CN112708786A - Method for recycling scandium from aluminum-scandium alloy target material waste - Google Patents
Method for recycling scandium from aluminum-scandium alloy target material waste Download PDFInfo
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- CN112708786A CN112708786A CN202011468583.2A CN202011468583A CN112708786A CN 112708786 A CN112708786 A CN 112708786A CN 202011468583 A CN202011468583 A CN 202011468583A CN 112708786 A CN112708786 A CN 112708786A
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- scandium
- aluminum
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- oxalate
- acid
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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
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
The invention relates to a method for recycling scandium from aluminum-scandium alloy target waste, which comprises the following steps: 1) crushing: crushing the aluminum-scandium alloy target material waste to obtain a recovered raw material; 2) acid leaching: leaching the recovered raw materials, pure water and acid according to a certain proportion to obtain scandium-containing pickle liquor; 3) oxalic acid precipitation: adding oxalic acid solution into the scandium-containing pickle liquor, carrying out precipitation purification to recover scandium, filtering to obtain aluminum-rich filtrate and crude scandium oxalate, and washing the separated crude scandium oxalate to obtain scandium oxalate; 4) and (3) calcining: and calcining scandium oxalate to obtain a high-purity scandium oxide product. The method disclosed by the invention has the advantages that scandium is recovered by treating the aluminum-scandium alloy target material waste material by adopting an acid leaching-oxalic acid precipitation method, the complex steps of traditional scandium extraction and recovery are optimized, valuable scandium metal in the scandium is recovered, the technological process of scandium recovery is greatly shortened, the chemical reagent dosage is reduced, the recovery cost is low, the recovery rate is high, the method is environment-friendly, and the product purity is more than 99.9%.
Description
Technical Field
The invention relates to the field of resource recovery, in particular to a method for recovering scandium from aluminum-scandium alloy target material waste.
Background
Scandium is an important rare earth element and is a typical rare metal, and is widely applied to the aspects of national defense, metallurgy, chemical engineering, aerospace, nuclear technology, preparation of high-efficiency lasers, superconducting materials, electrolyte materials of solid fuel cells and the like, and is a national important strategic resource. Scandium has good alloying effect on alloy, and a certain amount of scandium is added into aluminum, so that the effects of refining crystal grains, improving recrystallization temperature, improving corrosion resistance, improving strength and plasticity and the like can be achieved, therefore, the aluminum-scandium alloy has comprehensive properties of high strength, corrosion resistance, high temperature resistance and good weldability, has wide application in advanced science and technology fields such as aerospace, nuclear engineering and the like, and fields such as transportation, household appliances and the like, and is a light structural material. However, in the process of preparing and using the aluminum-scandium alloy target, more than 30% of the aluminum-scandium alloy target becomes waste materials and needs to be recycled, so that a simple and rapid method for recycling scandium is researched and developed, and the method has very important significance for the development of the scandium use field.
In the existing recovery process of the aluminum-scandium alloy target material waste, an alkali transformation-leaching-extraction recovery technology is mainly adopted, and scandium is precipitated by oxalic acid for separation and impurity removal; other scandium-containing materials adopt a combined process of multiple acid dissolution-extraction-back extraction-acid dissolution-oxalic acid precipitation inorganic precipitation separation and extraction in the recovery process, the method has low scandium recovery rate, high cost and complex process flow, and simultaneously causes the waste of scandium resources. For scandium extraction, P350 can be back-extracted by hydrochloric acid, but the quality of P350 is unstable and cannot meet the continuous production requirement of a scandium production line.
Therefore, it is necessary to design a new recycling method to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a method for recycling scandium from aluminum-scandium alloy target material waste, which has the advantages of simple process flow, less chemical reagents, low recycling cost, high recycling rate and small environmental pollution.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for recycling scandium from aluminum-scandium alloy target waste materials comprises the following steps:
s1 crushing: crushing the aluminum-scandium alloy target material waste to obtain a recovered raw material;
acid leaching of S2: leaching the recovered raw materials, pure water and acid according to a certain proportion to obtain scandium-containing pickle liquor;
s3 oxalic acid precipitation: adding oxalic acid solution into scandium-containing pickle liquor for precipitation, and washing the separated solid matter to obtain scandium oxalate;
s4 calcination: and calcining scandium oxalate to obtain high-purity scandium oxide.
As a further improvement of the method, the mass fraction of aluminum in the aluminum-scandium alloy target material waste is 70-90%.
As a further improvement of the present invention, in S2, the raw material is recovered: pure water: the ratio of the acids is 1g to 10-15 ml.
As a further improvement of the invention, the acid used for leaching comprises one of sulfuric acid, hydrochloric acid and nitric acid.
As a further improvement of the method, the scandium concentration of the scandium-containing pickle liquor is controlled to be 5-20 g/L.
As a further improvement of the method, the addition amount of the oxalic acid as the precipitator is 1-2 times of the theoretical amount.
As a further improvement of the method, the reaction temperature of the oxalic acid precipitation is controlled to be 50-70 ℃.
As a further improvement of the invention, the calcining temperature of the scandium oxalate is controlled to be 600-800 ℃.
As a further improvement of the invention, the calcination time of the scandium oxalate is controlled to be 2-4 h.
As a further improvement of the present invention, the valuable metal in the aluminum-scandium alloy target scrap includes at least one of scandium and aluminum.
The invention provides a method for recovering scandium from aluminum-scandium alloy target material waste, which adopts a method of acid leaching, oxalic acid precipitation, washing and calcining, and has the following beneficial effects compared with the prior art: firstly, scandium is recovered through selective precipitation of acid leaching solution, so that the problems of difficult back extraction and difficult alkali back extraction and pressure filtration in the traditional process can be effectively avoided, and particularly the problem of scandium metal loss easily caused in the process can be effectively solved. Secondly, after scandium is selectively precipitated by oxalic acid, the content of scandium in the aluminum-enriched liquid is less than 100mg/L, the recovery rate of scandium can reach 99%, and the loss of scandium is reduced. The whole technological process is simple to operate, the equipment investment is low, the scandium metal recovery period is short, and the scandium oxide obtained by production can provide a raw material for preparation of the scandium metal at the front end of the aluminum scandium target material.
Detailed Description
The invention provides a method for recycling scandium from aluminum-scandium alloy target waste, which comprises the following steps:
s1 crushing: crushing the aluminum-scandium alloy target material waste to obtain a recovered raw material;
acid leaching of S2: leaching the recovered raw materials, pure water and acid according to a certain proportion to obtain scandium-containing pickle liquor;
s3 oxalic acid precipitation: adding oxalic acid solution into scandium-containing pickle liquor for precipitation, and washing the separated solid matter to obtain scandium oxalate;
s4 calcination: and calcining scandium oxalate to obtain high-purity scandium oxide.
Example 1.
A method for recycling scandium from aluminum-scandium alloy target waste materials comprises the following steps: crushing the aluminum-scandium alloy target material waste with the content of 10% Sc-90% Al, adding pure water according to the solid-to-liquid ratio of 1:15, starting stirring, heating to 60 ℃, beginning to dropwise add analytically pure hydrochloric acid by using a constant-pressure funnel, stopping adding acid when the temperature is higher than 75 ℃, and obtaining acid leaching solution after complete reaction. Adding oxalic acid solution with the amount being 1 time of the stoichiometric ratio into the pickle liquor, reacting for 1 hour at the temperature of 55 ℃, carrying out suction filtration on the obtained precipitation system solution to obtain crude scandium oxalate, wherein the scandium precipitation rate is more than 98%, and the filtrate is used as aluminum-rich solution, and the scandium concentration is less than 100 ppm. And (3) washing scandium oxalate with pure water for 3 times, and calcining in a muffle furnace at the calcining temperature of 750 ℃ for 2 hours to obtain a scandium oxide product with the purity of 99.95%, wherein the recovery rate of scandium can reach more than 99.95%.
Example 2.
A method for recycling scandium from aluminum-scandium alloy target waste materials comprises the following steps: crushing the aluminum scandium target material waste with the content of 30% Sc-70% Al, adding pure water according to the solid-to-liquid ratio of 1:10, starting stirring, heating to 65 ℃, beginning to dropwise add analytically pure hydrochloric acid by using a constant-pressure funnel, stopping adding acid when the temperature is higher than 75 ℃, and obtaining acid leaching solution after complete reaction. Adding oxalic acid solution with the amount of 1.4 times of the stoichiometric ratio into the pickle liquor, reacting at 60 ℃ for 1h, carrying out suction filtration on the obtained precipitation system solution to obtain crude scandium oxalate, wherein the scandium precipitation rate is more than 99%, and the filtrate is used as aluminum-rich solution, and the scandium concentration is less than 150 ppm. And (2) washing scandium oxalate with pure water, and calcining in a muffle furnace at 750 ℃ for 2h to obtain a scandium oxide product with the purity of 99.98%, wherein the recovery rate of scandium can reach more than 99.95%.
Example 3.
A method for recycling scandium from aluminum-scandium alloy target waste materials comprises the following steps: crushing the aluminum scandium target material waste with the content of 30% Sc-70% Al, adding pure water according to the solid-to-liquid ratio of 1:12, starting stirring, heating to 55 ℃, beginning to dropwise add analytically pure hydrochloric acid by using a constant pressure funnel, stopping adding acid when the temperature is higher than 75 ℃, and obtaining acid leaching solution after complete reaction. Adding oxalic acid solution with the amount of 1.8 times of the stoichiometric ratio into the pickle liquor, reacting at 55 ℃ for 1.5h, carrying out suction filtration on the obtained precipitation system solution to obtain crude scandium oxalate, wherein the scandium precipitation rate is more than 99.5%, the filtrate is used as aluminum-rich solution, and the scandium concentration is less than 120 ppm. And (2) washing scandium oxalate with pure water, and calcining in a muffle furnace at 800 ℃ for 2h to obtain a scandium oxide product with the purity of 99.98%, wherein the recovery rate of scandium can reach more than 99.99%.
The invention has the beneficial effects that: by adopting the method, scandium is recovered from the aluminum-scandium alloy target material waste material, scandium metal in the aluminum-scandium alloy target material waste material can be efficiently and quickly recovered, the obtained scandium oxide can be used for preparing metal scandium at the front end of the aluminum-scandium alloy target material, and the problems of difficult back extraction, high cost and wastewater treatment in the process of extracting and recovering scandium are avoided. The process has the advantages of simple technical process, high recovery rate, large batch processing capacity, low cost, high product purity and the like.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (10)
1. A method for recycling scandium from aluminum-scandium alloy target waste materials is characterized by comprising the following steps: the method comprises the following steps:
s1 crushing: crushing the aluminum-scandium alloy target material waste to obtain a recovered raw material;
acid leaching of S2: leaching the recovered raw materials, pure water and acid according to a certain proportion to obtain scandium-containing pickle liquor;
s3 oxalic acid precipitation: adding the scandium-containing pickle liquor into an oxalic acid solution for precipitation, and washing the separated solid matter to obtain scandium oxalate;
s4 calcination: and calcining scandium oxalate to obtain high-purity scandium oxide.
2. The method of claim 1, wherein the scandium recovery step comprises: the mass fraction of aluminum in the aluminum-scandium alloy target material waste is 70-90%.
3. The method of claim 1, wherein the scandium recovery step comprises: in S2, recovering the raw material: pure water: the ratio of the acids is 1g to 10-15 ml.
4. The method of claim 3, wherein the scandium recovery step comprises: the acid comprises one of sulfuric acid, hydrochloric acid and nitric acid.
5. The method of claim 1, wherein the scandium recovery step comprises: the scandium concentration of the scandium-containing pickle liquor is controlled to be 5-20 g/L.
6. The method of claim 1, wherein the scandium recovery step comprises: the addition amount of the oxalic acid solution as the precipitant is 1-2 times of the stoichiometric ratio.
7. The method of claim 1, wherein the scandium recovery step comprises: the reaction temperature of oxalic acid precipitation is controlled to be 50-70 ℃.
8. The method of claim 1, wherein the scandium recovery step comprises: the calcining temperature of scandium oxalate is controlled to be 600-800 ℃.
9. The method of claim 1, wherein the scandium recovery step comprises: the calcination time of the scandium oxalate is controlled to be 2-4 h.
10. The method of claim 1, wherein the scandium recovery step comprises: the valuable metal in the aluminum-scandium alloy target scrap comprises at least one of scandium and aluminum.
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| CN202011468583.2A CN112708786A (en) | 2020-12-15 | 2020-12-15 | Method for recycling scandium from aluminum-scandium alloy target material waste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265554A (en) * | 2021-05-07 | 2021-08-17 | 先导薄膜材料（广东）有限公司 | Aluminum-scandium intermediate alloy and preparation method thereof |
| CN113373312A (en) * | 2021-06-10 | 2021-09-10 | 广东先导稀材股份有限公司 | Method for separating and recovering tantalum, scandium and aluminum |
| CN114538495A (en) * | 2022-01-05 | 2022-05-27 | 四川顺应动力电池材料有限公司 | Method for extracting high-purity scandium oxide |
| CN115305367A (en) * | 2022-09-15 | 2022-11-08 | 先导薄膜材料（广东）有限公司 | Method for recycling scandium oxide from scandium carbonate |
| CN115872436A (en) * | 2022-12-30 | 2023-03-31 | 河南荣佳钪钒科技有限公司 | Scandium fluoride wet preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113265554A (en) * | 2021-05-07 | 2021-08-17 | 先导薄膜材料（广东）有限公司 | Aluminum-scandium intermediate alloy and preparation method thereof |
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| CN113373312A (en) * | 2021-06-10 | 2021-09-10 | 广东先导稀材股份有限公司 | Method for separating and recovering tantalum, scandium and aluminum |
| CN114538495A (en) * | 2022-01-05 | 2022-05-27 | 四川顺应动力电池材料有限公司 | Method for extracting high-purity scandium oxide |
| CN115305367A (en) * | 2022-09-15 | 2022-11-08 | 先导薄膜材料（广东）有限公司 | Method for recycling scandium oxide from scandium carbonate |
| CN115872436A (en) * | 2022-12-30 | 2023-03-31 | 河南荣佳钪钒科技有限公司 | Scandium fluoride wet preparation method |
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Application publication date: 20210427 |