CN1827860A - Process and apparatus for producing Dy-Fe alloy by molten salt electrolysis method - Google Patents
Process and apparatus for producing Dy-Fe alloy by molten salt electrolysis method Download PDFInfo
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- CN1827860A CN1827860A CN 200510054067 CN200510054067A CN1827860A CN 1827860 A CN1827860 A CN 1827860A CN 200510054067 CN200510054067 CN 200510054067 CN 200510054067 A CN200510054067 A CN 200510054067A CN 1827860 A CN1827860 A CN 1827860A
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Abstract
The invention relates the dysprosium-iron alloy technology with fused salt electrolysis process and device, belonging to rare-earth products preparing field. The method comprises the following steps: at high temperature, dysprosium oxide melting at fluoride, dysprosium oxide beginning ionizing; at the condition of 95V/M direct current field, separating out Dy3+ on the surface of iron cathode, deacidizing Dy3+ to Dy, and alloying Dy and Fe to form Dy-Fe. O2- is oxygenated to O2 on the surface of graphite cathode, and it reacts with carbite to form CO2. The melting point of dysprosium-iron (20%Fe) is 1046Deg.C, and the melting point of Dy is 1407Deg.C, so the electrolyzation is carried out at 1050Deg.C. The invention has the advantages of low investment, low cost, simple technology, continuous production and low impurity content.
Description
One, technical field
The present invention relates to a kind of technology of producing Dy-Fe alloy by molten salt electrolysis method, belongs to the rare-earth products preparation field.
Two, background technology
The method of China's existing production dysprosium iron has fluorochemical vacuum calciothermy and oxide compound vacuum iron reduction-diffusion process.
Fluorochemical calciothermy production technique comparative maturity is the main method of producing dysprosium and dysprosium iron, but fluorochemical calciothermic reduction technology needs complicated vacuum apparatus and expensive crucible material, the production cost height because of needs fluorination process and reductive agent calcium; The fluorination process contaminate environment; Foreign matter content height such as the O in the product, Ca, F, W.
Oxide compound iron reduction-diffusion process production technique owing to oxygen level height in the product, be not easy to the reasons such as the difficult control of ratio of continuous production, dysprosium and iron, is difficult to apply;
Adopt electrolytic process can obtain the liquid metal dysprosium in theory, but because its electrolysis temperature (1450 ℃) that needs is higher, make the selection and the complicated operationization of electrolyzer.
In addition because present anode electrolytic cell structure is a column, thus complicated operation, energy consumption height, and be unfavorable for effective electrolysis of electrolyzer different depths making raw material Dy
2O
3Amass bottom deeply, reduce yield at electrolyzer.
Three, summary of the invention
The technical problem that the present invention solves is: reduce electrolysis temperature, make electrolysis can continue to carry out; Reduce the ionogen fusing point, improve flowability and stable, environmental protection and energy saving, but continuous production Dy-Fe alloy, production cost reduces significantly; And can make all effectively electrolysis of electrolyzer different depths, prevent that raw material from amassing the Processes and apparatus at a kind of producing Dy-Fe alloy by molten salt electrolysis method of bottom of electrolytic tank deeply.
The present invention is raw material with the dysprosium oxide, and it is 950-1050 ℃ fluorochemical (DyF that dysprosium oxide is added temperature
3, LiF) in the melt, the fusion of dysprosium oxide in melt, melting degree is 2～5%, ionization takes place in the dysprosium oxide of fusion immediately; Under the effect of DC electric field (95V/M), Dy
3+Separate out on the iron cathode surface, be reduced to Dy, Dy and Fe alloying form Dy-Fe; O
2-At the graphite cathode surface oxidation is O
2, be CO with the graphite reaction
2Enter air.Dysprosium iron (20%Fe) fusing point is 1046 ℃, far below 1407 ℃ of the fusing points of pure Dy, electrolysis is carried out about 1050 ℃;
In fused binary villiaumite system, produce Dy-Fe alloy with consumable pure iron catholyte dysprosium oxide.
Rare earth oxide is a dysprosium oxide.
Melt is a fluoride molten salt, and fluoride molten salt is DyF
3, LiF, wherein dysprosium fluoride accounts for 80-90%, lithium fluoride accounts for 10-20%.
Electrolysis cathode adopts pure iron.
Electrolysis direct current piezoelectric voltage 8-10V, electrolysis temperature 950-1050 ℃, electrolysis time 90 minutes.
A kind of equipment of producing Dy-Fe alloy by molten salt electrolysis method comprises shell, receptor, anode, negative electrode, plumbago crucible, interior protective shell, lagging material, and the anode shape that invests the plumbago crucible internal surface is a back taper.
Technology of the present invention has been filled up autonomous region's blank, has reached leading domestic, international most advanced level, and quality product reaches international like product level.
Current efficiency greater than 68%, the metal direct yield is greater than 92%
Quality product: TREM (85～77) ± 0.5%, Fe (15～23) ± 0.5%, C＜0.05%, O＜0.05%, Ca＜0.01%, W+Mo＜0.01%
It is negative electrode that the present invention selects pure iron for use, and electrolysate is the Dy-Fe alloy, greatly reduces electrolysis temperature, makes electrolysis can continue to carry out;
Select the binary electrolyte system for use, reduce the ionogen fusing point, improve flowability and stable.Show as in actual production process: Dy-Fe separates fully with ionogen, avoids being mingled with, ionogen physical and chemical performance long-term stability;
Adopt special anode construction, not only can simplify the operation, cut down the consumption of energy, and help all effectively electrolysis of electrolyzer different depths, prevent raw material Dy
2O
3Amass bottom deeply, improve yield at electrolyzer.
The present invention not only can reduce investment, reduce production costs, simplifies production technique; and large-scale production continuously; the foreign matter content of product is also very low; the dysprosium oxide that hot reducing method has been saved in the direct electrolysis of dysprosium oxide is fluoridized processing step, the environmental protection and energy saving for dysprosium fluoride, is an innovative production technique.
Four, description of drawings
Accompanying drawing 1 is two yuan of system phase diagrams of Dy-Fe alloy of the present invention;
Accompanying drawing 2 is a cell construction synoptic diagram of the present invention.
Five, embodiment
The present invention is to be raw material with the dysprosium oxide, and dysprosium fluoride, lithium fluoride binary system are ionogen, and dysprosium oxide is melted in fluorochemical (DyF
3, LiF) in the melt, the melting degree 2～5% of dysprosium oxide in melt utilizes consumable iron cathode electrolysis rare-earth oxidation dysprosium, obtains Dy-Fe alloy.
Electrolyzer passes through thorough drying, and meets graphite starting the arc heating in electrolyzer, DyF with making the arc machine
3With LiF by slowly adding the electrolyzer fusing after 90: 10 the mixed, when electrolytic solution reaches required liquid level, temperature in the time of 950-1050 ℃, DyO
3Add by the automatic charging equipment equal and quantitative, under the effect of DC electric field (95V/M), Dy
3+Separate out on the iron cathode surface, be reduced to Dy, Dy and Fe alloying form Dy-Fe.O
2-At the graphite cathode surface oxidation is O
2, be CO with the graphite reaction
2Enter air.
Take out the susceptor of iron cathode bottom after 90 minutes, the Dy-Fe alloy in the reverse graft receiver is in the mold ingot casting.
Claims (6)
1, producing Dy-Fe alloy by molten salt electrolysis method technology is characterized in that:
(1) being is raw material with the dysprosium oxide, when temperature is 950-1050 ℃, dysprosium oxide is added in the fluorochemical melt, and the melting degree of dysprosium oxide in melt is 2～5%, and ionization takes place the dysprosium oxide of fusion immediately:
(2) under the effect of DC electric field (95V/M), Dy
3+Separate out on the iron cathode surface, be reduced to Dy, Dy and Fe alloying form Dy-Fe, O
2-At the graphite cathode surface oxidation is O
2, be CO with the graphite reaction
2Enter air;
(3) fusing point of dysprosium iron: 20%Fe is 1046 ℃, is lower than 1407 ℃ of the fusing points of pure Dy, and electrolysis is being carried out below 1050 ℃.
2, producing Dy-Fe alloy by molten salt electrolysis method technology according to claim 1 is characterized in that: rare earth oxide is a dysprosium oxide.
3, producing Dy-Fe alloy by molten salt electrolysis method technology according to claim 1 is characterized in that: melt is a fluoride molten salt, and fluoride molten salt is DyF
3, LiF, wherein dysprosium fluoride accounts for 80-90%, lithium fluoride accounts for 10-20%.
4, producing Dy-Fe alloy by molten salt electrolysis method technology according to claim 1 is characterized in that: electrolysis cathode adopts pure iron.
5, producing Dy-Fe alloy by molten salt electrolysis method technology according to claim 1 is characterized in that: electrolysis direct current piezoelectric voltage 8-10V, electrolysis temperature 950-1050 ℃, electrolysis time 90 minutes.
6, a kind of equipment of producing Dy-Fe alloy by molten salt electrolysis method; comprise shell (1), receptor (2), anode (3), negative electrode (4), plumbago crucible (5), interior protective shell (6), lagging material (7), it is characterized in that: the anode (3) that invests plumbago crucible (5) internal surface is shaped as back taper.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200806B (en) * | 2006-12-13 | 2010-05-19 | 北京有色金属研究总院 | Method for preparing gadolinium-iron alloy by molten salt electrolysis |
| CN101629308B (en) * | 2009-04-29 | 2010-12-08 | 江苏江南铁合金有限公司 | Preparation method of Tb-Fe, Dy-Fe and Tb-Dy-Fe alloys employing electro-deoxidization |
| CN106636830A (en) * | 2016-12-16 | 2017-05-10 | 包头稀土研究院 | Yttrium-ferrous alloy and preparation method thereof |
| CN106757170A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | Lanthanum ferroalloy and preparation method thereof |
| CN106757171A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | Praseodymium ferroalloy and preparation method thereof |
| CN106834905A (en) * | 2016-12-16 | 2017-06-13 | 包头稀土研究院 | Rare earth ferroalloy and preparation method thereof |
| CN106835205A (en) * | 2016-12-16 | 2017-06-13 | 包头稀土研究院 | Praseodymium neodymium-iron alloy and preparation method thereof |
| CN108538563A (en) * | 2018-04-09 | 2018-09-14 | 赣州鑫磊稀土新材料股份有限公司 | A kind of sintered NdFeB crystal boundary bleeding agent painting method |
| CN108977855A (en) * | 2018-08-30 | 2018-12-11 | 李鹏 | A kind of preparation method of magnetic material |
| CN114941079A (en) * | 2022-05-24 | 2022-08-26 | 国瑞科创稀土功能材料(赣州)有限公司 | Method for removing oxide inclusion in Dy-Fe alloy |
-
2005
- 2005-02-28 CN CN 200510054067 patent/CN1827860A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200806B (en) * | 2006-12-13 | 2010-05-19 | 北京有色金属研究总院 | Method for preparing gadolinium-iron alloy by molten salt electrolysis |
| CN101629308B (en) * | 2009-04-29 | 2010-12-08 | 江苏江南铁合金有限公司 | Preparation method of Tb-Fe, Dy-Fe and Tb-Dy-Fe alloys employing electro-deoxidization |
| CN106636830A (en) * | 2016-12-16 | 2017-05-10 | 包头稀土研究院 | Yttrium-ferrous alloy and preparation method thereof |
| CN106757170A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | Lanthanum ferroalloy and preparation method thereof |
| CN106757171A (en) * | 2016-12-16 | 2017-05-31 | 包头稀土研究院 | Praseodymium ferroalloy and preparation method thereof |
| CN106834905A (en) * | 2016-12-16 | 2017-06-13 | 包头稀土研究院 | Rare earth ferroalloy and preparation method thereof |
| CN106835205A (en) * | 2016-12-16 | 2017-06-13 | 包头稀土研究院 | Praseodymium neodymium-iron alloy and preparation method thereof |
| CN108538563A (en) * | 2018-04-09 | 2018-09-14 | 赣州鑫磊稀土新材料股份有限公司 | A kind of sintered NdFeB crystal boundary bleeding agent painting method |
| CN108977855A (en) * | 2018-08-30 | 2018-12-11 | 李鹏 | A kind of preparation method of magnetic material |
| CN114941079A (en) * | 2022-05-24 | 2022-08-26 | 国瑞科创稀土功能材料(赣州)有限公司 | Method for removing oxide inclusion in Dy-Fe alloy |
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