CN114574697A - Method for extracting and separating rare earth neodymium from phosphate ionic liquid - Google Patents
Method for extracting and separating rare earth neodymium from phosphate ionic liquid Download PDFInfo
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 128
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 118
- 229910052779 Neodymium Inorganic materials 0.000 title claims abstract description 100
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 48
- 239000010452 phosphate Substances 0.000 title claims abstract description 48
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 44
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 113
- 239000002994 raw material Substances 0.000 claims abstract description 49
- 239000012071 phase Substances 0.000 claims abstract description 34
- -1 rare earth chloride Chemical class 0.000 claims abstract description 33
- 238000000926 separation method Methods 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 238000005191 phase separation Methods 0.000 claims abstract description 3
- 230000010355 oscillation Effects 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 7
- 230000008929 regeneration Effects 0.000 claims description 7
- 238000011069 regeneration method Methods 0.000 claims description 7
- 239000002274 desiccant Substances 0.000 claims description 5
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 abstract description 14
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052746 lanthanum Inorganic materials 0.000 abstract description 13
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052777 Praseodymium Inorganic materials 0.000 abstract description 12
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 abstract description 12
- 239000003085 diluting agent Substances 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 3
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical group [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010790 dilution Methods 0.000 abstract description 2
- 239000012895 dilution Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000007127 saponification reaction Methods 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 description 38
- 239000004803 Di-2ethylhexylphthalate Substances 0.000 description 24
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 24
- 238000002360 preparation method Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000425 proton nuclear magnetic resonance spectrum Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 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
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VEVLRSAIDXLSEU-UHFFFAOYSA-N N,N-dimethyloctan-1-amine Chemical compound C(CCCCCCC)N(C)C.C(CCCCCCC)N(C)C VEVLRSAIDXLSEU-UHFFFAOYSA-N 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 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
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 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
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011410 subtraction method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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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 provides a method for extracting and separating rare earth neodymium by phosphate ionic liquid, which is used for solving the technical problems that the separation coefficient of neodymium from lanthanum, cerium and praseodymium is low, the efficient separation and purification of neodymium are difficult to realize, and the traditional diluent used in the extraction and separation process is easy to volatilize in the current industry, and specifically comprises the following steps: (1) adding rare earth chloride into an aqueous solution, adjusting the pH value by adopting hydrochloric acid, and preparing a hydrochloric acid rare earth raw material solution; (2) and (2) mixing phosphate ionic liquid with the rare earth hydrochloride raw material liquid prepared in the step (1), extracting in a constant-temperature water bath oscillator, centrifuging the extracted mixed solution, and then carrying out phase separation to obtain a rare earth element-loaded ionic liquid phase and raffinate. The phosphate ionic liquid designed and synthesized by the invention has the advantages that the selectivity can be obviously improved through the coordination effect of the phosphorus-oxygen functional group and neodymium, the addition of a diluent for dilution is not needed, the extraction rate of neodymium is high, the separation performance is good, the operation is simple, saponification is not needed, and the phosphate ionic liquid can be recycled for multiple times.
Description
Technical Field
The invention belongs to the technical field of solvent extraction separation of rare earth elements, and particularly relates to a method for extracting and separating rare earth neodymium by phosphate ionic liquid.
Background
Rare earth elements are composed of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd) and other sixteen rare earth elements, and classified into light rare earth elements of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Po), samarium (Sc), europium (Eu) and heavy rare earth elements of gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Th), ytterbium (Yb), lutetium (Lu), scandium (Sc), and yttrium (Y) according to the atomic electron shell structure and the difference in physicochemical properties of the rare earth elements. The rare earth elements have unique optical, electric and magnetic properties, and can be widely used for various functional materials, such as rare earth permanent magnet materials, rare earth luminescent materials, rare earth catalytic materials, rare earth hydrogen storage materials, rare earth polishing materials and the like. In recent years, with the continuous development of high and new technology industries, rare earth functional materials with excellent performance play an increasingly important role in a plurality of fields such as metallurgy, chemical engineering, agriculture, ceramics, electronics, environmental protection, superconduction, national defense and military industry and the like.
Neodymium is an important rare earth element and is widely applied to the fields of neodymium-iron-boron permanent magnet materials, non-ferrous metal materials, aerospace materials, automobile industry and the like. The reserves of rare earth minerals in China account for more than 80% of the reserves in the world, wherein the reserves of neodymium in monazite and bastnaesite account for 15%. Although neodymium resources are not scarce, the physical and chemical properties of neodymium are very similar to those of adjacent rare earth elements such as lanthanum, cerium and praseodymium, so that the separation and purification of neodymium are difficult. Currently, organic phosphoric acid extracting agents P204, P507 and Cyanex272 are generally used for extracting and separating neodymium in industry, but because the separation coefficient of neodymium from lanthanum, cerium and praseodymium is low (about 1.5), high-purity neodymium is difficult to obtain. In addition, organic solvents used in conventional liquid-liquid extraction processes, such as toluene, petroleum ether, n-heptane, etc., are generally volatile and tend to cause environmental pollution. Therefore, the development of a novel method for efficiently and cleanly separating neodymium is of great significance.
Compared with the traditional organic solvent, the ionic liquid has the advantages of non-volatility, designability and the like, and is widely applied to the fields of electrochemistry, organic synthesis, extraction separation and the like. At present, the extraction and separation of rare earth elements based on ionic liquid has become a research focus, for example, chinese patent CN102382982A discloses a method for extracting and separating rare earth elements lanthanum, europium, ytterbium and lutetium by adding hydrophobic ionic liquid to form a liquid-liquid three-phase system; chinese patent CN102409172A discloses a method for separating tetravalent cerium or tetravalent cerium and fluorine by using a bifunctional ionic liquid; chinese patent CN109517985 discloses a method for extracting and separating light rare earth elements of lanthanum, cerium, praseodymium and neodymium by using a bifunctional ionic liquid; chinese patent CN106048221A discloses a method for preparing a liquid crystal by using an ionic liquid OMIM]BF4A method for extracting light rare earth elements of lanthanum, cerium, praseodymium and neodymium from an acidic solution. However, the above extraction efficiency is low and the selective extraction ability for a specific element is poor.
Disclosure of Invention
The invention provides a method for extracting and separating rare earth neodymium by phosphate ionic liquid, aiming at the technical problems that the separation coefficient of neodymium from lanthanum, cerium and praseodymium is low, the efficient separation and purification of neodymium are difficult to realize, and the traditional diluent used in the extraction and separation process is easy to volatilize in the current industry, and the like, so that the aims of reducing the production energy consumption and improving the separation efficiency are fulfilled.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for extracting and separating rare earth neodymium by phosphate ionic liquid is disclosed, wherein the phosphate ionic liquid has a structural general formula as follows:
(1) adding rare earth chloride into an aqueous solution, adjusting the pH value by adopting hydrochloric acid, and preparing a hydrochloric acid rare earth raw material solution;
(2) and (2) mixing phosphate ionic liquid with the rare earth hydrochloride raw material liquid prepared in the step (1), extracting in a constant-temperature water bath oscillator, centrifuging the extracted mixed solution, and then carrying out phase separation to obtain a rare earth element-loaded ionic liquid phase and raffinate.
The rare earth element in the rare earth chloride in the step (1) comprises Nd3+Or Nd3+And Ce3+、Pr3+、La3+One or more of them.
The concentration of rare earth in the hydrochloric acid rare earth raw material liquid is 0.001-0.03 mol/L; the pH value of the hydrochloric acid rare earth raw material liquid is 0.82-6.26.
The extraction ratio in the step (2) is 1: 1-1: 6, the extraction temperature is 15-40 ℃, the extraction time is 1-40 min, and the oscillation rate is 200-500 r/min.
In the step (2), the centrifugal rotating speed is 5000-12000 r/min, and the centrifugal time is 1-5 min.
And (3) carrying out back extraction on the rare earth element-loaded ionic liquid phase in the step (2), mixing hydrochloric acid with the rare earth element-loaded ionic liquid phase, centrifuging the back-extracted mixed solution, and separating to obtain the phosphate ionic liquid after back extraction and regeneration.
The concentration of the hydrochloric acid is 0-0.3 mol/L, the back-extraction ratio is 1: 1-1: 6, the back-extraction temperature is 15-40 ℃, the back-extraction time is 1-40 min, and the back-extraction oscillation rate is 200-500 r/min; and in the separation process of the mixed solution, the centrifugal rotating speed is 5000-12000 r/min, and the centrifugal time is 5-10 min.
And recycling the phosphate ionic liquid after the back extraction regeneration.
The preparation method of the phosphate ionic liquid comprises the following steps: dripping di (2-ethylhexyl) phosphate into equimolar tertiary amine under the ice bath condition, then moving to room temperature for vigorous stirring, and purifying and drying a product after the reaction to obtain the phosphate ionic liquid.
The reaction time at room temperature is 12-36 h; the drying agent adopted for drying is P2O5The temperature is 60 ℃ and the time is 36-48 h.
Phosphate ionic liquid is a novel functionalized ionic liquid, phosphate functional groups are introduced to anions of the ionic liquid, on one hand, the interaction of static electricity and clusters of the ionic liquid and neodymium ions is utilized, on the other hand, the coordination of the phosphate functional groups and neodymium metal ions can be utilized, and the separation efficiency and selectivity of rare earth neodymium ions are improved through dual functions.
The invention has the beneficial effects that: the phosphate ionic liquid designed and synthesized by the invention has the advantages that the selectivity can be obviously improved through the coordination effect of phosphorus-oxygen functional groups and neodymium, in addition, no diluent is added for dilution, the extraction rate of neodymium is high, the separation performance is good, the extraction balance can be achieved within 10min, the high extraction rate can still be maintained at the room temperature of 25 ℃, the operation is simple, saponification is not needed, the loaded ionic liquid phase can be recycled for multiple times after low-acid back extraction, and the extraction performance is basically maintained unchanged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an infrared spectrum of ionic liquids prepared in examples 1-3.
FIG. 2 shows preparation of ionic liquid in example 11H NMR spectrum.
FIG. 3 is a schematic representation of the preparation of an ionic liquid according to example 21H NMR spectrum.
FIG. 4 is a preparation of example 3Of ionic liquids1H NMR spectrum.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
In the process of the specific embodiment, after the extraction and the back extraction processes are finished, the rare earth concentration in the lower raffinate is measured by an ICP method, and the rare earth ion concentration in the ionic liquid phase is obtained by a subtraction method.
The extraction rate of the rare earth elements is calculated according to formula 1:
the distribution ratio of the rare earth elements is calculated according to formula 2:
the separation coefficient of the rare earth element is calculated by equation 3:
the back extraction rate of rare earth elements was calculated as formula 4:
in the formula: [ M ]]iAnd [ M]fRepresents the rare earth concentration in the aqueous phase before and after extraction, [ V ]]aAnd [ V ]]oRespectively representing the volumes of the aqueous phase and the ionic liquid phase; d1And D2The distribution ratio of the rare earth elements 1 and 2 respectively; [ M ] A]aAnd [ M]oRespectively representing the rare earth concentration in the water phase after back extraction and the rare earth concentration in the ionic liquid phase before back extraction.
Example 1
Ionic liquid [ N ]1,1,8,H][DEHP]Preparation of
HDEHP was added dropwise to equimolar N, N-dimethyloctylamine (N, N-dimethyloctylamine) under ice bath conditions1,1,8) In the middle, the mixture is stirred vigorously for 12h at room temperature, the product is washed several times with deionized water and then with P2O5Drying with desiccant under vacuum at 60 deg.C for 48 hr to obtain yellowish ionic liquid [ N1,1,8,H][DEHP]The yield thereof was found to be 95.6%. 3417cm in FIG. 1-1Is located at 1647cm and is an N-H bond stretching vibration peak-1Is located at the peak of bending vibration of N-H bond, combined with that of FIG. 21The H NMR spectrum shows that [ N ] is successfully prepared1,1,8,H][DEHP]。
Example 2
Ionic liquid [ N ]1,1,10,H][DEHP]Preparation of
HDEHP was added dropwise to an equimolar amount of N, N, -dimethyloctyldecylamine (N) under ice bath conditions1,1,10) In (B), vigorously stirred at room temperature for 24h, washed several times with deionized water and then treated with P2O5Drying with desiccant under vacuum at 50 deg.C for 48 hr to obtain yellowish ionic liquid [ N1,1,10,H][DEHP]The yield thereof was found to be 96.1%. 3417cm in FIG. 1-1Is located at 1647cm and is an N-H bond stretching vibration peak-1Is located at the peak of bending vibration of N-H bond, combined with that of FIG. 31The HNMR spectrogram can know that the [ N ] is successfully prepared1,1,10,H][DEHP]。
Example 3
Ionic liquid [ N ]1,1,12,H][DEHP]Preparation of
HDEHP was added dropwise to an equimolar amount of N, N, -dimethyldodecylamine (N, N-dimethyldodecylamine) under ice bath conditions1,1,12) In the middle, the mixture is vigorously stirred for 36h at room temperature, washed with deionized water for multiple times and then with P2O5Drying with desiccant under vacuum at 70 deg.C for 36 hr to obtain yellowish ionic liquid [ N1,1,12,H][DEHP]The yield was 96.5%. 3417cm in FIG. 1-1Is a bond of N-HPeak of stretching vibration, 1647cm-1Is located at the peak of bending vibration of N-H bond, combined with that of FIG. 41The H NMR spectrum shows that [ N ] is successfully prepared1,1,12,H][DEHP]。
Example 4
Phosphate ionic liquid [ N ]1,1,8,H][DEHP]Extraction separation of neodymium
Preparing a neodymium-containing rare earth hydrochloride raw material solution, wherein the concentration of neodymium in the raw material solution is 0.005mol/L, and the pH value is 4.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator according to a volume ratio of 1:3, wherein the extraction time is 20min, the temperature is 30 ℃, and the oscillation rate in the extraction process is 200 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 10000r/min, the centrifugation time is 5min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 99.82%.
Example 5
Phosphate ionic liquid [ N ]1,1,10,H][DEHP]Extraction separation of neodymium
Preparing a neodymium-containing rare earth hydrochloride raw material solution, wherein the concentration of neodymium in the raw material solution is 0.005mol/L, and the pH value is 4.
Putting the ionic liquid extracting agent and the raw material liquid in a constant-temperature water bath oscillator according to the ratio of 1:3, wherein the extraction time is 20min, the temperature is 30 ℃, and the oscillation speed in the extraction process is 200 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 3min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 98.99%.
Example 6
Phosphate ionic liquid [ N ]1,1,12,H][DEHP]Extraction separation of neodymium
Preparing neodymium-containing rare earth hydrochloride raw material liquid, wherein the concentration of neodymium in the raw material liquid is 0.005mol/L, and the pH value is 4.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:3, wherein the extraction time is 20min, the temperature is 30 ℃, and the oscillation rate in the extraction process is 200 r/min; and (3) placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 2min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 98.17%.
Example 7
Phosphate ionic liquid [ N ]1,1,8,H][DEHP]Extraction separation of neodymium
Preparing a rare earth hydrochloride raw material solution containing neodymium, wherein the concentration of neodymium in the raw material solution is 0.008mol/L, and the pH value is 1.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:2, wherein the extraction time is 25min, the temperature is 35 ℃, and the oscillation rate in the extraction process is 200 r/min; and placing the mixed solution after extraction in a centrifuge at the centrifugal rotation speed of 12000r/min for 5min to obtain the rare earth element-loaded ionic liquid phase and the raffinate after centrifugation.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 55.95%.
Example 8
Phosphate ionic liquid [ N ]1,1,10,H][DEHP]Extraction separation of neodymium
Preparing a rare earth hydrochloride raw material solution containing neodymium, wherein the concentration of neodymium in the raw material solution is 0.008mol/L, and the pH value is 1.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:2, wherein the extraction time is 25min, the temperature is 35 ℃, and the oscillation rate in the extraction process is 300 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 2min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of the rare earth element in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 50.90%.
Example 9
Phosphate ionic liquid [ N ]1,1,12,H][DEHP]Extraction separation of neodymium
Preparing a rare earth hydrochloride raw material solution containing neodymium, wherein the concentration of neodymium in the raw material solution is 0.008mol/L, and the pH value is 1.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:2, wherein the extraction time is 25min, the temperature is 35 ℃, and the oscillation rate in the extraction process is 300 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 10min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 46.56%.
Example 10
Phosphate ionic liquid [ N ]1,1,8,H][DEHP]Extraction separation of neodymium
Preparing a neodymium-containing rare earth hydrochloride raw material solution, wherein the concentration of neodymium in the raw material solution is 0.003mol/L, and the pH value is 3.
Putting the ionic liquid extracting agent and the raw material liquid in a constant-temperature water bath oscillator according to the ratio of 1:1, wherein the extraction time is 15min, the temperature is 25 ℃, and the oscillation speed in the extraction process is 400 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 8000r/min, the centrifugation time is 3min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 99.80%.
Example 11
Phosphate ionic liquid [ N ]1,1,10,H][DEHP]Extraction separation of neodymium
Preparing a neodymium-containing rare earth hydrochloride raw material solution, wherein the concentration of neodymium in the raw material solution is 0.003mol/L, and the pH value is 3.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:1, wherein the extraction time is 15min, the temperature is 25 ℃, and the oscillation rate in the extraction process is 400 r/min; and (3) placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 5min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 99.05%.
Example 12
Phosphate ionic liquid [ N ]1,1,12,H][DEHP]Extraction separation of neodymium
Preparing a neodymium-containing rare earth hydrochloride raw material solution, wherein the concentration of neodymium in the raw material solution is 0.003mol/L, and the pH value is 3.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:1, wherein the extraction time is 15min, the temperature is 25 ℃, and the oscillation rate in the extraction process is 400 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 2min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of the rare earth element in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 98.98%.
Example 13
Phosphate ionic liquid [ N ]1,1,8,H][DEHP]Extraction separation of neodymium
Preparing a rare earth hydrochloride raw material solution containing neodymium, wherein the concentration of neodymium in the raw material solution is 0.008mol/L, and the pH value is 4.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:3, wherein the extraction time is 10min, the temperature is 40 ℃, and the oscillation rate in the extraction process is 250 r/min; and (3) placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 3min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of the rare earth element in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 99.96%.
Example 14
Phosphate ionic liquid [ N ]1,1,10,H][DEHP]Extraction separation of neodymium
Preparing a rare earth hydrochloride raw material solution containing neodymium, wherein the concentration of neodymium in the raw material solution is 0.008mol/L, and the pH value is 4.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:3, wherein the extraction time is 10min, the temperature is 40 ℃, and the oscillation rate in the extraction process is 250 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 3min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 99.94%.
Example 15
Phosphate ionic liquid [ N ]1,1,12,H][DEHP]Extraction separation of neodymium
Preparing a rare earth hydrochloride raw material solution only containing neodymium, wherein the concentration of neodymium in the raw material solution is 0.008mol/L, and the pH value is 4.
Putting the ionic liquid extractant and the raw material liquid in a constant-temperature water bath oscillator in a ratio of 1:3, wherein the extraction time is 10min, the temperature is 40 ℃, and the oscillation rate in the extraction process is 250 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 5000r/min, the centrifugation time is 3min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the result shows that the extraction rate of the ionic liquid to neodymium is 99.87%.
Example 16
Phosphate ionic liquid [ N ]1,1,8,H][DEHP]Selective separation of neodymium from lanthanum, cerium, praseodymium and neodymium
Preparing rare earth hydrochloride raw material liquid containing lanthanum, cerium, praseodymium and neodymium, wherein the concentration of the lanthanum, the cerium, the praseodymium and the neodymium in the raw material liquid is 0.002mol/L, and the pH value is 4.
Putting the ionic liquid extracting agent and the raw material liquid in a constant-temperature water bath oscillator according to the ratio of 1:2, wherein the extraction time is 25min, the temperature is 30 ℃, and the oscillation speed in the extraction process is 350 r/min; and placing the mixed solution after extraction in a centrifuge, wherein the centrifugation speed is 10000r/min, the centrifugation time is 1min, and obtaining the rare earth element-loaded ionic liquid phase and the raffinate after the centrifugation is finished.
The concentration of rare earth elements in the raffinate is measured by an ICP method, and the results show that the separation coefficients of the ionic liquid on neodymium/lanthanum, neodymium/cerium and neodymium/praseodymium are respectively 13.76, 6.90 and 3.40.
Example 17
Phosphate ionic liquid [ N ]1,1,10,H][DEHP]Regeneration of
The ionic liquid phase was the rare earth element-loaded ionic liquid phase obtained by centrifugation after extraction in example 14.
Placing the rare earth element-loaded ionic liquid phase and a dilute hydrochloric acid stripping agent in a constant-temperature water bath oscillator in a ratio of 1:1, wherein the concentration of hydrochloric acid is 0.2mol/L, the back extraction time is 10min, the temperature is 40 ℃, the oscillation rate in the back extraction process is 250r/min, centrifuging the back-extracted mixed solution at the centrifugal rotation speed of 5000r/min for 3min, and separating to obtain the ionic liquid phase.
The concentration of the element neodymium in the ionic liquid phase was measured by the ICP method, and the back extraction rate of the rare earth element neodymium was calculated. After 8 regeneration cycles, the back extraction rate of diluted hydrochloric acid to neodymium is 81.8%.
Example 18
Phosphate ionic liquid [ N ]1,1,8,H][DEHP]Is recycled
The ionic liquid phase was the rare earth element-loaded ionic liquid phase after extraction in example 13.
Placing the rare earth element-loaded ionic liquid phase and a dilute hydrochloric acid stripping agent in a constant-temperature water bath oscillator according to the ratio of 1:1, wherein the hydrochloric acid concentration is 0.16mol/L, the stripping time is 10min, the temperature is 40 ℃, the oscillation rate in the stripping process is 250r/min, centrifuging the mixed solution after stripping at the centrifugal rotation speed of 8000r/min for 2min, and separating to obtain an ionic liquid extract; the extraction procedure of example 13 was repeated using an ionic liquid extract to obtain a raffinate after the extraction was complete.
The concentration of the raffinate was measured by the ICP method, and the extraction rate of the rare earth element neodymium was calculated. After 6 regeneration cycles, the extraction rate of the ionic liquid on neodymium is 99.14%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for extracting and separating rare earth neodymium by phosphate ionic liquid is characterized in that the structural general formula of the phosphate ionic liquid is as follows:
the method specifically comprises the following steps:
(1) adding rare earth chloride into an aqueous solution, adjusting the pH value by adopting hydrochloric acid, and preparing a hydrochloric acid rare earth raw material solution;
(2) and (2) mixing phosphate ionic liquid with the rare earth hydrochloride raw material liquid prepared in the step (1), extracting in a constant-temperature water bath oscillator, centrifuging the extracted mixed solution, and then carrying out phase separation to obtain a rare earth element-loaded ionic liquid phase and raffinate.
2. The method for extracting and separating rare earth neodymium from phosphate ionic liquid according to claim 1, wherein the rare earth element in the rare earth chloride in the step (1) comprises Nd3+Or Nd3+And Ce3+、Pr3+、La3+One or more of them.
3. The method for extracting and separating rare earth neodymium by using the phosphate ionic liquid as claimed in claim 1, wherein the concentration of rare earth in the hydrochloric acid rare earth raw material liquid is 0.001-0.03 mol/L; the pH value of the hydrochloric acid rare earth raw material liquid is 0.82-6.26.
4. The method for extracting and separating rare earth neodymium by using the phosphate ionic liquid as claimed in claim 1, wherein the extraction ratio in the step (2) is 1: 1-1: 6, the extraction temperature is 15-40 ℃, the extraction time is 1-40 min, and the oscillation rate is 200-500 r/min.
5. The method for extracting and separating rare earth neodymium by using the phosphate ionic liquid as claimed in claim 1, wherein the centrifugal rotation speed in the step (2) is 5000-12000 r/min, and the centrifugal time is 1-5 min.
6. The method for extracting and separating rare earth neodymium from phosphate ionic liquid according to claim 1, wherein the ionic liquid phase loaded with the rare earth element in the step (2) is subjected to back extraction, hydrochloric acid is mixed with the ionic liquid phase loaded with the rare earth element, and a mixed solution after back extraction is centrifuged and separated to obtain the phosphate ionic liquid after back extraction and regeneration.
7. The method for extracting and separating rare earth neodymium by using the phosphate ionic liquid as claimed in claim 6, wherein the concentration of hydrochloric acid is 0-0.3 mol/L, the back-extraction ratio is 1: 1-1: 6, the back-extraction temperature is 15-40 ℃, the back-extraction time is 1-40 min, and the back-extraction oscillation rate is 200-500 r/min; and in the separation process of the mixed solution, the centrifugal rotating speed is 5000-12000 r/min, and the centrifugal time is 5-10 min.
8. The method for extracting and separating rare earth neodymium by using the phosphate ester ionic liquid as claimed in claim 6 or 7, wherein the phosphate ester ionic liquid after the back extraction and regeneration is recycled.
9. The method for extracting and separating rare earth neodymium by using the phosphate ionic liquid as claimed in claim 1, wherein the phosphate ionic liquid is prepared by the following steps: under the ice bath condition, dripping di (2-ethylhexyl) phosphate into equimolar tertiary amine, then moving to room temperature for vigorous stirring, and purifying and drying the product after the reaction is finished to obtain the phosphate ionic liquid.
10. The method for extracting and separating rare earth neodymium by using the phosphate ionic liquid as claimed in claim 9, wherein the reaction time at room temperature is 12-36 h; the drying agent adopted for drying is P2O5The temperature is 60 ℃ and the time is 36-48 h.
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