CN103936072B - A kind of directly utilization decomposes the technique that crystal level high purity niobium oxide produced by supernatant liquor - Google Patents
A kind of directly utilization decomposes the technique that crystal level high purity niobium oxide produced by supernatant liquor Download PDFInfo
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- CN103936072B CN103936072B CN201410177680.4A CN201410177680A CN103936072B CN 103936072 B CN103936072 B CN 103936072B CN 201410177680 A CN201410177680 A CN 201410177680A CN 103936072 B CN103936072 B CN 103936072B
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Abstract
The present invention relates to a kind of direct utilization and decompose the technique that crystal level high purity niobium oxide produced by supernatant liquor, this technique comprises following steps: separation of supernatant, acid adjustment, essence are filtered, adopted sec-octyl alcohol to be that extraction agent extracts, through extraction, reextraction obtains high purity niobium liquid, liquefied ammonia neutralization obtains niobium hydroxide and proceeds to pressure filter, solid-liquid separation obtains niobium hydroxide solid, and carry out press filtration, washing, oven dry, calcining with pure water, sieve after calcining, obtain crystal level high purity niobium oxide.Supernatant liquor after present invention process extracting directly niobite dissolves, high-purity niobium liquid based on it, preparation process adopts sec-octyl alcohol to be extraction agent, by controlling the acidity of comparing in extraction process, pickling agent and anti-niobium agent, only need single extraction operation can obtain standard compliant high purity niobium liquid, its Production Flow Chart is more simple, and all ingredients consumed and the energy are less, and quality product is more stable.
Description
Technical field:
The present invention relates to the technical field of producing of niobium oxides, refer in particular to a kind of direct utilization and decompose the technique that crystal level high purity niobium oxide produced by supernatant liquor.
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 impurity elements such as such as Fe, Mn, Ti.Current niobium liquid preparation is the rear directly acid adjustment of niobite dissolving and filters to obtain filtrate, first obtain niobium liquid through single extraction, then can obtain high purity niobium liquid with the niobium liquid that this extraction is qualified through again extracting, 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 that crystal level high purity niobium oxide produced by supernatant liquor.
The technical scheme that the present invention realizes the employing of its object is: a kind of direct utilization decomposes the technique that crystal level high purity niobium oxide produced by supernatant liquor, and this technique comprises following steps:
A. the niobite rear industrial hydrofluoric acid of grinding and industrial sulphuric acid are decomposed, separation of supernatant after decomposing;
B. in supernatant liquor, add industrial hydrofluoric acid and industrial sulphuric acid carries out acid adjustment, make acidity meet extraction requirement;
C. carry out essence to the supernatant liquor after acid adjustment to filter;
D. filter to essence the clean supernatant liquor obtained to extract, employing sec-octyl alcohol 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 niobium hydroxide through liquefied ammonia neutralization and proceeds to pressure filter, solid-liquid separation obtains niobium hydroxide solid, and carries out press filtration, washing with pure water;
F. the niobium hydroxide solid obtained after washing is proceeded to drying baker to dry;
G. calcining proceeding to push away in boat stove after the niobium hydroxide solid abrasive dust after oven dry, sieving after calcining, obtaining crystal level high purity niobium oxide.
In above-mentioned technique, in described step a, niobite decomposition is carried out at normal temperatures and pressures, during decomposition, by weight, and 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%, and industrial sulphuric acid density is 1.84g/cm
3, its concentration is 95%, resolving time 16h.
In described step b, acidity control is at HF 5.5 ~ 6mol/L, H
2sO
42.5 ~ 3mol/L.
Aperture is adopted to be that the PE microfiltration tube of 0.5 micron carries out essence and filters in described step c.
In described steps d extraction process, pickling extraction section is in a ratio of organic phase: aqueous phase=1:0.6 ~ 1, and reextraction section is in a ratio of organic phase: aqueous phase=2:1, and pickling agent is the chemical pure sulfuric acid of acidity 3.5mol/L, and anti-niobium agent is the chemical pure sulfuric acid of acidity 1.5mol/L.
In described step e, pure water consumption is by 60 ~ 80L/kgNb
2o
5.
Bake out temperature 100 ± 10 DEG C in described step f, drying time 10 ± 1h.
Calcining temperature 850 DEG C ± 10 DEG C in described step f, calcination time 6 ± 1h.
Supernatant liquor after present invention process extracting directly niobite dissolves, high-purity niobium liquid based on it, preparation process adopts sec-octyl alcohol to be extraction agent, by controlling the acidity of comparing in extraction process, pickling agent and anti-niobium agent, only need single extraction operation can obtain standard compliant high purity niobium liquid, its Production Flow Chart is more simple, and all ingredients consumed and the energy are less, and quality product is more stable.The high purity niobium oxide adopting production technique of the present invention to produce all can reach the quality standard of rower [YS/T 548-2007] 04 grade of crystal level high purity niobium oxide, 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. by dropping into the decomposer of diameter 3m × 3m after niobite grinding, decomposing with industrial hydrofluoric acid and industrial sulphuric acid, decomposing and carry out at normal temperatures and pressures, during 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%, and industrial sulphuric acid density is 1.84g/cm
3, its concentration is 95%, and resolving time 16h, isolates supernatant liquor after decomposition;
B. in supernatant liquor, add industrial hydrofluoric acid and industrial sulphuric acid carries out acid adjustment, make acidity control at HF 5.5 ~ 6mol/L, H
2sO
42.5 ~ 3mol/L, meets extraction requirement;
C. the PE microfiltration tube being 0.5 micron to the supernatant liquor employing aperture after acid adjustment carries out essence and filters; Its effect removes molecule in supernatant liquor and floating matter further, obtains clean supernatant liquor;
D. filter to essence the clean supernatant liquor obtained to extract, employing sec-octyl alcohol is extraction agent, add in extraction process acidity be 3.5mol/L (equivalent concentration 7N) chemical pure sulfuric acid control be in a ratio of organic phase: aqueous phase=1:0.6 ~ 1, in isolated organic phase, add acidity is again that the chemical pure sulfuric acid of 1.5mol/L (equivalent concentration 3N) is as anti-niobium agent, strip, and control reextraction section and be in a ratio of organic phase: aqueous phase=2:1, the aqueous phase obtained after reextraction is high purity niobium liquid; Extraction and anti-extraction process carry out in mixer-settler, and wherein pickling 10 grades, extracts 10 grades; Strip 12 grades;
E. high purity niobium liquid is obtained niobium hydroxide through liquefied ammonia neutralization and proceeds to pressure filter, make niobium hydroxide separate out under stress, 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 obtained after washing is proceeded to drying baker to dry, bake out temperature 100 ± 10 DEG C, drying time 10 ± 1h;
G. calcine proceeding to push away in boat stove after the niobium hydroxide solid abrasive dust after oven dry, calcining temperature 850 DEG C ± 10 DEG C, calcination time 6 ± 1h, sieves after calcining, obtains crystal level high purity niobium oxide.
The high purity niobium oxide adopting production technique of the present invention to produce all can reach the quality standard of rower [YS/T548-2007] 04 grade of crystal level high purity niobium oxide, and quality is more stable.
Adopt present invention process, metal recovery rate can reach 98.5%, the product of preparation identical weight, relatively existing technique, can save sulfuric acid dosage more than 40%, saves hydrofluoric acid consumption more than 70%, and saves energy more than 10%, therefore can reduce product cost greatly.
Claims (1)
1. directly utilize and decompose the technique that crystal level high purity niobium oxide produced by supernatant liquor, it is characterized in that: this technique comprises following steps:
A. the niobium minerals rear industrial hydrofluoric acid of grinding and industrial sulphuric acid are decomposed, separation of supernatant after decomposing;
B. in supernatant liquor, add industrial hydrofluoric acid and industrial sulphuric acid carries out acid adjustment, make acidity meet extraction requirement;
C. carry out essence to the supernatant liquor after acid adjustment to filter;
D. filter to essence the clean supernatant liquor obtained to extract, employing sec-octyl alcohol 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 obtained niobium hydroxide through liquefied ammonia neutralization and proceeds to pressure filter, carrying out solid-liquid separation, obtain niobium hydroxide solid, and carry out press filtration, washing with pure water;
F. the niobium hydroxide solid obtained after washing is proceeded to drying baker to dry;
G. calcining proceeding to push away in boat stove after the niobium hydroxide solid abrasive dust after oven dry, sieving after calcining, obtaining crystal level high purity niobium oxide;
Wherein, in described step a, niobite decomposition is carried out at normal temperatures and pressures, during decomposition, by weight, and 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%, and industrial sulphuric acid density is 1.84g/cm
3, its concentration is 95%, resolving time 16h;
In described step b, acidity control is at HF 5.5 ~ 6mol/L, H
2sO
42.5 ~ 3mol/L;
Aperture is adopted to be that the PE microfiltration tube of 0.5 micron carries out essence and filters in described step c;
In described steps d extraction process, pickling extraction section is in a ratio of organic phase: aqueous phase=1:0.6 ~ 1, and reextraction section is in a ratio of organic phase: aqueous phase=2:1, and pickling agent is the chemical pure sulfuric acid of acidity 3.5mol/L, and anti-niobium agent is the chemical pure sulfuric acid of acidity 1.5mol/L;
In described step e, pure water consumption is by 60 ~ 80L/kgNb
2o
5;
Bake out temperature 100 ± 10 DEG C in described step f, drying time 10 ± 1h;
Calcining temperature 850 DEG C ± 10 DEG C in described step f, calcination time 6 ± 1h.
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| CN201410177680.4A CN103936072B (en) | 2014-04-29 | 2014-04-29 | A kind of directly utilization decomposes the technique that crystal level high purity niobium oxide produced by supernatant liquor |
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| CN201410177680.4A CN103936072B (en) | 2014-04-29 | 2014-04-29 | A kind of directly utilization decomposes the technique that crystal level high purity niobium oxide produced by supernatant liquor |
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| 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 |
Citations (3)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1498391B1 (en) * | 2003-07-15 | 2010-05-05 | H.C. Starck GmbH | Niobium suboxide |
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2014
- 2014-04-29 CN CN201410177680.4A patent/CN103936072B/en active Active
Patent Citations (3)
| 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 |
| 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 |
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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 |