CN111961849A - Method for extracting and separating scandium - Google Patents

Method for extracting and separating scandium Download PDF

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CN111961849A
CN111961849A CN202010907235.4A CN202010907235A CN111961849A CN 111961849 A CN111961849 A CN 111961849A CN 202010907235 A CN202010907235 A CN 202010907235A CN 111961849 A CN111961849 A CN 111961849A
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scandium
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extracting
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CN111961849B (en
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孙国新
彭修静
赵奕铭
崔玉
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University of Jinan
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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
    • 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
    • C22B3/28—Amines
    • 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

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Abstract

The invention belongs to the technical field of scandium extraction and purification, and particularly relates to a method for separating scandium and other impurities by using an amide podand extracting agent. The method adopts N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide as an extractant to separate scandium from a nitric acid medium, has high selectivity to scandium, has poor extraction capability to impurities such as Fe, Mg, Ti, Ba, Al, Zr, Mn and the like, and realizes the separation of scandium and impurity elements. The technology has the advantages of simple operation, little pollution and low requirement on equipment.

Description

Method for extracting and separating scandium
Technical Field
The invention belongs to the technical field of hydrometallurgy, and particularly relates to a method for separating scandium and other impurities by using an amide pod ether extracting agent.
Background
The excellent performance of scandium makes scandium play an important role in the fields of electric light sources, space navigation, electronic industry, nuclear technology, superconducting technology and the like, but scandium is used as a rare earth element, is distributed dispersedly and has extremely rare independent ore deposit. The coarse scandium oxide contains impurities of Fe, Mg, Ti, Ba, Al, Zr, Mn and the like, Sc2O3The content is 80-90%. The industrial problem is how to enrich scandium with low cost in the scandium extraction process so as to obtain high-purity scandium oxide.
Chinese patent CN108754156A) discloses a method for separating iron and scandium in red mud acid leachate by an extraction method, wherein an extractant containing long-chain alkyl quaternary ammonium salt is used for extracting and separating iron complex ions, so that scandium ions are left in the leachate, and the separation of iron and scandium is realized. The method has the iron removal rate of more than 95 percent, which indicates that a certain amount of iron still remains in the leachate and influences the purity of scandium. Chinese patent (publication No. CN109022810B) discloses a method for separating and recovering valuable metals of iron, manganese and scandium from tungsten slag, wherein P204 is used for extracting a leaching solution of sulfuric acid, the single-stage extraction rates of the iron, the manganese and the scandium in the leaching solution are respectively 86.1%, 82.4% and 97.7%, and different stripping solutions are adopted for stripping metals, so that a high-purity scandium product is difficult to obtain. Chinese patent publication No. CN109022839A discloses a method for scandium enrichment, which adopts different extractants to enrich scandium, and adopts neutral, alkaline and organic chelating extractants to extract and back extract scandium, without mentioning the separation of impurities. Chinese patent (publication No. CN1844421A) discloses a method for extracting scandium from red mud, wherein P204 is adopted to extract and recover scandium in red mud, and a loaded organic phase needs to be purified by 2.5 mol/L concentrated sulfuric acid before back extraction, so that a large amount of concentrated acid with low iron content is generated and is difficult to treat. Chinese patent (publication No. CN101182601A) adopts concentrated hydrochloric acid with different mass fractions to carry out twice impregnation on red mud, P204 is utilized to extract scandium from the second leaching solution, and a small amount of impurity iron is contained in an organic phase, so that the purity of scandium is influenced.
Phosphorus-containing extracting agents (P204 and the like) are commonly used in the extraction separation, alkali is added in the extraction process, salt-containing and ammonia nitrogen-containing wastewater is generated, the treatment is difficult, and solid waste residues are left after combustion.
Disclosure of Invention
Sc in crude scandium oxide2O3The content of scandium is 80-90%, and scandium is purified by a common phosphorus-containing extractant, so that the environment is polluted. The N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide extractant designed and synthesized by the invention has large molecular weight, is hardly dissolved in water, does not need saponification in the extraction process, and is environment-friendly. The extracting agent has strong scandium extracting capability in a solution with nitric acid and nitrate coexisting, has low scandium extracting capability on coexisting impurity ions, and effectively separates scandium and other impurity elements by utilizing a high scandium and other impurity separation coefficient of the extracting agent.
The technical characteristics of the invention are implemented by the following technical scheme, and the method for extracting and separating scandium comprises the following steps:
(1) dissolving a scandium sample by using nitric acid to obtain an aqueous solution of impurities including Fe, Mg, Ti, Ba, Al, Zr and Mn, wherein the concentration of the nitric acid in the aqueous phase is 0.01-5 mol/L, or the concentration of the nitric acid is 0.01-1 mol/L and the concentration of the nitrate is 0.01-4 mol/L, and the total concentration of scandium is 1-200 g/L.
(2) Weighing a certain mass of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide extractant, and diluting the extractant to a certain concentration by using a diluent to obtain an organic phase, wherein the diluent is one of toluene, xylene, dichloromethane, chloroform or carbon tetrachloride; the concentration of the extractant is 0.01-2 mol/L.
(3) Mixing and stirring the water phase and the organic phase in a certain volume ratio (1: 10-10: 1) for 10-120 min, wherein the extraction temperature is 5-60%oC。
(4) And standing the extracted mixed solution for 1-5 min for phase separation to obtain a clear and transparent two phases, namely a scandium-loaded organic phase, and leaving impurities in a raffinate aqueous phase.
(5) Mixing oxalic acid or oxalate aqueous solution with a certain volume concentration of 0.1-1.0 mol/L with the scandium-loaded organic phase, stirring for 5-100 min, and controlling the temperature to be 5-60 DEGoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The organic phase after standing and layering can be reused.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
(1) the extracting agent used in the method has high identification capability on scandium, has a large separation coefficient on scandium and impurity elements, and is beneficial to effective separation of scandium and impurities.
(2) The extracting agent adopted by the invention has good thermal stability, difficult volatilization, small water solubility, good physical and chemical stability, repeated use, low price and easy obtainment of all used reagents, small investment and cost saving.
(3) Compared with phosphoric acid extractant, the extractant adopted by the invention does not need saponification, and belongs to environment-friendly extractant.
(4) The method is simple and convenient to operate, has low requirements on equipment, and is easy to realize continuous industrial production.
Detailed description of the invention
The extraction rate (E) represents the ratio of the metal concentration in the aqueous phase before and after extraction. The concentrations of metals Sc, Fe, Mg, Ti, Ba, Al, Zr and Mn in the patent are measured by ICP-AES.
36g of a scandium oxide product having a purity of 85% was weighed, and a scandium sample was dissolved by heating with nitric acid, and the following working solutions were each obtained by diluting this solution.
Example 1
(1) The concentration of Sc in the water phase is 5 g/L, and the concentration of nitric acid is 0.6 mol/L.
(2) Toluene is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL each, stirring for 30 min, and extracting at 10 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 99.89%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 98 percent, and the scandium purity is more than 99.8 percent.
Example 2
(1) The concentration of Sc in the water phase is 5 g/L, and the concentration of nitric acid is 0.6 mol/L.
(2) Toluene is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL each, stirring for 30 min, and extracting at 40 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 98.85%.
(4) Mixing 20 mL of 0.5 mol/L oxalate aqueous solution with the extracted organic phase, stirring for 30 min at 30 deg.CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600o2 hours of C calcinationThen, scandium oxide is obtained. The scandium recovery rate is more than 97%, and the scandium purity is more than 99.3%.
Example 3
(1) The concentration of Sc in the water phase is 10 g/L, and the concentration of nitric acid is 3.0 mol/L.
(2) Toluene is used as a diluent, and 1 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL respectively, stirring for 30 min, and extracting at 20 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 99.98%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 98 percent, and the scandium purity is more than 99.9 percent.
Example 4
(1) The concentration of Sc in the water phase is 10 g/L, the concentration of nitric acid is 0.2 mol/L, and the concentration of lithium nitrate is 0.4 mol/L.
(2) Toluene is used as a diluent, and 1 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL respectively, stirring for 30 min, and extracting at 20 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 86.96%.
(4) Mixing 20 mL of 1.0 mol/L oxalate aqueous solution with the extracted organic phase, stirring for 30 min at 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 85 percent, and the scandium purity is more than 99.7 percent.
Example 5
(1) The concentration of Sc in the water phase is 10 g/L, the concentration of nitric acid is 0.2 mol/L, and the concentration of lithium nitrate is 3 mol/L.
(2) Toluene is used as a diluent, and 1 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL respectively, stirring for 30 min, and extracting at 20 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 99.68%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 98 percent, and the scandium purity is more than 99.7 percent.
Example 6
(1) The concentration of Sc in the water phase is 5 g/L, the concentration of nitric acid is 0.2 mol/L, and the concentration of lithium nitrate is 3 mol/L.
(2) Toluene is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL respectively, stirring for 60 min, and extracting at 20 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 99.98%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 98 percent, and the scandium purity is more than 99.6 percent.
Example 7
(1) The concentration of Sc in the water phase is 10 g/L, and the concentration of nitric acid is 1 mol/L.
(2) Toluene is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing aqueous phase 20 mL and organic phase 40mL, stirring for 30 min, and extracting at 20 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 98.32%.
(4) Mixing 40mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min, and heatingDegree of 30oC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 97%, and the scandium purity is more than 99.6%.
Example 8
(1) The concentration of Sc in the water phase is 5 g/L, and the concentration of nitric acid is 1 mol/L.
(2) Toluene is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing aqueous phase 40mL and organic phase 20 mL, stirring for 30 min, and extracting at 20 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 72.56%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 70 percent, and the scandium purity is more than 99.7 percent.
Example 9
(1) The concentration of Sc in the water phase is 5 g/L, and the concentration of nitric acid is 2 mol/L.
(2) Toluene is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing 80 mL of water phase and 20 mL of organic phase, stirring for 30 min, and extracting at 30 deg.CoC, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 45.80%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 44%, and the scandium purity is more than 99.8%.
Example 10
(1) The concentration of Sc in the water phase is 5 g/L, and the concentration of nitric acid is 0.6 mol/L.
(2) Carbon tetrachloride is used as a diluent, and 0.5 mol/L of N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide is prepared as an organic phase.
(3) Mixing the water phase and the organic phase 20 mL each, stirring for 30 min, and extracting at 10 deg.CoAnd C, measuring the concentration of Sc in the raffinate, wherein the extraction rate is 98.76%.
(4) Mixing 20 mL of oxalic acid aqueous solution with the concentration of 0.5 mol/L with the extracted organic phase, stirring for 30 min at the temperature of 30 DEG CoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oAnd C, calcining for 2 hours to obtain scandium oxide. The scandium recovery rate is more than 97%, and the scandium purity is more than 99.8%.

Claims (5)

1. A method for extracting and separating scandium is characterized in that an extracting agent used is N, N, N ', N' -tetracyclohexyl-3-oxoglutaramide, the extracting agent is diluted by a diluent and then used as an extraction organic phase, one or two of nitric acid and nitrate are added into an extraction aqueous phase, and high-purity scandium is obtained through extraction and back extraction, wherein the step of extracting and purifying scandium comprises the following steps:
(1) dissolving a scandium sample by using nitric acid to obtain an aqueous solution of impurities including Fe, Mg, Ti, Ba, Al, Zr and Mn, and adding one or two of nitric acid and nitrate as a water phase, wherein the total concentration of scandium is 1-200 g/L, and the concentrations of nitric acid and nitrate are 0.01-5 mol/L;
(2) weighing a certain mass of an extracting agent, and diluting the extracting agent to a certain concentration by using a diluent to obtain an organic phase, wherein the diluent is one of toluene, xylene, dichloromethane, chloroform or carbon tetrachloride; the concentration of the extracting agent is 0.01-2 mol/L;
(3) mixing and stirring the water phase and the organic phase according to a certain volume ratio for 10-120 min, wherein the extraction temperature is 5-60 DEGoC；
(4) Standing the extracted mixed solution for phase splitting to obtain a scandium-loaded organic phase, and leaving impurities in the raffinate;
(5) mixing oxalic acid or oxalate aqueous solution with a certain volume concentration of 0.1-1.0 mol/L with the scandium-loaded organic phase in the step (4), stirring for 5-100 min, and keeping the temperature at 5-60 DEGoC, standing to separate organic phase, filtering water phase to obtain precipitate, 120oC drying for 2 hours, 600oCalcining for 2 hours to obtain scandium oxide, and repeatedly using the organic phase after standing and layering.
2. The method for extracting and separating scandium according to claim 1, wherein in the step (3), the mixing volume ratio of the aqueous phase to the organic phase is 1: 10-10: 1.
3. The method for extracting and separating scandium according to claim 1, wherein in the step (3), the extraction time is 20-60 min, and the extraction temperature is 10-50oC。
4. The method for extracting and separating scandium according to claim 1, wherein in the step (4), the standing time is 1-5 min, and the mixed solution becomes clear and transparent two phases.
5. The method for extracting and separating scandium according to claim 1, wherein in the step (5), the stripping agent is oxalic acid or an oxalate solution, the stripping time is 10-30 min, and an organic phase after stripping can be reused.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114672650A (en) * 2022-05-06 2022-06-28 济南大学 Method for extracting scandium from titanium white waste acid by utilizing diphosphonic acid extracting agent

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180142321A1 (en) * 2015-05-07 2018-05-24 Commissariat A L'energie Atomique Et Aux Energies Alternatives Use of novel compounds for selectively extracting rare earths from aqueous solutions including phosphoric acid and associated extraction method
CN108300878A (en) * 2018-01-26 2018-07-20 中国科学院长春应用化学研究所 A kind of extraction process with acid phosphine enriching and recovering scandium from secondary resource leachate
CN111471860A (en) * 2020-06-17 2020-07-31 济南大学 Method for separating lanthanum and cerium from mixed rare earth by using amide podophyllum ether extracting agent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180142321A1 (en) * 2015-05-07 2018-05-24 Commissariat A L'energie Atomique Et Aux Energies Alternatives Use of novel compounds for selectively extracting rare earths from aqueous solutions including phosphoric acid and associated extraction method
CN108300878A (en) * 2018-01-26 2018-07-20 中国科学院长春应用化学研究所 A kind of extraction process with acid phosphine enriching and recovering scandium from secondary resource leachate
CN111471860A (en) * 2020-06-17 2020-07-31 济南大学 Method for separating lanthanum and cerium from mixed rare earth by using amide podophyllum ether extracting agent

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114672650A (en) * 2022-05-06 2022-06-28 济南大学 Method for extracting scandium from titanium white waste acid by utilizing diphosphonic acid extracting agent

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