CN104404573A - Preparation method of vanadium metal - Google Patents
Preparation method of vanadium metal Download PDFInfo
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- CN104404573A CN104404573A CN201410794842.9A CN201410794842A CN104404573A CN 104404573 A CN104404573 A CN 104404573A CN 201410794842 A CN201410794842 A CN 201410794842A CN 104404573 A CN104404573 A CN 104404573A
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- preparation
- vanadium metal
- vanadium
- metal
- inert gas
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
Abstract
The invention relates to a preparation method of vanadium metal, in particular to a method for preparing vanadium metal by electro-deoxidation in molten salt. The preparation method comprises the following steps: carbon powder and vanadium pentoxide are uniformly mixed, subjected to slurry casting or press forming, and then sintered for 5-8 h at the temperature of 600-900 DEG C under inert gas shielding, and a sintered body is obtained; then the sintered body and a metal wire are assembled to form a cathode, graphite is taken as an anode, CaCl2 melt is taken as an electrolyte, electrolysis is performed for 2-10 h under the conditions of the temperature of 850-900 DEG C and the voltage of 2.0-3.1 V under inert gas shielding, and the vanadium metal is obtained. The preparation method of the vanadium metal has the characteristics of low production process and energy consumption, little pollution, facilitation of continuous production and the like.
Description
Technical field
The present invention relates to the preparation method of vanadium metal, be specially and utilize electrodeoxidation to prepare vanadium metal method.
Background technology
Vanadium metal has the advantages that fusing point is high, good processability, erosion resistance strong, fast neutron absorption interface is little, is widely used in the aspects such as nuclear industry, superconductive alloy materials, refining special alloy and electronic industry.Produce vanadium metal and have kinds of processes perhaps, mainly comprise, vacuum carbothermal reduction method, silicothermic process, vanadium nitride thermal decomposition method, barium oxide or muriatic metallothermics, wherein general with the application of the thermit reduction of barium oxide.These method energy consumptions are high, complex process, and produce pollution.
Summary of the invention
For above-mentioned technical problem, the object of the invention is the preparation technology proposing a kind of vanadium metal, this explained hereafter flow process is short, and energy consumption is low, pollutes few, is easy to continuous seepage.
The preparation method of vanadium metal, comprises the following steps:
(1) be that the Vanadium Pentoxide in FLAKES of 2:0.5 ~ 1.5 and carbon dust mix by mol ratio, after slurry casting or pressed sizing, under protection of inert gas, 600 ~ 900 DEG C of sintering 5 ~ 8 hours, obtain sintered compact;
(2) sintered compact and groups of metal filaments being dressed up negative electrode, is anode with graphite, with CaCl
2melt is ionogen, and at 850 ~ 900 DEG C, electrolysis 2 ~ 10 hours under 2.0 ~ 3.1V voltage, electrolytic process carries out under protection of inert gas, the vanadium metal that final acquisition is pure.
Preferred electrolysis time is 2 ~ 8 hours.
The preparation method of vanadium metal provided by the invention, raw material is simple and easy to get, and production process is simple, with short production cycle, pollutes few, and the one-tenth reducing vanadium metal produces cost.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the sintered compact that embodiment 1 obtains;
Fig. 2 is the XRD figure spectrum of the vanadium metal that embodiment 1 obtains;
Fig. 3 is the SEM collection of illustrative plates of the vanadium metal that embodiment 1 obtains.
Embodiment
Specific implementation method of the present invention is described in conjunction with the embodiments.
Embodiment 1
Take Vanadium Pentoxide in FLAKES and carbon dust, by V
2o
5: C mol ratio is to mix at 2: 1, adds the PVB polyvinyl butyral acetal of mass concentration 1.5%, adds dehydrated alcohol, be placed in ball mill wet-milling 15 hours, then seasoning in atmosphere.
Under 20MP, powder compression become diameter to be 10mm, thickness is the disk of 2mm, and it is sintered 6 hours at 800 DEG C under argon shield, and Fig. 1 is the XRD figure spectrum after sintering;
The sintered wafer obtained and Fe-Cr-Al wire are assembled into negative electrode, adopt high purity graphite rod as anode, be inserted into and CaCl is housed
2in the alumina crucible of fused salt, under the protection of argon gas 850 DEG C, electrolysis 8 hours under control 2.8V voltage, after electrolysis terminates, cathode product cleaning also obtains vanadium metal after drying.Fig. 2 is the XRD figure spectrum of product, and Fig. 3 is the SEM photo of product.
Embodiment 2
Take Vanadium Pentoxide in FLAKES and carbon dust, by V
2o
5: C mol ratio is to mix at 2: 0.5, add the PVB polyvinyl butyral acetal of mass concentration 1.5%, add dehydrated alcohol, be placed in ball mill wet-milling 15 hours, then be poured in mould, obtaining diameter in atmosphere after seasoning is 12mm, and thickness is the disk of 3mm, and it is sintered 6 hours at 800 DEG C under argon shield;
The sintered wafer obtained and Fe-Cr-Al wire are assembled into negative electrode; adopt high purity graphite rod as anode; be inserted in the alumina crucible that CaCl2 fused salt is housed; under the protection of argon gas 850 DEG C; electrolysis 5 hours under control 3.0V voltage; after electrolysis terminates, cathode product cleaning also obtains vanadium metal after drying.
Claims (2)
1. the preparation method of vanadium metal, is characterized in that, comprises the following steps:
(1) be that the Vanadium Pentoxide in FLAKES of 2:0.5 ~ 1.5 and carbon dust mix by mol ratio, after slurry casting or pressed sizing, under protection of inert gas, 600 ~ 900 DEG C of sintering 5 ~ 8 hours, obtain sintered compact;
(2) sintered compact and groups of metal filaments being dressed up negative electrode, is anode with graphite, with CaCl
2melt is ionogen, and at 850 ~ 900 DEG C, electrolysis 2 ~ 10 hours under 2.0 ~ 3.1V voltage, electrolytic process carries out under protection of inert gas, the vanadium metal that final acquisition is pure.
2. the preparation method of vanadium metal according to claim 1, is characterized in that, described electrolysis time is 2 ~ 8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410794842.9A CN104404573A (en) | 2014-12-18 | 2014-12-18 | Preparation method of vanadium metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410794842.9A CN104404573A (en) | 2014-12-18 | 2014-12-18 | Preparation method of vanadium metal |
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|---|---|
| CN104404573A true CN104404573A (en) | 2015-03-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410794842.9A Pending CN104404573A (en) | 2014-12-18 | 2014-12-18 | Preparation method of vanadium metal |
Country Status (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105780059A (en) * | 2016-03-11 | 2016-07-20 | 西安建筑科技大学 | Electrolytic preparation method of vanadium-aluminum alloy |
| CN112251619A (en) * | 2020-09-11 | 2021-01-22 | 河钢承德钒钛新材料有限公司 | Preparation method and device of metal vanadium |
| CN113106496A (en) * | 2021-03-31 | 2021-07-13 | 北京科技大学 | Method for electrolyzing high-purity metal vanadium by vanadium-carbon-oxygen solid solution anode molten salt |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3098021A (en) * | 1960-04-15 | 1963-07-16 | Union Carbide Corp | Process for producing ductile vanadium |
| CN1837411A (en) * | 2006-02-17 | 2006-09-27 | 武汉大学 | Method for preparing refractory active metal or alloy |
| CN101440507A (en) * | 2008-11-28 | 2009-05-27 | 攀枝花新钢钒股份有限公司 | Preparation of metal vanadium |
| CN102121123A (en) * | 2011-04-18 | 2011-07-13 | 北京科技大学 | Vanadium metal smelting process |
| CN102978664A (en) * | 2011-09-05 | 2013-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of metal vanadium and metal vanadium obtained by same |
-
2014
- 2014-12-18 CN CN201410794842.9A patent/CN104404573A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3098021A (en) * | 1960-04-15 | 1963-07-16 | Union Carbide Corp | Process for producing ductile vanadium |
| CN1837411A (en) * | 2006-02-17 | 2006-09-27 | 武汉大学 | Method for preparing refractory active metal or alloy |
| CN101440507A (en) * | 2008-11-28 | 2009-05-27 | 攀枝花新钢钒股份有限公司 | Preparation of metal vanadium |
| CN102121123A (en) * | 2011-04-18 | 2011-07-13 | 北京科技大学 | Vanadium metal smelting process |
| CN102978664A (en) * | 2011-09-05 | 2013-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of metal vanadium and metal vanadium obtained by same |
Non-Patent Citations (2)
| Title |
|---|
| ZHUO-FEI CAI: "Direct electrochemical reduction of solid vanadium oxide to metal vanadium at low temperature in molten CaCl2-NaCl", 《INTERNATIONAL JOURNAL OF MINERALS, METALLURGY AND MATERIALS》 * |
| 杨保祥: "《钒基材料制造》", 31 March 2014 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105780059A (en) * | 2016-03-11 | 2016-07-20 | 西安建筑科技大学 | Electrolytic preparation method of vanadium-aluminum alloy |
| CN105780059B (en) * | 2016-03-11 | 2018-05-04 | 西安建筑科技大学 | A kind of electrolytic preparation method of vananum |
| CN112251619A (en) * | 2020-09-11 | 2021-01-22 | 河钢承德钒钛新材料有限公司 | Preparation method and device of metal vanadium |
| CN112251619B (en) * | 2020-09-11 | 2023-08-04 | 河钢承德钒钛新材料有限公司 | Preparation method and device of vanadium metal |
| CN113106496A (en) * | 2021-03-31 | 2021-07-13 | 北京科技大学 | Method for electrolyzing high-purity metal vanadium by vanadium-carbon-oxygen solid solution anode molten salt |
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Application publication date: 20150311 |
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| RJ01 | Rejection of invention patent application after publication |