CN112429760A - Method for purifying crude scandium oxide - Google Patents
Method for purifying crude scandium oxide Download PDFInfo
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- CN112429760A CN112429760A CN202011165667.9A CN202011165667A CN112429760A CN 112429760 A CN112429760 A CN 112429760A CN 202011165667 A CN202011165667 A CN 202011165667A CN 112429760 A CN112429760 A CN 112429760A
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- scandium
- scandium oxide
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- acid
- leaching
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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
Abstract
The invention discloses a method for purifying crude scandium oxide, which comprises the following steps: (1) primary acid leaching: adding water into the crude scandium oxide for size mixing, adding inorganic acid to adjust the pH value of the slurry to 1.0-3.0, and filtering after reaction to obtain first-stage leaching residue and first-stage leaching liquid; (2) secondary acid leaching: putting the obtained first-stage leaching residue into an inorganic acid solution, and reacting to obtain a second-stage leaching solution rich in scandium; (3) and (3) scandium precipitation by oxalic acid: adding oxalic acid solution into the two-stage leaching solution, adding a regulator to adjust the pH of the reaction material to 0.5-2.0, and filtering after reaction to obtain scandium oxalate precipitate; (4) and (3) calcining: and drying and calcining the obtained scandium oxalate precipitate to obtain the purified and refined scandium oxide. The method effectively utilizes the difference of acid solubility of the impurities and the scandium oxide to leach the impurities and the scandium oxide respectively, has good impurity separation effect, greatly simplifies the existing scandium oxide purification process and operation flow, and saves operation cost to a certain extent.
Description
Technical Field
The invention relates to the field of hydrometallurgy, in particular to a method for purifying crude scandium oxide through sectional leaching.
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. Scandium is not easy to extract and purify because independent ore deposits are few but widely distributed in ore deposits of cobalt, aluminum, nickel, titanium, tungsten, zirconium and the like or are enriched in metallurgical waste residues or smoke dust, and as a kind of associated ore or by-product, scandium is low in content of raw materials or waste residues, and impurities in the raw materials are various and high in content.
Because the chemical property of scandium metal is relatively active and is easy to oxidize, scandium metal is generally prepared into scandium oxide for storage and utilization after scandium is industrially extracted. Because the raw material for extracting scandium is complex and has more impurities, scandium is generally extracted and then prepared into coarse scandium oxide for enrichment, and then a series of purification operations such as refining and impurity removal are carried out to prepare high-purity scandium oxide which is then stored and utilized. At present, the process for industrially purifying scandium oxide mostly comprises the steps of dissolving scandium oxide completely by acid, then separating impurities by an extraction method, finally precipitating by oxalic acid and calcining to obtain high-purity scandium oxide, or repeatedly precipitating and calcining crude scandium oxide directly after acid dissolution to prepare high-purity scandium oxide. The extraction method also needs to be subjected to back extraction, impurity removal and precipitation again, the extraction agent needs to be regenerated, the process flow is long, and the operation is complicated. The impurity separation by the direct acid dissolution precipitation method is not thorough, the purification effect can be achieved only by repeated operation, and a large amount of acid is consumed by repeated acid dissolution, so that the cost is increased.
Disclosure of Invention
The invention provides a method for purifying scandium oxide through sectional leaching, aiming at the defects of the existing scandium oxide purification method. The method effectively utilizes the difference of acid solubility of the impurities and scandium oxide to leach the impurities and the scandium oxide respectively, has good impurity separation effect, greatly simplifies the existing scandium oxide purification process and operation flow, and saves operation cost to a certain extent.
The invention provides a method for purifying crude scandium oxide, which comprises the following steps:
a method of purifying crude scandium oxide, comprising the steps of:
(1) primary acid leaching: adding water into the crude scandium oxide for size mixing, adding inorganic acid (at least one of hydrochloric acid, sulfuric acid or nitric acid) for adjusting the pH value of the slurry to 1.0-3.0, reacting and filtering. Under the condition, impurities are mainly leached out, most of the impurities enter the solution, scandium oxide still remains in the slag, the reaction is carried out, the leaching solution and the slag are separated, and one-time separation of the impurities and the scandium oxide can be realized.
(2) Secondary acid leaching: putting the obtained first-stage leaching residue into a solution of inorganic acid (at least one of hydrochloric acid, sulfuric acid or nitric acid), wherein H of the inorganic acid+The content is 2-10 mol/L, and a scandium-rich two-stage leaching solution is obtained through reaction;
(3) and (3) scandium precipitation by oxalic acid: adding oxalic acid solution into the two-stage leaching solution, adding a regulator to adjust the pH of the reaction material to 0.5-2.0, and filtering after reaction to obtain scandium oxalate precipitate;
(4) and (3) calcining: and drying and calcining the obtained scandium oxalate precipitate to obtain the purified and refined scandium oxide.
In the invention, in the step (1), the reaction temperature is 5-100 ℃, and the reaction time is 0.5-5 h;
in the invention, in the step (2), the reaction temperature is 60-100 ℃, and the reaction time is 1-10 h;
in the step (3), the addition amount of the oxalic acid solution is 1.5-2.5 times of the theoretical addition amount of the generated scandium oxalate, the back regulator is one or more of ammonia water, ammonium bicarbonate and ammonium carbonate, and the addition amount of the back regulator is adjusted to enable the reaction pH to reach and maintain 0.5-2.0 of the reaction requirement.
In the invention, in the step (3), the reaction time is 0.5-3 h.
In the invention, in the step (4), the calcining temperature is 700-900 ℃, and the calcining time is 1-3 h.
The invention has the beneficial technical effects that:
the method effectively utilizes the difference of acid solubility of the impurities and the scandium oxide to leach the impurities and the scandium oxide respectively, has good impurity separation effect, greatly simplifies the existing scandium oxide purification process and operation flow, and saves operation cost to a certain extent.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
(1) Primary acid leaching: adding water into the crude scandium oxide for size mixing, adding hydrochloric acid for adjusting the pH value of the slurry to 1.2, reacting for 4 hours at room temperature of 25 ℃, mainly leaching out impurities under the condition, enabling most of the impurities to enter the solution, still retaining the scandium oxide in the slag, filtering after reaction, and separating leachate and the slag, thus realizing primary separation of the impurities and the scandium oxide.
(2) Secondary acid leaching: putting the obtained first-stage leaching residue into a hydrochloric acid solution H+The content is 5mol/L, and the reaction is carried out for 8 hours at 70 ℃ to obtain scandium-rich second-stage leaching solution;
(3) and (3) scandium precipitation by oxalic acid: adding oxalic acid solution into the two-stage leachate, wherein the addition amount of the oxalic acid solution is 2 times of the theoretical addition amount of the generated scandium oxalate, adding a back regulator to regulate the pH value of the reaction material to 1.0, wherein the back regulator is ammonia water, maintaining the pH value of the reaction material to 1.0 by adding the back regulator, reacting for 2 hours, and filtering to obtain scandium oxalate precipitate;
(4) and (3) calcining: and drying the obtained scandium oxalate precipitate, putting the dried scandium oxalate precipitate into a muffle furnace, and calcining the scandium oxalate precipitate for 2 hours at the temperature of 800 ℃ to obtain the purified and refined scandium oxide.
Example 2
(1) Primary acid leaching: adding water into the crude scandium oxide for size mixing, adding hydrochloric acid for adjusting the pH value of the slurry to 1.5, reacting for 3 hours at 60 ℃, mainly leaching out impurities under the condition, enabling most of the impurities to enter the solution, still retaining scandium oxide in slag, filtering after reaction, and separating leachate and slag, thus realizing primary separation of the impurities and scandium oxide.
(2) Secondary acid leaching: putting the obtained first-stage leaching residue into a hydrochloric acid solution H+The content is 7mol/L, and the reaction is carried out for 4 hours at the temperature of 80 ℃ to obtain a scandium-rich two-stage leaching solution;
(3) and (3) scandium precipitation by oxalic acid: adding oxalic acid solution into the two-stage leachate, wherein the addition amount of the oxalic acid solution is 2.2 times of the theoretical addition amount of the generated scandium oxalate, adding a back regulator to adjust the pH value of the reaction material to 0.8, wherein the back regulator is ammonium bicarbonate, maintaining the pH value of the reaction material to 0.8 by adding the back regulator, reacting for 2 hours, and filtering to obtain scandium oxalate precipitate;
(4) and (3) calcining: and drying the obtained scandium oxalate precipitate, putting the dried scandium oxalate precipitate into a muffle furnace, and calcining for 1h at the temperature of 850 ℃ to obtain the purified and refined scandium oxide.
Example 3
(1) Primary acid leaching: adding water into the crude scandium oxide for size mixing, adding sulfuric acid to adjust the pH value of the slurry to 1.8, reacting for 2.5h at 70 ℃, mainly leaching out impurities under the condition, enabling most of the impurities to enter the solution, keeping scandium oxide in the slag, filtering after reaction, and separating leachate and slag to realize primary separation of the impurities and scandium oxide.
(2) Secondary acid leaching: putting the obtained first-stage leaching residue into a hydrochloric acid solution H+The content is 10mol/L, and the reaction is carried out for 2 hours at the temperature of 90 ℃ to obtain a scandium-rich two-stage leaching solution;
(3) and (3) scandium precipitation by oxalic acid: adding oxalic acid solution into the two-stage leachate, wherein the addition amount of the oxalic acid solution is 2.1 times of the theoretical addition amount of the generated scandium oxalate, adding a back regulator to adjust the pH value of the reaction material to 1.2, wherein the back regulator is ammonium carbonate, maintaining the pH value of the reaction material to be 1.2 by adding the back regulator, reacting for 1.5h, and filtering to obtain scandium oxalate precipitate;
(4) and (3) calcining: and drying the obtained scandium oxalate precipitate, putting the dried scandium oxalate precipitate into a muffle furnace, and calcining the scandium oxalate precipitate for 2 hours at the temperature of 750 ℃ to obtain the purified and refined scandium oxide.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (7)
1. A method of purifying crude scandium oxide, comprising the steps of:
(1) primary acid leaching: adding water into the crude scandium oxide for size mixing, adding inorganic acid to adjust the pH value of the slurry to 1.0-3.0, and filtering after reaction to obtain first-stage leaching residue and first-stage leaching liquid;
(2) secondary acid leaching: putting the obtained first-stage leaching residue into an inorganic acid solution, wherein H of the inorganic acid solution+The content is 2-10 mol/L, and a scandium-rich two-stage leaching solution is obtained through reaction;
(3) and (3) scandium precipitation by oxalic acid: adding oxalic acid solution into the two-stage leaching solution, adding a regulator to adjust the pH of the reaction material to 0.5-2.0, and filtering after reaction to obtain scandium oxalate precipitate;
(4) and (3) calcining: and drying and calcining the obtained scandium oxalate precipitate to obtain the purified and refined scandium oxide.
2. The method for purifying crude scandium oxide according to claim 1, wherein in the step (1), the reaction temperature is 5 to 100 ℃ and the reaction time is 0.5 to 5 hours.
3. The method of purifying crude scandium oxide according to claim 1, wherein the inorganic acid used in the acid leaching is at least one of hydrochloric acid, sulfuric acid, or nitric acid.
4. The method for purifying crude scandium oxide according to claim 1, wherein in the step (2), the reaction temperature is 60 to 100 ℃ and the reaction time is 1 to 10 hours.
5. The method for purifying crude scandium oxide according to claim 1, wherein in the step (3), the oxalic acid solution is added in an amount of 1.5 to 2.5 times a theoretical addition amount for generating scandium oxalate, the adjustment agent is one or more of ammonia water, ammonium bicarbonate and ammonium carbonate, and the adjustment agent is added in an amount so as to maintain a reaction pH of 0.5 to 2.0 required for the reaction.
6. The method for purifying crude scandium oxide according to claim 1, wherein in the step (3), the reaction time is 0.5 to 3 hours.
7. The method for purifying crude scandium oxide according to claim 1, wherein in the step (4), the calcination temperature is in a range of 700 to 900 ℃ and the calcination time is in a range of 1 to 3 hours.
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| CN202011165667.9A CN112429760A (en) | 2020-10-27 | 2020-10-27 | Method for purifying crude scandium oxide |
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| CN202011165667.9A CN112429760A (en) | 2020-10-27 | 2020-10-27 | Method for purifying crude scandium oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113371751A (en) * | 2021-05-13 | 2021-09-10 | 中国恩菲工程技术有限公司 | Preparation method and application of ultra-high-purity scandium oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102863004A (en) * | 2011-07-05 | 2013-01-09 | 北京有色金属研究总院 | Purification and preparation method of high-purity scandium oxide |
| CN105980585A (en) * | 2014-02-19 | 2016-09-28 | 住友金属矿山株式会社 | Scandium recovery process |
| CN107082443A (en) * | 2017-04-21 | 2017-08-22 | 闫博文 | A kind of preparation method of solid fuel cell scandium oxide |
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- 2020-10-27 CN CN202011165667.9A patent/CN112429760A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863004A (en) * | 2011-07-05 | 2013-01-09 | 北京有色金属研究总院 | Purification and preparation method of high-purity scandium oxide |
| CN105980585A (en) * | 2014-02-19 | 2016-09-28 | 住友金属矿山株式会社 | Scandium recovery process |
| CN107082443A (en) * | 2017-04-21 | 2017-08-22 | 闫博文 | A kind of preparation method of solid fuel cell scandium oxide |
Non-Patent Citations (1)
| Title |
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| 《中国商品大辞典》编辑委员会: "《中国商品大辞典 化学试剂分册》", vol. 978, 冶金工业出版社, pages: 230 - 231 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113371751A (en) * | 2021-05-13 | 2021-09-10 | 中国恩菲工程技术有限公司 | Preparation method and application of ultra-high-purity scandium oxide |
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