CN107227404A - A kind of method of extract and separate lanthanum - Google Patents
A kind of method of extract and separate lanthanum Download PDFInfo
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- CN107227404A CN107227404A CN201710364288.4A CN201710364288A CN107227404A CN 107227404 A CN107227404 A CN 107227404A CN 201710364288 A CN201710364288 A CN 201710364288A CN 107227404 A CN107227404 A CN 107227404A
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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
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
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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
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention discloses a kind of method of extract and separate lanthanum, its step is as follows：1）LaCePr aqueous phases and PrNd organic phases are obtained using extractant separation LaCePrNd chloride solutions；2）LaCePr aqueous phases are separated using extractant, thick La aqueous phases, CePr aqueous phases and organic phase containing Pr is obtained；3）Separation PrNd organic phases obtain PrNd aqueous phases and Nd organic phases；4）Nd organic phases are stripped using hydrochloric acid, Nd strip aqueous is obtained；5）Thick La is separated using extractant, non-RE waste water and La organic phases is obtained；Using CeCl3Solution is stripped La organic phases, obtains La products and Ce organic phases；6）Using PrCl3Solution and the organic phase separation CePr aqueous phases of Ce, obtain Ce aqueous phases and Pr organic phases；7）Pr aqueous phases are obtained using hydrochloric acid back extraction Pr organic phases, Pr aqueous phases are used as product.Realize that extract and separate lanthanum technique productions cost is lower, production waste water is less.
Description
Technical field
The present invention relates to a kind of separation method of rare earth element, more particularly to a kind of method of extract and separate lanthanum.
Background technology
In recent years, country is greatly developed towards the research of high-endization, intellectuality, the new and high technology of precision and Material Field,
High-purity La2O3As the basic raw material of the forward position such as precision optics glass, thermoelectric material, laser material material, belong to grand strategy
Property resource.
Current La2O3Production technology mainly uses the conventional method and stream of extract and separate lanthanum in extraction and separation technology, light rare earth
Journey is suitable by LaCePr/Nd, LaCe/Pr, La/Ce separation using P204- kerosene-hydrochloric acid system or P507- kerosene-hydrochloric acid system
Sequence successively obtains Nd, Pr and La, Ce products, or by LaCe/PrNd, La/Ce, Pr/Nd separation sequence successively obtain La, Ce and
Pr, Nd product, both conventional methods fill groove material and acid and alkali consumption is big, and fixed investment and production cost are high.Therefore, Yan Chunhua
Et al. improvement was done to bastnaesite rare earth extraction separation process, develop band three outlet light rare earth separating technology flow, Deng
Also research is optimized to mixed light rare earth extraction and separation technology in assistant state et al., develops the light rare earth separation of the fuzzy separation of band
Technological process.But current south ion rare-earth smelting enterprise La2O3Product separation costs are higher, cause corporate profit margin relatively low, money
Source wastes serious.
The content of the invention
The invention discloses a kind of method from extract and separate lanthanum, it is desirable to provide a kind of low extract and separate lanthanum of separation costs
Technology.
The method of the extract and separate lanthanum of the present invention is as follows：
1）P507 concentration is used for extractant and [H that 1.0 ~ 1.5mol/L, solvent are kerosene+] concentration be 0.1 ~ 2mol/L,
[Nd3++Pr3+] concentration be 0.3 ~ 2mol/L (PrNd) Cl3Solution separation LaCePrNd chloride solutions obtain LaCePr aqueous phases
With PrNd organic phases；
2）P507 concentration is used for extractant and [H that 1.0 ~ 1.5mol/L, solvent are kerosene+] concentration be 0.1 ~ 2mol/L,
[Nd3++Pr3+] concentration be 0.3 ~ 2mol/L (PrNd) Cl3Solution separating step 1）LaCePr aqueous phases, obtain thick La aqueous phases,
CePr aqueous phases and organic phase containing Pr；
3）Using [H+] concentration be 0.3 ~ 2mol/L, [Nd3+] concentration be 0.3 ~ 2mol/L NdCl3Solution separating step 1）'s
PrNd organic phases and step 2）The mixing organic phase of the organic phase containing Pr obtain PrNd aqueous phases and Nd organic phases；By PrNd aqueous phases
10 ~ 30% are used as product, 20 ~ 50% return to step 1）For separating LaCePrNd chlorides, 20 ~ 50% return to step 2）For dividing
From LaCePr aqueous phases；
4）Use concentration to be stripped Nd organic phases for 4 ~ 6mol/L hydrochloric acid, obtain Nd strip aqueous；10 ~ 30%Nd is stripped
Aqueous phase is used as product, 70 ~ 90% return to step steps 3）For separating mixing organic phase；
5）P507 concentration is used for 1.0 ~ 1.5mol/L, the extractant separating step 2 that solvent is kerosene）Thick La, obtain non-dilute
Native waste water and La organic phases；Using [H+] concentration be 0.3 ~ 2mol/L, [Ce3+] concentration be 0.3 ~ 2mol/L CeCl3Solution is anti-
La organic phases are extracted, La products and Ce organic phases is obtained；
6）Using [H+] concentration be 0.3 ~ 2mol/L, [Pr3+] concentration be 0.3 ~ 2mol/L PrCl3Solution and step 5）Ce have
Machine phase separation step 2）CePr aqueous phases, obtain Ce aqueous phases and Pr organic phases；3 ~ 10%Ce aqueous phases are returned as product, 90 ~ 97%
Step 5）For being stripped La organic phases；
7）Use concentration for 4 ~ 6mol/L hydrochloric acid back extraction Pr organic phases obtain Pr aqueous phases, 10 ~ 30%Pr aqueous phases as product,
70 ~ 90% return to step 6）For separating step 2）CePr aqueous phases.
Rare Earth Separation cost height is evaluated, extraction quantity is important evaluation index.Ce/Nd separations are than Ce/Pr or Pr/Nd
Greatly, use and principle is separated into Ce/Nd, be LaCePr and PrNd by LaCePrNd extract and separates, according to tandem Optimized Extraction work
Skill design theory is calculated, and the extraction quantity or washing amount so separated can be much smaller, substantially reduces technological process, reduces extraction
Sump volume, reduces and fills groove one-time investment and chemical materials unit consumption, and production cost can decline to a great extent.LaCePrNd is separated,
La/CePr, PrNd/Nd, non-rare earth/La, La/Ce and Ce/P separation combination, form interactive.Using La/CePr separation and
The extraction quantity of the load organic phases of LaCePrNd separation substitutes the extraction quantity of PrNd/Nd separation, realizes that PrNd/Nd separates organic phase
Without saponification, so as to reduce alkali consumption；A part of aqueous phase that PrNd/Nd is separated substitutes traditional La/ as cleaning solution
The hydrochloric acid cleaning solution that CePr separation is separated with LaCePrNd, makes La/CePr separation and LaCePrNd separating, washings without acid, so that
Saving acid and alkali consumption is reached, the purpose of production cost is reduced, extract and separate is also reduced and produces the discharge capacity of waste water, and reduce
Acidity and salinity in waste water.PrNd/Nd separation employs organic phase fed technology, reduces the previous separation of LaCePr/PrNd
The consumption of the back extraction acid of load organic phases.An anti-stripping agent shunting part is as washing lotion, and this cleaning solution is easily extraction component material
Liquid, improves washing and separating effect, and reduce sour consumption.
The above-mentioned technological process of the present invention is short, and realization is filled groove material and more saved, and acid and alkali consumption is lower, reduces production cost,
Reduce equipment and fill groove investment, reduce production discharge of wastewater.
Brief description of the drawings
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings, but not constituted to the present invention's
Any limitation.
Fig. 1 is the process flow diagram of the present invention.
Embodiment
The LaCePrNd chloride solutions component of table 1 (is calculated) by oxide
| Element | La2O3 | CeO2 | Pr6O11 | Nd2O3 |
| WRE/% | 52.69 | 5.52 | 12.80 | 29.00 |
The above-mentioned chloride solution containing LaCePrNd is separated into tetra- Rare Earth Elements Determination products of La, Ce, Pr, Nd, product matter
Figureofmerit is as shown in table 2.
The product quality indicator of table 2 La, Ce, Pr, Nd rare earth element
| Element term | Purity（%） | Non-rare earth impurity（%） |
| La | ＞ 99.99 | CeO2、Pr6O11、Nd2O3Equal ＜ 0.002 |
| Ce | ＞ 99.99 | La2O3、Pr6O11、Nd2O3Equal ＜ 0.002 |
| Pr | ＞ 99.9 | La2O3、CeO2The equal ＜ 0.04 of equal ＜ 0.01, Nd2O3 |
| Nd | ＞ 99.9 | La2O3、CeO2Equal ＜ 0.01, Pr6O11 ＜ 0.04 |
| PrNd | Pr+Nd ＞ 99.9 | La2O3、CeO2Equal ＜ 0.01 |
Embodiment 1
P507 concentration is used for extractant that 1.5mol/L, solvent are kerosene（Saponification rate is 36%）[H+] concentration be 0.5mol/
L、[Nd3++Pr3+] concentration be 1.5mol/L (PrNd) Cl3Solution, be by 26 grades of extractions, 50 grades of washing separation concentration
1.5mol/L, acidity obtains LaCePr aqueous phases and PrNd organic phases for pH3.5 LaCePrNd chloride solutions；It is dense using P507
The extractant that degree is 1.5mol/L, solvent is kerosene（Saponification rate is 36%）[H+] concentration be 0.5mol/L, [Nd3++Pr3+] dense
Spend (PrNd) Cl for 1.5mol/L3Solution, by 26 grades extraction 50 grades washing separation LaCePr aqueous phases, obtain thick La aqueous phases,
CePr aqueous phases and organic phase containing Pr；Using [H+] concentration be 0.5mol/L, [Nd3+] concentration be 1.5mol/L NdCl3Solution, warp
The mixing organic phase for crossing 40 grades of washing separation PrNd organic phases and the organic phase containing Pr obtains PrNd aqueous phases and Nd organic phases；By PrNd
The 30% of aqueous phase is as product, and 35% returns for separating LaCePrNd chlorides, and 35% returns for separating LaCePr aqueous phases；Adopt
The hydrochloric acid for being 5mol/L with concentration is stripped Nd organic phases, obtains Nd strip aqueous；30%Nd strip aqueous as product,
70% returns for separating mixing organic phase；P507 concentration is used to extract for the extractant that 1.5mol/L, solvent are kerosene by 10 grades
30 grades of washing thick La of separation are taken, non-RE waste water and La organic phases is obtained；Using [H+] concentration be 0.5mol/L, [Ce3+] concentration
For 1.5mol/L CeCl3Solution, is stripped La organic phases by 50 grades of washings, obtains La products and Ce organic phases；Using [H+]
Concentration is 0.5mol/L, [Pr3+] concentration be 1.5mol/L PrCl3Solution and Ce organic phases, by 35 grades of extractions, 25 grades of washings
CePr aqueous phases are separated, Ce aqueous phases and Pr organic phases is obtained；5%Ce aqueous phases are as product, and 95% returns for being stripped La organic phases；
Concentration is used to obtain Pr aqueous phases for 5mol/L hydrochloric acid back extraction Pr organic phases, 30%Pr aqueous phases are as product, and 70% returns and is used for
Separate CePr aqueous phases.Through measuring and calculating, the method for the extract and separate lanthanum is deposited groove organic phase and reduced about compared with the method for traditional SEPARATION OF La
35%, groove amount of rare earth depositing reduces about 35%, and hydrochloric acid consumption reduces about 50%, and liquid caustic soda consumption reduces about 50%.
Embodiment 2
The LaCePrNd chloride solutions component such as upper table 1 of the present embodiment, product quality indicator is as shown in table 2.
P507 concentration is used for extractant that 1.2mol/L, solvent are kerosene（Saponification rate is 36%）[H+] concentration is
1.2mol/L、[Nd3++Pr3+] concentration be 0.5mol/L (PrNd) Cl3Solution, by 30 grades of extractions, 60 grades of washing separation concentration
For 1.5mol/L, acidity obtains LaCePr aqueous phases and PrNd organic phases for pH3.5 LaCePrNd chloride solutions；Using P507
The extractant that concentration is 1.2mol/L, solvent is kerosene（Saponification rate is 36%）[H+] concentration be 1.2mol/L, [Nd3++Pr3+]
Concentration is 0.5mol/L (PrNd) Cl3Solution, by 35 grades of extractions, 56 grades of washing separation LaCePr aqueous phases, obtains thick La water
Phase, CePr aqueous phases and organic phase containing Pr；Using [H+] concentration be 1.2mol/L, [Nd3+] concentration be 0.5mol/L NdCl3It is molten
Liquid, the mixing organic phase for separating PrNd organic phases and the organic phase containing Pr by 50 grades of washings obtains PrNd aqueous phases and Nd organic phases；
Using the 10% of PrNd aqueous phases as product, 45% returns for separating LaCePrNd chlorides, and 45% returns for separating LaCePr water
Phase；Use concentration to be stripped Nd organic phases for 6mol/L hydrochloric acid, obtain Nd strip aqueous；10%Nd strip aqueous conducts
Product, 90% returns for separating mixing organic phase；P507 concentration is used to pass through 8 for the extractant that 1.2mol/L, solvent are kerosene
36 grades of washing thick La of separation of level extraction, obtain non-RE waste water and La organic phases；Using [H+] concentration be 1.2mol/L, [Ce3+]
Concentration is 0.5mol/L CeCl3Solution, is stripped La organic phases by 60 grades of washings, obtains La products and Ce organic phases；Adopt
With [H+] concentration be 1.2mol/L, [Pr3+] concentration be 0.5mol/L PrCl3Solution and Ce organic phases, by 35 grades of extractions 25
Level washing separation CePr aqueous phases, obtain Ce aqueous phases and Pr organic phases；10%Ce aqueous phases are as product, and 90% returns for being stripped La
Organic phase；Concentration is used to obtain Pr aqueous phases for 5mol/L hydrochloric acid back extraction Pr organic phases, 10%Pr aqueous phases are returned as product, 90%
It is back to separation CePr aqueous phases.Through measuring and calculating, the method for the extract and separate lanthanum deposits groove organic phase compared with the method for traditional SEPARATION OF La
About 35% is reduced, groove amount of rare earth depositing reduces about 35%, and hydrochloric acid consumption reduces about 50%, and liquid caustic soda consumption reduces about 50%.
Through measuring and calculating, the method for extract and separate lanthanum of the invention deposits the reduction of groove organic phase compared with the method for traditional SEPARATION OF La
About 32%, groove amount of rare earth depositing reduces about 30%, and hydrochloric acid consumption reduces about 43%, and liquid caustic soda consumption reduces about 47%.The extraction of Optimal improvements
The method of separation reduces production cost, reduces equipment and fills groove investment, reduces production discharge of wastewater, technique is advanced conjunction
Reason.
Claims (1)
1. a kind of method from extract and separate lanthanum, it is characterized in that comprising the steps of：
1）P507 concentration is used for extractant and [H that 1.0 ~ 1.5mol/L, solvent are kerosene+] concentration be 0.1 ~ 2mol/L, [Nd3 ++Pr3+] concentration be 0.3 ~ 2mol/L (PrNd) Cl3Solution separation LaCePrNd chloride solutions obtain LaCePr aqueous phases and
PrNd organic phases；
2）P507 concentration is used for extractant and [H that 1.0 ~ 1.5mol/L, solvent are kerosene+] concentration be 0.1 ~ 2mol/L, [Nd3 ++Pr3+] concentration be 0.3 ~ 2mol/L (PrNd) Cl3Solution separating step 1）LaCePr aqueous phases, obtain thick La aqueous phases, CePr
Aqueous phase and organic phase containing Pr；
3）Using [H+] concentration be 0.3 ~ 2mol/L, [Nd3+] concentration be 0.3 ~ 2mol/L NdCl3Solution separating step 1）'s
PrNd organic phases and step 2）The mixing organic phase of the organic phase containing Pr obtain PrNd aqueous phases and Nd organic phases；By PrNd aqueous phases
10 ~ 30% are used as product, 20 ~ 50% return to step 1）For separating LaCePrNd chlorides, 20 ~ 50% return to step 2）For dividing
From LaCePr aqueous phases；
4）Use concentration to be stripped Nd organic phases for 4 ~ 6mol/L hydrochloric acid, obtain Nd strip aqueous；10 ~ 30%Nd is stripped
Aqueous phase is used as product, 70 ~ 90% return to step steps 3）For separating mixing organic phase；
5）P507 concentration is used for 1.0 ~ 1.5mol/L, the extractant separating step 2 that solvent is kerosene）Thick La, obtain non-dilute
Native waste water and La organic phases；Using [H+] concentration be 0.3 ~ 2mol/L, [Ce3+] concentration be 0.3 ~ 2mol/L CeCl3Solution is anti-
La organic phases are extracted, La products and Ce organic phases is obtained；
6）Using [H+] concentration be 0.3 ~ 2mol/L, [Pr3+] concentration be 0.3 ~ 2mol/L PrCl3Solution and step 5）Ce have
Machine phase separation step 2）CePr aqueous phases, obtain Ce aqueous phases and Pr organic phases；3 ~ 10%Ce aqueous phases are returned as product, 90 ~ 97%
Step 5）For being stripped La organic phases；
7）Use concentration for 4 ~ 6mol/L hydrochloric acid back extraction Pr organic phases obtain Pr aqueous phases, 10 ~ 30%Pr aqueous phases as product,
70 ~ 90% return to step 6）For separating step 2）CePr aqueous phases.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306048A (en) * | 2019-08-01 | 2019-10-08 | 南昌航空大学 | A method of preparing high-purity lanthanum, high-purity cerium and high-purity praseodymium neodymium |
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| WO1998014621A1 (en) * | 1996-09-30 | 1998-04-09 | Basf Aktiengesellschaft | Use of hydrocarbon-soluble aminomethylenephosphonic acid derivatives for the solvent extraction of metal ions from aqueous solutions |
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| CN110306048A (en) * | 2019-08-01 | 2019-10-08 | 南昌航空大学 | A method of preparing high-purity lanthanum, high-purity cerium and high-purity praseodymium neodymium |
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Effective date of registration: 20230308 Address after: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee after: Institute of resource utilization and rare earth development, Guangdong Academy of Sciences Address before: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee before: Institute of rare metals, Guangdong Academy of Sciences |