CN108220632B - Rare earth recovery and enrichment process - Google Patents
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- 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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- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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Abstract
The invention relates to a rare earth elementA collecting and enriching process for collecting and enriching P507 and OH‑Compared with the rare earth product separated by the multi-rare earth solution prepared by the conventional separation methods such as a fractional crystallization method, a fractional precipitation method, an ion exchange chromatography, an extraction chromatography and the like in the prior art, the technical scheme of the invention has the advantages of full separation of rare earth products such as lanthanum, cerium, dysprosium and ytterbium, high purity, high yield, suitability for large-scale production, simple and convenient operation, low production cost, convenience for industrial production and the like.
Description
Technical Field
The invention relates to the field of rare earth extraction and separation, in particular to a rare earth recovery and enrichment process.
Background
The separation method of rare earth elements is mostly based on a wet method, although the physicochemical properties of the rare earth elements are similar, the rare earth compounds still have slight difference, in the field of the wet method, the rare earth is separated mainly by means of an extractant or a precipitator, and the slight difference is enlarged by repeatedly carrying out extraction or precipitation reaction, so that the rare earth elements are separated from each other. The separation method of rare earth elements mainly comprises a fractional crystallization method, a fractional precipitation method, an ion exchange chromatography, an extraction chromatography, a solvent extraction method and the like. The separation principle of solvent extraction is that the extracted substance is transferred from the water phase to the organic phase by utilizing the difference of the distribution coefficients of the extracted substance in the water phase and the organic phase, and the vast majority of the extracted substance is separated through multi-stage extraction and is enriched and extracted in a designated stage. The solvent extraction method has the advantages of simple process, large treatment capacity, strong selectivity to extracted substances, thorough intermetallic separation and the like, and is a mainstream separation method for certain metals.
P507 exists basically as dimer in non-polar or weak polar solvent, and the extraction mechanism is in accordance with D2EHPA is substantially similar and the ratio of P507 to D is known from the structural formula2EHPA has one alkoxy (OR) and one alkyl (R) less, and the H on P507 is increased by the electron-pushing effect of the alkyl+Is difficult to dissociate, and has an acid ratio D2The EHPA is weak, so that the extraction capacity of the EHPA to rare earth is reduced, and the stability of the EHPA is higher than that of the generated extract compound, so that the EHPA is easier to back extract than the P204. P507 is suitable for the extraction separation of mixed rare earth mainly comprising heavy rare earth, in recent years, China researches a process for continuously extracting and separating single light rare earth element and medium rare earth element by using P507, and achieves the purpose of continuously separating lanthanum, cerium, praseodymium, neodymium, samarium, europium and gadolinium in a medium by using a single extracting agent; seven single high-purity rare earth products are obtained simultaneously, and the process has the characteristics of high yield, low cost and the like. However, in the current process, the separation of light and medium rare earths is still concentrated, and for the extraction and enrichment of multi-element rare earth feed liquid containing heavy rare earths, the technical difficulty of how to improve the purity and recovery rate of the separated product still exists.
Disclosure of Invention
In order to solve the technical problems, the invention provides a rare earth recovery and enrichment process, which takes P507 as an extracting agent and rare earth chloride feed liquid containing lanthanum, cerium, dysprosium and ytterbium with the pH value range of 3-5 as a solution to be extracted, and comprises the following steps:
1) adding the solution to be extracted, P507 and OH into an extraction reactor in sequence-The preparation method comprises the following steps of stirring and reacting type strongly basic anion exchange resin for 10-15 min under a heating condition, standing for 0.5-1 h, and separating an organic phase, a water phase and an anion exchange resin phase, wherein the water phase is a feed liquid containing lanthanum and cerium, and the organic phase is an organic phase loaded with dysprosium and ytterbium.
2) And adding hydrochloric acid with the concentration of 3-4 mol/L into the dysprosium ytterbium-loaded organic phase for back extraction, and obtaining an acid-containing dysprosium ytterbium chloride solution after the back extraction.
3) Adding conventional saponification P204 into the feed liquid containing lanthanum and cerium for re-extraction to obtain a separated product lanthanum and a cerium-loaded organic phase, performing back extraction on the cerium-loaded organic phase by adopting hydrochloric acid with the concentration of 1.5-1.7 mol/L, and separating the back-extracted water phase to obtain a product cerium.
4) And carrying out countercurrent extraction on the acid-containing dysprosium ytterbium chloride solution to remove residual hydrochloric acid in the solution, wherein an acid extraction organic phase is N235, the concentration of the N235 is 0.6mol/L, and the ratio of the number of moles of the N235 to the number of moles of the residual hydrochloric acid is controlled to be 2: 1, so as to obtain the acid-removed dysprosium ytterbium chloride solution.
5) Adding conventional saponification P204 into the deacidified dysprosium ytterbium chloride solution for re-extraction to obtain a separated product dysprosium and ytterbium-loaded organic phase, performing back extraction on the ytterbium-loaded organic phase by adopting hydrochloric acid with the concentration of 3-4 mol/L, controlling the ratio of the mole number of the hydrochloric acid to the mole number of rare earth in the organic phase to be 3-3.5: 1, and separating the back-extracted aqueous phase to obtain a product ytterbium.
In the step 1), the molar ratio of the rare earth element to P507 in the solution to be extracted is 0.3-0.5: 1, and the OH is-The molar ratio of the type strong-base anion exchange resin to chloride ions in the solution to be extracted is 10-15: 1.
In the step 2), the ratio of the mole number of the hydrochloric acid to the mole number of dysprosium and ytterbium in the organic phase is 4-5: 1.
The OH group-The strongly basic anion exchange resin is styrene anion exchange resin, and the effective exchange capacity is 5-6 mol/kg.
And the P507 is a sulfonated kerosene solution of the P507.
The concentration of the rare earth in the solution to be extracted is 0.3-0.5 mol/L.
The purity of the lanthanum product, the purity of the cerium product, the purity of the dysprosium product and the purity of the ytterbium product are all higher than 99.99%, and the yield is higher than 95.21%.
The invention has the technical effects that: compared with the rare earth products separated by the multi-rare earth solution prepared by the conventional separation methods such as a fractional crystallization method, a fractional precipitation method, an ion exchange chromatography method, an extraction chromatography method and the like, the technical scheme of the extraction, enrichment and separation of the multi-rare earth element feed liquid adopted by the invention has the advantages of full separation of products such as lanthanum, cerium, dysprosium and ytterbium, high purity and yield, suitability for large-scale production, simple and convenient operation, low production cost, convenience for industrial production and the like.
Detailed Description
The present invention will be described in further detail with reference to examples and comparative examples.
Example 1:
the sulfonated kerosene solution of P507 is used as an extracting agent. The rare earth chloride feed liquid with the pH value of 3 and containing lanthanum, cerium, dysprosium and ytterbium elements is a solution to be extracted, and the rare earth concentration of the solution to be extracted is 0.3 mol/L. Adding the solution to be extracted, P507 and OH into an extraction reactor in sequence-The preparation method comprises the following steps of stirring and reacting type strongly basic anion exchange resin for 15min under a heating condition, standing for 1h, and separating an organic phase, a water phase and an anion exchange resin phase, wherein the water phase is a feed liquid containing lanthanum and cerium, and the organic phase is an organic phase loaded with dysprosium and ytterbium. The molar ratio of the rare earth elements to P507 in the solution to be extracted is 0.3: 1, and the OH-The molar ratio of the type strong base anion exchange resin to chloride ions in the solution to be extracted is 15: 1. The OH group-The strongly basic anion exchange resin is phenylethyleneThe effective exchange capacity of the alkene anion exchange resin is 5 mol/kg. And adding hydrochloric acid with the concentration of 3mol/L into the dysprosium and ytterbium-loaded organic phase for back extraction to obtain an acid-containing dysprosium and ytterbium chloride solution, wherein the ratio of the number of moles of the hydrochloric acid to the number of moles of dysprosium and ytterbium in the organic phase is 4: 1. Adding conventional saponification P204 into the feed liquid containing lanthanum and cerium for re-extraction to obtain a separated product of lanthanum and a cerium-loaded organic phase, performing back extraction on the cerium-loaded organic phase by adopting hydrochloric acid with the concentration of 1.7mol/L, and separating the back-extracted water phase to obtain a product of cerium. And carrying out countercurrent extraction on the acid-containing dysprosium ytterbium chloride solution to remove residual hydrochloric acid in the solution, wherein an acid extraction organic phase is N235, the concentration of the N235 is 0.6mol/L, and the ratio of the number of moles of the N235 to the number of moles of the residual hydrochloric acid is controlled to be 2: 1, so as to obtain the acid-removed dysprosium ytterbium chloride solution. Adding conventional saponification P204 into the deacidified dysprosium ytterbium chloride solution for re-extraction to obtain a separated product dysprosium and ytterbium-loaded organic phase, performing back extraction on the ytterbium-loaded organic phase by adopting hydrochloric acid with the concentration of 3mol/L, controlling the ratio of the mole number of the hydrochloric acid to the mole number of rare earth in the organic phase to be 3: 1, and separating the back-extracted aqueous phase to obtain a product ytterbium. The purity of the product lanthanum, the purity of the product cerium, the purity of the product dysprosium and the purity of the product ytterbium are 99.990%, and the yield is 96.13%.
Example 2:
the sulfonated kerosene solution of P507 is used as an extracting agent. The rare earth chloride feed liquid with the pH value of 4 and containing lanthanum, cerium, dysprosium and ytterbium elements is a solution to be extracted, and the rare earth concentration of the solution to be extracted is 0.4 mol/L. Adding the solution to be extracted, P507 and OH into an extraction reactor in sequence-The preparation method comprises the following steps of stirring and reacting type strongly basic anion exchange resin for 12min under a heating condition, standing for 0.5h, and separating an organic phase, a water phase and an anion exchange resin phase, wherein the water phase is a feed liquid containing lanthanum and cerium, and the organic phase is an organic phase loaded with dysprosium and ytterbium. The molar ratio of the rare earth elements to P507 in the solution to be extracted is 0.4: 1, and the OH-The molar ratio of the type strong base anion exchange resin to chloride ions in the solution to be extracted is 10: 1. The OH group-The strongly basic anion exchange resin is styrene anion exchange resin, and the effective exchange capacity is 5.5 mol/kg. Loading the organic phase of dysprosium and ytterbiumAnd adding hydrochloric acid with the concentration of 3.5mol/L for back extraction to obtain an acid-containing dysprosium ytterbium chloride solution, wherein the ratio of the mole number of the added hydrochloric acid to the mole number of dysprosium and ytterbium in the organic phase is 4: 1. Adding conventional saponification P204 into the feed liquid containing lanthanum and cerium for re-extraction to obtain a separated product of lanthanum and a cerium-loaded organic phase, performing back extraction on the cerium-loaded organic phase by adopting hydrochloric acid with the concentration of 1.6mol/L, and separating the back-extracted water phase to obtain a product of cerium. And carrying out countercurrent extraction on the acid-containing dysprosium ytterbium chloride solution to remove residual hydrochloric acid in the solution, wherein an acid extraction organic phase is N235, the concentration of the N235 is 0.6mol/L, and the ratio of the number of moles of the N235 to the number of moles of the residual hydrochloric acid is controlled to be 2: 1, so as to obtain the acid-removed dysprosium ytterbium chloride solution. Adding conventional saponification P204 into the deacidified dysprosium ytterbium chloride solution for re-extraction to obtain a separated product dysprosium and ytterbium-loaded organic phase, performing back extraction on the ytterbium-loaded organic phase by adopting hydrochloric acid with the concentration of 3.5mol/L, controlling the ratio of the mole number of the hydrochloric acid to the mole number of rare earth in the organic phase to be 3.5: 1, and separating the back-extracted aqueous phase to obtain a product ytterbium. The purity of the product lanthanum, the purity of the product cerium, the purity of the product dysprosium and the purity of the product ytterbium are 99.995%, and the yield is 97.05%.
Example 3:
the sulfonated kerosene solution of P507 is used as an extracting agent. The rare earth chloride feed liquid with the pH value of 5 and containing lanthanum, cerium, dysprosium and ytterbium elements is a solution to be extracted, and the rare earth concentration of the solution to be extracted is 0.5 mol/L. Adding the solution to be extracted, P507 and OH into an extraction reactor in sequence-The preparation method comprises the following steps of stirring and reacting type strongly basic anion exchange resin for 10min under a heating condition, standing for 0.5h, and separating an organic phase, a water phase and an anion exchange resin phase, wherein the water phase is a feed liquid containing lanthanum and cerium, and the organic phase is an organic phase loaded with dysprosium and ytterbium. The molar ratio of the rare earth elements to P507 in the solution to be extracted is 0.5: 1, and the OH-The molar ratio of the type strong base anion exchange resin to chloride ions in the solution to be extracted is 12: 1. The OH group-The strongly basic anion exchange resin is styrene anion exchange resin, and the effective exchange capacity is 6 mol/kg. Adding hydrochloric acid with the concentration of 4mol/L into the organic phase loaded with dysprosium and ytterbium for back extraction to obtain a solution containing acid dysprosium and ytterbium chloride, and adding the solutionThe ratio of the mole number of the hydrochloric acid to the mole number of dysprosium and ytterbium in the organic phase is 4: 1. Adding conventional saponification P204 into the feed liquid containing lanthanum and cerium for re-extraction to obtain a separated product of lanthanum and a cerium-loaded organic phase, performing back extraction on the cerium-loaded organic phase by adopting hydrochloric acid with the concentration of 1.7mol/L, and separating the back-extracted water phase to obtain a product of cerium. And carrying out countercurrent extraction on the acid-containing dysprosium ytterbium chloride solution to remove residual hydrochloric acid in the solution, wherein an acid extraction organic phase is N235, the concentration of the N235 is 0.6mol/L, and the ratio of the number of moles of the N235 to the number of moles of the residual hydrochloric acid is controlled to be 2: 1, so as to obtain the acid-removed dysprosium ytterbium chloride solution. Adding conventional saponification P204 into the deacidified dysprosium ytterbium chloride solution for re-extraction to obtain a separated product dysprosium and ytterbium-loaded organic phase, performing back extraction on the ytterbium-loaded organic phase by adopting hydrochloric acid with the concentration of 4mol/L, controlling the ratio of the mole number of the hydrochloric acid to the mole number of rare earth in the organic phase to be 3: 1, and separating the back-extracted aqueous phase to obtain a product ytterbium. The purity of the product lanthanum, the purity of the product cerium, the purity of the product dysprosium and the purity of the product ytterbium are 99.992%, and the yield is 95.56%.
Comparative example 1:
when the extraction separation process different from the extraction separation process of the invention is adopted, particularly if the first-step separation is only carried out by adopting the conventional separation mode in the prior art, the rare earth elements cannot be completely separated, and the purity of the obtained rare earth products, particularly lanthanum and cerium, is lower than 98 percent, and the yield is lower than 92 percent.
Comparative example 2:
by adopting the extraction enrichment process parameters different from those of the invention, the purity and yield of the obtained rare earth product are obviously reduced due to the lack of enough extractant organic phase or different pH value environments and reaction liquid concentrations.
As can be seen from examples 1-3 and comparative examples 1-2, the present invention uses the P507 and OH-The strong alkaline anion exchange resin carries out fractional extraction and separation on the rare earth chloride feed liquid, and compared with the rare earth product separated by the multi-rare earth solution prepared by the conventional separation methods such as fractional crystallization, fractional precipitation, ion exchange chromatography, extraction chromatography and the like in the prior art, the technical scheme of the invention adopts the multi-rare earth element feed liquid extraction, enrichment and separationThe method has the advantages of full separation of rare earth element products such as lanthanum, cerium, dysprosium and ytterbium, high purity, high yield, suitability for large-scale production, simple and convenient operation, low production cost, convenience for industrial production and the like.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (1)
1. A rare earth recovery and enrichment process is characterized in that: taking P507 as an extracting agent, a rare earth chloride feed liquid containing lanthanum, cerium, dysprosium and ytterbium and having a pH value of 3 as a solution to be extracted, wherein the rare earth concentration of the solution to be extracted is 0.3mol/L, and the process specifically comprises the following steps:
1) adding the solution to be extracted, P507 and OH into an extraction reactor in sequence-The preparation method comprises the following steps of (1) stirring and reacting type strongly basic anion exchange resin for 15min under a heating condition, standing for 1h, and separating an organic phase, an aqueous phase and an anion exchange resin phase, wherein the aqueous phase is a feed liquid containing lanthanum and cerium, and the organic phase is an organic phase loaded with dysprosium and ytterbium;
2) adding hydrochloric acid with the concentration of 3mol/L into the dysprosium ytterbium-loaded organic phase for back extraction to obtain an acid-containing dysprosium ytterbium chloride solution after the back extraction;
3) adding conventional saponification P204 into the feed liquid containing lanthanum and cerium for re-extraction to obtain a separated product lanthanum and a cerium-loaded organic phase, performing back extraction on the cerium-loaded organic phase by adopting hydrochloric acid with the concentration of 1.7mol/L, and separating the back-extracted water phase to obtain a product cerium;
4) carrying out countercurrent extraction on the dysprosium ytterbium chloride solution containing acid to remove residual hydrochloric acid in the solution, wherein an acid extraction organic phase is N235, the concentration of the N235 is 0.6mol/L, and the ratio of the number of moles of the N235 to the number of moles of the residual hydrochloric acid is controlled to be 2: 1 to obtain the dysprosium ytterbium chloride solution after acid removal;
5) adding conventional saponification P204 into the deacidified dysprosium ytterbium chloride solution for re-extraction to obtain a separated product dysprosium and ytterbium-loaded organic phase, performing back extraction on the ytterbium-loaded organic phase by adopting hydrochloric acid with the concentration of 3mol/L, controlling the ratio of the mole number of the hydrochloric acid to the mole number of rare earth in the organic phase to be 3: 1, and separating the back-extracted water phase to obtain a product ytterbium;
in the step 1), the molar ratio of the rare earth element to P507 in the solution to be extracted is 0.3: 1, and the OH is-The molar ratio of the type strong-base anion exchange resin to chloride ions in the solution to be extracted is 15: 1;
in the step 2), the ratio of the mole number of the added hydrochloric acid to the mole number of dysprosium and ytterbium in the organic phase is 4: 1;
the purity of the product lanthanum, the purity of the product cerium, the purity of the product dysprosium and the purity of the product ytterbium are 99.990%, and the yield is 96.13%;
the OH group-The type strongly basic anion exchange resin is styrene anion exchange resin, and the effective exchange capacity is 5 mol/kg;
and the P507 is a sulfonated kerosene solution of the P507.
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Effective date of registration: 20210601 Address after: 731601 Industrial Park, Yanguoxia Town, Yongjing County, Linxia Hui Autonomous Prefecture, Gansu Province Applicant after: Gansu Guangsheng rare earth new material Co.,Ltd. Address before: Room 203, building 23, Xin'an Lake Garden, Xin'an street, Bao'an District, Shenzhen City, Guangdong Province Applicant before: SHENZHEN WANJIA INTERDYNAMIC TECHNOLOGY Co.,Ltd. |
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