CN102465204A - Preparation method of niobium pentoxide with high apparent density - Google Patents
Preparation method of niobium pentoxide with high apparent density Download PDFInfo
- Publication number
- CN102465204A CN102465204A CN2010105480276A CN201010548027A CN102465204A CN 102465204 A CN102465204 A CN 102465204A CN 2010105480276 A CN2010105480276 A CN 2010105480276A CN 201010548027 A CN201010548027 A CN 201010548027A CN 102465204 A CN102465204 A CN 102465204A
- Authority
- CN
- China
- Prior art keywords
- niobium
- density
- hydrochloric acid
- niobium hydroxide
- hours
- 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.)
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- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 title abstract 3
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims abstract description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000010955 niobium Substances 0.000 claims abstract description 18
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 16
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 238000011026 diafiltration Methods 0.000 claims description 5
- 238000006115 defluorination reaction Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 6
- 239000000047 product Substances 0.000 abstract description 3
- 238000007873 sieving Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 4
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 3
- 235000011613 Pinus brutia Nutrition 0.000 description 3
- 241000018646 Pinus brutia Species 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of niobium pentoxide with high apparent density, which comprises the steps of neutralizing a niobium liquid with ammonia water to obtain niobium hydroxide precipitate, separating, transferring into a vacuum filtering and washing tank, washing with pure water, filtering until the filtrate contains less than 0.02g/L, adding 15-25L of concentrated hydrochloric acid with the concentration of 20-30% into the obtained defluorinated niobium hydroxide slurry according to 100Kg of niobium oxide, blending, uniformly mixing, drying in a drying machine at 80 ℃ for 7-9 hours, transferring into a converter for calcination, controlling the furnace temperature at 850 +/-10 ℃ and the calcination time at 2-4 hours, and sieving to obtain niobium pentoxide with high apparent density after calcination. The method has the advantages that: the bulk density of the produced niobium hydroxide reaches 1.5g/ml to 1.8g/ml, and is improved by more than one time compared with the product produced by 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, earlier niobium liquid is squeezed into the neutralization precipitation groove, under agitation feeds NH
3Gas makes solution PH=8～9, generates Nb (OH)
5Deposition is then with its solid-liquid separation, through washing, remove by filter Nb (OH)
5In fluorion impurity, dry again, 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, influences steel product quality.
Summary of the invention
The objective of the invention is to propose a kind of new process of producing High-density Niobium Oxide, to overcome the existing drawback of preparation Niobium Pentxoxide to above-mentioned prior art problems.
Technical scheme of the present invention is following:
Neutralization obtains the niobium hydroxide deposition through ammoniacal liquor with niobium liquid, isolates niobium hydroxide, changes in the vacuum diafiltration groove again; Wash, filter with pure water, be washed till filtrate and contain F＜0.02g/L, obtain the niobium hydroxide slurry behind the 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, prepares burden, after mixing; Behind drying machine drying, move in the converter and calcine; Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 2～4 hours, and sieving after the calcining promptly obtains 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 gets into oven dry, calcination process then.
The batching of described niobium hydroxide slip and concentrated hydrochloric acid is dried to move in the converter after 7～9 hours in 80 ℃ dryer and is calcined.
Know-why of the present invention: 1, add hydrochloric acid in the niobium hydroxide after, make the niobium hydroxide system become acid system by alkalescence; 2, strengthened the adsorptive power between the molecule behind the adding hydrochloric acid, made the niobium hydroxide cohere agglomerating under the high temperature more easily, 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 behind sintering not to have influence to quality product, evaporable HCl recyclable utilization after water absorbs simultaneously fully.
Embodiment
Following embodiment further specifies the present invention, but should be as the restriction to protection scope of the present invention.
Embodiment one
1, neutralization obtains the niobium hydroxide deposition through ammoniacal liquor with niobium liquid, after the solid-liquid separation, niobium hydroxide is changed in the vacuum diafiltration groove, washs with pure water, filters, and is washed till filtrate and contains F＜0.02g/L;
2, will be 25% concentrated hydrochloric acid 20L by 100Kg niobium oxides adding concentration through washing, the niobium hydroxide slurry that filters the back gained, prepare burden, mix;
3, the material after will mixing changes in the dryer and dries 80 ℃ of bake out temperatures, 8 hours time.
4, the material after will drying moves in the converter and calcines, and Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 3 hours, and the calcining back is crossed and is sieved to high pine dress Niobium Pentxoxide.
Embodiment two
1, neutralization obtains the niobium hydroxide deposition through ammoniacal liquor with niobium liquid, after the solid-liquid separation, niobium hydroxide is changed in the vacuum diafiltration groove, washs with pure water, filters, and is washed till filtrating and contains F＜0.02g/L;
2, will be 22% concentrated hydrochloric acid 15L by 100Kg niobium oxides adding concentration through washing, the niobium hydroxide slurry that filters the back gained, prepare burden, mix;
3, the material after will mixing changes in the dryer and dries 80 ℃ of bake out temperatures, 9 hours time.
4, the material after will drying moves in the converter and calcines, and Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 4 hours, and the calcining back is crossed and is sieved to high pine dress Niobium Pentxoxide.
Embodiment three
1, neutralization obtains the niobium hydroxide deposition through ammoniacal liquor with niobium liquid, after the solid-liquid separation, niobium hydroxide is changed in the vacuum diafiltration groove, washs with pure water, filters, and is washed till filtrate and contains F＜0.02g/L;
2, will be 20% concentrated hydrochloric acid 15L by 100Kg niobium oxides adding concentration through washing, the niobium hydroxide slurry that filters the back gained, prepare burden, mix;
3, the material after will mixing changes in the dryer and dries 80 ℃ of bake out temperatures, 7 hours time.
4, the material after will drying moves in the converter and calcines, and Control for Kiln Temperature is at 850 ℃ ± 10 ℃, and calcination time is 2 hours, and the calcining back is crossed and is sieved to high pine dress Niobium Pentxoxide.
Claims (3)
1. method of producing High-density Niobium Oxide, technical scheme is following: neutralization obtains the niobium hydroxide deposition through ammoniacal liquor with niobium liquid, isolates niobium hydroxide; Change over to again in the vacuum diafiltration groove, wash, filter, be washed till filtrate and contain F＜0.02g/L with pure water; Obtain the niobium hydroxide slurry behind the 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, prepares burden; After mixing, behind drying machine drying, move in the converter and calcine, Control for Kiln Temperature is at 850 ℃ ± 10 ℃; Calcination time is 2～4 hours, sieves after the calcining promptly to 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 gets into oven dry, calcination process then.
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 the converter after 7～9 hours in 80 ℃ dryer 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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102465204A true CN102465204A (en) | 2012-05-23 |
| CN102465204B CN102465204B (en) | 2013-11-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105480276A Expired - Fee Related CN102465204B (en) | 2010-11-16 | 2010-11-16 | Method for preparing niobium pentoxide with high apparent density |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102465204B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310478A (en) * | 2014-10-10 | 2015-01-28 | 九江有色金属冶炼有限公司 | Preparation method of high-tap-density niobium oxide and high-tap-density niobium oxide prepared by same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107657A (en) * | 1986-11-11 | 1987-12-09 | 北京有色金属研究总院 | The production method of purification of spherical Niobium Pentxoxide |
| WO1997013724A1 (en) * | 1995-10-12 | 1997-04-17 | Cabot Corporation | Niobium and tantalum pentoxide compounds |
| JP2002321917A (en) * | 2002-03-25 | 2002-11-08 | Mitsui Mining & Smelting Co Ltd | Method for manufacturing granulated niobium oxide |
| JP2004051383A (en) * | 2002-07-16 | 2004-02-19 | Mitsui Mining & Smelting Co Ltd | Method for manufacturing tantalum oxide powder as well as niobium oxide powder, and tantalum oxide powder and niobium oxide powder obtained by the manufacturing method |
| CN101565207A (en) * | 2009-06-01 | 2009-10-28 | 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 |
-
2010
- 2010-11-16 CN CN2010105480276A patent/CN102465204B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107657A (en) * | 1986-11-11 | 1987-12-09 | 北京有色金属研究总院 | The production method of purification of spherical Niobium Pentxoxide |
| WO1997013724A1 (en) * | 1995-10-12 | 1997-04-17 | Cabot Corporation | Niobium and tantalum pentoxide compounds |
| JP2002321917A (en) * | 2002-03-25 | 2002-11-08 | Mitsui Mining & Smelting Co Ltd | Method for manufacturing granulated niobium oxide |
| JP2004051383A (en) * | 2002-07-16 | 2004-02-19 | Mitsui Mining & Smelting Co Ltd | Method for manufacturing tantalum oxide powder as well as niobium oxide powder, and tantalum oxide powder and niobium oxide powder obtained by the manufacturing method |
| CN101565207A (en) * | 2009-06-01 | 2009-10-28 | 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李济华等: "高松装密度五氧化二铌的研究", 《稀有金属与硬质合金》, no. 145, 30 June 2001 (2001-06-30) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310478A (en) * | 2014-10-10 | 2015-01-28 | 九江有色金属冶炼有限公司 | Preparation method of high-tap-density niobium oxide and high-tap-density niobium oxide prepared by same |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102465204B (en) | 2013-11-06 |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
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Granted publication date: 20131106 Termination date: 20161116 |