CN109517985A - A method of light rare earth elements is separated using difunctional ion liquid abstraction - Google Patents
A method of light rare earth elements is separated using difunctional ion liquid abstraction Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B59/00—Obtaining rare earth metals
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Abstract
The invention belongs to Rare Earth Separations and ion liquid abstraction technical field, and in particular to a method of light rare earth elements is separated using difunctional ion liquid abstraction.Using the aqueous solution containing light rare earth elements as material liquid, it is combined using di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester with N- octylpyridinium villaumite, sodium hydroxide is added to adjust, the anion for retaining di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester is combined with the cation of N- octylpyridinium villaumite, it synthesizes difunctional ionic liquid and acid material liquid carries out hybrid extraction, the organic phase and raffinate of centrifuged supported rare earth, rare earth is stripped using strippant, centrifuged pure earth solution and recyclable ionic liquid.Extraction efficiency of the present invention is high, and equilibration time is short, easy to operate, does not generate emulsion.
Description
Technical field
The invention belongs to Rare Earth Separations and ion liquid abstraction technical field, and in particular to a kind of to utilize difunctional ionic liquid
The method of body extraction and separation light rare earth elements.
Background technique
Rare earth is non-renewable grand strategy resource, by chemical property and separating technology requirement, can be divided into light rare earth and
Two class of heavy rare earth is widely used in new material and new technical field, and China's rare earth reserves rank first in the world, wherein southern ion
The content of light rare earth elements is all very high in absorbent-type Rare Earth Mine and northern bastnaesite, and light rare earth elements has a wide range of application,
Rare earth application in play the role of it is very important, therefore, light rare earth elements efficiently separate purifying to expand its application field have
Significance.
Rare earth element physics is similar with chemical property, and separation and purification difficult, solvent extraction are industrial Rare Earth Separations
The method generally used uses extractant di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (P507) and two (2- ethylhexyl) phosphines
Acid esters (P204), although acid phosphine extractant has good effect of extracting to light rare earth elements, in the process of rare-earth separating
In that there is also back extraction acidity is high, back extraction is not thorough, and generates the great number of issues such as ammonia nitrogen waste water, high-salt wastewater.Therefore,
High efficiency is explored, environmentally friendly extraction and separation technology is extremely urgent.
Ionic liquid steam forces down, and thermal stability is good, can be applied to extraction and separation field, has and made using ionic liquid
For extractant application Rare Earth Separation research report, Chinese patent (publication number CN102876893A) disclose it is a kind of use quaternary amine
The method that ion liquid abstraction agent extracts rare earth element in sulfuric acid system；Chinese patent CN103320629A discloses a kind of difunctional
The method of ionic liquid efficient extracting rare-earth cerium in sulfuric acid system, Chinese patent (publication number CN102618736A) are open a kind of
The method of difunctional ionic liquid extracting rare-earth element in nitric acid salt system.But do not have also using N- octylpyridinium villaumite
([OPy] [Cl]) and di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (P507) it is combined into difunctional ion liquid abstraction rare earth member
The research report of element.
Summary of the invention
It is difficult for being stripped in current Rare-Earth Extraction Process using acid phosphine extractant, easily cause secondary pollution etc. to ask
Topic, the purpose of the present invention is to provide it is a kind of using difunctional ion liquid abstraction separation light rare earth elements method, using from
The features such as sub- liquid is non-volatile, chemical property has been stablized, by traditional extraction agent P507It is combined with ionic liquid, use is difunctional
Ion liquid abstraction rare earth, extraction efficiency is high, and does not generate ammonia nitrogen waste water pollution problem.
The technical scheme is that
A method of light rare earth elements being separated using difunctional ion liquid abstraction, is followed the steps below:
(1) aqueous solution of the configuration containing light rare earth elements is material liquid, in material liquid light rare earth concentration be 0.01~
0.04mol/L, pH value of solution are 1~5.5；
(2) difunctional ionic liquid is configured as extractant, N- octylpyridinium villaumite ([OPy] [Cl]) and 2- ethylhexyl
Phosphonic acids single 2-ethyl hexyl ester (P507) molar ratio be 1:1~1:3, P507Concentration be 0.03~0.1mol/L, N- octyl pyrrole
The concentration of pyridine villaumite is 0.03~0.1mol/L；
(3) material liquid and difunctional ionic liquid hybrid extraction in an oscillator, mixing are comparably 1:1, in extraction process
Revolving speed is 50~150r/min, and extraction time is 15~30min, and extraction temperature is 5~35 DEG C, the mixed solution after the completion of extracting
It is centrifuged to obtain the organic phase of supported rare earth and raffinate；
(4) organic phase of supported rare earth is stripped using strippant, is stripped the centrifugal rotational speed of centrifuge separation
For 2000~3500r/min, centrifugation time is 2~8min, centrifuged pure earth solution and ionic liquid.
The method using difunctional ion liquid abstraction separation light rare earth elements, light rare earth elements are lanthanum, cerium, praseodymium
Or neodymium.
The method using difunctional ion liquid abstraction separation light rare earth elements, contains the water-soluble of light rare earth elements
Liquid is re chloride or rare earth nitrate solution, and optimal is re chloride.
The described method using difunctional ion liquid abstraction separation light rare earth elements, in difunctional ionic liquid, sun
Ion is N- octylpyridinium [Opy]+, anion is [P507]-, the structural formula of difunctional ionic liquid zwitterion is as shown in Equation 1:
The described method using difunctional ion liquid abstraction separation light rare earth elements, in step (3), centrifugal rotational speed is
2000~3500r/min, centrifugation time are 2~8min.
The described method using difunctional ion liquid abstraction separation light rare earth elements, in difunctional ionic liquid, N-
Octylpyridinium villaumite ([OPy] [Cl]) and di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (P507) select n-amyl alcohol as dilution
Agent.
The method using difunctional ion liquid abstraction separation light rare earth elements, P507Saponification rate 100%.
The described method using difunctional ion liquid abstraction separation light rare earth elements, strippant use concentration for
The aqueous ammonium chloride solution of 0.05~0.3mol/L.
Design philosophy of the invention is:
Ionic liquid steam forces down, and thermal stability is good, is subject in terms of hydrometallurgy as a kind of green solvent extensive
It pays close attention to, often achievees the purpose that separating-purifying using dissolubility of the ionic liquid to substance in previous research.And the present invention is with new
Science, probe into the effect that ionic liquid plays in light rare earth separation process as extractant, realize ionic liquid by
" supporting role " identity of " green solvent " to extractant " leading role " identity counteroffensive, using pyridine ionic liquid and convention acidic
Phosphine extractant is organic to cooperatively form difunctional ionic liquid, completes P507By the function of convention acidic extractant to ionic liquid
Transformation, while retaining its high extraction ability, realizes the environmentally friendly separation of rare earth element.
The invention has the advantages and beneficial effects that:
The present invention is using the aqueous solution containing light rare earth elements as material liquid, using di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester
It is combined with N- octylpyridinium villaumite, sodium hydroxide is added and adjusts, retains the yin of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester
Ion is combined with the cation of N- octylpyridinium villaumite, is synthesized difunctional ionic liquid and is carried out mixing extraction with acid material liquid
It takes, the organic phase and raffinate of centrifuged supported rare earth are stripped rare earth using strippant, centrifuged
Pure earth solution and recyclable ionic liquid.While the present invention had not only retained ionic liquid intrinsic advantage, but also have both biography
Unite extractant high extractibility the advantages of.Extraction efficiency of the present invention is high, and good separating effect, equilibration time is short, easy to operate, does not generate
Emulsion, ionic liquid can be recycled, and difunctional ionic liquid has a extensive future as a kind of green extractant.
Specific embodiment
In the specific implementation process, the present invention is extracted and is stripped after the completion of separation process, in raffinate and anti-stripping agent
Rare earth concentration can refer to GB/T14635-2008 rare earth metal and its compound chemical analysis method, pass through EDTA titration (second
Ethylenediamine tetraacetic acid (EDTA) titration) it measures, rare earth concentration is obtained by minusing in ionic liquid.
Rare earth extraction rate E is calculated by formula 2:
Formula 2
Rare earth stripping rate S is calculated by formula 3:
Formula 3.
In formula: Ct、CeRare earth concentration respectively in the water phase of extraction front and back, mol/L.[M]aRare earth in water phase when to balance
Concentration, mol/L.[M]oFor the initial concentration of organic phase, mol/L.
In order to further appreciate that the present invention, embodiment of the present invention is described in detail below in conjunction with example, but
It is it will be understood to those of skill in the art that following Examples is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.
The person that is not specified actual conditions in embodiment, carries out, instrument and reagent are not according to conventional conditions or manufacturer's recommended conditions
Manufacturer person is indicated, being can be by the conventional products of commercially available purchase.
Embodiment 1
In the present embodiment, using difunctional ion liquid abstraction separation light rare earth elements method, according to the following steps into
Row:
(1) using the re chloride containing lanthanum as material liquid, the concentration of lanthanum is 0.04mol/L, pH 5.5 in material liquid.
(2) configure difunctional ionic liquid and be used as extractant, select n-amyl alcohol as diluent, N- octylpyridinium villaumite with
P507Molar ratio be 1:1, P507Concentration be 0.1mol/L, the concentration of N- octylpyridinium villaumite is 0.1mol/L, P507Saponification
Rate is 100%.
(3) by material liquid and difunctional ionic liquid, hybrid extraction, mixing are comparably O/A=1:1 in an oscillator, extract
Revolving speed is 50r/min in the process, and extraction time 30min, 25 DEG C of extraction temperature, mixed solution is centrifuged after the completion of extraction
The organic phase and raffinate of supported rare earth are obtained, centrifugal rotational speed 2000r/min, centrifugation time 5min are measured in raffinate
The concentration of lanthanum, obtaining extraction yield is 27.19%.
(4) organic phase of supported rare earth is stripped using strippant, strippant is the chlorination of 0.3mol/L
Aqueous ammonium is 1:1 compared to O/A, and revolving speed is 50r/min, back-extraction time 30min during back extraction, and back extraction is completed
Mixed solution afterwards is centrifuged recovering rare earth, and the centrifugal rotational speed of centrifuge separation is 2000r/min, centrifugation time 5mim, divides
From ionic liquid carry out regeneration, be computed, stripping rate 17.12%.
Embodiment 2
In the present embodiment, using difunctional ion liquid abstraction separation light rare earth elements method, according to the following steps into
Row:
(1) using the re chloride containing cerium as material liquid, the concentration of cerium is 0.02mol/L, pH 1 in material liquid.
(2) configure difunctional ionic liquid and be used as extractant, select n-amyl alcohol as diluent, N- octylpyridinium villaumite with
P507Molar ratio be 1:3, P507Concentration be 0.08mol/L, the concentration of N- octylpyridinium villaumite is 0.08mol/L, P507Soap
Rate is 100%.
(3) by material liquid and difunctional ionic liquid, hybrid extraction, mixing are comparably O/A=1:1 in an oscillator, extract
Revolving speed is 75r/min in the process, and extraction time 25min, 35 DEG C of extraction temperature, mixed solution is centrifuged after the completion of extraction
The organic phase and raffinate of supported rare earth are obtained, centrifugal rotational speed 3000r/min, centrifugation time 8min are measured in raffinate
The concentration of lanthanum, obtaining extraction yield is 15%.
(4) organic phase of supported rare earth is stripped using strippant, strippant is the chlorination of 0.1mol/L
Aqueous ammonium is 1:1 compared to O/A, and revolving speed is 75r/min, back-extraction time 25min during back extraction, and back extraction is completed
Mixed solution afterwards is centrifuged recovering rare earth, and the centrifugal rotational speed of centrifuge separation is 3000r/min, centrifugation time 8mim, divides
From ionic liquid carry out regeneration, be computed, stripping rate 57.15%.
Embodiment 3
In the present embodiment, using difunctional ion liquid abstraction separation light rare earth elements method, according to the following steps into
Row:
(1) using the re chloride containing praseodymium as material liquid, the concentration of praseodymium is 0.01mol/L, pH 2.5 in material liquid.
(2) configure difunctional ionic liquid and be used as extractant, select n-amyl alcohol as diluent, N- octylpyridinium villaumite with
P507Molar ratio be 1:1, P507Concentration be 0.05mol/L, the concentration of N- octylpyridinium villaumite is 0.05mol/L, P507Soap
Rate is 100%.
(3) by material liquid and difunctional ionic liquid, hybrid extraction, mixing are comparably O/A=1:1 in an oscillator, extract
Revolving speed is 100r/min, extraction time 20min in the process, and 15 DEG C of extraction temperature, mixed solution is through centrifugation point after the completion of extraction
From the organic phase and raffinate of supported rare earth is obtained, centrifugal rotational speed 2500r/min, centrifugation time 3min measure raffinate
The concentration of middle lanthanum, obtaining extraction yield is 89.87%.
(4) organic phase of supported rare earth is stripped using strippant, strippant is the chlorination of 0.08mol/L
Aqueous ammonium is 1:4 compared to O/A, and revolving speed is 100r/min, back-extraction time 20min during back extraction, and back extraction is completed
Mixed solution afterwards is centrifuged recovering rare earth, and the centrifugal rotational speed of centrifuge separation is 2500r/min, centrifugation time 3mim, divides
From ionic liquid carry out regeneration, be computed, stripping rate 11%.
Embodiment 4
In the present embodiment, using difunctional ion liquid abstraction separation light rare earth elements method, according to the following steps into
Row:
(1) using the rare earth nitrate solution containing neodymium as material liquid, the concentration of neodymium is 0.01mol/L, pH 3 in material liquid.
(2) configure difunctional ionic liquid and be used as extractant, select n-amyl alcohol as diluent, N- octylpyridinium villaumite with
P507Molar ratio be 1:1, P507Concentration be 0.03mol/L, the concentration of N- octylpyridinium villaumite is 0.03mol/L, P507Soap
Rate is 100%.
(3) by material liquid and difunctional ionic liquid, hybrid extraction, mixing are comparably O/A=1:1 in an oscillator, extract
Revolving speed is 150r/min in the process, and extraction time 15min, 5 DEG C of extraction temperature, mixed solution is centrifuged after the completion of extraction
The organic phase and raffinate of supported rare earth are obtained, centrifugal rotational speed 3500r/min, centrifugation time 2min are measured in raffinate
The concentration of lanthanum, obtaining extraction yield is 60.02%%.
(4) organic phase of supported rare earth is stripped using strippant, strippant is the chlorination of 0.05mol/L
Aqueous ammonium is 1:2 compared to O/A, and revolving speed is 150r/min, back-extraction time 15min during back extraction, and back extraction is completed
Mixed solution afterwards is centrifuged recovering rare earth, and the centrifugal rotational speed of centrifuge separation is 3500r/min, centrifugation time 2mim, divides
From ionic liquid carry out regeneration, be computed, stripping rate 15%.
Embodiment the result shows that, the present invention has the advantages that extraction efficiency using difunctional ion liquid abstraction rare earth
Height, equilibration time is short, and two phase stratification is clear after extraction, and no emulsion generates, and does not generate secondary pollution in extraction process.
Claims (8)
1. a kind of method using difunctional ion liquid abstraction separation light rare earth elements, which is characterized in that according to the following steps
It carries out:
(1) aqueous solution of the configuration containing light rare earth elements is material liquid, and light rare earth concentration is 0.01~0.04mol/ in material liquid
L, pH value of solution are 1~5.5；
(2) difunctional ionic liquid is configured as extractant, N- octylpyridinium villaumite ([OPy] [Cl]) and 2- ethylhexyl phosphonic acids
Single 2-ethyl hexyl ester (P507) molar ratio be 1:1~1:3, P507Concentration be 0.03~0.1mol/L, N- octylpyridinium chlorine
The concentration of salt is 0.03~0.1mol/L；
(3) hybrid extraction, mixing are comparably 1:1, revolving speed in extraction process in an oscillator for material liquid and difunctional ionic liquid
For 50~150r/min, extraction time is 15~30min, and extraction temperature is 5~35 DEG C, the mixed solution after the completion of extracting pass through from
The organic phase and raffinate of the isolated supported rare earth of the heart；
(4) organic phase of supported rare earth is stripped using strippant, the centrifugal rotational speed for being stripped centrifuge separation is
2000~3500r/min, centrifugation time are 2~8min, centrifuged pure earth solution and ionic liquid.
2. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In light rare earth elements is lanthanum, cerium, praseodymium or neodymium.
3. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In the aqueous solution containing light rare earth elements is re chloride or rare earth nitrate solution, and optimal is re chloride.
4. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In in difunctional ionic liquid, cation is N- octylpyridinium [Opy]+, anion is [P507]-, difunctional ionic liquid yin-yang
The structural formula of ion is as shown in Equation 1:
5. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In in step (3), centrifugal rotational speed is 2000~3500r/min, and centrifugation time is 2~8min.
6. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In, in difunctional ionic liquid, N- octylpyridinium villaumite ([OPy] [Cl]) and di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester
(P507) select n-amyl alcohol as diluent.
7. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In P507Saponification rate 100%.
8. the method described in accordance with the claim 1 using difunctional ion liquid abstraction separation light rare earth elements, feature exist
In strippant uses concentration for the aqueous ammonium chloride solution of 0.05~0.3mol/L.
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| CN112588274A (en) * | 2020-12-21 | 2021-04-02 | 江苏南方永磁科技有限公司 | Extraction material for separating cerium and preparation method thereof |
| CN112695214A (en) * | 2020-12-21 | 2021-04-23 | 江苏南方永磁科技有限公司 | Lanthanum extraction material and preparation method thereof |
| CN113106271A (en) * | 2021-04-06 | 2021-07-13 | 中国科学院过程工程研究所 | Method for purifying rare earth element gadolinium with high purity by using carboxylic acid functionalized ionic liquid |
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