CN1188162A - Rare earth molten salt electrolytic ceramic anode and preparation method thereof - Google Patents
Rare earth molten salt electrolytic ceramic anode and preparation method thereof Download PDFInfo
- Publication number
- CN1188162A CN1188162A CN97121917A CN97121917A CN1188162A CN 1188162 A CN1188162 A CN 1188162A CN 97121917 A CN97121917 A CN 97121917A CN 97121917 A CN97121917 A CN 97121917A CN 1188162 A CN1188162 A CN 1188162A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- anode
- preparation
- salt electrolysis
- ceramic anode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 28
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 28
- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 150000003839 salts Chemical class 0.000 title abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 24
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 9
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 8
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 12
- 229960004643 cupric oxide Drugs 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052799 carbon Inorganic materials 0.000 abstract description 12
- 239000010405 anode material Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000005751 Copper oxide Substances 0.000 abstract 1
- 229910000431 copper oxide Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 description 16
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
Landscapes
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
A ceramic anode for rare earth molten salt electrolysis and a preparation method thereof relate to an anode material for rare earth molten salt electrolysis. The material is characterized by comprising 60-84% of neodymium oxide, 1-20% of cerium oxide and 15-20% of copper oxide. When in preparation, firstly mixed uniformly mixed neodymium oxide, cerium oxide and copper oxide powder is prepared, then isostatic pressing is carried out to prepare a blank, and finally sintering is carried out. The ceramic anode of the invention has excellent performance and high-temperature conductivity, does not bring carbon impurities to products, and is an ideal substitute for the anode for rare earth molten salt electrolysis.
Description
A kind of rare earth molten-salt electrolysis relates to a kind of anode material that uses and anodic preparation method thereof with ceramic anode and preparation method thereof in the rare earth molten-salt electrolysis process.
The preparation of rare earth metal mainly contains two kinds of methods, i.e. fused salt electrolysis process and metallothermics.Fused salt electrolysis process has simple, the use equipment characteristics few, with short production cycle of technology, has obtained general application in China rare metal factory.At present, extensively adopting graphite in the fused salt electrolysis process is electrode materials.Because graphite has good conduction, heat conduction, high temperature resistant, acid and alkali-resistance erosion performance, and extensively be used for the smelting of rare earth metal as electrode materials.But because graphite oxidized easily and corrosion under the high-temperature electrolysis condition, making has higher carbon content in the metal that makes, up to 500ppm.Carbon content is higher in the rare earth, causes the quality of metal to descend, and then has influenced the use properties of metal, final from being directed in price of product the decline of enterprise's productivity effect.At present, adopt metallothermics to prepare rare earth metal, can avoid that carbon fuses into metal in the rare earth metal production process.Because it is reductive agent that metallothermics adopts calcium metal, be easy to cause in the metal oxygen level higher.Because this method also needs high precision equipment, and the operational condition harshness makes the use of this method, particularly the use in China is restricted simultaneously.Adopt fused salt electrolysis process to produce rare earth, solve the high problem of carbon containing in the rare earth metal, people have done many trials.As in the carbon electrodes coating, and in smelting process method such as oxygen blast carbon drop, but effect is all undesirable, its major cause is that the fusion processes of carbon is difficult to control.
Purpose of the present invention is exactly in order to overcome the deficiency that exists in the above-mentioned prior art, a kind of novel rare-earth molten-salt electrolysis ceramic anode to be provided, can eliminate effectively in the rare earth molten-salt electrolysis process, owing to the dissolving of carbon in the carbon anode makes the too high phenomenon of carbon content in the metal.Thereby realize adopting fused salt electrolysis process, the purpose of producing the low high quality rare earth metal of carbon containing.
A kind of rare earth molten-salt electrolysis ceramic anode is characterized in that the material composition of ceramic anode is (weight %): Neodymium trioxide 60%～84%, cerium oxide 1%～20%, cupric oxide 15%～20%.
A kind of preparation method of rare earth molten-salt electrolysis ceramic anode, it is characterized in that: a. at first prepares Neodymium trioxide, cerium oxide, the cupric oxide powder mix that composition is prepared in ceramic anode composition ratio uniformly, b. carry out isostatic pressing then and make the anode blank, c. carries out sintering at last; Processing condition are: isostatic pressing pressure is 0.5～2 * 10
8Handkerchief, sintering temperature are 800～1000 ℃, and sintering time is 10～20 hours.
By the rare earth molten-salt electrolysis ceramic anode that method of the present invention is prepared, excellent property, its high-temperature conductivity＞1 * 10
2(Ω cm)
-1, fusing point＞1300 ℃, the density of material＞95%, the corrosion rate of material are (1～2) * 10
-2G/cm
2H has reached rare earth molten-salt electrolysis and has produced rare earth metal anodic requirement, and brings carbon impurity can for the rare earth metal product, is rare earth molten-salt electrolysis anodic ideal substitute.
, be further described a kind of rare earth molten-salt electrolysis ceramic anode of the present invention and preparation method thereof below in conjunction with example.
A kind of rare earth molten-salt electrolysis ceramic anode, the material composition of its ceramic anode are (weight %): Neodymium trioxide 60%～84%, cerium oxide 1%～20%, cupric oxide 15%～20%.The preparation method of molten-salt electrolysis ceramic anode at first prepares Neodymium trioxide, cerium oxide, the cupric oxide powder mix that composition is prepared in ceramic anode composition ratio uniformly, 0.5～2
8Under the pressure of handkerchief, carrying out isostatic pressing and make the anode blank, is under 800～1000 ℃ in temperature again, and sintering 10～20 hours just can make satisfactory anode material.
Embodiment 1
Adopt the coprecipitation method preparation to consist of 65%Nd
2O
3, 17%CeO
2And the mixed powder of 18%CuO, powder is through 1 * 10
8Isostatic pressing under the handkerchief pressure again 900 ℃ of following sintering 10 hours, promptly makes ceramic anode of the present invention after the moulding.This anodic analytical results shows that the material of electrode consists of and contains Nd
2O
365.4%, CeO
216.7%, CuO17.9%, the fusing point of material are 1320 ℃, and actual density is 6.48g/cm
3
Embodiment 2
Adopt the coprecipitation method preparation to consist of 74%Nd
2O
3, 6%CeO
2And the mixed powder of 20%CuO, powder is through 2 * 10
8Isostatic pressing under the handkerchief pressure again 1000 ℃ of following sintering 20 hours, promptly makes ceramic anode of the present invention after the moulding, and this anodic analytical results shows that the material of electrode consists of and contains Nd
2O
374.5%, CeO
25.8%, CuO19.7%, the fusing point of material are 1321 ℃, and actual density is 6.53g/cm
3
Embodiment 3
Adopt the coprecipitation method preparation to consist of 7865%Nd
2O
3, 4%CeO
2And the mixed powder of 17%CuO, powder is through 1 * 10
8Isostatic pressing under the handkerchief pressure again 1000 ℃ of following sintering 15 hours, promptly makes ceramic anode of the present invention after the moulding.This anodic analytical results shows that the material of electrode consists of and contains Nd
2O
379.5%, CeO
23.7%, CuO16.8%, the fusing point of material are 1323 ℃, and actual density is 6.50g/cm
3
Claims (2)
1. a rare earth molten-salt electrolysis ceramic anode is characterized in that the material composition of ceramic anode is (weight %): Neodymium trioxide 60%～84%, cerium oxide 1%～20%, cupric oxide 15%～20%.
2. the preparation method of a rare earth molten-salt electrolysis ceramic anode is characterized in that:
A. at first prepare Neodymium trioxide, cerium oxide, cupric oxide powder mix that composition is prepared in ceramic anode composition ratio uniformly;
B. carry out isostatic pressing then and make the anode blank;
C. carry out sintering at last;
Processing condition are:
Isostatic pressing pressure is 0.5～2 * 10
8Handkerchief,
Sintering temperature is 800～1000 ℃,
Sintering time is 10～20 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121917A CN1055140C (en) | 1997-11-19 | 1997-11-19 | Ceramic anode for rare earth molten salt electrolysis and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121917A CN1055140C (en) | 1997-11-19 | 1997-11-19 | Ceramic anode for rare earth molten salt electrolysis and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1188162A true CN1188162A (en) | 1998-07-22 |
| CN1055140C CN1055140C (en) | 2000-08-02 |
Family
ID=5176540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97121917A Expired - Lifetime CN1055140C (en) | 1997-11-19 | 1997-11-19 | Ceramic anode for rare earth molten salt electrolysis and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1055140C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093569C (en) * | 1999-12-24 | 2002-10-30 | 江西南方稀土高技术股份有限公司 | Application technology for lumpy multiple anode in fluoride system molten salt electrolysis process |
| CN104276825A (en) * | 2014-09-30 | 2015-01-14 | 苏州普京真空技术有限公司 | Preparation method of rare-earth neodymium electrolysis ceramic crucible |
| CN104556308A (en) * | 2014-12-12 | 2015-04-29 | 江苏省陶瓷研究所有限公司 | Preparation method of multivariate micro-electrolysis ceramic for water treatment |
| CN112921360A (en) * | 2019-12-05 | 2021-06-08 | 乐山有研稀土新材料有限公司 | Method for preparing rare earth metal by molten salt electrolysis |
| CN115304379A (en) * | 2022-06-16 | 2022-11-08 | 江苏南方永磁科技有限公司 | Anode material and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1003458B (en) * | 1987-09-01 | 1989-03-01 | 东北工学院 | Anode |
| EP0306102B1 (en) * | 1987-09-02 | 1993-03-31 | MOLTECH Invent S.A. | Molten salt electrolysis with non-consumable anode |
| CN1026504C (en) * | 1992-04-25 | 1994-11-09 | 北京科技大学 | Inert anode for molten-salt electrolysis producing neodymium |
-
1997
- 1997-11-19 CN CN97121917A patent/CN1055140C/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093569C (en) * | 1999-12-24 | 2002-10-30 | 江西南方稀土高技术股份有限公司 | Application technology for lumpy multiple anode in fluoride system molten salt electrolysis process |
| CN104276825A (en) * | 2014-09-30 | 2015-01-14 | 苏州普京真空技术有限公司 | Preparation method of rare-earth neodymium electrolysis ceramic crucible |
| CN104556308A (en) * | 2014-12-12 | 2015-04-29 | 江苏省陶瓷研究所有限公司 | Preparation method of multivariate micro-electrolysis ceramic for water treatment |
| CN104556308B (en) * | 2014-12-12 | 2017-01-18 | 江苏省陶瓷研究所有限公司 | Preparation method of multivariate micro-electrolysis ceramic for water treatment |
| CN112921360A (en) * | 2019-12-05 | 2021-06-08 | 乐山有研稀土新材料有限公司 | Method for preparing rare earth metal by molten salt electrolysis |
| CN112921360B (en) * | 2019-12-05 | 2023-01-03 | 乐山有研稀土新材料有限公司 | Method for preparing rare earth metal by molten salt electrolysis |
| CN115304379A (en) * | 2022-06-16 | 2022-11-08 | 江苏南方永磁科技有限公司 | Anode material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1055140C (en) | 2000-08-02 |
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Granted publication date: 20000802 |