CN102021343A - Method for separating and recovering scandium oxide from aluminum-scandium alloy smelting waste - Google Patents
Method for separating and recovering scandium oxide from aluminum-scandium alloy smelting waste Download PDFInfo
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- CN102021343A CN102021343A CN2010105058180A CN201010505818A CN102021343A CN 102021343 A CN102021343 A CN 102021343A CN 2010105058180 A CN2010105058180 A CN 2010105058180A CN 201010505818 A CN201010505818 A CN 201010505818A CN 102021343 A CN102021343 A CN 102021343A
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Abstract
The invention discloses a method for separating and recovering scandium oxide from aluminum-scandium alloy smelting waste. In the invention, aluminum-scandium alloy smelting waste is taken as a raw material, and high-purity scandium oxide is obtained through raw material pulverization, alkali transition, hydrochloric acid decomposition, oxalate sediment and calcination at intermediate temperature. In the invention, single-stage solvent is utilized for extraction. The invention has the advantages of simple technique process, little chemical material consumption, low recovery cost, good extraction and separation effect, little investment and more than 99.9 percent of product purity.
Description
Technical field
The present invention relates to a kind of rare earth metallurgy technology, particularly a kind ofly smelt Separation and Recovery method of scandium oxide the waste material from aluminum scandium alloy.
Technical background
China is the relatively abundanter country of scandium resource, and relevant with scandium is big as bauxite and phosphorite ore reserve, and scandium reserves wherein are about 290,000 tons according to estimates, account for 51% of all scandium ore deposit type total reservess, are the important mineral deposit and the main sources of China's scandium.The independent mineral wealth of scandium are few, and obtaining scandium on the general industry is when comprehensive treating process non-ferrous metal and rare metal ore, realize by recovery association scandium.
Scandium is typical dissipated metal element, and in the periodic table of elements, ordination number is 21, is the neighbour of aluminium, titanium, and its lattice parameter, physics, mechanical property more are bordering on aluminium, and yttrium and titanium are aluminium alloy ideal alloy elements.Add a spot of scandium in aluminium and aluminium alloy, remarkable refinement cast alloy crystal grain, improve the intensity and the toughness of aluminium alloy, and can significantly improve weldability, thermotolerance, corrosion stability, thermostability and the anti-neutron radiation of aluminium alloy, therefore, aluminum scandium alloy is considered to high-performance aluminium alloy structured material such as space flight and aviation of new generation, naval vessel, nuclear energy, defence and military leading-edge field.
Fused salt electrolysis process, thermit reduction and magnesium reduction process are generally adopted in the preparation of scandium bearing master alloy, and any smelting process no matter exists all that the resource that contains the scandium metallurgical slag reclaims, recycle.
Summary of the invention
The object of the present invention is to provide and a kind ofly smelt Separation and Recovery method of scandium oxide the waste material, reclaim resource scarcity and expensive Scium trioxide, turn waste into wealth, realize the resource circulation utilization with lower production cost, high yield, high purity from aluminum scandium alloy.
Technical scheme of the present invention is: with rare earth metal fused salt electrolysis waste material is raw material, carries out according to the following steps:
Smelting waste material with aluminum scandium alloy is raw material, carries out according to the following steps:
1. raw material pulverizing: raw material filters out foreign material and metal through fragmentation, carries out fine crushing again, is ground to the 50-200 order;
2. alkali makes the transition: powder and alkali that 1. above-mentioned steps is obtained are 1 by weight: the 0.5-1.5 thorough mixing is even, puts into reaction transition of container intensification carrying out alkali, generates scandium hydroxide; The temperature that alkali makes the transition is 100-600 ℃, and the reaction times is 1-5 hour;
3. hydrochloric acid decomposes: put into reaction vessel after the scandium hydroxide that 2. step is obtained washs, add 30% technical hydrochloric acid and carry out decomposition reaction, purify Scium trichloride;
4. single-stage extraction is purified: with the 3. Scium trichloride solution of gained of step, enter the specially designed single-stage extraction groove of 500L and adopt the colour band hierarchical control technology of independent research.Basic technology parameter: 1.5mol/LP507, compare 1: 2～5, extraction mixing-time 10min, extraction settling time 15min, washing lotion be after 0.6～1.0NHCL. separates through three counter-current extractions, with Sc3+ and Fe2+, AL3+, Re3+ separates, and obtains Scium trichloride solution with 4mol/LHCl back extraction organic phase.Reached the separating effect of conventional cascade extraction.
5. producing of High-purity Sc Oxide: with step 4. the Scium trichloride solution of gained be heated to more than 70 ℃, add 60-70 ℃, 20% oxalic acid solution reacts, the oxalic acid scandium that obtains is through washing, horse arc stove is done, put into to suction filtration, 800 ℃ of down insulations 2 hours, make purity greater than 99.9% Scium trioxide.
The invention has the beneficial effects as follows that the present invention adopts the single-stage solvent extraction, technical process is simple, and it is few to consume chemical materials, and cost recovery is low, and extracting and separating is respond well, invests lowly, and product purity is greater than 99.9%.
Embodiment
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Below in conjunction with drawings and Examples the present invention is done and to describe in further detail.
With certain the 200kg AL-Sc of unit alloy smelting waste material is example, and analysis of components is as follows:
| Title | Sc 2O 3 | AL | Na | K | F - |
| wt％ | 2.5 | 55.5 | 15.2 | 8.8 | 22 |
1. raw material pulverizing: raw material filters out foreign material or metal through fragmentation, carries out fine crushing again, is ground to negative 20-200 order;
2. alkali makes the transition: powder and solid caustic soda that 1. above-mentioned steps is obtained are 1 by weight: the 0.5-1.5 thorough mixing is even, puts into the steel basin, the reaction that in electric furnace, makes the transition (temperature 100-600 ℃, reaction times 1-5 hour), and the gained scandium hydroxide washs;
3. hydrochloric acid decomposes: washing back scandium hydroxide is put into 5m
3In the reactor, slowly add technical hydrochloric acid and carry out the acid decomposition, obtain Scium trichloride solution after removal of impurities, the filtration.Slag is 30kg heavily, and scandium content is 0.7% in the acid non-soluble substance, and sour rate of decomposition is greater than 95%;
4. single-stage extraction is purified: with the 3. Scium trichloride solution of gained of step, enter 500L single-stage solvent extraction groove, extraction agent is selected the P507 of concentration 1.5mol/L for use, control compares 1: 2-5, extraction mixing-time 10min, extraction settling time 15min, after three counter-current extractions separation, with Sc3+ and Fe2+, AL3+, Re3+ separates, and obtains Scium trichloride solution with 4mol/L HCl back extraction organic phase;
5. producing of High-purity Sc Oxide:: with the 4. Scium trichloride solution of gained of step, be heated to more than 70 ℃, add 60-70 ℃, 20% oxalic acid solution and carry out precipitin reaction, the calcination of horse arc stove is done, put into to the oxalic acid scandium that obtains through washing, suction filtration, be incubated 2 hours down at 800 ℃, obtain the 4.56kg Scium trioxide.
The total yield of scandium reaches more than 91%, and analysis list is as follows:
| TREO | 98.09 |
| La 2O 3 | 0.0010 |
| CeO 2 | 0.0017 |
| Pr 6o 11 | 0.0010 |
| Nd 2O 3 | 0.0010 |
| Sm 2O 3 | 0.0010 |
| Eu 2O 3 | 0.0010 |
| Gd 2O 3 | 0.0010 |
| Tb 4O 7 | 0.0010 |
| Dy 2O 3 | 0.0012 |
| Ho 2O 3 | 0.0010 |
| Er 2O 3 | 0.0010 |
| Tm 2O 3 | 0.0010 |
| Yb 2O 3 | 0.0014 |
| Lu 2O 3 | 0.0010 |
| Y 2O 3 | 0.0048 |
| Sc 2O 3 | Matrix |
Claims (3)
1. a Separation and Recovery method of scandium oxide from aluminum scandium alloy smelting waste material is characterized in that with aluminum scandium alloy smelting waste material be raw material, carries out according to the following steps:
1. raw material pulverizing: raw material filters out foreign material and metal through fragmentation, carries out fine crushing again, is ground to the 50-200 order;
2. alkali makes the transition: powder and alkali thorough mixing that 1. above-mentioned steps obtains is even, put into reaction transition of container intensification carrying out alkali, and generate scandium hydroxide;
3. hydrochloric acid decomposes: put into reaction vessel after the scandium hydroxide that 2. step is obtained washs, add 30% technical hydrochloric acid and carry out decomposition reaction, purify Scium trichloride;
4. single-stage extraction is purified: with the 3. Scium trichloride solution of gained of step, enter 500L single-stage solvent extraction groove, the basic technology parameter: extraction agent be 1.5mol/L P507, compare 1: 2-5, extraction mixing-time 10min, extraction settling time 15min, washing lotion are the HCL of 0.6-1.0N; After separating through three counter-current extractions, obtain Scium trichloride solution with the HCl back extraction organic phase of 4mol/L;
5. producing of High-purity Sc Oxide: with step 4. the Scium trichloride solution of gained be heated to more than 70 ℃, add 60-70 ℃, 20% oxalic acid solution reacts, the oxalic acid scandium that obtains is through washing, horse arc stove is done, put into to suction filtration, 800 ℃ of down insulations 2 hours, make purity greater than 99.9% Scium trioxide.
2. according to claim 1ly a kind ofly smelt Separation and Recovery method of scandium oxide the waste material from aluminum scandium alloy, it is characterized in that: the powder that 1. step obtains and the weight ratio of solid caustic soda are 1: 0.5-1.5.
3. according to claim 1ly a kind ofly smelt Separation and Recovery method of scandium oxide the waste material from aluminum scandium alloy, it is characterized in that: the temperature of alkali transition is 100-600 ℃, and the reaction times is 1-5 hour.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605199A (en) * | 2012-04-17 | 2012-07-25 | 湖南东方钪业股份有限公司 | Method for recovering scandium from zirconium oxychloride acid pickle, and extracting agent for method |
| 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 |
| CN103103361A (en) * | 2013-02-28 | 2013-05-15 | 包头稀土研究院 | Method for preparing rare earth oxide from rare earth polishing powder waste |
| CN103215439A (en) * | 2013-04-16 | 2013-07-24 | 内蒙古科技大学 | Method for extracting scandium from scandium enrichment |
| CN103361486A (en) * | 2013-07-18 | 2013-10-23 | 攀枝花市精研科技有限公司 | Method for extracting high purity scandium oxide and titanium from waste acid solution containing scandium and titanium |
| CN103361488A (en) * | 2013-07-31 | 2013-10-23 | 湖南永利化工股份有限公司 | Recycling method of scandium in titanium white waste water |
| CN104232945A (en) * | 2013-06-08 | 2014-12-24 | 淄博广通化工有限责任公司 | Method for preparing high pure scandium oxide from hydrochloric acid mother liquid for producing zirconium oxychloride |
| 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 |
| CN104726718A (en) * | 2015-04-07 | 2015-06-24 | 杨秋良 | Method for producing high-purity discandium trioxide from alkali fusion separated anode slime/silver separating residue by use of total wet process |
| EP3078757A4 (en) * | 2014-01-27 | 2016-11-16 | Sumitomo Metal Mining Co | Scandium chloride and scandium chloride production method |
| JP2018035391A (en) * | 2016-08-30 | 2018-03-08 | 住友金属鉱山株式会社 | Recovery method of scandium |
| CN110470140A (en) * | 2019-08-30 | 2019-11-19 | 王一浩 | A kind of aluminium-scandium alloy smelting waste separation scandium oxide recovery furnace |
| CN112708786A (en) * | 2020-12-15 | 2021-04-27 | 广东先导稀材股份有限公司 | Method for recycling scandium from aluminum-scandium alloy target material waste |
| CN115747533A (en) * | 2022-11-15 | 2023-03-07 | 广东先导稀材股份有限公司 | Method for recovering scandium from scandium-containing salt slag |
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Cited By (17)
| 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 |
| CN102605199A (en) * | 2012-04-17 | 2012-07-25 | 湖南东方钪业股份有限公司 | Method for recovering scandium from zirconium oxychloride acid pickle, and extracting agent for method |
| CN103103361B (en) * | 2013-02-28 | 2014-11-26 | 包头稀土研究院 | Method for preparing rare earth oxide from rare earth polishing powder waste |
| CN103103361A (en) * | 2013-02-28 | 2013-05-15 | 包头稀土研究院 | Method for preparing rare earth oxide from rare earth polishing powder waste |
| CN103215439A (en) * | 2013-04-16 | 2013-07-24 | 内蒙古科技大学 | Method for extracting scandium from scandium enrichment |
| CN104232945A (en) * | 2013-06-08 | 2014-12-24 | 淄博广通化工有限责任公司 | Method for preparing high pure scandium oxide from hydrochloric acid mother liquid for producing zirconium oxychloride |
| CN103361486A (en) * | 2013-07-18 | 2013-10-23 | 攀枝花市精研科技有限公司 | Method for extracting high purity scandium oxide and titanium from waste acid solution containing scandium and titanium |
| CN103361486B (en) * | 2013-07-18 | 2014-10-29 | 攀枝花市精研科技有限公司 | Method for extracting high purity scandium oxide and titanium from waste acid solution containing scandium and titanium |
| CN103361488A (en) * | 2013-07-31 | 2013-10-23 | 湖南永利化工股份有限公司 | Recycling method of scandium in titanium white waste water |
| 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 |
| EP3078757A4 (en) * | 2014-01-27 | 2016-11-16 | Sumitomo Metal Mining Co | Scandium chloride and scandium chloride production method |
| CN104726718A (en) * | 2015-04-07 | 2015-06-24 | 杨秋良 | Method for producing high-purity discandium trioxide from alkali fusion separated anode slime/silver separating residue by use of total wet process |
| JP2018035391A (en) * | 2016-08-30 | 2018-03-08 | 住友金属鉱山株式会社 | Recovery method of scandium |
| CN109563566A (en) * | 2016-08-30 | 2019-04-02 | 住友金属矿山株式会社 | The recovery method of scandium |
| CN110470140A (en) * | 2019-08-30 | 2019-11-19 | 王一浩 | A kind of aluminium-scandium alloy smelting waste separation scandium oxide recovery furnace |
| CN112708786A (en) * | 2020-12-15 | 2021-04-27 | 广东先导稀材股份有限公司 | Method for recycling scandium from aluminum-scandium alloy target material waste |
| CN115747533A (en) * | 2022-11-15 | 2023-03-07 | 广东先导稀材股份有限公司 | Method for recovering scandium from scandium-containing salt slag |
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Application publication date: 20110420 |