CN101979680A - Method for removing aluminum from rare-earth feed liquid - Google Patents
Method for removing aluminum from rare-earth feed liquid Download PDFInfo
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Abstract
The invention discloses a method for removing aluminum from rare-earth feed liquid, belongs to rare-earth feed liquid treatment technology and aims to provide the method for removing the aluminum from the rare-earth feed liquid, of which the aluminum-removing effect is good, the aluminum-removing cost is low, the rare-earth recovery rate is high, the operation and control are convenient, the process is simple and the investment in equipment is small. The key point of the technical scheme mainly comprises the following steps of: (1) preparing an organic phase from 15 to 25 volume percent of naphthenic acid and 15 to 25 volume percent of alcohol-kerosene; (2) adding the prepared organic phase and the rare-earth feed liquid into a stirring tank in a volume ratio of 2-5:1, starting the tank, stirring and uniformly mixing; (3) adding alkaline solution into the mixed liquid obtained in the step (2) with stirring, wherein the total number of moles of the added alkali is 50 to 100 percent of that of rare-earth elements in the rare-earth feed liquid; and (4) after adding the alkaline solution, continuously stirring for a certain time, stopping stirring and standing for a certain time, wherein the solution is separated into an aqueous phase and an organic phase and the aqueous phase is the rare-earth feed liquid from which the aluminum is removed. The method is applied to aluminum removal for the rare-earth feed liquid.
Description
Technical field
The present invention relates to a kind of rare earth feed liquid treatment technology, more particularly, it relates to a kind of method of removing aluminium from rare earth feed liquid.
Background technology
In the ion adsorption type rare earth ore, rare earth element is to be adsorbed on the clay mineral surface with ionic state.When the leaching ion type rareearth ore, a large amount of aluminum ions enter in the leach liquor with rare earth in the clay mineral.When the concentrate of ion adsorption type rare earth ore prepares in early days, adopt the rare earth in the oxalic acid precipitation leach liquor, removed a large amount of non-rare earth impurities that comprise aluminium.Yet ion adsorption type rare earth ore leach liquor oxalic acid precipitation technology is progressively substituted by ammonium bicarbonate precipitation in recent years, though the cost of concentrate preparation is greatly descended, non-rare earth impurities such as the aluminium in the concentrate but do not obtain good pre-separation; Aluminium content is up to 4% (massfraction) in southern ion type rareearth concentrate, the high hydrolysis easily of aluminium composition causes extraction agent emulsification in the rare earth ore concentrate, increased difficulty not only for the later separation flow process, and charge capacity is descended, cause processing power to descend, the separation that also influences rare earth is purified, it extensively distributes in P507-kerosene-hydrochloric acid system segregation section, quite disperse, all have in elements such as Pr, Nd, Sm, Eu outlets and to accumulate enrichment in various degree, especially with Nd, Sm for very, aluminium content accounts for 3% of rare earth weight ratio up to 8g/l in the rare earth feed liquid.Because aluminium is close with rare-earth hydroxide precipitation pH, and forms colloid, aluminium has both sexes, so aluminium is difficult to separate with rare earth in the rare earth feed liquid.Produce aluminum removing method upward commonly used at present and mainly contain alkaline process, acid system, hydrolysis method, extraction process etc.(1) alkaline process wherein: because aluminium generates soluble meta-aluminate under the highly basic condition, rare earth then generates oxyhydroxide, make aluminium and rare earth reach isolating purpose by leave standstill, filtration etc., but rare earth hydrate be key in the operation of this method separating of mother liquor.This law is suitable for separating aluminium and rare earth in the rare-earth alkali conversion process, and the baotite alkaline process prepares and promptly comprised this step in the rare earth chloride step, and the effect of removing aluminium is general.(2) acid system: claim oxalate precipitation method again, add in the earth solution with oxalic acid, because oxalic acid aluminium solubleness in acidic solution is bigger, aluminium is stayed in the solution, it is fine that this method is removed the aluminium effect, is suitable for separating the small amount of aluminum in a large amount of rare earths, and this method generally is used for the final step feed liquid and handles, owing to need complicated transforming process, process links is many, removal of impurities cost height, oxalate solution loss are big, oxalic acid wastewater treatment difficulty and shortage practical significance for middle feed liquid.(3) hydrolysis method: the pH value with alkali lye or bicarbonate of ammonia adjustment rare earth feed liquid makes Al
3+Hydrolysis and removing.Because Al
3+With RE
3+The pH value of beginning hydrolysis is just quite approaching, thereby causes aluminium and rare earth hydrolytic precipitation simultaneously, and the gelatinous precipitate subsequent disposal that generates is very difficult.It is low that this method is removed aluminium efficient, and the rare earth loss is big, therefore can't effectively remove aluminium with hydrolysis method.(4) extraction process: traditional extraction process is to be that 25% naphthenic acid-20% isooctyl alcohol-kerosene is formed organic phase with volume ratio, add ammoniacal liquor or sodium hydroxide saponification earlier, saponification value is 0.35M, utilize the rare earth feed liquid of single-stage steel basin or multi-stage solvent extraction groove and pH value 3.0 to mix then, it is about 30% that aluminium extracts, but the rare earth extraction loss is greater than 10%, and it is general that this method is removed the aluminium effect, and the necessary strict control of the pH value of rare earth feed liquid, otherwise easily cause system emulsification that extraction process can't be carried out.
Summary of the invention
The present invention solves the deficiency that present rare earth feed liquid aluminum removing method exists, and provides a kind of effective except that aluminium, and it is low to remove the aluminium cost, the rare earth yield height, and convenient operation and control, operation is simple, the rare earth feed liquid aluminum removing method that facility investment is few.
Technical scheme of the present invention is such: a kind of method of removing aluminium from rare earth feed liquid comprises the steps:
(1) is 15～25% naphthenic acid-15～25% alcohol-kerosene preparation organic phase by volume;
(2) above-mentioned organic phase for preparing and rare earth feed liquid are added in steel basin by volume at 2～5: 1, open and stir, mix;
(3) under agitation condition, in the mixed solution of step (2) gained, add basic solution, the alkali total moles of adding is 50%～100% of a rare earth feed liquid middle-weight rare earths element total moles;
(4) add alkali and finish back continuation stirring for some time, stop then stirring, leave standstill for some time, solution separating is water and organic phase, and water is except that the rare earth feed liquid behind the aluminium.
Further, above-mentioned a kind ofly from rare earth feed liquid, remove in the method for aluminium, the alcohol described in the step (1) is selected from one of them of octanol or isooctyl alcohol or C8～C10 alcohol mixture; Rare earth feed liquid described in the step (2) is rare earth chloride liquid or sulfuric acid rare earth feed liquid; Basic solution described in the step (3) is one of them of ammoniacal liquor or aqueous sodium hydroxide solution or aqueous sodium carbonate or ammonium bicarbonate aqueous solution, and described basic solution volumetric molar concentration is 3～6mol/L; Churning time described in the step (4) is 10～30 minutes, and time of repose is 10～30 minutes.
Further, organic phase described in the step (4) is under agitation condition, regenerate with the acidic solution back extraction, the total moles of acid is 100～150% of a rare earth feed liquid middle-weight rare earths element total moles in the acidic solution that adds, the regeneration organic phase that obtains recycles, and strip liquor reclaims wherein rare earth element with oxalate precipitation method; Described acidic solution is one of them of hydrochloric acid soln or sulphuric acid soln; Described acidic solution concentration is 3～5mol/L.
The present invention compared with prior art has except that aluminium effectively, and it is low to remove the aluminium cost, the rare earth yield height, and easy to operate, operation is simple, and facility investment is few, practical advantage.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but do not constitute any limitation of the invention.
Embodiment 1
Mishmetal extraction grouping separates post chlorization neodymium feed liquid 2500L, rare earth concentration 1.26mol/L, Al
2O
3Be 8232.2mg/L, to contain Neodymium trioxide be 525.63Kg to the Neodymium trichloride feed liquid as calculated.At first prepare organic phase, organic phase consists of 25% naphthenic acid-25% alcohol mixture-kerosene by volume, and the 5000L organic phase is joined 10M
3In the steel basin; The Neodymium trichloride feed liquid that adds 2500L is opened and is stirred to steel basin, mixes; Under agitation condition, adding 358L concentration is the ammoniacal liquor of 6mol/L; Ammoniacal liquor add finish after, continue to stir and stop after 30 minutes stirring, leave standstill phase-splitting in 30 minutes after, emit water, water is except that the Neodymium trichloride feed liquid behind the aluminium; Under agitation condition, organic phase concentration is that 5mol/L, volume are the hydrochloric acid soln back extraction regeneration of 716L, and organic phase recycles, and strip liquor reclaims neodymium with the oxalic acid precipitation method.
Except that obtaining the Neodymium trichloride material liquid volume behind the aluminium is 2813L, detects by analysis: rare earth concentration 1.05 mol/L, Al
2O
3Be 1.2mg/L, to contain Neodymium trioxide be 496.8Kg to the Neodymium trichloride feed liquid as calculated, and promptly rare earth yield is 94.51%, and aluminium clearance 99.98% removes the aluminium cost and is no more than 700 yuan/ton (in Neodymium trioxide).
Embodiment 2
Mishmetal extraction grouping separates post chlorization praseodymium feed liquid 1250L, rare earth concentration 1.22 mol/L, Al
2O
3Be 2453mg/L, to contain Praseodymium trioxide be 259.56Kg to the praseodymium chloride feed liquid as calculated.At first prepare organic phase, organic phase consists of 15% naphthenic acid-15% alcohol mixture-kerosene by volume, and the 5000L organic phase is joined 10M
3In the steel basin; The praseodymium chloride feed liquid that adds 1250L is opened and is stirred to steel basin, mixes; Under agitation condition, adding 280L concentration is the sodium hydroxide solution of 3mol/L; Sodium hydroxide solution add finish after, continue to stir and stop after 30 minutes stirring, leave standstill phase-splitting in 20 minutes after, emit water, water is except that the praseodymium chloride feed liquid behind the aluminium; Under agitation condition, organic phase concentration is that 3mol/L, volume are the hydrochloric acid soln back extraction regeneration of 400L, and organic phase recycles, and strip liquor reclaims praseodymium with the oxalic acid precipitation method.
Except that obtaining the praseodymium chloride material liquid volume behind the aluminium is 1503L, detects by analysis: rare earth concentration 0.95mol/L, Al
2O
3＜0.1mg/L, to contain Praseodymium trioxide be 243.02Kg to the praseodymium chloride feed liquid as calculated, and promptly rare earth yield is 93.63%, and aluminium clearance＞99.996% removes the aluminium cost and is no more than 700 yuan/ton (in Praseodymium trioxides).
Embodiment 3
Mishmetal extraction grouping separates post chlorization samarium feed liquid 2000L, rare earth concentration 1.18mol/L, Al
2O
3Be 6723mg/L, to contain Samarium trioxide be 411.58Kg to the samarium trichloride feed liquid as calculated.At first prepare organic phase, organic phase consists of 20% naphthenic acid-20% isooctyl alcohol-kerosene by volume, and the 5000L organic phase is joined 10M
3In the steel basin; The samarium trichloride feed liquid that adds 2000L is opened and is stirred to steel basin, mixes; Under agitation condition, adding 460L concentration is the ammonium bicarbonate aqueous solution of 3mol/L; Ammonium bicarbonate aqueous solution add finish after, continue to stir and stop after 20 minutes stirring, leave standstill phase-splitting in 20 minutes after, emit water, water is except that the samarium trichloride feed liquid behind the aluminium; Under agitation condition, organic phase concentration is that 4mol/L, volume are the hydrochloric acid soln back extraction regeneration of 700L, and organic phase recycles, and strip liquor reclaims samarium with the oxalic acid precipitation method.
Except that obtaining the samarium trichloride material liquid volume behind the aluminium is 2436L, detects by analysis: rare earth concentration 0.92 mol/L, Al
2O
3Be 1.1mg/L, to contain Samarium trioxide be 390.85Kg to the samarium trichloride feed liquid as calculated, and promptly rare earth yield is 94.96%, and aluminium clearance 99.98% removes the aluminium cost and is no more than 900 yuan/ton (in Samarium trioxides).
Embodiment 4
Mixed chlorinated rare earth feed liquid 2000L, rare earth concentration 1.52 mol/L, Al
2O
3Be 3533mg/L, through its partition of spectroscopic analysis and calculating, the mixed chlorinated rare earth feed liquid contains and mixes rare earth oxide is 480.32Kg.At first prepare organic phase, organic phase consists of 25% naphthenic acid-25% isooctyl alcohol-kerosene by volume, and the 5000L organic phase is joined 10M
3In the steel basin; The mixed chlorinated rare earth feed liquid that adds 2000L is opened and is stirred to steel basin, mixes; Under agitation condition, adding 380L concentration is the ammoniacal liquor of 6mol/L; Ammoniacal liquor add finish after, continue to stir and stop after 25 minutes stirring, leave standstill phase-splitting in 25 minutes after, emit water, water is except that the mixed chlorinated rare earth feed liquid behind the aluminium; Under agitation condition, organic phase concentration is that 5mol/L, volume are the hydrochloric acid soln back extraction regeneration of 900L, and organic phase recycles, and strip liquor reclaims its middle-weight rare earths with the oxalic acid precipitation method.
Except that obtaining the mixed chlorinated rare earth material liquid volume behind the aluminium is 2351L, detects by analysis: rare earth concentration 1.19 mol/L, Al
2O
3＜0.1mg/L, to contain and mix rare earth oxide be 442.04Kg to the mixed chlorinated rare earth feed liquid as calculated, and promptly rare earth yield is 92.03%, and aluminium clearance＞99.997% removes the aluminium cost and is no more than 900 yuan/ton (in mixed rare-earth oxides).
Embodiment 5
Mishmetal extraction grouping separates back sulfuric acid pr-nd enriched product feed liquid 1500L, rare earth concentration 0.28 mol/L, Al
2O
3Be 3685mg/L, its partition of spectroscopic analysis is Pr
6O
1125.32%, Nd
2O
374.63%, to contain the oxidation pr-nd enriched product be 70.85Kg to sulfuric acid pr-nd enriched product feed liquid as calculated.At first prepare organic phase, organic phase consists of 18% naphthenic acid-18% isooctyl alcohol-kerosene by volume, and the 5000L organic phase is joined 10M
3In the steel basin; The sulfuric acid pr-nd enriched product feed liquid that adds 1500L is opened and is stirred to steel basin, mixes; Under agitation condition, adding 80L concentration is the sodium hydroxide solution of 5mol/L; Sodium hydroxide solution add finish after, continue to stir and stop after 15 minutes stirring, leave standstill phase-splitting in 15 minutes after, emit water, water is except that the sulfuric acid pr-nd enriched product feed liquid behind the aluminium; Under agitation condition, organic phase concentration is that 4mol/L, volume are the sulphuric acid soln back extraction regeneration of 150L, and organic phase recycles, and strip liquor reclaims pr-nd enriched product with the oxalic acid precipitation method.
Except that obtaining sulfuric acid pr-nd enriched product material liquid volume behind the aluminium is 1562L, detects by analysis: rare earth concentration 0.25mol/L, Al
2O
3＜0.1mg/L, to contain the oxidation pr-nd enriched product be 65.88Kg to sulfuric acid pr-nd enriched product feed liquid as calculated, and promptly rare earth yield is 92.98%, and aluminium clearance＞99.997% removes the aluminium cost and is no more than 700 yuan/ton (in oxidation pr-nd enriched products).
Embodiment 6
Mix sulphur acid rare earth feed liquid 1000L, rare earth concentration 0.32 mol/L, Al
2O
3Be 3826mg/L, through its partition of spectroscopic analysis and calculating, mix sulphur acid rare earth feed liquid contains and mixes rare earth oxide is 101.12Kg.At first prepare organic phase, organic phase consists of 22% naphthenic acid-22% alcohol mixture-kerosene by volume, and the 3000L organic phase is joined 5M
3In the steel basin; The mix sulphur acid rare earth feed liquid that adds 1000L is opened and is stirred to steel basin, mixes; Under agitation condition, adding 80L concentration is the sodium carbonate solution of 3mol/L; Sodium carbonate solution add finish after, continue to stir and stop after 10 minutes stirring, leave standstill phase-splitting in 10 minutes after, emit water, water is except that the mix sulphur acid rare earth feed liquid behind the aluminium; Under agitation condition, organic phase concentration is that 4mol/L, volume are the sulphuric acid soln back extraction regeneration of 120L, and organic phase recycles, and strip liquor reclaims its middle-weight rare earths with the oxalic acid precipitation method.
Except that obtaining mix sulphur acid rare earth material liquid volume behind the aluminium is 1062L, detects by analysis: rare earth concentration 0.28 mol/L, Al
2O
3＜0.1mg/L, to contain and mix rare earth oxide be 93.97Kg to mix sulphur acid rare earth feed liquid as calculated, and promptly rare earth yield is 92.93%, and aluminium clearance＞99.997% removes the aluminium cost and is no more than 1000 yuan/ton (in mixed rare-earth oxides).
Show from analysis result: the present invention has except aluminium effective, and it is low to remove the aluminium cost, the rare earth yield height, and easy to operate, operation is simple, and equipment investment is few, practical characteristics.
Claims (9)
1. a method of removing aluminium from rare earth feed liquid is characterized in that comprising the steps:
(1) is 15～25% naphthenic acid-15～25% alcohol-kerosene preparation organic phase by volume;
(2) above-mentioned organic phase for preparing and rare earth feed liquid are added in steel basin by volume at 2～5: 1, open and stir, mix;
(3) under agitation condition, in the mixed solution of step (2) gained, add basic solution, the alkali total moles of adding is 50～100% of a rare earth feed liquid middle-weight rare earths element total moles;
(4) add alkali and finish back continuation stirring for some time, stop then stirring, leave standstill for some time, solution separating is water and organic phase, and water is except that the rare earth feed liquid behind the aluminium.
2. a kind of method of removing aluminium from rare earth feed liquid according to claim 1 is characterized in that the alcohol described in the step (1) is selected from one of them of octanol or isooctyl alcohol or C8～C10 alcohol mixture.
3. a kind of method of removing aluminium from rare earth feed liquid according to claim 1 is characterized in that the rare earth feed liquid described in the step (2) is rare earth chloride liquid or sulfuric acid rare earth feed liquid.
4. a kind of method of removing aluminium from rare earth feed liquid according to claim 1 is characterized in that the basic solution described in the step (3) is one of them of ammoniacal liquor or aqueous sodium hydroxide solution or aqueous sodium carbonate or ammonium bicarbonate aqueous solution.
5. according to claim 1 or 4 described a kind of methods of from rare earth feed liquid, removing aluminium, it is characterized in that described basic solution volumetric molar concentration is 3～6mol/L.
6. a kind of method of removing aluminium from rare earth feed liquid according to claim 1 is characterized in that the churning time described in the step (4) is 10～30 minutes, and time of repose is 10～30 minutes.
7. a kind of method of from rare earth feed liquid, removing aluminium according to claim 1, it is characterized in that, organic phase described in the step (4) is under agitation condition, regenerate with the acidic solution back extraction, the total moles of acid is 100～150% of a rare earth feed liquid middle-weight rare earths element total moles in the acidic solution that adds, the regeneration organic phase that obtains recycles, and strip liquor reclaims wherein rare earth element with oxalate precipitation method.
8. a kind of method of removing aluminium from rare earth feed liquid according to claim 7 is characterized in that described acidic solution is one of them of hydrochloric acid soln or sulphuric acid soln.
9. according to claim 7 or 8 described a kind of methods of from rare earth feed liquid, removing aluminium, it is characterized in that described acidic solution concentration is 3～5mol/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN103343245A (en) * | 2013-07-15 | 2013-10-09 | 福州大学 | Method for removing impurity aluminum in rare earth solution by neutralization-magnetic flocculation-magnetic separation |
| CN103602812A (en) * | 2013-11-18 | 2014-02-26 | 江西理工大学 | Rare-earth organic extractant and back-extraction process thereof |
| CN103773955A (en) * | 2013-11-04 | 2014-05-07 | 中铝广西有色金源稀土股份有限公司 | Method for removing aluminium in tombarthite feed liquid |
| 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 |
| CN105624440A (en) * | 2016-01-25 | 2016-06-01 | 江西理工大学 | Method for complex-precipitation aluminum removal in rare earth solution |
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| CN108950251A (en) * | 2018-08-01 | 2018-12-07 | 连云港高品再生资源有限公司 | The recovery method of rare earth element |
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| CN103343245A (en) * | 2013-07-15 | 2013-10-09 | 福州大学 | Method for removing impurity aluminum in rare earth solution by neutralization-magnetic flocculation-magnetic separation |
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| CN103602812A (en) * | 2013-11-18 | 2014-02-26 | 江西理工大学 | Rare-earth organic extractant and back-extraction process thereof |
| 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 |
| CN105624440A (en) * | 2016-01-25 | 2016-06-01 | 江西理工大学 | Method for complex-precipitation aluminum removal in rare earth solution |
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| CN107502762A (en) * | 2017-08-29 | 2017-12-22 | 江西理工大学 | The method that ion type rareearth leaches mother liquor one-step method removing impurity by means of precipitation Extraction of rare earth |
| CN107502762B (en) * | 2017-08-29 | 2022-01-07 | 江西理工大学 | Method for extracting rare earth by one-step precipitation and impurity removal of ionic rare earth leaching mother liquor |
| CN108085493A (en) * | 2017-11-29 | 2018-05-29 | 中铝广西国盛稀土开发有限公司 | A kind of method that impurity in rare earth chloride liquid is removed using batch process |
| CN108085493B (en) * | 2017-11-29 | 2019-10-25 | 中铝广西国盛稀土开发有限公司 | A method of impurity in rare earth chloride liquid is removed using batch process |
| CN108642310A (en) * | 2018-05-08 | 2018-10-12 | 江西理工大学 | A method of complex-precipitation removes aluminium from rare earth feed liquid |
| CN108950251B (en) * | 2018-08-01 | 2021-08-24 | 连云港高品再生资源有限公司 | Method for recovering rare earth elements |
| CN108950251A (en) * | 2018-08-01 | 2018-12-07 | 连云港高品再生资源有限公司 | The recovery method of rare earth element |
| CN111944998A (en) * | 2020-08-25 | 2020-11-17 | 赣州有色冶金研究所 | Method for removing aluminum from rare earth feed liquid |
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