CN101274777A - Method for extracting vanadic anhydride from vanadium-containing liquid - Google Patents
Method for extracting vanadic anhydride from vanadium-containing liquid Download PDFInfo
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- CN101274777A CN101274777A CN 200710034640 CN200710034640A CN101274777A CN 101274777 A CN101274777 A CN 101274777A CN 200710034640 CN200710034640 CN 200710034640 CN 200710034640 A CN200710034640 A CN 200710034640A CN 101274777 A CN101274777 A CN 101274777A
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Abstract
The invention discloses a method for extracting vanadic oxide from a solution that contains vanadium, which is characterized in that: an extractant (N-235) and synergic reagents (sulfonated kerosene and TPB) are added to the solution containing the vanadium, then technical procedures of extraction, washing, back extraction, filtration, vanadium precipitation and calcination, etc. are carried out to obtain products that contain more than 98 percent of vanadium. The method of the invention selects the extractant (N-235) and the synergic reagents (sulfonated kerosene and TPB) of the solution that has high efficient separation, is concentrating, has low content and contains vanadium, thereby simplifying process flow, reducing production cost, improving the recovery ratio of the vanadium and realizing more than 97 percent of the recovery ratio of the vanadium in the solution containing vanadium; the total recovery ratio is more than 95 percent and the purity of the products is more than 98 percent.
Description
Technical field
The present invention relates to a kind of method of from the solution containing vanadium body, extracting Vanadium Pentoxide in FLAKES.
Background technology
Both at home and abroad the method for vanadium extraction has from liquid: (1) hydrolysis precipitation technology: vanadium liquid heating hydrolysis precipitation-dissolving-removal of impurities-filtration-precipitation-filter-calcine Vanadium Pentoxide in FLAKES technology.The reaction of this technological process is complicated, is subjected to the influence of factors such as character, concentration, acidity, temperature, impurity of solution bigger, and quality product is restive, about yield 70-80%.(2) ion exchange process, vanadium liquid are regulated certain pH value, vanadium liquid through upper prop-wash-out-removal of impurities-filtration-precipitation-filter-calcine Vanadium Pentoxide in FLAKES product technology.This technology has had raising to selectivity, and impurity has obtained effective control, and still, because the adsorptivity of resin still has impurity to bring product into, the removal of impurities meeting brings loss, and total recovery is about 80%.(3) precipitation technology adds precipitation agent in the solution containing vanadium body, through precipitation-filtration-leaching-removal of impurities-filtration-ammonium salt precipitation-filter-calcine Vanadium Pentoxide in FLAKES product technology.This technology precipitation and leaching process are complicated, wayward.(4) extraction process, vanadium liquid through extraction-washing-back extraction-precipitation-filter-calcine Vanadium Pentoxide in FLAKES product technology, this technology is because the difference of the extraction agent that adopts, all there are very big difference in yield, quality product, benefit.
Summary of the invention
The few method of from the solution containing vanadium body, extracting Vanadium Pentoxide in FLAKES of rate of recovery height, impurity that the purpose of this invention is to provide a kind of vanadium.
Technical scheme of the present invention is as follows: in the solution containing vanadium body in 5-25: 90-70: 5 ratio adds extraction agent (N-235) and synergist (sulfonated kerosene and TPB), the pH value of regulating the solution containing vanadium body is 1-3, water and organic phase extracted by 4: 1, vibrated 5-10 minute, left standstill 20-60 minute, and treated layering; After aqueous phase separation, use technology water washing organic phase 3-5 time; Adopt 1molNaCl-1mol NaOH system that organic phase is carried out back extraction, control aqueous phase content of vanadium is more than 20g/L; Through back extraction gained solution containing vanadium, regulate its pH value and be 7-8, add vanadiumcontent 1-3 NH doubly
4Cl, normal temperature stirred 10-30 minute down, left standstill 24 hours to such an extent that ammonium meta-vanadate precipitates; Filtration obtained the solid ammonium meta-vanadate, obtained the smart vanadium of purity＞98.% at 550 ℃ of oxidizing roasting 2-4 hours.
Method of the present invention is owing to selected a kind of extraction agent (N-235) and synergist (sulfonated kerosene and TPB) of high efficiency separation enrichment low levels solution containing vanadium body, simplified technical process, reduced production cost, improved the rate of recovery of vanadium, made that the yield of vanadium reaches more than 97% in the solution containing vanadium; Its total yield reaches more than 95%, and product purity reaches more than 98%.
Embodiment:
Embodiment one:
(1) extraction: with extraction agent (N-235), synergist (sulfonated kerosene and TPB), by 5: 90: 5 mixed, regulating the pH value that contains vanadium (2.15g/L) liquid was 1.5, and water and organic phase extracted by 4: 1, vibrated 5 minutes, left standstill 20 minutes, treated layering;
(2) washing: after aqueous phase separation, use technology water washing organic phase 4 times;
(3) back extraction: adopt 1mol NaCl-1mol NaOH system that organic phase is carried out back extraction, control aqueous phase content of vanadium is more than 20g/L;
(4) precipitation: through back extraction gained solution containing vanadium, regulating its pH value is 7.2, adds the NH of 2.5 times of vanadiumcontents
4Cl, normal temperature stirred 15 minutes down, left standstill 24 hours to such an extent that ammonium meta-vanadate precipitates;
(5) filter: filter and obtain the solid ammonium meta-vanadate;
(6) calcining: the smart vanadium that the solid ammonium meta-vanadate was obtained purity＞98.% at 550 ℃ of oxidizing roastings in 4 hours.
Embodiment two:
According to above-mentioned technological process,, mix by a certain percentage (10: 85: 5) extraction agent (N-235), synergist (sulfonated kerosene and TPB), the pH value that adjusting contains vanadium (2.15g/L) liquid is 2.0, water and organic phase extracted by 4: 1, vibrated 8 minutes, left standstill 40 minutes; After the water phase separated, use technology water washing organic phase 4 times; Adopt 1mol NaCl-1mol NaOH system that organic phase is carried out back extraction, control aqueous phase content of vanadium is more than 20g/L; Regulating its pH value is 7.4, adds the NH4Cl of 2 times of vanadiumcontents, and normal temperature stirred 20 minutes down, leaves standstill 24 hours to such an extent that ammonium meta-vanadate precipitates; Filtration obtains the solid ammonium meta-vanadate, obtains the smart vanadium of purity＞98.% in 3 hours at 550 ℃ of oxidizing roastings.
Embodiment three:
According to above-mentioned technological process,, mix by a certain percentage (20: 75: 5) extraction agent (N-235), synergist (sulfonated kerosene and TPB), the pH value that adjusting contains vanadium (2.15g/L) liquid is 2.5, water and organic phase extracted by 4: 1, vibrated 10 minutes, left standstill 50 minutes; After the water phase separated, use technology water washing organic phase 4 times; Adopt 1mol NaCl-1mol NaOH system that organic phase is carried out back extraction, control aqueous phase content of vanadium is more than 20g/L; Regulating its pH value is 7.1, adds the NH4Cl of 2.1 times of vanadiumcontents, and normal temperature stirred 15 minutes down, leaves standstill 24 hours to such an extent that ammonium meta-vanadate precipitates; Filtration obtains the solid ammonium meta-vanadate, obtains the smart vanadium of purity＞98.% in 4 hours at 550 ℃ of oxidizing roastings.
Claims (1)
1. method of from the solution containing vanadium body, extracting Vanadium Pentoxide in FLAKES, comprise processing steps such as extraction, washing, back extraction, filtration 1, precipitation and calcination, it is characterized in that it be in the solution containing vanadium body in 5-25: 90-70: 5 ratio adds extraction agent (N-235) and synergist (sulfonated kerosene and TPB), the pH value of regulating the solution containing vanadium body is 1-3, water and organic phase are by 1-4: 1 extracts, vibrated 5-10 minute, and left standstill and treated layering in 20-60 minute; After aqueous phase separation, use technology water washing organic phase 3-5 time; Adopt 1mol NaCl-1mol NaOH system that organic phase is carried out back extraction, control aqueous phase content of vanadium is more than 20g/L; Through back extraction gained solution containing vanadium, regulate its pH value and be 7-8, add vanadiumcontent 1-3 NH doubly
4Cl, normal temperature stirred 10-30 minute down, left standstill 24 hours to such an extent that ammonium meta-vanadate precipitates; Filtration obtained the solid ammonium meta-vanadate, obtained the smart vanadium of purity＞98.% at 550 ℃ of oxidizing roasting 2-4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200710034640 CN101274777A (en) | 2007-03-26 | 2007-03-26 | Method for extracting vanadic anhydride from vanadium-containing liquid |
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| CN 200710034640 CN101274777A (en) | 2007-03-26 | 2007-03-26 | Method for extracting vanadic anhydride from vanadium-containing liquid |
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| CN101274777A true CN101274777A (en) | 2008-10-01 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928830A (en) * | 2010-09-25 | 2010-12-29 | 吉首大学 | Method for extracting vanadium from vanadium-containing liquid |
| CN102826603A (en) * | 2012-09-20 | 2012-12-19 | 电子科技大学 | Preparation method of vanadium pentoxide nanofibers |
| CN102849795A (en) * | 2011-07-02 | 2013-01-02 | 全喆 | Preparation of high-purity vanadium pentoxide |
| WO2015161659A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for simultaneously preparing high-purity vanadium and heteropolyacid catalyst |
| CN106966431A (en) * | 2017-05-15 | 2017-07-21 | 天津市风船化学试剂科技有限公司 | A kind of preparation method of the high-purity ammonium metavanadate of 4N assigned stages |
-
2007
- 2007-03-26 CN CN 200710034640 patent/CN101274777A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928830A (en) * | 2010-09-25 | 2010-12-29 | 吉首大学 | Method for extracting vanadium from vanadium-containing liquid |
| CN102849795A (en) * | 2011-07-02 | 2013-01-02 | 全喆 | Preparation of high-purity vanadium pentoxide |
| CN102849795B (en) * | 2011-07-02 | 2014-12-17 | 全喆 | Preparation of high-purity vanadium pentoxide |
| CN102826603A (en) * | 2012-09-20 | 2012-12-19 | 电子科技大学 | Preparation method of vanadium pentoxide nanofibers |
| WO2015161659A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for simultaneously preparing high-purity vanadium and heteropolyacid catalyst |
| CN106966431A (en) * | 2017-05-15 | 2017-07-21 | 天津市风船化学试剂科技有限公司 | A kind of preparation method of the high-purity ammonium metavanadate of 4N assigned stages |
| CN106966431B (en) * | 2017-05-15 | 2018-10-16 | 天津市风船化学试剂科技有限公司 | A kind of preparation method of the high-purity ammonium metavanadate of 4N assigned stages |
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Open date: 20081001 |