid mouth at settling tank (8) top;
By detecting the concentration of the required rare earth element from the light constituent solution that settling tank (8) is discharged, judgement is extracted or whether extraction is completed;
After extracting or extraction complete, stop the input of light liquid, open the blow-off valve (7) of settling tank (8) below, emptying settling tank (8);
Extraction is carried the heavy liquid exit that the heavy-fluid in tank (1) carries tank (1) bottom through extraction emits;
Extraction is carried tank (1) for adopting the jacketed type tank body of hot steam or hot water heating, insulation;
In described startup stir shaft (2), extraction is proposed tank (1) heating, the feed liquid that allows extraction carry in tank (1) remains on preset temp;
Each stirs ring (3) and is evenly distributed on described stir shaft (2), and each stationary ring (5) is evenly distributed on the inwall that described extraction is carried tank (1).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105255845A CN102936665B (en) | 2011-08-04 | 2011-08-04 | Method for extracting rare earth elements |
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| CN2012105255845A CN102936665B (en) | 2011-08-04 | 2011-08-04 | Method for extracting rare earth elements |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011102223585A Division CN102277493B (en) | 2011-08-04 | 2011-08-04 | Method for extracting rare earth elements and rare earth extraction system |
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| CN102936665A CN102936665A (en) | 2013-02-20 |
| CN102936665B true CN102936665B (en) | 2013-11-06 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042570A (en) * | 1989-12-04 | 1990-05-30 | 北京大学 | High-purity terbium oxide preparation by use of fractional extraction method |
| CN1121843A (en) * | 1995-08-01 | 1996-05-08 | 新疆大学 | Method and apparatus for separating several metal chlorides by electrolysis and extraction |
| CN1154416A (en) * | 1995-12-13 | 1997-07-16 | Cytec技术有限公司 | Extraction of rare earth elements |
| CN2507536Y (en) * | 2001-08-26 | 2002-08-28 | 龚贺 | Tank mixing and clarifying device for extraction or reaction |
| CN101787438A (en) * | 2009-01-23 | 2010-07-28 | 胡建康 | Method for precipitating rare earth by adopting carbon dioxide |
| CN201648485U (en) * | 2010-03-25 | 2010-11-24 | 江阴加华新材料资源有限公司 | Device for removing slag in return pipe of rare earth extraction tank body |
| CN201664526U (en) * | 2009-11-16 | 2010-12-08 | 陆文光 | Centrifugal stirring type extracting tower |
-
2011
- 2011-08-04 CN CN2012105255845A patent/CN102936665B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042570A (en) * | 1989-12-04 | 1990-05-30 | 北京大学 | High-purity terbium oxide preparation by use of fractional extraction method |
| CN1121843A (en) * | 1995-08-01 | 1996-05-08 | 新疆大学 | Method and apparatus for separating several metal chlorides by electrolysis and extraction |
| CN1154416A (en) * | 1995-12-13 | 1997-07-16 | Cytec技术有限公司 | Extraction of rare earth elements |
| CN2507536Y (en) * | 2001-08-26 | 2002-08-28 | 龚贺 | Tank mixing and clarifying device for extraction or reaction |
| CN101787438A (en) * | 2009-01-23 | 2010-07-28 | 胡建康 | Method for precipitating rare earth by adopting carbon dioxide |
| CN201664526U (en) * | 2009-11-16 | 2010-12-08 | 陆文光 | Centrifugal stirring type extracting tower |
| CN201648485U (en) * | 2010-03-25 | 2010-11-24 | 江阴加华新材料资源有限公司 | Device for removing slag in return pipe of rare earth extraction tank body |
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| CN102936665A (en) | 2013-02-20 |
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