FR2826667A1 - Treatment of rare earth mineral with high iron content for recuperation of rare earth metals as an aqueous solution involves reacting the mineral with sulfuric acid, firing, mixing the calcined material with aqueous solution, and separating - Google Patents
Treatment of rare earth mineral with high iron content for recuperation of rare earth metals as an aqueous solution involves reacting the mineral with sulfuric acid, firing, mixing the calcined material with aqueous solution, and separating Download PDFInfo
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- FR2826667A1 FR2826667A1 FR0108653A FR0108653A FR2826667A1 FR 2826667 A1 FR2826667 A1 FR 2826667A1 FR 0108653 A FR0108653 A FR 0108653A FR 0108653 A FR0108653 A FR 0108653A FR 2826667 A1 FR2826667 A1 FR 2826667A1
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- ore
- rare earth
- aqueous solution
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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
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/06—Sulfating roasting
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
Description
<Desc/Clms Page number 1> <Desc / Clms Page number 1>
PROCEDE DE TRAITEMENT D'UN MINERAI DE TERRES RARES A
TENEUR ELEVEE EN FER
La présente invention concerne un procédé de traitement d'un minerai de terres rares à teneur élevée en fer, par exemple de type monazite
On connaît des procédés pour la récupération des terres rares à partir de concentrés de minerais de terres rares par attaque acide ou alcaline. Toutefois, dans le cas de certains minerais, ces procédés connus ne donnent pas entièrement satisfaction. Ils ne permettent pas en effet une séparation efficace des terres rares des autres éléments et impuretés, notamment du fer, et leur mise en oeuvre n'est pas simple. PROCESS FOR TREATING A RARE EARTH ORE IN
HIGH IRON CONTENT
The present invention relates to a method for processing a rare earth ore with a high iron content, for example of the monazite type.
Processes are known for the recovery of rare earths from concentrates of rare earth ores by acid or alkaline attack. However, in the case of certain ores, these known methods are not entirely satisfactory. They do not in fact allow an effective separation of the rare earths from the other elements and impurities, in particular iron, and their implementation is not simple.
L'objet de l'invention est la mise au point d'un procédé qui permet d'obtenir à partir d'un minerai riche en fer des terres rares de bonne pureté, en particulier vis à vis du fer. The object of the invention is the development of a process which makes it possible to obtain, from an iron-rich ore, rare earths of good purity, in particular with respect to iron.
Dans ce but, le procédé de l'invention, pour le traitement d'un minerai de terres rares à teneur élevée en fer, est caractérisé en ce qu'il comprend les étapes suivantes : - on fait réagir le minerai avec de l'acide sulfurique ; - on effectue une cuisson du mélange obtenu à une température d'au moins 780 C ; - on mélange avec une solution aqueuse le produit issu de la cuisson de l'étape précédente ; - on sépare la phase liquide de la phase solide de ce mélange, ce par quoi on obtient une première phase aqueuse contenant des terres rares. For this purpose, the process of the invention, for the treatment of a rare earth ore with a high iron content, is characterized in that it comprises the following stages: - the ore is reacted with acid sulfuric; - Cooking the mixture obtained at a temperature of at least 780 C; - The product from the cooking of the previous step is mixed with an aqueous solution; - The liquid phase is separated from the solid phase of this mixture, whereby a first aqueous phase containing rare earths is obtained.
D'autres caractéristiques, détails et avantages de l'invention apparaîtront encore plus complètement à la lecture de la description qui va suivre, ainsi que d'un exemples concret mais non limitatif destiné à l'illustrer. Other characteristics, details and advantages of the invention will appear even more completely on reading the description which follows, as well as a concrete but nonlimiting example intended to illustrate it.
Il est précisé ici que par terres rares on entend les éléments du groupe constitué par le scandium, l'yttrium et les éléments de la classification périodique de numéro atomique compris inclusivement entre 57 et 71. It is specified here that by rare earth is understood the elements of the group constituted by scandium, yttrium and the elements of the periodic classification with atomic number included inclusively between 57 and 71.
Le procédé de l'invention s'applique au traitement de tout minerai de terres rare à teneur élevée en fer. The method of the invention is applicable to the treatment of any rare earth ore with a high iron content.
Par teneur élevée en fer, on entend une teneur en fer d'au moins 10%, plus particulièrement d'au moins 20%, cette teneur pouvant être d'au moins 40%, voire d'au moins 50% dans le cas de minerais bruts. Cette teneur est exprimée ici en masse de Fe203 par rapport au minerai. By high iron content is meant an iron content of at least 10%, more particularly of at least 20%, this content being able to be at least 40%, or even at least 50% in the case of raw ores. This content is expressed here by mass of Fe 2 O 3 relative to the ore.
Plus particulièrement, le procédé de'l'invention s'applique au traitement de minerais altérés, c'est à dire de minerais dans lesquels les minéraux sont More particularly, the method of the invention applies to the treatment of altered ores, that is to say ores in which the minerals are
<Desc/Clms Page number 2><Desc / Clms Page number 2>
disséminés, fins et imbriqués et pour lesquels les séparations physiques sont habituellement peu efficaces. scattered, thin and nested and for which physical separations are usually ineffective.
Comme minerais à teneur élevée en fer et susceptibles d'être traités par le procédé de l'invention, on peut citer certaines monazites et les monazites altérées ou secondaires, minerais dans lesquels les terres rares sont présentes principalement sous forme de phosphates plus ou moins complexes. On peut mentionner ainsi la rabophanite ou la florencite. As ores with a high iron content and capable of being treated by the process of the invention, mention may be made of certain monazites and altered or secondary monazites, ores in which the rare earths are present mainly in the form of more or less complex phosphates . We can thus mention rabophanite or florencite.
On peut aussi citer des minerais mixtes monazite-basnésite-fer. Mention may also be made of mixed monazite-basnesite-iron ores.
L'invention s'applique aussi au traitement d'un minerai concentré, c'est à dire d'un minerai dont la teneur en terres rares a été augmentée et celle en fer diminuée en mettent en oeuvre des méthodes d'enrichissement connues du type flottation ou gravimétrie par exemple. The invention also applies to the treatment of a concentrated ore, that is to say an ore whose content of rare earths has been increased and that of iron decreased by using known enrichment methods of the type flotation or gravimetry for example.
La première étape du procédé de l'invention consiste à faire réagir le minerai, brut ou concentré, avec de l'acide sulfurique. Préalablement à l'attaque sulfurique, le minerai est broyé, de préférence à une granulométrie (diamètre moyen des particules) d'environ 100um, plus particulièrement d'au plus 50um. The first step of the process of the invention consists in reacting the ore, raw or concentrated, with sulfuric acid. Prior to the sulfuric attack, the ore is ground, preferably at a particle size (mean particle diameter) of approximately 100 μm, more particularly at most 50 μm.
On utilise de préférence un acide sulfurique concentré, par exemple à 95%. On travaille avec une quantité d'acide qui est comprise entre une quantité minimale pour attaquer le minerai et une quantité maximale pour que le mélange obtenu se présente sous la forme d'une pâte. De préférence, on travaille avec une quantité d'acide telle que le rapport poids d'acide/poids de minerai est compris entre 1 et 2, plus particulièrement entre 1 et 1,5. A concentrated sulfuric acid, for example 95%, is preferably used. We work with an amount of acid which is between a minimum amount to attack the ore and a maximum amount so that the mixture obtained is in the form of a paste. Preferably, one works with an amount of acid such that the weight ratio of acid / weight of ore is between 1 and 2, more particularly between 1 and 1.5.
Il est avantageux, lors de la réaction avec l'acide sulfurique, de chauffer le mélange minerai/acide, par exemple à une température d'au moins 150 C. It is advantageous, during the reaction with sulfuric acid, to heat the ore / acid mixture, for example to a temperature of at least 150 C.
Le mélange se fait en utilisant tout appareil convenable. Mixing is done using any suitable device.
La deuxième étape du procédé de l'invention consiste à effectuer une cuisson du mélange obtenu à l'étape précédente. Cette cuisson se fait à une température d'au moins 780 C. Cette température peut être comprise par exemple entre 7800C et 820 C. Dans cette gamme de températures on obtient la séparation la plus efficace des terres rares vis à vis du fer. The second step of the process of the invention consists in cooking the mixture obtained in the previous step. This cooking is done at a temperature of at least 780 C. This temperature can be for example between 7800C and 820 C. In this range of temperatures, the most effective separation of the rare earths from iron is obtained.
La durée de la cuisson peut varier par exemple entre 1 et 3 heures, une fois atteinte la température de cuisson. The cooking time can vary for example between 1 and 3 hours, once the cooking temperature is reached.
A l'issue de la cuisson et dans une troisième étape du procédé, on mélange le produit ainsi obtenu avec une solution aqueuse ou de l'eau. On obtient de ce fait un milieu comprenant une phase liquide qui contient les terres rares solubilisées et une phase solide constituée par les impuretés insolubles, notamment le fer. La séparation des phases se fait par tout moyen After cooking and in a third step of the process, the product thus obtained is mixed with an aqueous solution or water. There is thus obtained a medium comprising a liquid phase which contains the solubilized rare earths and a solid phase consisting of insoluble impurities, in particular iron. The separation of the phases is done by any means
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connu et elle permet d'obtenir ainsi à l'issue du procédé de l'invention les terres rares en phase aqueuse. known and thus makes it possible to obtain, at the end of the process of the invention, the rare earths in the aqueous phase.
Il est possible, selon une variante de l'invention, d'ajouter une base à la phase aqueuse précitée contenant des terres rares et qui a été obtenue à l'issue du procédé tel que décrit plus haut. Cette addition de base peut se faire sous la forme d'une solution aqueuse, la base pouvant être plus particulièrement l'ammoniaque. Cette addition se fait généralement avec une quantité de base telle que le milieu obtenu présente un pH compris entre environ 3 et environ 4 et elle provoque une précipitation d'impuretés résiduelles. On sépare la phase liquide de la phase solide du mélange ainsi obtenu ce par quoi on obtient une seconde phase aqueuse contenant des terres rares dont la pureté est augmentée. It is possible, according to a variant of the invention, to add a base to the above-mentioned aqueous phase containing rare earths and which was obtained at the end of the process as described above. This addition of base can be in the form of an aqueous solution, the base being more particularly ammonia. This addition is generally carried out with an amount of base such that the medium obtained has a pH of between approximately 3 and approximately 4 and it causes precipitation of residual impurities. The liquid phase is separated from the solid phase of the mixture thus obtained, whereby a second aqueous phase is obtained containing rare earths whose purity is increased.
Les phases aqueuses contenant les terres rares (première ou seconde phase précitée) qui ont été obtenues de la manière décrite ci-dessus peuvent subir ensuite différents types de traitements pour récupérer les terres rares sous des formes spécifiques. The aqueous phases containing the rare earths (first or second phase mentioned above) which have been obtained in the manner described above can then undergo different types of treatment to recover the rare earths in specific forms.
Ainsi, il est possible d'ajouter aux phases aqueuses précitées un anion, carbonate par exemple pour obtenir un précipité de carbonate de terres rares. Thus, it is possible to add to the above aqueous phases an anion, carbonate for example to obtain a precipitate of rare earth carbonate.
Il est également possible de soumettre ces phase aqueuses à une extraction liquide-liquide pour en extraire les terres rares. It is also possible to subject these aqueous phases to a liquid-liquid extraction in order to extract the rare earths therefrom.
Un exemple va maintenant être donné. An example will now be given.
EXEMPLE
On part d'un minerai de monazite présentant la composition massique suivante :
Oxydes de terres rares (TR203) : 19% Fe203 : 49,2% SiOz 4, 3% Art203 : 4, 1%
P205 : 9,3%
S04 : 0,7%
60g de ce minerai sont mélangés avec 95g d'acide sulfurique à 95%. Le mélange se fait en 15 minutes en chauffant à 1800C de manière à obtenir un solide. EXAMPLE
We start from a monazite ore with the following mass composition:
Rare earth oxides (TR203): 19% Fe203: 49.2% SiOz 4.3% Art203: 4.1%
P205: 9.3%
S04: 0.7%
60g of this ore are mixed with 95g of 95% sulfuric acid. The mixing is done in 15 minutes by heating to 1800C so as to obtain a solid.
On calcine ensuite le mélange en creuset 2 heures à 800 C. Après calcination on récupère 59g de produit calciné et ce produit est mélangé 1 heure avec 0, 41 d'eau. On filtre. On obtient'41 g de résidu sec et 0, 361 de filtrat. The mixture is then calcined in a crucible for 2 hours at 800 C. After calcination, 59g of calcined product are recovered and this product is mixed 1 hour with 0.41 of water. We filter. 41 g of dry residue and 0.361 of filtrate are obtained.
Le résidu présente la composition massique suivante : The residue has the following mass composition:
<Desc/Clms Page number 4> <Desc / Clms Page number 4>
TR203 : 6% (2,46g)
Fe203 : 59% Si02 : 8% Ah03 : 6%
P205 : 12%
S04 : 6%
Ce résidu est lavé. Les eaux de lavage de ce résidu contiennent 0, 428g de TR203. TR203: 6% (2.46g)
Fe203: 59% Si02: 8% Ah03: 6%
P205: 12%
S04: 6%
This residue is washed. The washing water of this residue contains 0.428 g of TR203.
Le filtrat présente la composition suivante :
TR203 : 21, 4g/l (7, 70g) Fe203 : 0, 00g/1 P205 : O, 02gl1
S04 : 27, 5g/1
Le taux de terres rares solubilisées et obtenues à partir du minerai de départ est de 80%.The filtrate has the following composition:
TR203: 21.4g / l (7.70g) Fe203: 0.00g / 1 P205: O, 02gl1
S04: 27.5g / 1
The rate of rare earth solubilized and obtained from the starting ore is 80%.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0108653A FR2826667A1 (en) | 2001-06-29 | 2001-06-29 | Treatment of rare earth mineral with high iron content for recuperation of rare earth metals as an aqueous solution involves reacting the mineral with sulfuric acid, firing, mixing the calcined material with aqueous solution, and separating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0108653A FR2826667A1 (en) | 2001-06-29 | 2001-06-29 | Treatment of rare earth mineral with high iron content for recuperation of rare earth metals as an aqueous solution involves reacting the mineral with sulfuric acid, firing, mixing the calcined material with aqueous solution, and separating |
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| Publication Number | Publication Date |
|---|---|
| FR2826667A1 true FR2826667A1 (en) | 2003-01-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR0108653A Pending FR2826667A1 (en) | 2001-06-29 | 2001-06-29 | Treatment of rare earth mineral with high iron content for recuperation of rare earth metals as an aqueous solution involves reacting the mineral with sulfuric acid, firing, mixing the calcined material with aqueous solution, and separating |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
| WO2009021389A1 (en) * | 2007-08-10 | 2009-02-19 | Grirem Advanced Materials Co., Ltd. | A PROCESS OF SMELTING MONAZITE RARE EARTH ORE RICH IN Fe |
| AU2008286599B2 (en) * | 2007-08-10 | 2010-11-18 | Grirem Advanced Materials Co., Ltd. | A metallurgical process for iron-rich monazite rare earth ore or concentrate |
| WO2013163711A1 (en) | 2012-05-04 | 2013-11-07 | Vale S.A. | System and method for rare earths extraction |
| CN106460087A (en) * | 2014-05-15 | 2017-02-22 | 淡水河谷公司 | System and process for selective rare earth extraction with sulfur recovery |
| WO2017100933A1 (en) * | 2015-12-16 | 2017-06-22 | Quest Rare Minerals Ltd. | Rare earth ore processing methods by acid mixing, sulphating and decomposing |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4464344A (en) * | 1979-05-25 | 1984-08-07 | Saikkonen Pekka J | Process for recovering non-ferrous metal values from ores, concentrates, oxidic roasting products or slags |
| US4670228A (en) * | 1983-09-21 | 1987-06-02 | A/S Megon & Co. | Process for the recovery of valuable metals, particularly rare earths and similar metals, from a carbonate-containing raw material |
| EP0629712A1 (en) * | 1993-05-12 | 1994-12-21 | Rhone-Poulenc Chimie | A process for treating compositions containing noble metals and, optionally, other valuable elements in order to recover said valuables |
| EP0834584A1 (en) * | 1996-09-26 | 1998-04-08 | Fansteel Inc. | Recovery of tantalum and/or niobium from metalfluoride containing materials and ore residues with use of sulfuric acid roasting |
-
2001
- 2001-06-29 FR FR0108653A patent/FR2826667A1/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4464344A (en) * | 1979-05-25 | 1984-08-07 | Saikkonen Pekka J | Process for recovering non-ferrous metal values from ores, concentrates, oxidic roasting products or slags |
| US4670228A (en) * | 1983-09-21 | 1987-06-02 | A/S Megon & Co. | Process for the recovery of valuable metals, particularly rare earths and similar metals, from a carbonate-containing raw material |
| EP0629712A1 (en) * | 1993-05-12 | 1994-12-21 | Rhone-Poulenc Chimie | A process for treating compositions containing noble metals and, optionally, other valuable elements in order to recover said valuables |
| EP0834584A1 (en) * | 1996-09-26 | 1998-04-08 | Fansteel Inc. | Recovery of tantalum and/or niobium from metalfluoride containing materials and ore residues with use of sulfuric acid roasting |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
| WO2009021389A1 (en) * | 2007-08-10 | 2009-02-19 | Grirem Advanced Materials Co., Ltd. | A PROCESS OF SMELTING MONAZITE RARE EARTH ORE RICH IN Fe |
| AU2008286599B2 (en) * | 2007-08-10 | 2010-11-18 | Grirem Advanced Materials Co., Ltd. | A metallurgical process for iron-rich monazite rare earth ore or concentrate |
| WO2013163711A1 (en) | 2012-05-04 | 2013-11-07 | Vale S.A. | System and method for rare earths extraction |
| AU2013255066B2 (en) * | 2012-05-04 | 2015-11-05 | Vale S.A. | System and method for rare earths extraction |
| RU2618975C2 (en) * | 2012-05-04 | 2017-05-11 | Вале С.А. | System and method of extraction of rare earth elements |
| CN106460087A (en) * | 2014-05-15 | 2017-02-22 | 淡水河谷公司 | System and process for selective rare earth extraction with sulfur recovery |
| RU2701777C2 (en) * | 2014-05-15 | 2019-10-01 | Вале С.А. | System and method of selective extraction of rare-earth elements with regeneration of sulfur |
| US10597754B2 (en) | 2014-05-15 | 2020-03-24 | Vale S.A. | System and process for selective rare earth extraction with sulphur recovery |
| WO2017100933A1 (en) * | 2015-12-16 | 2017-06-22 | Quest Rare Minerals Ltd. | Rare earth ore processing methods by acid mixing, sulphating and decomposing |
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