CN112320832A - Method for purifying and refining high-purity scandium oxide from scandium hydroxide intermediate product - Google Patents
Method for purifying and refining high-purity scandium oxide from scandium hydroxide intermediate product Download PDFInfo
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- CN112320832A CN112320832A CN202011143998.2A CN202011143998A CN112320832A CN 112320832 A CN112320832 A CN 112320832A CN 202011143998 A CN202011143998 A CN 202011143998A CN 112320832 A CN112320832 A CN 112320832A
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product, which comprises the following steps: calcining the scandium hydroxide intermediate product to obtain crude scandium oxide; adding water into the crude scandium oxide for slurrying, adding inorganic acid to adjust the pH value to 1.0-3.0, filtering and washing to obtain first-stage leaching residue; putting the first-stage leaching residue into an inorganic acid solution, and filtering to obtain a second-stage leaching solution; extracting and phase-splitting the second-stage leachate by using an extractant P350, and then performing back extraction and phase splitting to obtain a scandium-containing back extraction solution; adding an oxalic acid solution into the scandium-containing back extraction solution, adding a back regulator to adjust the pH value to 0.5-2.0, filtering and washing to obtain scandium oxalate precipitate; and calcining the scandium oxalate precipitate to obtain the refined high-purity scandium oxide. The invention combines the sectional leaching and extraction processes aiming at the characteristic difference of scandium oxide and impurity elements to prepare the high-purity scandium oxide, and can greatly shorten the process flow.
Description
Technical Field
The invention belongs to the field of rare earth metallurgy, and particularly relates to a method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product.
Background
Scandium as a rare earth metal element has wide application in the fields of lighting industry, alloy industry, ceramic materials, catalytic materials and the like. For example, an aluminum-scandium alloy made of scandium and aluminum is widely used in the fields of aerospace, aviation, missile, ship and the like due to the advantages of small density, high strength, high hardness, good thermal stability and the like, and gradually turns to civil use, such as moving devices, computers, mobile phone shells and the like. Scandium-sodium halogen and the like prepared from scandium oxide are widely applied to illumination in various occasions due to the characteristics of good luminosity, energy conservation, long service life, strong fog breaking capability and the like. Lasers and various electric light source devices made of high-purity scandium oxide are widely applied to the fields of military industry, civil use and the like, and particularly, in recent years, with the rapid development of communication technology, the market demand of scandium as an important additive of electric light source materials is further increased. However, the purity of scandium oxide has an important influence on the applicable field, the purity of scandium oxide produced in China is mostly below 99.9%, the scandium oxide cannot be directly applied to high-precision fields such as laser, electric light source and the like, and if the scandium oxide is used in the fields, further purification is needed.
At present, there are many reports on recovering and extracting scandium oxide from various scandium-containing raw materials and waste materials, and common raw materials or waste materials for extracting scandium oxide include scandium-containing ores, red mud, titanium white waste acid, zirconium oxychloride waste acid, chlorinated smoke dust, slag generated by smelting tungsten, manganese and iron, and the like. The method for extracting scandium basically comprises the steps of firstly transferring scandium into a solution through a certain leaching process, then carrying out concentration enrichment and impurity removal on scandium in the solution through an extraction process, then precipitating scandium in a certain solid form, and finally further processing and purifying a solid intermediate product rich in scandium to prepare scandium oxide. In the preparation process of scandium oxide, scandium hydroxide is a common important intermediate product in the process, and there are various routes for preparing scandium oxide by processing scandium hydroxide. Scandium hydroxide is generally dissolved by acid, and then is subjected to impurity separation and oxalic acid precipitation by an extraction or ion exchange method to prepare scandium oxide, but the scandium oxide prepared by the method is generally not high in purity, and if certain use conditions are met, further dissolution and purification of crude scandium oxide are required. And at present, no extracting agent can be used for separating scandium and all impurity elements in one-time extraction in a targeted manner. The preparation of high-purity scandium oxide usually requires the combined use of more than two extracting agents, and the required purity can be achieved after multiple times of extraction and back extraction, which undoubtedly makes the scandium extraction process long and complicated and increases the operation cost.
Disclosure of Invention
Aiming at the problems of complicated process and weak pertinence in the prior art for preparing high-purity scandium oxide, the invention prepares the high-purity scandium oxide by taking scandium hydroxide as a starting raw material and combining the processes of sectional leaching and extraction according to the characteristic difference of scandium oxide and impurity elements, and can greatly shorten the process flow.
The invention adopts the following technical scheme:
a method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product is characterized by comprising the following steps:
(1) calcining the scandium hydroxide intermediate product at 700-900 ℃ for 1-2 h to obtain crude scandium oxide;
(2) adding water into the crude scandium oxide for slurrying to obtain slurry, adding inorganic acid into the slurry to adjust the pH value to 1.0-3.0, filtering to obtain first filter residue, and washing the first filter residue with pure water to obtain first-stage leaching residue;
(3) putting the first-stage leaching residue into an inorganic acid solution with the hydrogen ion concentration of 2-10 mol/L, and filtering to obtain a scandium-rich second-stage leaching solution;
(4) extracting and phase-splitting the two-stage leachate by using an extractant P350 to obtain a scandium-rich organic phase;
(5) carrying out back extraction and phase splitting on the scandium-rich organic phase to obtain a scandium-containing back extraction solution;
(6) adding an oxalic acid solution into the scandium-containing back extraction solution to obtain a reaction material, adding a back regulator into the reaction material to adjust the pH value to 0.5-2.0, filtering to obtain second filter residue, and washing the second filter residue with pure water or a dilute oxalic acid solution to obtain scandium oxalate precipitate;
(7) and (3) calcining the scandium oxalate precipitate at 700-900 ℃ for 1-2 h to obtain the refined high-purity scandium oxide.
The method for purifying and refining high-purity scandium oxide from the scandium hydroxide intermediate product is characterized in that in the step (2), inorganic acid is added into slurry, and then the pH value is maintained to be 1.0-3.0 for reaction for 1-5 h; and (3) adjusting the pH of the slurry in the step (2) by using one or more of sulfuric acid, hydrochloric acid and nitric acid.
The method for purifying and refining high-purity scandium oxide from the scandium hydroxide intermediate product is characterized in that in the step (3), a first-stage leaching residue is put into an inorganic acid solution and reacts for 1-8 h at the temperature of 60-100 ℃; and (3) the inorganic acid in the inorganic acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid.
The method for purifying and refining high-purity scandium oxide from the scandium hydroxide intermediate product is characterized in that the volume concentration of the extracting agent P350 in the step (4) is 5-50%, and the diluent used for extracting and phase-separating the two-stage leaching solution by the extracting agent P350 in the step (4) is sulfonated kerosene.
The method for purifying and refining high-purity scandium oxide from the scandium hydroxide intermediate product is characterized in that a stripping agent used for stripping the scandium-rich organic phase in the step (5) is an inorganic acid solution with the concentration of 0.01-5 mol/L.
The method for purifying and refining high-purity scandium oxide from the scandium hydroxide intermediate product is characterized in that the inorganic acid in the stripping agent inorganic acid solution used for stripping the scandium-rich organic phase in the step (5) is one or more of sulfuric acid, hydrochloric acid and nitric acid.
The method for purifying and refining high-purity scandium oxide from the scandium hydroxide intermediate product is characterized in that in the step (6), a reaction material is added with a back-regulating agent to adjust the pH value to 0.5-2.0, and then the pH value is maintained for reaction for 0.5-3 h; and (6) adding the Chinese herbal acid solution into the scandium-containing back extraction solution in the step (6) in an amount which is 1.5-2.5 times of the theoretical oxalic acid dosage for generating scandium oxalate, and using at least one of ammonia water, ammonium bicarbonate and ammonium carbonate as a tempering agent.
The invention has the beneficial technical effects that: the combined sectional leaching and extracting process provided by the invention utilizes the difference of acid solubility of the oxide and the selective extraction principle to purposefully separate different impurities from the main element scandium step by step, thereby preparing the high-purity scandium oxide. After the combined operation of sectional leaching and extraction, high-purity scandium oxide with the purity of more than 99.99 percent can be obtained. Compared with other processes for preparing the same-grade scandium oxide, the method has the advantages of short flow, simplicity in operation and capability of greatly reducing the operation cost.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Referring to fig. 1, the method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product comprises the following steps:
(1) calcining the scandium hydroxide intermediate product at 700-900 ℃ for 1-2 h to obtain crude scandium oxide;
(2) adding water into the crude scandium oxide for slurrying to obtain slurry, adding inorganic acid into the slurry to adjust the pH value to 1.0-3.0, maintaining the pH value to 1.0-3.0, reacting for 1-5 h, filtering to obtain first filter residue, and washing the first filter residue with pure water to obtain first-stage leaching residue; the inorganic acid for adjusting the pH of the slurry is one or more of sulfuric acid, hydrochloric acid and nitric acid.
(3) Putting the first-stage leaching residue into an inorganic acid solution with the hydrogen ion concentration of 2-10 mol/L, reacting for 1-8 h at 60-100 ℃, and filtering to obtain a scandium-rich second-stage leaching solution; the inorganic acid in the inorganic acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid.
(4) Extracting and phase-separating the second-stage leachate by using an extractant P350 (dimethylheptyl methylphosphonate) to obtain a scandium-rich organic phase; the volume concentration of the extractant P350 is 5-50%, and the diluent used when the second-stage leaching solution is extracted and phase-separated by the extractant P350 is sulfonated kerosene. The number of extraction stages is 1 to 20 stages compared with the ratio of O/A (1: 20) to (20: 1).
(5) Carrying out back extraction and phase splitting on the scandium-rich organic phase to obtain a scandium-containing back extraction solution; the stripping agent used for stripping is 0.01 mol/L-5 mol/L inorganic acid solution, and the inorganic acid in the stripping agent inorganic acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid. The stripping ratio O/A is (1: 20) - (20: 1), and the number of stripping stages is 1-20.
(6) Adding an oxalic acid solution into the scandium-containing back extraction solution to obtain a reaction material, adding a back regulator into the reaction material to adjust the pH to 0.5-2.0, maintaining the pH to 0.5-2.0, reacting for 0.5-3 h, filtering to obtain second filter residue, and washing the second filter residue with pure water or a dilute oxalic acid solution to obtain scandium oxalate precipitate; the adding amount of the oxalic acid solution added into the scandium-containing strip liquor is 1.5-2.5 times of the theoretical oxalic acid dosage for generating scandium oxalate, and the tempering agent is at least one of ammonia water, ammonium bicarbonate and ammonium carbonate.
(7) And (3) calcining the scandium oxalate precipitate at 700-900 ℃ for 1-2 h to obtain the refined high-purity scandium oxide.
Example 1
1000g of scandium hydroxide intermediate was calcined at 800 ℃ for 2h to obtain crude scandium oxide.
Adding water into the crude scandium oxide for slurrying to obtain slurry, adding hydrochloric acid into the slurry to adjust the pH value to 1.5, maintaining the pH value to 1.5, reacting for 3 hours, filtering to obtain first filter residue, and washing the first filter residue with pure water to obtain first-stage leaching residue.
And putting the first-stage leaching residue into a hydrochloric acid solution with the hydrogen ion concentration of 6mol/L, reacting for 5 hours at 90 ℃, and filtering to obtain a second-stage leaching solution rich in scandium.
Extracting and phase-splitting the two-stage leachate by using an extractant P350 to obtain a scandium-rich organic phase; the volume concentration of the extractant P350 is 40 percent, and the diluent used for extracting and phase-splitting the second-stage leaching solution by the extractant P350 is sulfonated kerosene. And (3) extracting, wherein the ratio of O/A is 1: 1, the extraction stage number is 3.
Carrying out back extraction and phase splitting on the scandium-rich organic phase to obtain a scandium-containing back extraction solution; the stripping agent used in the stripping is 1mol/L hydrochloric acid solution. And the stripping phase ratio O/A is 1: 1, the back extraction stage number is 2.
Adding oxalic acid solution into the scandium-containing back extraction solution to obtain a reaction material, adding a back regulator into the reaction material to adjust the pH to 1.0, maintaining the pH to 1.0, reacting for 2 hours, filtering to obtain a second filter residue, and washing the second filter residue with pure water to obtain scandium oxalate precipitate; the adding amount of the oxalic acid solution added into the scandium-containing strip liquor is 2 times of the theoretical oxalic acid dosage for generating scandium oxalate, and the adjusting agent is ammonia water.
And calcining the scandium oxalate precipitate at 800 ℃ for 2h to obtain the refined high-purity scandium oxide.
Example 2
1000g of scandium hydroxide intermediate was calcined at 800 ℃ for 1.5h to obtain crude scandium oxide.
Adding water into the crude scandium oxide for slurrying to obtain slurry, adding hydrochloric acid into the slurry to adjust the pH value to 2.0, maintaining the pH value to 2.0, reacting for 4 hours, filtering to obtain first filter residue, and washing the first filter residue with pure water to obtain first-stage leaching residue.
And putting the first-stage leaching residue into a hydrochloric acid solution with the hydrogen ion concentration of 8mol/L, reacting for 3 hours at 90 ℃, and filtering to obtain a second-stage leaching solution rich in scandium.
Extracting and phase-splitting the two-stage leachate by using an extractant P350 to obtain a scandium-rich organic phase; the volume concentration of the extractant P350 is 30 percent, and the diluent used for extracting and phase-splitting the second-stage leaching solution by the extractant P350 is sulfonated kerosene. And (3) extracting, wherein O/A is 2: 1, the extraction stage number is 2 stages.
Carrying out back extraction and phase splitting on the scandium-rich organic phase to obtain a scandium-containing back extraction solution; the stripping agent used in the stripping is 1.5mol/L hydrochloric acid solution. And the stripping phase ratio O/A is 1: 1, the back extraction stage number is 3.
Adding oxalic acid solution into the scandium-containing back extraction solution to obtain a reaction material, adding a back regulator into the reaction material to adjust the pH to 1.0, maintaining the pH to 1.0, reacting for 2 hours, filtering to obtain a second filter residue, and washing the second filter residue with pure water to obtain scandium oxalate precipitate; the adding amount of the oxalic acid solution added into the scandium-containing strip liquor is 2 times of the theoretical oxalic acid dosage for generating scandium oxalate, and the adjusting agent is ammonium bicarbonate.
And calcining the scandium oxalate precipitate at 800 ℃ for 1.5h to obtain the refined high-purity scandium oxide.
The above description is only a preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product is characterized by comprising the following steps:
(1) calcining the scandium hydroxide intermediate product at 700-900 ℃ for 1-2 h to obtain crude scandium oxide;
(2) adding water into the crude scandium oxide for slurrying to obtain slurry, adding inorganic acid into the slurry to adjust the pH value to 1.0-3.0, filtering to obtain first filter residue, and washing the first filter residue with pure water to obtain first-stage leaching residue;
(3) putting the first-stage leaching residue into an inorganic acid solution with the hydrogen ion concentration of 2-10 mol/L, and filtering to obtain a scandium-rich second-stage leaching solution;
(4) extracting and phase-splitting the two-stage leachate by using an extractant P350 to obtain a scandium-rich organic phase;
(5) carrying out back extraction and phase splitting on the scandium-rich organic phase to obtain a scandium-containing back extraction solution;
(6) adding an oxalic acid solution into the scandium-containing back extraction solution to obtain a reaction material, adding a back regulator into the reaction material to adjust the pH value to 0.5-2.0, filtering to obtain second filter residue, and washing the second filter residue with pure water or a dilute oxalic acid solution to obtain scandium oxalate precipitate;
(7) and (3) calcining the scandium oxalate precipitate at 700-900 ℃ for 1-2 h to obtain the refined high-purity scandium oxide.
2. The method for purifying and refining high-purity scandium oxide from scandium hydroxide intermediate product according to claim 1, wherein in the step (2), the slurry is added with inorganic acid, and then the pH value is maintained to be 1.0-3.0, and the reaction is carried out for 1-5 h; and (3) adjusting the pH of the slurry in the step (2) by using one or more of sulfuric acid, hydrochloric acid and nitric acid.
3. The method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product according to claim 1, wherein in the step (3), the first-stage leaching residue is put into an inorganic acid solution and reacts for 1h to 8h at 60 ℃ to 100 ℃; and (3) the inorganic acid in the inorganic acid solution is one or more of sulfuric acid, hydrochloric acid and nitric acid.
4. The method for purifying and refining high-purity scandium oxide from a scandium hydroxide intermediate product according to claim 1, wherein a volume concentration of the extractant P350 in the step (4) is 5% to 50%, and a diluent used for extraction and phase separation of the second-stage leachate with the extractant P350 in the step (4) is sulfonated kerosene.
5. The method for purifying and refining scandium hydroxide intermediate product according to claim 1, wherein the stripping agent used for stripping the scandium-rich organic phase in the step (5) is an inorganic acid solution of 0.01mol/L to 5 mol/L.
6. The method for purifying and refining scandium hydroxide intermediate products according to claim 5, wherein the inorganic acid in the back extractant inorganic acid solution used for back extracting the scandium-rich organic phase in the step (5) is one or more of sulfuric acid, hydrochloric acid and nitric acid.
7. The method for purifying and refining high-purity scandium oxide from scandium hydroxide intermediate products according to claim 1, wherein in the step (6), the reaction material is added with a pH adjusting agent to adjust the pH to 0.5-2.0, and then the pH is maintained for reaction for 0.5-3 h; and (6) adding the Chinese herbal acid solution into the scandium-containing back extraction solution in the step (6) in an amount which is 1.5-2.5 times of the theoretical oxalic acid dosage for generating scandium oxalate, and using at least one of ammonia water, ammonium bicarbonate and ammonium carbonate as a tempering agent.
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| CN113184892A (en) * | 2021-04-25 | 2021-07-30 | 烟台金堃新材料科技有限公司 | Method for preparing ultra-high-purity scandium oxide from crude scandium hydroxide |
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