DE19858560C2 - Crystallization stripping of a rare earth-loaded liquid ion exchanger with sodium hydroxide solution of high concentration - Google Patents
Crystallization stripping of a rare earth-loaded liquid ion exchanger with sodium hydroxide solution of high concentrationInfo
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- DE19858560C2 DE19858560C2 DE19858560A DE19858560A DE19858560C2 DE 19858560 C2 DE19858560 C2 DE 19858560C2 DE 19858560 A DE19858560 A DE 19858560A DE 19858560 A DE19858560 A DE 19858560A DE 19858560 C2 DE19858560 C2 DE 19858560C2
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- scandium
- sodium hydroxide
- ion exchanger
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- hydroxide 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
- 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
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
- C01F17/13—Preparation or treatment, e.g. separation or purification by using ion exchange resins, e.g. chelate resins
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
- C01F17/17—Preparation or treatment, e.g. separation or purification involving a liquid-liquid extraction
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/212—Scandium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/218—Yttrium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
-
- 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
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
-
- 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
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Analytical Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
Die Erfindung bezieht sich auf ein Verfahren zum Kristallisationsstrippen von Scandium, Yttrium oder Neodym beladenen flüssigen Ionenaustauscher mit Natronlauge hoher Konzentration.The invention relates to a method for crystallization stripping of Scandium, yttrium or neodymium loaded liquid ion exchanger Sodium hydroxide solution of high concentration.
Bei der Erzeugung und dem Recycling von scandiumhaltigen Magnesium- und
Aluminiumwerkstoffen fallen Reststoffe mit hohen Scandiumgehalten an, deren
Metallgehalt niedrig ist. Durch Laugung mit Salzsäure wird Scandium in die
wässrige Lösung überführt und anschließend mit dem Extraktionsmittel Di(2-
ethylhexyl)phosphorsäure (DEHPA) und bestimmten Anteilen von Modifiern
gelöst in Kerosin extrahiert. Die bei der Laugung von scandiumhaltigen
Rohstoffen mit Mineralsäuren anfallenden Lösungen haben z. B.
Zusammensetzungen von 0,1-6 g/l Sc, 10-40 g/l Mg oder bis 10 g/l Al sowie
0,1-1 g/l Fe. Die Extraktion erfolgt gemäß
During the production and recycling of scandium-containing magnesium and aluminum materials, residues with high scandium contents occur, the metal content of which is low. Scandium is transferred to the aqueous solution by leaching with hydrochloric acid and then extracted with the extractant di (2-ethylhexyl) phosphoric acid (DEHPA) and certain proportions of modifiers dissolved in kerosene. The solutions resulting from the leaching of scandium-containing raw materials with mineral acids have, for. B. Compositions of 0.1-6 g / l Sc, 10-40 g / l Mg or up to 10 g / l Al and 0.1-1 g / l Fe. The extraction takes place according to
Sc3+ + 3[H2(DEHP)2] = Sc(DEHP)3 . [H(DEHP)]3 + 3H+ (1)
Sc 3+ + 3 [H 2 (DEHP) 2 ] = Sc (DEHP) 3 . [H (DEHP)] 3 + 3H + (1)
während Magnesium, Aluminium, Natrium, Calcium, Barium, Kalium, Eisen etc. im Raffinat verbleiben.while magnesium, aluminum, sodium, calcium, barium, potassium, iron etc. remain in the raffinate.
Nach der Extraktion wird das Scandium einstufig mit Natronlauge gestrippt:
After the extraction, the scandium is stripped in one step with sodium hydroxide solution:
Sc(DEHP)3 . [H(DEHP)]3 + 6NaOH = Sc(OH)3↓ + 6Na(DEHP) + 3H2O (2)Sc (DEHP) 3 . [H (DEHP)] 3 + 6NaOH = Sc (OH) 3 ↓ + 6Na (DEHP) + 3H 2 O (2)
Für die Extraktion Seltener Erden wird vorwiegend das kostengünstige DEHPA verwendet, das üblicherweise mit 2-2,5 molarer Natronlauge gestrippt wird (Xu Shaoquan, Li Suquing: Review of the extractive metallurgy of scandium in China (1978-1991), Hydrometallurgy 42 (1996) pp 337-343).The inexpensive DEHPA is mainly used for the extraction of rare earths used, which is usually stripped with 2-2.5 molar sodium hydroxide solution (Xu Shaoquan, Li Suquing: Review of the extractive metallurgy of scandium in China (1978-1991), Hydrometallurgy 42 (1996) pp 337-343).
Bei dieser Arbeitsweise fällt das Scandiumhydroxid so an, daß eine Filtration des Hydroxides zwar möglich ist. Allerdings führt die Verwendung dieser geringen Natronlaugekonzentrationen zu einer erhöhten Löslichkeit des Extraktionsmittels DEHPA, wie Fig. 1 (Ritcey, G. M. and Ashbrook, A. W.: Solvent Extraction Part I, Elsevier 1984, p 237) zeigt. Der Verlust von DEHPA muß demzufolge regelmäßig kompensiert werden. J09-291320 beschreibt ebenfalls einen Prozeß zur Extraktion von Scandium und Yttrium aus wässriger Lösung, die außerdem Fe, Al, Ca, Mn, Cr und Mg enthält. Als Extraktionsmittel wird dort allerdings das teurere PC 88 A (2-ethyl-hexyl phosphonic acid-mono-2- ethyl-hexyl-ester) verwendet, welches mit 1-4 molarer, bevorzugt 2-3 molarer Natronlauge in 1-4 Schritten, bevorzugt in 2-3 Schritten, gestrippt wird. Eine Extraktion von Sc aus einer Lösung mit in g/l 0,015 Sc, 56 FeO, 5,6 TiO2, 8,2 MgO, 2,3 Al2O3, 0,9 MnO, 0,9 V2O5, 73,5 H2SO4 mit einer 20 Vol.% Alkylphosphorsäure in Kerosin beschreiben auch Palant, A. A., Petrova, V. A. u. Reznichenko, V. A.: Recovery of scandium from wastes from manufacture of pigment titaniumdioxide, Kompleksn. Ispol'z. Miner. Syr'ya (1993), 1 pp 56-59. Die Reextraktion erfolgt mit 10-20%iger KOH oder NaOH. Das schließlich nach der Kalzination erzeugte Produkt hat die Zusammensetzung 0,97% Sc2O3, 50,5% TiO2 und 23,5% Na2O. Das Erzeugnis ist kein vorwiegend Seltene Erden enthaltendes Hydroxid sondern ein Natriumtitanat mit wenig Sc2O3.With this procedure, the scandium hydroxide is obtained in such a way that the hydroxide can be filtered. However, the use of these low sodium hydroxide concentrations leads to an increased solubility of the extracting agent DEHPA, as shown in FIG. 1 (Ritcey, GM and Ashbrook, AW: Solvent Extraction Part I, Elsevier 1984, p 237). The loss of DEHPA must therefore be regularly compensated for. J09-291320 also describes a process for the extraction of scandium and yttrium from aqueous solution, which also contains Fe, Al, Ca, Mn, Cr and Mg. However, the more expensive PC 88 A (2-ethyl-hexylphosphonic acid-mono-2-ethyl-hexyl ester) is used as the extracting agent. preferably in 2-3 steps. An extraction of Sc from a solution with in g / l 0.015 Sc, 56 FeO, 5.6 TiO 2 , 8.2 MgO, 2.3 Al 2 O 3 , 0.9 MnO, 0.9 V 2 O 5 , 73.5 H 2 SO 4 with a 20 vol.% Alkylphosphorsäure in kerosene also describe Palant, AA, Petrova, VA and. Reznichenko, VA: Recovery of scandium from wastes from manufacture of pigment titanium dioxide, Kompleksn. Ispol'z. Miner. Syr'ya (1993), 1 pp 56-59. The re-extraction is done with 10-20% KOH or NaOH. The product finally produced after the calcination has the composition 0.97% Sc 2 O 3 , 50.5% TiO 2 and 23.5% Na 2 O. The product is not a predominantly rare earth-containing hydroxide but a sodium titanate with a low Sc 2 O 3 .
Der Erfindung liegt daher die Aufgabe zugrunde, unter Verwendung von
DEHPA, einen gut filtrierbaren Scandiumniederschlag zu erzeugen und die
Löslichkeit von DEHPA in der wässrigen Phase stark zu reduzieren.
Diese Aufgabe wird durch das Verfahren nach Anspruch 1 gelöst. Das
erfindungsgemäße Verfahren des Kristallisationsstrippens des mit Scandium
beladenen Ionenaustauschers mit Natronlauge hoher Konzentration und die
kontrollierte Zugabe der Natronlauge ermöglicht die Fällung des Scandiums und
anderer Seltenen Erden wie Yttrium und Neodym als Hydroxid in einer
filtrierbaren Form. Erfindungsgemäß wird der benötigte
Natronlaugevolumenstrom, der das Absetz- und Filtrierverhalten bestimmt,
gemäß nachstehender Funktion ermittelt:
The invention is therefore based on the object, using DEHPA, to produce a readily filterable scandium precipitate and to greatly reduce the solubility of DEHPA in the aqueous phase. This object is achieved by the method according to claim 1. The process according to the invention of stripping crystallization of the ion exchanger loaded with scandium with sodium hydroxide solution of high concentration and the controlled addition of the sodium hydroxide solution enables the precipitation of the scandium and other rare earths such as yttrium and neodymium as hydroxide in a filterable form. According to the invention, the required volume of sodium hydroxide solution, which determines the settling and filtering behavior, is determined according to the following function:
V-Hydroxid/V-aqu. . 100 = a + b . ln(v/Va . 1000) (3)
V-hydroxide / V-aqu. . 100 = a + b. ln (v / Va. 1000) (3)
wobei
V-Hydroxid = Volumen, welches das Scandiumhydroxid in der wässrigen Phase
einnimmt
V-aqu. = gesamtes wässriges Volumen nach dem Strippen
v = Volumenstrom in ml/s der zugepumpten Natronlauge
Va = Anfangsvolumen der Natronlauge in ml
a, b = durch Regression für verschiedene Seltene Erdenhydroxide zu ermittelnde
Faktoren. Für Scandiumhydroxid a = 35,5 und b = 14,7.in which
V-hydroxide = volume which the scandium hydroxide occupies in the aqueous phase
V-aqu. = total aqueous volume after stripping
v = volume flow in ml / s of the pumped sodium hydroxide solution
Va = initial volume of the sodium hydroxide solution in ml
a, b = factors to be determined by regression for various rare earth hydroxides. For scandium hydroxide a = 35.5 and b = 14.7.
Überraschenderweise wurde gefunden, daß die Erzeugung filtrierbarer Niederschläge nach der erfindungsgemäßen Methode des Kristallisationsstrippens nur mit einer Zusammensetzung des Ionenaustauschers von 10-30 Vol.% bevorzugt 15-25 Vol.% Extraktionsmittel Di(2- ethylhexyl)phosphorsäure (DEHPA), 1-5 Vol.% bevorzugt 2-3 Vol.% Mono(2- ethylhexyl)phosphorsäure (MEHPA) und 1-5 Vol.% bevorzugt 2-3 Vol.% Tributylphosphat (TBP) und Rest Kerosin oder ein anderes aliphatisches Lösungsmittel, möglich ist. Das Verhältnis von organischer zu wässriger Phase (desweiteren als O/A-Verhältnis bezeichnet) muß dabei abhängig vom Scandiumgehalt der organischen Phase so eingestellt werden, daß der Scandiumgehalt der wässrigen Phase nach dem Strippen (Scandium liegt als Hydroxid vor) nicht mehr als 6-7 g/l beträgt, damit genügend Volumen zum Absetzen zur Verfügung steht. Dabei ist zu berücksichtigen, daß das Volumen der wässrigen Phase nach dem Strippen kleiner als das Anfangsvolumen der Natronlauge ist. Es beträgt bei einem O/A-Verhältnis von zwei im Durchschnitt 77% des Anfangsvolumens.Surprisingly, it was found that the production was filterable Precipitation by the method of the invention Crystallization stripping only with a composition of the ion exchanger from 10-30 vol.% preferably 15-25 vol.% extractant Di (2- ethylhexyl) phosphoric acid (DEHPA), 1-5 vol.% preferably 2-3 vol.% mono (2- ethylhexyl) phosphoric acid (MEHPA) and 1-5 vol.% preferably 2-3 vol.% Tributyl phosphate (TBP) and balance kerosene or other aliphatic Solvent, is possible. The ratio of organic to aqueous phase (further referred to as O / A ratio) must depend on Scandium content of the organic phase can be adjusted so that the Scandium content of the aqueous phase after stripping (Scandium lies as Hydroxide before) is not more than 6-7 g / l, so enough volume to Settling is available. It should be noted that the volume the aqueous phase after stripping is smaller than the initial volume of the Caustic soda is. It is on average with an O / A ratio of two 77% of the initial volume.
Der Nachweis zu dem beschriebenen erfindungsgemäßen Verfahren des Kristallisationsstrippens wird in Form von Absetzkurven und den sich bei diesen Versuchen ergebenden Hydroxidvolumina in der verwendeten 4-6, vorzugsweise 4,5-5,5 molaren Natronlauge erbracht. Die quantitative Bestimmung der Hydroxidvolumina erfolgt in Standzylindern gemäß Fig. 2, aus der auch die Anordnung der verschiedenen Phasen hervorgeht.Evidence of the crystallization stripping process according to the invention described is provided in the form of settling curves and the hydroxide volumes resulting from these tests in the 4-6, preferably 4.5-5.5 molar sodium hydroxide solution used. The hydroxide volumes are determined quantitatively in stationary cylinders according to FIG. 2, from which the arrangement of the different phases is also evident.
Erfindungsgemäß wird das Kristallisationsstrippen durch Zupumpen der Natronlauge mittels einer geregelten Pumpe in einen Behälter, in dem sich der mit Scandium beladene genannte Ionenaustauscher befindet, durchgeführt. Die Rührerdrehzahl wird so eingestellt, daß gerade eine Vermischung der vorliegenden Phasen gewährleistet ist. Dann wird ein Scandiumhydroxid, bei einem geeigneten Volumenstrom der Natronlaugekonzentration von 4-6 Mol/l, bevorzugt 4,5-5,5 Mol/l, erzeugt, das ohne Verdünnung dekantierbar und filtrierbar ist - im Gegensatz zu einem Hydroxid, das bei einer unkontrollierten schnellen Zugabe entsteht.According to the crystallization stripping by pumping the Sodium hydroxide solution by means of a regulated pump in a container in which the ion exchanger loaded with scandium is carried out. The Stirrer speed is set so that just a mixing of the existing phases is guaranteed. Then a scandium hydroxide, at a suitable volume flow of the sodium hydroxide concentration of 4-6 mol / l, preferably 4.5-5.5 mol / l, which can be decanted without dilution and is filterable - in contrast to a hydroxide, which is used in an uncontrolled quick encore arises.
Fig. 3 zeigt die Veränderung der prozentualen Hydroxidvolumina mit zunehmender Absetzdauer bei konstanten Verhältnissen aus Volumenstrom (v) zu Anfangsvolumen 5-molarer Natronlauge (Va) anhand ausgewählter Absetzversuche. Fig. 3 shows the change in percentage Hydroxidvolumina with increasing settling time at constant ratios of flow (v) to initial volume of 5 molar sodium hydroxide solution (Va) by means of selected Absetzversuche.
Eine langsame Zugabe der Natronlauge begünstigt das Kristallwachstum im Vergleich zur Keimbildung. Da die Absetzgeschwindigkeit quadratisch von der Korngröße abhängt, beeinflussen bereits geringe Korngrößenveränderungen das Absetzverhalten stark. Die Korngrößen des Scandiumhydroxides im Bereich v/Va von 0 bis 2 . 10-3 1/s und der ebenfalls untersuchten Yttrium- und Neodymhydroxide liegen bei d[10%] ca. 3 µm, d[50%] ca. 7 µm und d[90%] ca. 19 µm. Der Vergleich mit einem gestrippten Hydroxid, bei dem die Natronlauge unkontrolliert zugegeben wurde, lieferte dagegen Korngrößen von d[10%] ca. 1 µm, d[50%] ca. 1,5 µm und d[90%] ca. 2 µm für das Scandium- und Yttriumhydroxid. Die Bestimmung erfolgte mit dem Particle-System-Analyser von MTS (Meßtechnik Schwartz GmbH, Düsseldorf) durch Ausmessen der Partikel mittels Laserlicht.A slow addition of sodium hydroxide promotes crystal growth compared to nucleation. Since the settling speed depends quadratically on the grain size, even small grain size changes strongly influence the settling behavior. The grain sizes of the scandium hydroxide in the range v / Va from 0 to 2. 10 -3 1 / s and the yttrium and neodymium hydroxides also examined are d [10%] approx. 3 µm, d [50%] approx. 7 µm and d [90%] approx. 19 µm. The comparison with a stripped hydroxide, in which the sodium hydroxide solution was added in an uncontrolled manner, gave grain sizes of d [10%] about 1 µm, d [50%] about 1.5 µm and d [90%] about 2 µm for the scandium and yttrium hydroxide. The determination was carried out with the particle system analyzer from MTS (Meßtechnik Schwartz GmbH, Dusseldorf) by measuring the particles using laser light.
Die erreichten prozentualen Endvolumina des Scandiumhydroxides, für ein O/A-Verhältnis von zwei, nach dem Absetzen zeigt Fig. 4. Hieraus ergibt sich die eindeutige Abhängigkeit des Absetzverhaltens vom Volumenstrom der Natronlauge, die der gefundenen Funktion (3) entspricht.The final percentage volumes of the scandium hydroxide achieved, for an O / A ratio of two, are shown in FIG. 4 after settling . This results in the clear dependence of the settling behavior on the volume flow of the sodium hydroxide solution, which corresponds to the function found (3).
Die Erfindung wird durch Ausführungsbeispiele näher erläutert.The invention is explained in more detail by means of exemplary embodiments.
Ein mit 2,5 g/l Scandium beladener Ionenaustauscher (20% DEHPA, 3%
-MEHPA, 3% TBP, Rest Kerosin) wird mit 5molarer Natronlauge in einem
Rührreaktor gestrippt. Tabelle 1 zeigt die Bedingungen und Ergebnisse:
An ion exchanger (20% DEHPA, 3% MEHPA, 3% TBP, rest kerosene) loaded with 2.5 g / l scandium is stripped with 5 molar sodium hydroxide solution in a stirred reactor. Table 1 shows the conditions and results:
Ein mit 2,5 g/l Scandium beladener Ionenaustauscher (20% DEHPA, 3%
MEHPA, 3% TBP, Rest Kerosin) wird mit 5molarer Natronlauge in einem
Rührreaktor gestrippt. Tabelle 2 zeigt die Bedingungen und Ergebnisse:
An ion exchanger loaded with 2.5 g / l scandium (20% DEHPA, 3% MEHPA, 3% TBP, rest kerosene) is stripped with 5 molar sodium hydroxide solution in a stirred reactor. Table 2 shows the conditions and results:
Das Volumen der organischen Phase beträgt 100 l, beladen mit 2,5 g/l Scandium. Der maximale Gehalt der wässrigen Phase nach dem Strippen beträgt 6,5 g Sc als Hydroxid/l.The volume of the organic phase is 100 l, loaded with 2.5 g / l Scandium. The maximum content of the aqueous phase after stripping is 6.5 g Sc as hydroxide / l.
Endvolumen der wässrigen Phase nach dem Strippen 100 . 2,5/6,5 = 38,5 l = 77% des Anfangsvolumens.Final volume of the aqueous phase after stripping 100. 2.5 / 6.5 = 38.5 l = 77% of the initial volume.
Anfangsvolumen 5 m Natronlauge 38,5/77. 100 = 50 l.Initial volume 5 m sodium hydroxide solution 38.5 / 77. 100 = 50 l.
Es wird ein Hydroxidvolumen von 20 Vol.% für ein gutes Dekantieren mit
anschließender Filtration gewünscht.
A hydroxide volume of 20 vol.% Is required for good decanting with subsequent filtration.
V-Hydroxid/V-aqu. . 100 = 20%
V-hydroxide / V-aqu. . 100 = 20%
eingesetzt in die Regressionsfunktion (3) mit a = 35,5 und b = 14,7:
used in the regression function (3) with a = 35.5 and b = 14.7:
V-Hydroxid/V-aqu. . 100 = 35,5 + 14,7 ln(v/Va . 1000)
V-hydroxide / V-aqu. . 100 = 35.5 + 14.7 ln (v / Va. 1000)
ergibt sich
surrendered
v/Va = 0,35 . 10-3 1/s und der Volumenstrom errechnet sich zu
v / Va = 0.35. 10 -3 1 / s and the volume flow is calculated
v = 50 . 103 . 0,35 . 10-3 = 17,5 ml/s = 63 l/hv = 50. 10 3 . 0.35. 10 -3 = 17.5 ml / s = 63 l / h
Die Zugabe an 5molarer Natronlauge muß mit einem Volumenstrom von 63 l/h erfolgen.The addition of 5 molar sodium hydroxide solution must be at a volume flow of 63 l / h respectively.
Claims (4)
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WO2016209178A1 (en) * | 2015-06-22 | 2016-12-29 | Meta Ni̇kel Kobalt Madenci̇li̇k Sanayi̇ Ve Ti̇caret Anoni̇m Şi̇rketi̇ | Recovering scandium and derivatives thereof from a leach solution loaded with metals obtained as a result of leaching lateritic ores comprising nickel, cobalt and scandium, and secondary sources comprising scandium |
CN114890450B (en) * | 2022-05-11 | 2024-03-26 | 湖南东方钪业股份有限公司 | Method for preparing scandium oxide |
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1998
- 1998-12-18 DE DE19858560A patent/DE19858560C2/en not_active Expired - Fee Related
Non-Patent Citations (2)
Title |
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Chem.Abstr. 121 (1994) Ref.-Nr. 39576 * |
Chem.Abstr. 127 (1997) Ref.-Nr. 349163r * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015021926A1 (en) * | 2013-08-15 | 2015-02-19 | 中国恩菲工程技术有限公司 | Method for processing laterite-nickel ore and method for recycling scandium |
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