CN1710119A - Process for removing impurity element aluminium from rate-earth solution by fatty acid extraction - Google Patents
Process for removing impurity element aluminium from rate-earth solution by fatty acid extraction Download PDFInfo
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- CN1710119A CN1710119A CNA200510083431XA CN200510083431A CN1710119A CN 1710119 A CN1710119 A CN 1710119A CN A200510083431X A CNA200510083431X A CN A200510083431XA CN 200510083431 A CN200510083431 A CN 200510083431A CN 1710119 A CN1710119 A CN 1710119A
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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
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Abstract
The invention relates to a technique which removes extraneous component aluminum from rare-earth solution using fatty acid extracting method. It relates to wet refining preparation technique in rare-earth refining. The features of the technique are explained as following: long chain fatty acid is adopted as extractor, alcohol or N235 or fossil is adopted as lacquer solvent, and coal oil as diluent, together forming a long chain fatty acid-diluent-coal oil extracting organic phase with volume ratio of fatty acid taking 5 to 50 percent, alcohol or N235 or fossil taking 2 to 25 percent, and coal oil taking the rest. Saponify thus organic phase with saponification agent at a ratio of 0 to 80 percent, extract rare-earth solution with above saponified organic phase to obtain rare-earth solution of low aluminum content. Advantages of the technique are simple process, rational adaptation, low agent consumption. Single extraction reduces the aluminum content in rare-earth solution to 20 to 40 mg/l, multiple extractions restrains the content below 1 mg/L.
Description
Technical field
The present invention relates to a kind of lipid acid extraction process and remove the technology of impurity element aluminium in the earth solution, belong to the preparation technology of hydrometallurgy rare earth metal.
Background technology
Along with rare earth element use increasingly extensive, people not only rest in the requirement to Purity of Rare Earth the requirement of rare-earth products, more be physicals such as size-grade distribution, specific surface etc. to rare-earth products, and the requirement of non-rare earth impurity index, aluminium is exactly by one of increasing desired non-rare earth impurity of client.Aluminium is amphoteric element, and it can be with Al in solution
3+, Al (OH)
2+, Al (OH)
2 +, Al (OH)
3, AlO
2 -Exist etc. various ways, therefore increased itself and the isolating difficulty of rare earth element.The isolating method of rare earth and non-rare earth impurity mainly contains neutralisation, oxalate precipitation method, sulphide precipitation and extraction process etc.Because the pH value and the rare earth of aluminum precipitation are approaching, neutralisation is difficult to separate aluminium and rare earth; When preparation high-purity rare-earth solution, adopt a spot of rare earth of loss, promptly add small amount of H
2O
2The hydrolysate (colloid oxyhydroxide) that the hydrolysis of trivalent cerium partial oxidation is generated tetravalence cerous hydroxide precipitation absorption impurity A l together precipitates, and has obtained satisfied effect.But then can not use this method to mishmetal or other single rare earth products that does not contain cerium.Sulphide precipitation has effect preferably to separation Hg, Cu, Pb, Sn, Cd, Ni, Zn, Fe, most of non-rare earth impurities such as Mn, Mg.The oxalate precipitation method can be removed a large amount of non-rare earth impurities, especially aluminium is had decontamination effect improving preferably, can make that aluminium drops to 10 in the solution
-4, but too high for some mishmetal products production costs at a low price.Method--the complexometry that also has a kind of new separation aluminium adds some organic complexing agent and removes aluminium in product when producing carbonated rare earth, the clearance of aluminium can reach 60%, but acquires a certain degree of difficulty in the production operation.Extraction process is considered to a kind of method of separating non-rare earth impurity preferably, can make Cu, Pb, Zn, Co, Ni etc. drop to 10
-6, but also do not have the ripe technical process of using for the extracting and separating of aluminium.Literature research has been arranged at P
507The distribution situation of aluminium in extracting and separating Sm/Eu/Gd and the Gd/Tb/Dy process is utilized the apparent separation factor β of cell body data computation aluminium and samarium in two extracting and separating sections
Sm/Al=4--6 is at P
507--the difficult extraction of aluminum ratio samarium in the HCl system, aluminium has the part accumulation in cell body in the process of extracting and separating rear earth, and most of aluminium is enriched in the middle of the surplus liquid of extraction, and small part is discharged from the 3rd outlet and organic phase.Therefore use P
507Extraction agent rare-earth separating and aluminium is difficulty.Also had literature research and extracted the iron aluminium of removing in the re chloride with naphthenic acid, with 32% naphthenic acid-20% isooctyl alcohol-48% kerosene system, extract through 4 stage countercurrents with centrifugal extractor, in the re chloride, iron is reduced to 2mg/L by 20mg/L, aluminium is reduced to about 160mg/L by 250mg/L, and visible de-ferrous effect is obvious but unsatisfactory except that the aluminium effect, can only remove 30% aluminium.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of technology that the effective lipid acid extraction process of impurity element aluminium in the earth solution is removed impurity element aluminium in the earth solution of removing is provided.
Processing step of the present invention is as follows:
The employing longer chain fatty acid is an extraction agent, adopting alcohols or N235 or petrolenum sulfoxide is solubility promoter, employing kerosene is thinner, form longer chain fatty acid-solubility promoter-kerosene extraction organic phase, this extracted organic phase composition is counted with volume ratio: 5-50% longer chain fatty acid, 2～25% alcohols or N235 or petrolenum sulfoxide, surplus are kerosene, with saponifying agent extracted organic phase is carried out saponification, the saponification degree of extracted organic phase is 0～80%, the earth solution of impure element aluminum is extracted the earth solution that obtains low aluminium with the extracted organic phase after the above-mentioned saponification.
The earth solution of described impure element aluminum is re chloride, rare earth nitrate solution or rare earth sulfate solution, and the rare earth concentration of solution is 0.01～2mol/L, acidity PH1～4.
Described extraction agent longer chain fatty acid is the dehydrated castor oil fatty acid of C18;
Described extraction agent longer chain fatty acid is the not dehydrated castor oil fatty acid of C18;
Described extraction agent longer chain fatty acid is the soya fatty acid of C18.
Described co-solvent is one or more the mixture in isooctyl alcohol, secondary octanol, primary isoamyl alcohol, the alcohol mixture.
Described saponifying agent is ammoniacal liquor, sodium hydroxide, bicarbonate of ammonia.
The described earth solution of impure element aluminum the extraction with the extracted organic phase after the saponification is single-stage extraction or multi-stage solvent extraction.Extracted organic phase after the single-stage extraction saponification and rare earth raw material liquid are by comparing 1～5: 1～3; Extracted organic phase after the multi-stage solvent extraction saponification and rare earth raw material liquid by stream than being 1: 1～5.
Load organic phases is stripped with the mineral acid strip liquor, can reclaim its middle-weight rare earths.Can be recycled after the organic phase washing.
Advantage of the present invention is: technical process is simple, is connected rationally, and chemical reagent consumption is few.Single-stage extraction can make the content of impurity element aluminium in the earth solution reduce to 20--40mg/L; Multi-stage solvent extraction can make that aluminum concentration drops to less than 1mg/L in the earth solution.
Embodiment
It is that stock liquid extracts that technology of the present invention can be directly obtains re chloride with baotite sulfuric acid high-temperature roasting infusion transition, and raffinate directly can be used for follow-up extracting and separating; Also can carry out extracting and separating to the single re chloride that extracting and separating obtains and remove aluminium, raffinate directly carries out carbon ammonium precipitation, and technical process is simple, is connected rationally, and chemical reagent consumption is few.
Embodiment 1: the chlorination spectrum neodymium solution that Inner Mongol rare earth enterprise extracting and separating obtains, the about 190g/L of rare earth concentration, impurity aluminum content 728mg/L, acidity pH2-3.Extracted organic phase consists of longer chain fatty acid 20%--isooctyl alcohol 10%--kerosene 70%, strong aqua saponification, saponification deg 20%.Organic phase is compared 1: 1 single-stage extraction with water, impurity aluminum is reduced to 14mg/L in the raffinate.The clearance of aluminium is 98%.
Embodiment 2: the chlorination spectrum neodymium solution that Inner Mongol rare earth enterprise extracting and separating obtains, the about 150g/L of rare earth concentration, impurity aluminum content 550mg/L, acidity pH2-3.Extracted organic phase consists of longer chain fatty acid 15%--isooctyl alcohol 10%--kerosene 75%, strong aqua saponification, saponification deg 25%.Organic phase is compared 1: 1 single-stage extraction with water, impurity aluminum is reduced to 35mg/L in the raffinate, and the aluminium clearance is 93.6%.
Embodiment 3: lanthanum chloride solution, the about 80g/L of rare earth concentration, impurity aluminum content 18.6mg/L, acidity pH1-2.Extracted organic phase consists of longer chain fatty acid 20%--isooctyl alcohol 10%--kerosene 70%, strong aqua saponification, saponification deg 20%.The extraction of 4 stage countercurrents, stream is than being organic phase: water=1: 3, impurity aluminum is reduced to less than 0.5mg/L in the raffinate.
Claims (10)
1. a lipid acid extraction process is removed the technology of impurity element aluminium in the earth solution, it is characterized in that: the employing longer chain fatty acid is an extraction agent, adopting alcohols or N235 or petrolenum sulfoxide is solubility promoter, employing kerosene is thinner, form longer chain fatty acid-solubility promoter-kerosene extraction organic phase, this extracted organic phase composition is counted with volume ratio: the 5-50% longer chain fatty acid, 2～25% alcohols or N235 or petrolenum sulfoxide, surplus is a kerosene, with saponifying agent extracted organic phase is carried out saponification, the saponification degree of extracted organic phase is 0～80%, the earth solution of impure element aluminum is extracted the earth solution that obtains low aluminium with the extracted organic phase after the above-mentioned saponification.
2. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, it is characterized in that: the earth solution of impure element aluminum is re chloride, rare earth nitrate solution or rare earth sulfate solution, the rare earth concentration of solution is 0.01～2mol/L, acidity PH1～4.
3. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, and it is characterized in that: the extraction agent longer chain fatty acid is the dehydrated castor oil fatty acid of C18.
4. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, and it is characterized in that: the extraction agent longer chain fatty acid is the not dehydrated castor oil fatty acid of C18.
5. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, and it is characterized in that: the extraction agent longer chain fatty acid is the soya fatty acid of C18.
6. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, it is characterized in that: co-solvent is one or more the mixture in isooctyl alcohol, secondary octanol, primary isoamyl alcohol, the alcohol mixture.
7. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, and it is characterized in that: saponifying agent is ammoniacal liquor, sodium hydroxide, bicarbonate of ammonia.
8. lipid acid extraction process according to claim 1 is removed the technology of impurity element aluminium in the earth solution, it is characterized in that: the described earth solution of impure element aluminum the extraction with the extracted organic phase after the saponification is single-stage extraction or multi-stage solvent extraction.
9. lipid acid extraction process according to claim 8 is removed the technology of impurity element aluminium in the earth solution, and it is characterized in that: extracted organic phase after the single-stage extraction saponification and rare earth raw material liquid are by being in a ratio of: 1～5: 1～3.
10. lipid acid extraction process according to claim 8 is removed the technology of impurity element aluminium in the earth solution, it is characterized in that: the extracted organic phase after the multi-stage solvent extraction saponification with rare earth raw material liquid by stream than being: 1: 1～5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200510083431XA CN1710119A (en) | 2005-07-12 | 2005-07-12 | Process for removing impurity element aluminium from rate-earth solution by fatty acid extraction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200510083431XA CN1710119A (en) | 2005-07-12 | 2005-07-12 | Process for removing impurity element aluminium from rate-earth solution by fatty acid extraction |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100381550C (en) * | 2006-06-26 | 2008-04-16 | 山东恒利石油化工有限公司 | Oil cleaning agent and cleaning method for heat-conducting oil heating system |
| CN101813932B (en) * | 2009-02-03 | 2012-07-04 | 东北大学 | Method for component content prediction and optimization operation in wet-process metallurgic extraction process |
| CN103146921A (en) * | 2013-04-07 | 2013-06-12 | 内蒙古包钢稀土(集团)高科技股份有限公司 | Method for removing aluminum in rare-earth solution |
| CN103966441A (en) * | 2014-05-08 | 2014-08-06 | 广东省工业技术研究院(广州有色金属研究院) | Method for continuously extracting aluminum from rare earth liquid |
| CN107130120A (en) * | 2017-04-28 | 2017-09-05 | 广西师范大学 | A kind of non-rare earth impurity and rare earth element extraction separating method |
| CN110408777A (en) * | 2019-07-25 | 2019-11-05 | 厦门熙途科技有限公司 | A kind of method of fatty acid extracting metals ion |
| CN112921176A (en) * | 2021-01-21 | 2021-06-08 | 中国科学院过程工程研究所 | Phenoxycarboxylic acid rare earth solution aluminum-removing extracting agent |
-
2005
- 2005-07-12 CN CNA200510083431XA patent/CN1710119A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100381550C (en) * | 2006-06-26 | 2008-04-16 | 山东恒利石油化工有限公司 | Oil cleaning agent and cleaning method for heat-conducting oil heating system |
| CN101813932B (en) * | 2009-02-03 | 2012-07-04 | 东北大学 | Method for component content prediction and optimization operation in wet-process metallurgic extraction process |
| CN103146921A (en) * | 2013-04-07 | 2013-06-12 | 内蒙古包钢稀土(集团)高科技股份有限公司 | Method for removing aluminum in rare-earth solution |
| CN103966441A (en) * | 2014-05-08 | 2014-08-06 | 广东省工业技术研究院(广州有色金属研究院) | Method for continuously extracting aluminum from rare earth liquid |
| CN107130120A (en) * | 2017-04-28 | 2017-09-05 | 广西师范大学 | A kind of non-rare earth impurity and rare earth element extraction separating method |
| CN110408777A (en) * | 2019-07-25 | 2019-11-05 | 厦门熙途科技有限公司 | A kind of method of fatty acid extracting metals ion |
| CN112921176A (en) * | 2021-01-21 | 2021-06-08 | 中国科学院过程工程研究所 | Phenoxycarboxylic acid rare earth solution aluminum-removing extracting agent |
| CN112921176B (en) * | 2021-01-21 | 2021-12-21 | 中国科学院过程工程研究所 | Phenoxycarboxylic acid rare earth solution aluminum-removing extracting agent |
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