CN104593591B - A kind of method of separation of rare earth elements - Google Patents
A kind of method of separation of rare earth elements Download PDFInfo
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- CN104593591B CN104593591B CN201510039016.8A CN201510039016A CN104593591B CN 104593591 B CN104593591 B CN 104593591B CN 201510039016 A CN201510039016 A CN 201510039016A CN 104593591 B CN104593591 B CN 104593591B
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000000926 separation method Methods 0.000 title claims abstract description 40
- 238000000605 extraction Methods 0.000 claims abstract description 73
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000001179 sorption measurement Methods 0.000 claims abstract description 9
- 238000005194 fractionation Methods 0.000 claims abstract description 8
- 238000002386 leaching Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 10
- 239000011574 phosphorus Substances 0.000 claims description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 150000001412 amines Chemical class 0.000 claims description 9
- 238000005342 ion exchange Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- -1 2-ethyl hexyl esters Chemical class 0.000 claims description 7
- 239000006210 lotion Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical class CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003456 ion exchange resin Substances 0.000 abstract description 5
- 229920003303 ion-exchange polymer Polymers 0.000 abstract description 5
- 238000007127 saponification reaction Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 238000000638 solvent extraction Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 239000000320 mechanical mixture Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- NPSJHQMIVNJLNN-UHFFFAOYSA-N 2-ethylhexyl 4-nitrobenzoate Chemical compound CCCCC(CC)COC(=O)C1=CC=C([N+]([O-])=O)C=C1 NPSJHQMIVNJLNN-UHFFFAOYSA-N 0.000 description 1
- 239000004808 2-ethylhexylester Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- WFXRJNDIBXZNJK-KVVVOXFISA-N azanium;(z)-octadec-9-enoate Chemical compound N.CCCCCCCC\C=C/CCCCCCCC(O)=O WFXRJNDIBXZNJK-KVVVOXFISA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of method of separation of rare earth elements, step are as follows：(1) prepared by hybrid resin, (2) dress post, (3) post separation, (4) post wash and the circulation of (5) post.The advantage of the invention is that：Using ion-exchange-resin process separation of rare earth elements, solve because of problem of environmental pollution caused by saponification；Invention is using N235 resins to H+Adsorption capacity, solve the problems, such as that rare earth adsorbance is low caused by rare earth ion extraction equilibrium acidity is low；Absorbability using N235 to acid, can control the exchange acidity of adsorption zone, resin is had preferable separating capacity to light rare earth；The mode connected using multicolumn is realized using fractionation extraction leaching technique separation of rare earth elements, and a kind of new method is provided for the separation of rare earth element.
Description
Technical field
The present invention relates to rare earths separation technical field, more particularly to a kind of method of separation of rare earth elements.
Background technology
Rare earth element causes the ion between rare earth element because of its similar electron structure and rare earth " lanthanide contract " phenomenon
Radius is close, determines the similitude of the physicochemical properties of rare earth element, causes the separation between rare earth element difficult.Rare earth
The separation method of element is numerous, and separation principle is to rely on the fine difference between rare earth compound, by certain extractant or
Precipitating reagent is through separating step is repeated several times and by rare earths separation.Technique uses Solvent Extraction Separation rare earth element at present,
But Solvent Extraction Separation rare earth largely contains because neutralizing saponification organic phase using ammonia soap or soda soap, calcium soap, magnesium soap etc. under exchange
The inorganic salts waste water of ammonium or alkali metal ion, it is high to pollute environment or treatment cost, while also brings along the environment such as water body COD is exceeded
Pollution problem.Requirement of the solvent extraction to feed liquid impurity is higher, Ca2+、Mg2+、Al3+、Fe3+、Si4+Impurity content is high easily to be occurred
Third phase, cause split-phase difficult, it is low to extract the rare earth feed liquid extraction efficiency of low concentration, influences plant produced efficiency.Solvent simultaneously
Series needed for extraction is more, and the isolated single rare earth of mischmetal is taken around into 3,000 multistage extraction tanks, rare earth pressure
Groove amount is big, and fixed cost investment is big.In recent years country has also been proposed new requirement in terms of the green smelting of rare earth, therefore exploitation is ground
The method for studying carefully new separation of rare earth elements is particularly important.
Ion exchange resin is a kind of reticular polymer compound for carrying active group, has and exchanges, selects, inhaling
Attached enrichment and catalysis.Resin adsorbs different ions according to the difference of active group, alternative, reaches the mesh of enrichment
's.Existing Patent Publication (patent 89101932, patent 85101874, patent CN85101611) is carried using Strong acid ion-exchanger
Pure rare earth element, obtain the single rare earth product of high-purity.It is but dilute in absorption in simple phosphorus extractant ion exchange resin
During native ion, a large amount of H can be exchanged down+, the relatively low rare earth ion of extraction equilibrium acidity is parsed, causes the absorption of resin dilute
Soil amount is low, and the effective rate of utilization of extractant reduces in resin.Therefore the adsorption capacity and control exchange process of resin how to be improved
In acidity change turn into key problem in technology.
The content of the invention
To realize the separation of rare earth, the invention provides a kind of method of separation of rare earth elements.Invention is Phosphorus using acidity
Extractant coordinates and added to H to the extracting power of rare earth ion+Amine extractant with effect of extracting, is prepared for compound tree
Fat is used for the separation of rare earth element.
The present invention adopts the following technical scheme that：
The method of the separation of rare earth elements of the present invention comprises the following steps that：
(1) preparation of hybrid resin：
It is 1 in mass ratio by single phosphorus extractant resin and single amine extracted resin:It is prepared by 0.1~5 mechanical mixture
Hybrid resin；Or by phosphorus extractant and amine extractant it is 1 in mass ratio:Prepared by the mixed extractant of 0.1~5 composition
Hybrid resin；
(2) post is filled：
By the hybrid resin obtained by step (1) with wet method dress post method load post footpath be 1~300cm, ratio of height to diameter be 1~
80:1 ion exchange column；
(3) post separation：
The ion exchange column that step (2) dress post obtains carries out multicolumn and connects to obtain splitter, wherein, splitter is according to pillar
Jointing is divided into extraction column (F), column scrubber (W) and re-extraction column (H), and post trend is along extraction column (F), column scrubber (W) and instead
Extract post (H) direction；First extraction column (F1) be connected with the n-th column scrubber (Wn), the first column scrubber (W1) connect with the n-th re-extraction column (Hn)
Connect；With the rare earth feed liquid that pH value is 3~5 with 0.1~20cmmin-1Flow velocity from the first extraction column (F1) place flows through splitter,
With the hydrochloric acid that concentration is 0.1~6mol/L with 0.1~20cmmin-1Flow velocity from the first re-extraction column (H1) place flows through splitter,
The strip liquor flowed out from the n-th re-extraction column (Hn) is in the form of washing lotion with 0.1~20cmmin-1Flow velocity from the first column scrubber
(W1) flow through splitter；Elapsed timeAfterwards, wherein：DmaxFor single pillar rare earth adsorption saturation amount, MFFor material
Liquid mass flow, fAEasily extract component molar fraction for feed liquid, λ was extraction coefficient, the first extraction column (F1) enter washing section, first
Column scrubber (W1) enter stripping section；In the n-th extraction column (Fn) place obtains the difficult extraction component of rare earth, obtained at the n-th re-extraction column (Hn) place dilute
Native easily extraction component；
(4) post washs
Eluate pH value is washed with distilled water to more than 3 containing acid separation column after use, obtains blank post；
(5) post circulates
Realize using fractionation extraction leaching technique separation of rare earth elements blank post recirculation step (3)~(4) after washing.
In step (1), described phosphorus extractant is two (2- ethylhexyl phosphoric acids) or 2- ethylhexyl phosphoric acid list 2- second
Base hexyl ester；Described amine extractant is trialkyl tertiary amine.
In step (1), described hybrid resin is pressed including single phosphorus extractant resin with single amine extractant resin
Mass ratio is 1:Hybrid resin prepared by 0.1~5 mechanical mixture, or extractant are 1 in mass ratio:0.1~5 is formed
Hybrid resin prepared by P204-N235, P507-N235 mixed extractant.
In step (4), the pH value of described rare earth feed liquid is 3~5.
In step (3), the separation of rare earth element is realized in multicolumn series connection using fractionation extraction leaching technique；In the first extraction column (F1)
Feeding liquid, the first column scrubber (W is flowed through in the form of washing lotion by the n-th re-extraction column (Hn) shunting1) post, in the first re-extraction column (H1) enter
Back extraction acid；Elapsed timeAfterwards, wherein：DmaxFor single pillar rare earth adsorption saturation amount, MFFor feed liquid quality
Flow, fAEasily extract component molar fraction for feed liquid, λ was extraction coefficient, the first extraction column (F1) enter washing section as the n-th washing
Post (Wn), the first column scrubber (W1) post enter stripping section turn into the n-th re-extraction column (Hn), in the n-th extraction column (Fn), the n-th re-extraction column
(Hn) place respectively obtains the difficult extraction component of rare earth, rare earth easily extracts component.
Ion exchange column can be substituted with tank diameter described in fractionation extraction leaching process technology scheme.
The positive effect of the present invention is as follows：
(1) ion-exchange-resin process separation of rare earth elements is used, is solved because of problem of environmental pollution caused by saponification；
(2) using N235 resins to H+Adsorption capacity, solve dilute caused by rare earth ion extraction equilibrium acidity is low
The problem of native adsorbance is low；
(3) Strong acid ion-exchanger rare earth element is used, eliminates the split-phase difficult problem that traditional solvent extraction is brought；
(4) ion-exchange-resin process technique is simple, and prepared hybrid resin stablizes reusable, easy to operate, nothing
It is malicious, pollution-free；
(5) realized using the mode of multicolumn series connection and leaching technique separation of rare earth elements is extracted using fractionation, be point of rare earth element
From providing a kind of new method.
Brief description of the drawings
Fig. 1 is the process chart of the inventive method；
Fig. 2 is the series system figure of the ion exchange column of the inventive method；
In figure, F- extraction columns, W- column scrubbers, H- re-extraction columns, F1- the first extraction column, the extraction columns of Fn- n-th, W1- the first washing
Post, the column scrubbers of Wn- n-th, H1- the first re-extraction column, the re-extraction columns of Hn- n-th, VF- feed velocity, VW- washing lotion flow velocity, VH- back extraction acid stream
Speed.
Embodiment
The following examples are that the present invention is described in further detail.
As shown in figure 1 and 2, the method for separation of rare earth elements of the invention comprises the following steps that：
(1) preparation of hybrid resin：
It is 1 in mass ratio by single phosphorus extractant resin and single amine extracted resin:It is prepared by 0.1~5 mechanical mixture
Hybrid resin；Or by phosphorus extractant and amine extractant it is 1 in mass ratio:Prepared by the mixed extractant of 0.1~5 composition
Hybrid resin；
(2) post is filled：
It is 1~300cm, ratio of height to diameter that active carbon adsorption material wet method dress post method obtained by step (1) is loaded into post footpath
For 1~80:1 ion exchange column；
(3) post separation：
The ion exchange column that step (2) dress post obtains carries out multicolumn and connects to obtain splitter, series system such as Fig. 2, separation
Post is divided into extraction column F, column scrubber W and re-extraction column H according to pillar jointing, and post trend is along extraction column F, column scrubber W and anti-
Extract post H directions；First extraction column F1With the n-th washing
Post Wn connections, the first column scrubber W1It is connected with the n-th re-extraction column Hn；With the rare earth feed liquid that pH value is 2~5 with 0.1~
20cm·min-1Flow velocity from the first extraction column F1Place flows through splitter, with the hydrochloric acid that concentration is 0.1~6mol/L with 0.1~
20cm·min-1Flow velocity from the first re-extraction column H1Place flows through splitter, and the strip liquor flowed out at the n-th re-extraction column Hn is with washing lotion
Form with 0.1~20cmmin-1Flow velocity as washing lotion from the first column scrubber W1Flow through splitter；Elapsed timeAfterwards, wherein：DmaxFor single pillar rare earth adsorption saturation amount, MFFor feed liquid mass flow, fAEasily extract for feed liquid
Component molar fraction, λ were extraction coefficient, the first extraction column F1Into washing section, the first column scrubber W1Into stripping section；In the n-th extraction
Take FnPlace obtains the difficult extraction component of rare earth, and obtaining rare earth at the n-th re-extraction column Hn easily extracts component；
(4) post washs
Eluate pH value is washed with distilled water to more than 3 containing acid separation column after use, obtains blank post；
(5) post circulates
Realize using fractionation extraction leaching technique separation of rare earth elements blank post recirculation step (3)~(4) after washing.
Embodiment 1
Dry 2- ethylhexyl phosphoric acid single 2-ethyl hexyl ester (P507) resins are weighed to set with trialkyl tertiary amine (N235)
Fat is 1 in mass ratio:1 it is well mixed form hybrid resin, add distilled water and be completely soaked resin, then filled with wet method dress post method
Enter the ion exchange column that post footpath is 20mm, pillar height is 1000mm, dress pillar height degree is 850mm.
Separation circuit contains splitter 15, wherein extraction column 6, column scrubber 6, re-extraction column 3.Rare earth material used in experiment
Liquid concentration is 0.3mol/L, partition of rare earth element Pr3+：51.30%th, Nd3+：48.60%, other elements are equal<0.1%, feed liquid
PH is 3.5, and rare earth feed liquid is with 0.76cmmin-1Flow velocity from F1Place flows through splitter, with concentration be 5.0mol/L hydrochloric acid with
2.5cm·min-1Flow velocity from H1Place flows through splitter, from H3Locate the back extraction acid moieties of outflow with 1.40cmmin-1Flow velocity
Flow into W1Post.After 2min, F1Post enters washing section, W1Post enters stripping section.In F6Place obtains Pr3+Concentration is 0.054mol/
L, purity 99.89%, other elements are equal<0.1%；In H3Place obtains Nd3+Concentration is 1.15mol/L, purity 99.90%,
Other elements are equal<0.1%.
Eluate pH value being washed with distilled water to containing acid separation column blank post being formed more than 3, blank post is used further to rare earth material
The enrichment of liquid, so recycles splitter.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
- A kind of 1. method of separation of rare earth elements, it is characterised in that：Methods described comprises the following steps that：（1）The preparation of hybrid resin：It is 1 in mass ratio by phosphorus extractant and amine extractant:Compound tree prepared by the mixed extractant of 0.1 ~ 5 composition Fat；（2）Fill post：By step（1）Resulting hybrid resin wet method dress post method loading post footpath is 1 ~ 300cm, ratio of height to diameter is 1 ~ 80:1 from Sub- exchange column；（3）Post separation：Step（2）The ion exchange column that dress post obtains carries out multicolumn and connects to obtain splitter, wherein, splitter connects according to pillar Section is divided into extraction column（F）, column scrubber（W）And re-extraction column（H）, post trend is along extraction column（F）, column scrubber（W）And re-extraction column （H）Direction；First extraction column（F1）With the n-th column scrubber（Wn）Connection, the first column scrubber（W1）With the n-th re-extraction column（Hn）Connection；With The rare earth feed liquid that pH value is 3 ~ 5 is with 0.1 ~ 20cmmin-1Flow velocity from the first extraction column（F1）Place flows through splitter, uses concentration For 0.1 ~ 6mol/L hydrochloric acid with 0.1 ~ 20cmmin-1Flow velocity from the first re-extraction column（H1）Place flows through splitter, anti-from n-th Extract post（Hn）The strip liquor for locating to flow out is in the form of washing lotion with 0.1 ~ 20cmmin-1Flow velocity from the first column scrubber（W1）Flow through Splitter；After elapsed time, wherein：DmaxFor single pillar rare earth adsorption saturation amount, MFFor feed liquid mass flow,f AIt is easy for feed liquid Extract component molar fraction, λ was extraction coefficient, the first extraction column（F1）Into washing section, the first column scrubber（W1）Into stripping section； In the n-th extraction column（Fn）Place obtains the difficult extraction component of rare earth, in the n-th re-extraction column（Hn）Place obtains rare earth and easily extracts component；（4）Post washs:Eluate pH value is washed with distilled water to more than 3 containing acid separation column after use, obtains blank post；（5）Post circulates:Blank post recirculation step after washing（3）~（4）Realize using fractionation extraction leaching technique separation of rare earth elements.
- A kind of 2. method of separation of rare earth elements as claimed in claim 1, it is characterised in that：Step（1）In, described is Phosphorus Extractant is two (2- ethylhexyl phosphoric acids) or 2- ethylhexyl phosphoric acid single 2-ethyl hexyl esters；Described amine extractant is three Alkyl tertiary amine.
- A kind of 3. method of separation of rare earth elements as claimed in claim 1, it is characterised in that：Step（4）In, described rare earth The pH value of feed liquid is 3 ~ 5 and is not 3.
- A kind of 4. method of separation of rare earth elements as described in claim any one of 1-3, it is characterised in that：Fractionation extraction leaching technique Ion exchange column is substituted with tank diameter described in technical scheme.
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Effective date of registration: 20240411 Address after: Building 1-28, Jinmaowan North Garden, Huanjin Road, Yazhou District, Sanya City, Hainan Province, 572024 Patentee after: Hainan Tongbao New Materials Technology Co.,Ltd. Country or region after: China Address before: No.63 Innovation Park, Yinchuan Economic and Technological Development Zone, Ningxia Hui Autonomous Region, 750000 Patentee before: Ningxia Tongle New Material Technology Co.,Ltd. Country or region before: China |
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