CN103936072A - Process for directly producing crystal-level high-purity niobium oxide from decomposition supernate - Google Patents
Process for directly producing crystal-level high-purity niobium oxide from decomposition supernate Download PDFInfo
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- CN103936072A CN103936072A CN201410177680.4A CN201410177680A CN103936072A CN 103936072 A CN103936072 A CN 103936072A CN 201410177680 A CN201410177680 A CN 201410177680A CN 103936072 A CN103936072 A CN 103936072A
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- supernatant liquor
- niobium
- high purity
- purity niobium
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Abstract
The invention relates to a process for directly producing crystal-level high-purity niobium oxide from decomposition supernate, which comprises the following steps: separating supernate, regulating the acidity, performing fine filtration, and extracting by taking sec-octyl alcohol as extractant; performing extraction and back extraction to obtain a high-purity niobium solution, neutralizing with liquid ammonia to obtain niobium hydroxide, and transferring into a filter press; performing solid-liquid separation to obtain solid niobium hydroxide; and performing pressure filtration with pure water, washing, drying, calcining, and then screening to obtain the crystal-level high-purity niobium oxide. According to the process provided by the invention, the supernate with niobite dissolved is directly extracted, the high-purity niobium solution is prepared by taking the supernate as the basis, and the sec-octyl alcohol is used as the extractant in the preparation process; and by controlling the phase ratio, pickling agent and the acidity of anti-niobium agent in the extraction process, the high-purity niobium solution conforming to the standard can be prepared through only one extraction procedure. Thus, the production process is simpler, less reagents and energy sources are consumed, and the product quality is more stable.
Description
Technical field:
The present invention relates to the technical field of producing of niobium oxides, refer in particular to the technique that supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization.
Background technology:
High purity niobium oxide refers to the niobium oxides that purity is greater than 99.95%, is mainly used in opticglass, ceramic condenser LiNbO
3the high-tech areas such as crystal are a kind of important electronic materials.
The raw materials for production of niobium oxides, mainly with niobite, tantalite etc., wherein all contain higher tantalum, simultaneously with as impurity elements such as Fe, Mn, Ti.Current niobium liquid preparation is that after niobite dissolves, direct acid adjustment is also filtered and obtained filtrate, first obtain niobium liquid through single extraction, then can obtain high purity niobium liquid through extraction again with the qualified niobium liquid of this extraction, its whole processing procedure is long, energy consumption is large, the high and unstable product quality of cost.
Summary of the invention:
The object of the invention is to overcome the deficiencies in the prior art part, provide a kind of direct utilization to decompose the technique of supernatant liquor production crystal level high purity niobium oxide.
The technical scheme that the present invention realizes its object employing is: the technique of supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization, and this technique comprises following steps:
A. after niobite being ground, decompose separation of supernatant after decomposing with industrial hydrofluoric acid and industrial sulphuric acid;
B. in supernatant liquor, add industrial hydrofluoric acid and industrial sulphuric acid to carry out acid adjustment, make acidity meet extraction requirement;
C. the supernatant liquor after acid adjustment being carried out to essence filters;
D. essence is filtered to the clean supernatant liquor obtaining and extract, adopting secondary octanol is extraction agent, and chemical pure sulfuric acid is pickling agent and anti-niobium agent, and supernatant liquor obtains high purity niobium liquid through extraction, reextraction;
E. high purity niobium liquid is obtained to niobium hydroxide and proceeds to pressure filter through liquefied ammonia neutralization, solid-liquid separation obtains niobium hydroxide solid, and carries out press filtration, washing with pure water;
F. the niobium hydroxide solid obtaining after washing being proceeded to drying baker dries;
G. calcine proceeding to push away in boat stove after the niobium hydroxide solid abrasive dust after drying, after calcining, sieve, obtain crystal level high purity niobium oxide.
In above-mentioned technique, in described step a, niobite decomposition is carried out at normal temperatures and pressures, when decomposition, by weight, niobite: hydrofluoric acid is 1:2; Niobite: sulfuric acid is 1:1.5; The density of industrial hydrofluoric acid used is 1.21g/cm
3, its concentration is 40%, industrial sulphuric acid density is 1.84g/cm
3, its concentration is 95%, resolving time 16h.
In described step b, acidity control is at HF5.5～6mol/L, H
2sO
42.5～3mol/L.
In described step c, adopting aperture is that the PE microfiltration tube of 0.5 micron carries out essence and filters.
In described steps d extraction process, pickling extraction section is in a ratio of organic phase: water=1:0.6～1, and the section of stripping is in a ratio of organic phase: water=2:1, and pickling agent is the chemical pure sulfuric acid of acidity 3.5mol/L, the chemical pure sulfuric acid that anti-niobium agent is acidity 1.5mol/L.
In described step e, pure water consumption is by 60～80L/kgNb
2o
5.
100 ± 10 DEG C of bake out temperatures in described step f, drying time 10 ± 1h.
850 DEG C ± 10 DEG C of calcining temperatures in described step f, calcination time 6 ± 1h.
Technique of the present invention is directly extracted the supernatant liquor after niobite dissolves, taking it as basic high-purity niobium liquid, it is extraction agent that preparation process adopts secondary octanol, by controlling the acidity of comparing in extraction process, pickling agent and anti-niobium agent, only need single extraction operation can make standard compliant high purity niobium liquid, its Production Flow Chart is more simple, and still less, and quality product is more stable for all ingredients consuming and the energy.The high purity niobium oxide that adopts production technique of the present invention to produce all can reach the quality standard of 04 grade of crystal level high purity niobium oxide of rower [YS/T548-2007], and compared with old technology product, quality is more stable, and production cost is lower.
Embodiment:
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment
A. after niobite being ground, drop into the decomposer of diameter 3m × 3m, decompose with industrial hydrofluoric acid and industrial sulphuric acid, decomposition is carried out at normal temperatures and pressures, when decomposition, by weight, niobite: hydrofluoric acid is 1:2; Niobite: sulfuric acid is 1:1.5; The density of industrial hydrofluoric acid used is 1.21g/cm
3, its concentration is 40%, industrial sulphuric acid density is 1.84g/cm
3, its concentration is 95%, resolving time 16h isolates supernatant liquor after decomposition;
B. in supernatant liquor, add industrial hydrofluoric acid and industrial sulphuric acid to carry out acid adjustment, make acidity control at HF5.5～6mol/L, H
2sO
42.5～3mol/L, meets extraction requirement;
C. the PE microfiltration tube that is 0.5 micron to the supernatant liquor employing aperture after acid adjustment carries out essence and filters; Its effect is molecule and the floating matter of further removing in supernatant liquor, obtains clean supernatant liquor;
D. essence being filtered to the clean supernatant liquor obtaining extracts, adopting secondary octanol is extraction agent, in extraction process, adding acidity is that the chemical pure sulfuric acid control of 3.5mol/L (equivalent concentration 7N) is in a ratio of organic phase: water=1:0.6～1, be that the chemical pure sulfuric acid of 1.5mol/L (equivalent concentration 3N) is as anti-niobium agent to adding acidity in isolated organic phase again, strip, and control strip section be in a ratio of organic phase: water=2:1, the water obtaining after reextraction is high purity niobium liquid; Extraction and anti-extraction process carry out in mixer-settler, and wherein 10 grades of pickling, extract 10 grades; Strip 12 grades;
E. by high purity niobium liquid, through liquefied ammonia, neutralization obtains niobium hydroxide and proceeds to pressure filter, under pressure, niobium hydroxide is separated out, and solid-liquid separation obtains niobium hydroxide solid, then carries out press filtration, washing with pure water, and pure water consumption is by 60～80L/kgNb
2o
5can control F content below 0.2%;
F. the niobium hydroxide solid obtaining is proceeded to drying baker and dry after washing, 100 ± 10 DEG C of bake out temperatures, drying time 10 ± 1h;
G. calcine proceeding to push away in boat stove after the niobium hydroxide solid abrasive dust after drying, 850 DEG C ± 10 DEG C of calcining temperatures, calcination time 6 ± 1h, sieves after calcining, obtains crystal level high purity niobium oxide.
The high purity niobium oxide that adopts production technique of the present invention to produce all can reach the quality standard of 04 grade of crystal level high purity niobium oxide of rower [YS/T548-2007], and quality is more stable.
Adopt technique of the present invention, metal recovery rate can reach 98.5%, the product of preparation identical weight, relatively existing technique, can save sulfuric acid consumption more than 40%, saves hydrofluoric acid consumption more than 70%, and saves energy more than 10%, therefore can reduce product cost greatly.
Claims (8)
1. directly utilize a technique of decomposing supernatant liquor production crystal level high purity niobium oxide, it is characterized in that: this technique comprises following steps:
A. after niobium minerals being ground, decompose separation of supernatant after decomposing with industrial hydrofluoric acid and industrial sulphuric acid;
B. in supernatant liquor, add industrial hydrofluoric acid and industrial sulphuric acid to carry out acid adjustment, make acidity meet extraction requirement;
C. the supernatant liquor after acid adjustment being carried out to essence filters;
D. essence is filtered to the clean supernatant liquor obtaining and extract, adopting secondary octanol is extraction agent, and chemical pure sulfuric acid is pickling agent and anti-niobium agent, and supernatant liquor obtains high purity niobium liquid through extraction, reextraction;
E. high purity niobium liquid is obtained to niobium hydroxide and proceeds to pressure filter through liquefied ammonia neutralization, carry out solid-liquid separation, obtain niobium hydroxide solid, and carry out press filtration, washing with pure water;
F. the niobium hydroxide solid obtaining after washing being proceeded to drying baker dries;
G. calcine proceeding to push away in boat stove after the niobium hydroxide solid abrasive dust after drying, after calcining, sieve, obtain crystal level high purity niobium oxide.
2. the technique of supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization according to claim 1, it is characterized in that: in described step a, niobite decomposition is carried out at normal temperatures and pressures, and when decomposition, by weight, niobite: hydrofluoric acid is 1:2; Niobite: sulfuric acid is 1:1.5; The density of industrial hydrofluoric acid used is 1.21g/cm
3, its concentration is 40%, industrial sulphuric acid density is 1.84g/cm
3, its concentration is 95%, resolving time 16h.
3. the technique that a kind of direct utilization according to claim 1 is decomposed supernatant liquor and produced crystal level high purity niobium oxide, is characterized in that: in described step b acidity control at HF5.5～6mol/L, H
2sO
42.5～3mol/L.
4. the technique that a kind of direct utilization according to claim 1 is decomposed supernatant liquor and produced crystal level high purity niobium oxide, is characterized in that: in described step c, adopting aperture is that the PE microfiltration tube of 0.5 micron carries out essence filtration.
5. the technique of supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization according to claim 1, it is characterized in that: in described steps d extraction process, pickling extraction section is in a ratio of organic phase: water=1:0.6～1, the section of stripping is in a ratio of organic phase: water=2:1, pickling agent is the chemical pure sulfuric acid of acidity 3.5mol/L, the chemical pure sulfuric acid that anti-niobium agent is acidity 1.5mol/L.
6. the technique of supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization according to claim 1, it is characterized in that: in described step e, pure water consumption is by 60～80L/kgNb
2o
5.
7. the technique of supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization according to claim 1, it is characterized in that: 100 ± 10 DEG C of bake out temperatures in described step f, drying time 10 ± 1h.
8. the technique of supernatant liquor production crystal level high purity niobium oxide is decomposed in a kind of direct utilization according to claim 1, it is characterized in that: 850 DEG C ± 10 DEG C of calcining temperatures in described step f, calcination time 6 ± 1h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109292822A (en) * | 2018-12-17 | 2019-02-01 | 株洲硬质合金集团有限公司 | A kind of preparation method of High-density Niobium Oxide |
| CN110563038A (en) * | 2019-09-25 | 2019-12-13 | 九江有色金属冶炼有限公司 | method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108543A (en) * | 1986-12-15 | 1988-07-13 | 包钢钢铁研究所 | The method of preparing optical grade niobium oxide from waste slags of niobium metallurgy |
| US20080291605A1 (en) * | 2003-07-15 | 2008-11-27 | H.C. Starck Gmbh | Niobium suboxide powder |
| CN102424420A (en) * | 2011-09-15 | 2012-04-25 | 宜春市金洋稀有金属有限公司 | Method for preparing niobium pentoxide by using ferrocolumbium as raw material |
| CN103408070A (en) * | 2013-08-09 | 2013-11-27 | 九江有色金属冶炼有限公司 | Technological method for removing antimony in preparation of high-pure niobium oxide by niobium tantalite |
-
2014
- 2014-04-29 CN CN201410177680.4A patent/CN103936072B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108543A (en) * | 1986-12-15 | 1988-07-13 | 包钢钢铁研究所 | The method of preparing optical grade niobium oxide from waste slags of niobium metallurgy |
| US20080291605A1 (en) * | 2003-07-15 | 2008-11-27 | H.C. Starck Gmbh | Niobium suboxide powder |
| CN102424420A (en) * | 2011-09-15 | 2012-04-25 | 宜春市金洋稀有金属有限公司 | Method for preparing niobium pentoxide by using ferrocolumbium as raw material |
| CN103408070A (en) * | 2013-08-09 | 2013-11-27 | 九江有色金属冶炼有限公司 | Technological method for removing antimony in preparation of high-pure niobium oxide by niobium tantalite |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109292822A (en) * | 2018-12-17 | 2019-02-01 | 株洲硬质合金集团有限公司 | A kind of preparation method of High-density Niobium Oxide |
| CN109292822B (en) * | 2018-12-17 | 2021-01-26 | 株洲硬质合金集团有限公司 | Preparation method of niobium pentoxide with high apparent density |
| CN110563038A (en) * | 2019-09-25 | 2019-12-13 | 九江有色金属冶炼有限公司 | method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite |
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| CN103936072B (en) | 2015-08-26 |
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Address after: 510900 Conghua Province, Guangzhou City, the town of red grass Patentee after: Guangdong Guangsheng photoelectric rare metal new material Co Ltd Address before: 510900 Conghua Province, Guangzhou City, the town of red grass Patentee before: CONGHUA TANTALUM & NIOBIUM SMELTERY |