CN1772963A - Common-battery deposition producing method for Mg La Pr Ce intermediate alloy - Google Patents
Common-battery deposition producing method for Mg La Pr Ce intermediate alloy Download PDFInfo
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- CN1772963A CN1772963A CN 200510017209 CN200510017209A CN1772963A CN 1772963 A CN1772963 A CN 1772963A CN 200510017209 CN200510017209 CN 200510017209 CN 200510017209 A CN200510017209 A CN 200510017209A CN 1772963 A CN1772963 A CN 1772963A
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Abstract
The present invention belongs to a coelectrodeposition prepartion method of magnesium-lanthanum, praseodymium and cerium intermediate alloy. In the electrolytic furnace said invention uses potassium chloride, magnesium chloride and lanthanum-praseodymium-cerium chloride as electrolyte, its cathodic current density is 10-30 A/ sq.cm, and its temperature is 700-900 deg.C, so that said invention can utilize the coelectrodeposition process to prepare the invented magnesium-lanthanum-praseodymium-cerium intermediate alloy.
Description
Technical field
The invention belongs to the coelectrodeposition preparation method of magnesium-lanthanum praseodymium cerium master alloy, belong to the fused salt electrolysis metallurgical technology field.
Background technology
Magnesium-rare earth intermediate alloy is the basic raw material that the advanced novel corrosion resistant high temperature of preparation is used magnesium alloy.Preparation magnesium-rare earth intermediate alloy mainly contains following three kinds of methods, and the one, to the method for mixing, the 2nd, magnesium reduction process, the 3rd, come-up liquid cathode electrolytic process.These three kinds of methods respectively have problem: the method for mixing is difficult to avoid the alloying constituent segregation, because magnesium and most rare earth metal differ greatly on proportion and fusing point, rare earth can not be distributed in the magnesium well; Magnesium reduction process batch production cost height; Come-up liquid cathode electrolytic process product is scattered in electrolyzer upper, middle and lower each several part, bad collection.No matter which kind of method all must adopt MAGNESIUM METAL; What have also will make rare earth metal earlier.
Summary of the invention
The present invention provides the preparation method of magnesium-lanthanum praseodymium cerium master alloy.The invention reside in without magnesium and rare earth metal, only with the compound of rare earth and magnesium as raw material, allow the ion of rare earth and magnesium coelectrodeposition and directly produce the magnesium rare earth intermediate alloy on negative electrode.Its purpose is to provide a kind of industrialized novel process of producing magnesium-lpc rare-earth mixture master alloy that is easy to.
Technology of preparing scheme of the present invention is: used raw material is the commercially available crystallization material that extracts remaining mishmetal behind neodymium, cerium, the praseodymium from common mixed light rare earth, dewaters in vacuum drying oven, and the water-content after the dehydration is controlled at 15～25wt%; Magnesium chloride content of water after dewatering is controlled at 2～8wt%.
In electrolytic furnace, with the plumbago crucible is anode, molybdenum bar is a negative electrode, in plumbago crucible, add magnesium chloride, the lanthanum praseodymium cerium rare earth chloride of dehydration, Repone K ionogen through dehydration, they are 5 by the quality proportioning: (30-40): (55-65), at electrolysis temperature is 700-900 ℃, and cathode current density is 10-30A/cm
2Condition under, prepare magnesium-lanthanum praseodymium cerium master alloy.Its content is 24-65%.Current efficiency 60-85%, the direct yield of magnesium and rare earth reaches 80-95% and 80-93% respectively.
The invention provides a kind of economical rationality, rare earth-magnesium master alloy preparation method that cost performance is higher.The invention reside in without magnesium and rare earth metal, only the compound of using rare earth and magnesium is saved resource as raw material.Magnesium-the rare earth intermediate alloy of method preparation of the present invention is the basic raw material that the advanced novel corrosion resistant high temperature of preparation is used magnesium alloy.
Embodiment
Embodiment one:
In electrolytic furnace, be anode with the plumbago crucible, molybdenum bar is a negative electrode, adding commercially available industrial Repone K, the lanthanum praseodymium cerium mischmetal muriate of not exclusively dehydration and the magnesium chloride that has dewatered in plumbago crucible is ionogen.Magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, are 700 ℃ at electrolysis temperature, cathode current density 10A/cm
2, interpole gap is to prepare under the condition of 8cm that content of rare earth is 56.4%, current efficiency is 73%, the direct yield of rare earth and magnesium reaches 92% and 94%.
Embodiment two:
In electrolytic furnace, be anode with the plumbago crucible, molybdenum bar is a negative electrode, adding commercially available industrial Repone K, the lanthanum praseodymium cerium mischmetal muriate of not exclusively dehydration and the magnesium chloride that has dewatered in plumbago crucible is ionogen.Magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 40: 55 ratio preparation in the quality proportioning, are 800 ℃ at electrolysis temperature, cathode current density 20A/cm
2, interpole gap is to prepare under the condition of 4cm that content of rare earth is 24%, current efficiency is 60%, the direct yield of rare earth and magnesium reaches 92% and 95%.
Embodiment three:
In electrolytic furnace, be anode with the plumbago crucible, molybdenum bar is a negative electrode, adding commercially available industrial Repone K, the lanthanum praseodymium cerium mischmetal muriate of not exclusively dehydration and the magnesium chloride that has dewatered in plumbago crucible is ionogen.Magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, are 900 ℃ at electrolysis temperature, cathode current density 30A/cm
2, interpole gap is to prepare under the condition of 8cm that content of rare earth is 65%, current efficiency is 75%, the direct yield of rare earth and magnesium reaches 80% and 80%.
Embodiment four:
In electrolytic furnace, be anode with the plumbago crucible, molybdenum bar is a negative electrode, adding commercially available industrial Repone K, the lanthanum praseodymium cerium mischmetal muriate of not exclusively dehydration and the magnesium chloride that has dewatered in plumbago crucible is ionogen.Magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, are 800 ℃ at electrolysis temperature, cathode current density 15A/cm
2, interpole gap is to prepare under the condition of 6cm that content of rare earth is 38%, current efficiency is 76%, the direct yield of rare earth and magnesium reaches 89% and 93%.
Embodiment five:
In electrolytic furnace, be anode with the plumbago crucible, molybdenum bar is a negative electrode, adding commercially available industrial Repone K, the lanthanum praseodymium cerium mischmetal muriate of not exclusively dehydration and the magnesium chloride that has dewatered in plumbago crucible is ionogen.Magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, are 780 ℃ at electrolysis temperature, cathode current density 15A/cm
2, interpole gap is to prepare under the condition of 6cm that content of rare earth is 53%, current efficiency is 83%, the direct yield of rare earth and magnesium reaches 88% and 95%.
Embodiment six:
In electrolytic furnace, be anode with the plumbago crucible, molybdenum bar is a negative electrode, adding commercially available industrial Repone K, the lanthanum praseodymium cerium mischmetal muriate of not exclusively dehydration and the magnesium chloride that has dewatered in plumbago crucible is ionogen.Magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 40: 55 ratio preparation in the quality proportioning, are 780 ℃ at electrolysis temperature, cathode current density 15A/cm
2, interpole gap is to prepare under the condition of 6cm that content of rare earth is 60%, current efficiency is 80%, the direct yield of rare earth and magnesium reaches 90% and 92%.
Claims (9)
1, a kind of coelectrodeposition preparation method of magnesium-lanthanum-praseodymium-cerium master alloy, it is characterized in that: in electrolytic furnace, with the plumbago crucible is anode, molybdenum bar is a negative electrode, in plumbago crucible, add magnesium chloride, the lanthanum praseodymium cerium rare earth chloride of dehydration, Repone K ionogen through dehydration, they are 5 by the quality proportioning: (30-40): (55-65), be 700-900 ℃ at electrolysis temperature, cathode current density is 10-30A/cm
2Condition under, prepare the magnesium-lanthanum-praseodymium-cerium master alloy.
2, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1, it is characterized in that: said Lanthanum trichloride praseodymium cerium mischmetal is the commercially available crystallization material of residue rare earth behind extraction neodymium, cerium, the praseodymium, through dehydration, the content of water is 15～25wt%; Magnesium chloride is through dehydration, and the content of water is 2～8wt%.
3, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, electrolysis temperature is 700 ℃, cathode current density 10A/cm
2
4, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 40: 55 ratio preparation in the quality proportioning, at electrolysis temperature is 800 ℃, cathode current density 20A/cm
2
5, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, at electrolysis temperature is 900 ℃, cathode current density 30A/cm
2？？
6, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, at electrolysis temperature is 900 ℃, cathode current density 30A/cm
2
7, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, at electrolysis temperature is 800 ℃, cathode current density 15A/cm
2
8, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 30: 65 ratio preparation in the quality proportioning, at electrolysis temperature is 780 ℃, cathode current density 15A/cm
2
9, the coelectrodeposition preparation method of a kind of magnesium-lanthanum-praseodymium-cerium master alloy as claimed in claim 1 or 2, it is characterized in that: magnesium chloride, lanthanum praseodymium cerium rare earth chloride, Repone K are the ionogen of 5: 40: 55 ratio preparation in the quality proportioning, at electrolysis temperature is 780 ℃, cathode current density 15A/cm
2
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302594B (en) * | 2008-06-04 | 2010-06-02 | 哈尔滨工程大学 | Mg-Li-Ce-La alloy and fused salt electrolysis preparation thereof |
| CN102220607A (en) * | 2011-05-25 | 2011-10-19 | 中国科学院青海盐湖研究所 | Molten salt electrolyte composition for preparing magnesium-rare earth alloy by using water-containing chloride to electrolyze |
| CN102330118A (en) * | 2011-03-03 | 2012-01-25 | 华东理工大学 | Method for preparing Mg-Sr alloy through molten salt electrolytic codeposition |
| CN101724769B (en) * | 2008-10-13 | 2012-03-28 | 北京有色金属研究总院 | Rare earth aluminum alloy, and method and device for preparing same |
| CN101767594B (en) * | 2010-01-22 | 2012-12-05 | 大连交通大学 | Magnesium alloy ventilation window of railway coach and manufacturing process thereof |
| CN103556023A (en) * | 2013-11-14 | 2014-02-05 | 扬州宏福铝业有限公司 | Lanthanum cerium-magnesium intermediate alloy and production method thereof |
| CN103590073A (en) * | 2013-11-14 | 2014-02-19 | 扬州宏福铝业有限公司 | Method for preparing mixed intermediate alloy of magnesium and light rare earth with double-cathode method |
| CN107630233A (en) * | 2017-10-20 | 2018-01-26 | 安吉绿金金属材料有限公司 | A kind of method using rare earth-iron-boron Electrowinning rare earth metal |
-
2005
- 2005-10-21 CN CN 200510017209 patent/CN1772963A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302594B (en) * | 2008-06-04 | 2010-06-02 | 哈尔滨工程大学 | Mg-Li-Ce-La alloy and fused salt electrolysis preparation thereof |
| CN101724769B (en) * | 2008-10-13 | 2012-03-28 | 北京有色金属研究总院 | Rare earth aluminum alloy, and method and device for preparing same |
| CN101767594B (en) * | 2010-01-22 | 2012-12-05 | 大连交通大学 | Magnesium alloy ventilation window of railway coach and manufacturing process thereof |
| CN102330118A (en) * | 2011-03-03 | 2012-01-25 | 华东理工大学 | Method for preparing Mg-Sr alloy through molten salt electrolytic codeposition |
| CN102330118B (en) * | 2011-03-03 | 2014-08-27 | 华东理工大学 | Method for preparing Mg-Sr alloy through molten salt electrolytic codeposition |
| CN102220607A (en) * | 2011-05-25 | 2011-10-19 | 中国科学院青海盐湖研究所 | Molten salt electrolyte composition for preparing magnesium-rare earth alloy by using water-containing chloride to electrolyze |
| CN103556023A (en) * | 2013-11-14 | 2014-02-05 | 扬州宏福铝业有限公司 | Lanthanum cerium-magnesium intermediate alloy and production method thereof |
| CN103590073A (en) * | 2013-11-14 | 2014-02-19 | 扬州宏福铝业有限公司 | Method for preparing mixed intermediate alloy of magnesium and light rare earth with double-cathode method |
| CN107630233A (en) * | 2017-10-20 | 2018-01-26 | 安吉绿金金属材料有限公司 | A kind of method using rare earth-iron-boron Electrowinning rare earth metal |
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