CN102465204B - Method for preparing niobium pentoxide with high apparent density - Google Patents
Method for preparing niobium pentoxide with high apparent density Download PDFInfo
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- CN102465204B CN102465204B CN2010105480276A CN201010548027A CN102465204B CN 102465204 B CN102465204 B CN 102465204B CN 2010105480276 A CN2010105480276 A CN 2010105480276A CN 201010548027 A CN201010548027 A CN 201010548027A CN 102465204 B CN102465204 B CN 102465204B
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- niobium
- niobium hydroxide
- hydrochloric acid
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- apparent density
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to a method for preparing niobium pentoxide with high apparent density. The method comprises the following steps of: neutralizing a niobium solution with ammonia water to obtain niobium hydroxide precipitation, separating the niobium hydroxide precipitation and transferring the separated niobium hydroxide precipitation into a vacuum filtering and washing tank, washing and filtering the niobium hydroxide precipitation with pure water till the content of F of percolate is less than 0.02g/L, adding niobium hydroxide slurry subjected to F removal into 12-25L of 20-30% concentrated hydrochloric acid according to 100Kg of niobium oxide, burdening and uniformly mixing, then drying for 7-9h in a drying machine with the temperature of 80 DEG C, then transferring to a converter for calcining for 2-4h with the furnace temperature being controlled at 850+/-10 DEG C, and screening after calcining to obtain the niobium pentoxide with high apparent density. The method disclosed by the invention has the advantage that: the apparent density of the prepared niobium pentoxide reaches 1.5-1.8g/ml and is increased by more than one time of that of a product prepared by using the traditional method.
Description
Technical field
The present invention relates to a kind of preparation method of High-density Niobium Oxide
Background technology
At present, traditional Niobium Pentxoxide is to produce with the niobium liquid in the liquid-liquid extraction sepn process, first niobium liquid is squeezed into the neutralization precipitation groove, under agitation passes into NH
3Gas makes solution PH=8～9, generates Nb (OH)
5Precipitation is then with its solid-liquid separation, through washing, remove by filter Nb (OH)
5In fluorion impurity, then dry, calcine and obtain Niobium Pentxoxide.
The traditional method shortcoming: the Niobium Pentxoxide loose density that produced in conventional processes goes out is low, generally at 0.7～0.8g/ml.The Niobium Pentxoxide that this method is produced can produce pore in adding special rolling-mill section to, and its homogeneity is bad, affects steel product quality.
Summary of the invention
The objective of the invention is the problem for above-mentioned prior art, propose a kind of new process of producing High-density Niobium Oxide, to overcome the existing drawback of preparation Niobium Pentxoxide.
Technical scheme of the present invention is as follows:
niobium liquid is obtained the niobium hydroxide precipitation through ammonia neutralization, isolate niobium hydroxide, change over to again in vacuum diafiltration groove, wash with pure water, filter, be washed till filtrate and contain F＜0.02g/L, obtain the niobium hydroxide slurry after defluorination, it is characterized in that it is concentrated hydrochloric acid 15～25L of 20%～25% that the niobium hydroxide slurry of gained is added concentration by the 100Kg niobium oxides, prepare burden, after mixing, move in converter after the oven dry of drying machine and calcine, Control for Kiln Temperature is at 850 ℃ ± 10 ℃, calcination time is 2～4 hours, sieve after calcining and namely obtain High-density Niobium Oxide.
Preferred scheme is:
It is 25% concentrated hydrochloric acid 20L that described niobium hydroxide slurry adds concentration by the 100Kg niobium oxides, prepares burden, and then enters oven dry, calcination process.
The batching of described niobium hydroxide slip and concentrated hydrochloric acid is dried to move in converter after 7～9 hours in the dryer of 80 ℃ and is calcined.
Know-why of the present invention: 1, add hydrochloric acid in niobium hydroxide after, make the niobium hydroxide system become acid system by alkalescence; 2, add the adsorptive power that has strengthened after hydrochloric acid between molecule, more easily make the niobium hydroxide cohere agglomerating under high temperature, the niobium hydroxide density of unit volume is increased; 3, the niobium hydroxide loose density produced of this method reaches 1.5g/ml～1.8g/ml, and loose density is doubled many; 4, the hydrochloric acid that adds is volatilizable after sintering not to be affected quality product fully, simultaneously the HCl of volatilization recoverable after water absorbs.
Embodiment
The present invention will be further described for the following examples, but should be as the restriction to protection scope of the present invention.
Embodiment one
1, niobium liquid is obtained the niobium hydroxide precipitation through ammonia neutralization, after solid-liquid separation, niobium hydroxide is changed in vacuum diafiltration groove, wash with pure water, filter, be washed till filtrate and contain F＜0.02g/L;
2, will be through washing, filter after the niobium hydroxide slurry of gained to add concentration by the 100Kg niobium oxides be 25% concentrated hydrochloric acid 20L, prepare burden, mix;
3, the material after mixing changes in dryer and dries, 80 ℃ of bake out temperatures, 8 hours time.
4, the material after drying moves in converter and calcines, and Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 3 hours, crosses after calcining to be sieved to high pine dress Niobium Pentxoxide.
Embodiment two
1, niobium liquid is obtained the niobium hydroxide precipitation through ammonia neutralization, after solid-liquid separation, niobium hydroxide is changed in vacuum diafiltration groove, wash with pure water, filter, be washed till filtrate and contain F＜0.02g/L;
2, will be through washing, filter after the niobium hydroxide slurry of gained to add concentration by the 100Kg niobium oxides be 22% concentrated hydrochloric acid 15L, prepare burden, mix;
3, the material after mixing changes in dryer and dries, 80 ℃ of bake out temperatures, 9 hours time.
4, the material after drying moves in converter and calcines, and Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 4 hours, crosses after calcining to be sieved to high pine dress Niobium Pentxoxide.
Embodiment three
1, niobium liquid is obtained the niobium hydroxide precipitation through ammonia neutralization, after solid-liquid separation, niobium hydroxide is changed in vacuum diafiltration groove, wash with pure water, filter, be washed till filtrate and contain F＜0.02g/L;
2, will be through washing, filter after the niobium hydroxide slurry of gained to add concentration by the 100Kg niobium oxides be 20% concentrated hydrochloric acid 15L, prepare burden, mix;
3, the material after mixing changes in dryer and dries, 80 ℃ of bake out temperatures, 7 hours time.
4, the material after drying moves in converter and calcines, and Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 2 hours, crosses after calcining to be sieved to high pine dress Niobium Pentxoxide.
Claims (3)
1. method of producing High-density Niobium Oxide, technical scheme is as follows: niobium liquid is obtained the niobium hydroxide precipitation through ammonia neutralization, isolate niobium hydroxide, change over to again in vacuum diafiltration groove, wash with pure water, filter, be washed till filtrate and contain F＜0.02g/L, obtain the niobium hydroxide slurry after defluorination, it is characterized in that it is concentrated hydrochloric acid 15～25L of 20%～25% that the niobium hydroxide slurry of gained is added concentration by the 100Kg niobium oxides, prepare burden, after mixing, move in converter after the oven dry of drying machine and calcine, Control for Kiln Temperature is at 850 ℃ ± 10 ℃, calcination time is 2～4 hours, sieve after calcining and namely obtain High-density Niobium Oxide.
2. the preparation method of High-density Niobium Oxide according to claim 1 is characterized in that it is 25% concentrated hydrochloric acid 20L that described niobium hydroxide slurry adds concentration by the 100Kg niobium oxides, prepares burden, and then enters oven dry, calcination process.
3. the preparation method of High-density Niobium Oxide according to claim 1, the batching that it is characterized in that described niobium hydroxide slip and concentrated hydrochloric acid is dried to move in converter after 7～9 hours in the dryer of 80 ℃ and is calcined.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105480276A CN102465204B (en) | 2010-11-16 | 2010-11-16 | Method for preparing niobium pentoxide with high apparent density |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105480276A CN102465204B (en) | 2010-11-16 | 2010-11-16 | Method for preparing niobium pentoxide with high apparent density |
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| Publication Number | Publication Date |
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| CN102465204A CN102465204A (en) | 2012-05-23 |
| CN102465204B true CN102465204B (en) | 2013-11-06 |
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| CN2010105480276A Expired - Fee Related CN102465204B (en) | 2010-11-16 | 2010-11-16 | Method for preparing niobium pentoxide with high apparent density |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104310478B (en) * | 2014-10-10 | 2016-12-07 | 九江有色金属冶炼有限公司 | The preparation method of a kind of big tap density niobium oxide and the big tap density niobium oxide of preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN86107657B (en) * | 1986-11-11 | 1988-01-13 | 北京有色金属研究总院 | Production for sphare niobium pentoxide |
| US6338832B1 (en) * | 1995-10-12 | 2002-01-15 | Cabot Corporation | Process for producing niobium and tantalum compounds |
| JP3907102B2 (en) * | 2002-03-25 | 2007-04-18 | 三井金属鉱業株式会社 | Method for producing granular niobium oxide |
| JP4025594B2 (en) * | 2002-07-16 | 2007-12-19 | 三井金属鉱業株式会社 | Method for producing tantalum oxide powder and niobium oxide powder, and tantalum oxide powder and niobium oxide powder obtained by the production method |
| CN101565207B (en) * | 2009-06-01 | 2010-12-01 | 肇庆多罗山蓝宝石稀有金属有限公司 | Producing method of low-fluorine high-purity tantalic oxide |
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Granted publication date: 20131106 Termination date: 20161116 |