CN1081240C - Process for producing metal dysprosium - Google Patents
Process for producing metal dysprosium Download PDFInfo
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- CN1081240C CN1081240C CN99108163A CN99108163A CN1081240C CN 1081240 C CN1081240 C CN 1081240C CN 99108163 A CN99108163 A CN 99108163A CN 99108163 A CN99108163 A CN 99108163A CN 1081240 C CN1081240 C CN 1081240C
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- metal
- dysprosium
- dym
- alloy
- fluoride
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Abstract
The present invention relates to the field of metal materials, particularly to the field of new and high materials. In the existing the production technology of metal dysprosium, dysprosium fluoride is reduced by calcium to obtain coarse dysprosium or dysprosium alloys, and then, the metal dysprosium is obtained by distillation. The technology has the disadvantages of hard requirement, high consumption of raw and auxiliary materials and high cost. The present invention uses fluoride and lithium fluoride as molten salts, DyM alloys are prepared by the co-electrolysis of dysprosium oxide and compounds of M, and the metal Dy and the metal M are obtained by separating the DyM alloys in a vacuum. The present invention has the advantages of unrestricted technological condition, no slag formation in processes, low material consumption and low cost, and the raw materials and the auxiliary materials are sufficiently utilized and recovered.
Description
The present invention relates to metal material field, particularly relate to high-performance Ne-Fe-B permanent-magnet material, magnetic cooling material, rare earth ultra-magnetostriction material, giant magnetic resistance, rare earth microwave material etc.
At present, calciothermic reduction---vacuum distilling technology is adopted in the metal dysprosium preparation, is reductive agent with calcium, and anhydrous dysprosium fluoride is starting material, and at first reduction makes calcic higher thick dysprosium or disprosium alloy, and the vacuum distilling deliming obtains the metal dysprosium product then.Though traditional technology is simple and easy to do, starting material preparation work is required harshness, the corrosion resistance nature of used device in the production process is had relatively high expectations, and output is little the cost height.
The object of the present invention is to provide a kind of production metal dysprosium novel process, thereby overcome the deficiency of traditional technology, reduce the preparation cost of metal dysprosium conscientiously.
Technical scheme of the present invention is to be fused salt with fluorochemical and lithium fluoride, make electrolyzer and anode with graphite, continue the mixture of the compound of adding dysprosium oxide and element M, carry out the common-battery of the compound of dysprosium oxide and M under the low temperature and separate, obtain the DyM alloy, obtain metal dysprosium and metal M by vacuum separation.This technology fluorochemical consist of DyF
3/ MFn=(0-100%)/(0-100%), the fused salt proportioning is lithium fluoride≤30%, 70%≤fluorochemical, the compound that consists of dysprosium oxide/M of mixture=(40-90%)/(10-60%), it is 1000 ± 200 ℃ that common-battery is separated temperature, and M is a metallic element, under common-battery is separated operational temperature conditions, M can form liquid alloy with Dy, and DyM alloy vacuum separation in 1200-1700 ℃ of scope obtains metal dysprosium and metal M.
The embodiment of the invention:
1, starting material are prepared:
Fused salt is pressed LaF
3The preparation of/LiF=83/17 ratio, mixture is pressed Dy
2O
3/ La
2O
3=70/30 preparation.
2, fused salt electrolysis:
In the 2000A electrolyzer, add the fused salt of being prepared in 1, the groove temperature control is made as 960 ℃-1040 ℃, adds mixture and carries out electrolysis, and electrolysis is tapping casting about 40 minutes, obtains the LaDy alloy after peeling off fused salt.
3, vacuum separation:
The LaDy alloy is placed tungsten crucible in the 10Kg vacuum intermediate frequency furnace, in 1200-1600 ℃ of scope, under the 1.33Pa air pressure, distilled 8 hours, Dy overflows with steam, condenses behind the chance condenser, obtains the Dy metal, and La still stays in tungsten crucible.Metal dysprosium, lanthanoid metal composition analysis such as following table:
| The composition name of product | RE(％) | Partition of rare earth element (%) | Non-rare earth (%) | ||||||||||
| La | Dy | All the other | Fe | Si | Al | Mg | Ca | W+Mo | O | N | S | ||
| Lanthanoid metal | 98.90 | 97.30 | 2.70 | All＜0.03 | 0.21 | 0.005 | 0.14 | / | / | 0.045 | 0.004 | ＜0.01 | ＜0.01 |
| Metal dysprosium | 99.53 | 0.34 | 99.64 | All＜0.03 | 0.04 | 0.005 | 0.003 | / | 0.005 | 0.007 | 0.009 | ＜0.01 | ＜0.01 |
Advantage of the present invention:
Replace calcium reduction route with common-battery solution method and produce disprosium alloy, operating temperature low (1000 ± 200 ℃) during the common-battery solution is produced and is easy to serialization; The fluoride that adopts in the production process is easy to preparation, and oxide is easily taken care of, and does not relate to the extremely strong metallic reducing agent of activity in addition, namely produces used raw and auxiliary material and easily prepares, preserves, and operating condition control is more loose; Obtain metal dysprosium and another metal product after the vacuum separation; Whole technical process realizes that without scorification all raw and auxiliary materials are all fully reclaimed, and material consumption is corresponding lower; Constant product quality, production and processing is with low cost.
Claims (3)
1, a kind of production metal dysprosium novel process comprises that fluoride molten salt system low temperature common-battery separates Dy
2O
3Make the DyM alloy with the compound of M, DyM alloy vacuum separation obtains operations such as metal dysprosium and metal M, and it is characterized in that: with fluorochemical and lithium fluoride is fused salt, fluorochemical consist of DyF
3/ MFn=(0-100%)/(0-100%), the fused salt proportioning is lithium fluoride≤30%, 70%≤fluorochemical; The compound that consists of dysprosium oxide/M of mixture=(40-90%)/(10-60%).
2, production metal dysprosium novel process according to claim 1 is characterized in that it is 1000 ± 200 ℃ that common-battery is separated service temperature.
3, according to claim 1,2 described production metal dysprosium novel procesies, it is characterized in that: under common-battery was separated operational temperature conditions, metal M and Dy formed liquid alloy, and the DyM alloy is under 1200～1700 ℃ of high temperature, and vacuum separation obtains metal Dy and metal M.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99108163A CN1081240C (en) | 1999-06-09 | 1999-06-09 | Process for producing metal dysprosium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99108163A CN1081240C (en) | 1999-06-09 | 1999-06-09 | Process for producing metal dysprosium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1243168A CN1243168A (en) | 2000-02-02 |
| CN1081240C true CN1081240C (en) | 2002-03-20 |
Family
ID=5273173
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99108163A Expired - Fee Related CN1081240C (en) | 1999-06-09 | 1999-06-09 | Process for producing metal dysprosium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1081240C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046820B (en) * | 2008-03-26 | 2013-07-10 | 财团法人生产技术研究奖励会 | Method and apparatus for collection of rare earth element |
| CN101550494B (en) * | 2008-03-31 | 2011-06-08 | 北京有色金属研究总院 | Method for preparing rare earth metals |
| JP6179699B1 (en) | 2016-03-28 | 2017-08-16 | 日立金属株式会社 | Method for separating both from an alloy containing Dy and Tb |
| WO2017170347A1 (en) * | 2016-03-28 | 2017-10-05 | 日立金属株式会社 | METHOD FOR SEPARATING Dy AND Tb FROM ALLOY CONTAINING BOTH |
| CN115821075A (en) * | 2022-11-23 | 2023-03-21 | 昆明理工大学 | Method for recovering rare earth metal in samarium cobalt permanent magnet waste |
-
1999
- 1999-06-09 CN CN99108163A patent/CN1081240C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1243168A (en) | 2000-02-02 |
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