CN103937978A - Method for extracting vanadium from vanadium-containing raw material roasted clinker through ammonia leaching - Google Patents
Method for extracting vanadium from vanadium-containing raw material roasted clinker through ammonia leaching Download PDFInfo
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- CN103937978A CN103937978A CN201410162944.9A CN201410162944A CN103937978A CN 103937978 A CN103937978 A CN 103937978A CN 201410162944 A CN201410162944 A CN 201410162944A CN 103937978 A CN103937978 A CN 103937978A
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- vanadium
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a method for extracting vanadium from vanadium-containing raw material roasted clinker through ammonia leaching. The method comprises the following steps: leaching the vanadium-containing raw material roasted clinker to extract vanadium, so as to enable vanadium to enter solution in a manner of ammonium vanadate, to obtain leaching residues and vanadium-containing liquid, and performing ammonia evaporation and separation, ammonium vanadate cooling crystallization and separation, and ammonium vanadium calcination to the vanadium-containing liquid, to obtain a vanadium pentoxide product. By adopting the ammonium water leaching technology, the method is simple in flow, and easy to operate, the vanadium extraction rate can achieve 85-99%, and the high-efficiency extraction of vanadium can be realized.
Description
Technical field
The invention belongs to vanadium chemical industry metallurgical technical field, relate in particular to a kind of method containing grog ammonia leaching and vanadium extraction after vanadium raw materials roasting.
Background technology
Vanadium titano-magnetite, vanadium slag, bone coal etc. are the vanadium extraction of roasting-water logging/pickling process containing the traditional extraction vanadium method of vanadium raw materials, are wherein the main stream approach of vanadium extraction containing vanadium raw materials sodium roasting-water logging.The ultimate principle of sodium roasting technique is with Na
2cO
3, NaCl, Na
2sO
4be additive Deng sodium salt, the sodium salt of water-soluble pentavalent vanadium will be converted into containing the vanadium of vanadium raw materials middle or low price state by high-temperature roasting (750-850 DEG C), again to the direct water logging of sodium roasting product, obtain the leaching liquid containing vanadium, after add ammonium salt to make ammonium poly-vanadate precipitation, after reducing roasting, obtain the oxide product of vanadium.Sodium roasting technique vanadium recovery is low, and single roasting vanadium recovery is 70% left and right, and after roasting repeatedly, the rate of recovery of vanadium is only also 80%; And need repeatedly roasting, energy consumption is higher; In roasting process, can produce harmful HCl, Cl
2deng aggressive gas, the heavy process of follow-up ammonia can obtain high salinity nitrogen-containing wastewater, not only contaminate environment, and also improvement cost is higher.
In order to solve the problem of sodium roasting, CN101161831A has proposed a kind of method of vanadium slag calcification baking, vanadium slag and lime or Wingdale are mixed and directly enter 600 DEG C of above stoving ovens and carry out calcification baking afterwards, make the vanadium in vanadium slag be converted into vanadic acid calcium, roasting grog makes vanadium dissolve and enters solution under the acidleach effect of sulphuric acid soln, and then produces the products such as barium oxide.The elements such as calcification baking grog acidleach process Fe, P also enter leach liquor together with vanadium, and later separation is more difficult.
The high temperature vanadium slag that also has CN1082617A to propose blowing to obtain is processed 900~1300 DEG C of direct oxygen blast, impel the Low Valent Vanadium in slag to be oxidized into pentavalent vanadium, after the cooling fragmentation of slag, vanadium under certain temperature, alkali concn, oxygen partial pressure in leached mud, the method needn't be in high-temperature roasting again after vanadium slag cooling, and energy consumption greatly reduces, and the environmental pollution of having avoided sodium roasting to cause, but exist metallic iron to reclaim, and the low problem of vanadium recovery.
CN101899582A proposes a kind of method of being extracted Vanadium Pentoxide in FLAKES by vanadium slag, vanadium slag is in 800~1000 DEG C of roastings, grog soaks through the alkali lye alkali of 20~50% alkali concns, after obtain sodium vanadate crystal through silica removal, crystallisation by cooling, after obtain ammonium vanadate through turning molten, acid ammonium salt precipitation.The method exists that impurity is difficult to remove, the problem of filtration difficulty, the problem of simultaneously keeping away unavoidable acid ammonia nitrogen waste water, and its vanadium recovery is lower than 90%.
But, at present there are no using ammonia soln directly to leach the relevant report containing vanadium raw materials roasting grog.
Summary of the invention
For the deficiencies in the prior art, one of object of the present invention is to provide a kind of method containing grog ammonia leaching and vanadium extraction after vanadium raw materials roasting.With respect to existing roasting grog leaching method, the method V leaching rate is high, and does not enter leach liquor containing other impurity in vanadium raw materials, and follow-up ammonium vanadate separates simple.
For reaching above-mentioned purpose, the present invention is achieved through the following technical solutions:
Containing a method for grog ammonia leaching and vanadium extraction after vanadium raw materials roasting, will in ammoniacal liquor, leach vanadium extraction containing grog after vanadium raw materials roasting, make vanadium enter solution with ammonium vanadate form, obtain leached mud and solution containing vanadium.Be converted into the pentavalent vanadium that can leach at roasting process containing trivalent vanadium wherein after vanadium raw materials roasting, pentavalent vanadium can react with ammoniacal liquor generation ammonium vanadate, thereby vanadium is extracted from raw material.
As optimal technical scheme, method of the present invention, the described vanadium raw materials that contains is vanadium titano-magnetite, bone coal, vanadium slag, contains the one kind or two or more mixture in chrome alum slag or vanadium containing catalysts; Wherein vanadium containing catalysts can be also the catalyzer that cannot reuse after using for the catalyzer before using;
As optimal technical scheme, method of the present invention, described roasting is the one kind or two or more combination in calcification baking, sodium roasting, blank roasting (being additive-free roasting).
As optimal technical scheme, method of the present invention, the mass concentration of described ammoniacal liquor is 0.1~40%, the mass concentration of ammoniacal liquor is lower than 0.1%, and the extraction yield of vanadium is very low, the more difficult acquisition of ammoniacal liquor higher than 40%, can greatly increase the cost of vanadium extraction, therefore, it is 0.1~40% that the present invention selects the mass concentration of ammoniacal liquor, is preferably 1~30%.
As optimal technical scheme, method of the present invention, the temperature of described leaching is normal temperature~180 DEG C, be for example 25 DEG C, 35 DEG C, 50 DEG C, 80 DEG C, 100 DEG C, 130 DEG C, 145 DEG C, 170 DEG C etc., temperature is too low low containing the vanadium leaching efficiency in grog after vanadium raw materials roasting, and 180 DEG C time, the leaching yield of various different roasting grog vanadium is very high, the extraction temperature that raises is again nonsensical, therefore, selectively leaching temperature of the present invention is normal temperature~180 DEG C, is preferably 120~150 DEG C.
As optimal technical scheme, method of the present invention, the time of described leaching is more than 0.5h, for example, be 1h, 2.5h, 3h, 4.5h etc., and extraction time is too short as lower than 0.5h, and the extraction efficiency of vanadium is low, is preferably 1~4h.
As optimal technical scheme, method of the present invention, in the process of described leaching, ammoniacal liquor and the liquid-solid ratio containing grog after vanadium raw materials roasting are 2:1~10:1ml/g, be for example 4:1ml/g, 7:1ml/g, 9:1ml/g etc., it is poor that liquid-solid ratio is reacted liquid-solid mass transfer below 2ml/g, is difficult to realize, and liquid-solid ratio vanadium meltage in 10ml/g leach liquor is enough, improve liquid-solid ratio nonsensical again, be preferably 3:1~6:1ml/g.
As optimal technical scheme, method of the present invention, comprises the steps:, by leaching vanadium extraction in the ammoniacal liquor that is 0.1~40% in mass concentration containing grog after vanadium raw materials roasting, to make vanadium enter solution with ammonium vanadate form, obtains leached mud and solution containing vanadium;
Wherein, the temperature of leaching is normal temperature~180 DEG C, and the time of leaching is more than 0.5h, and in the process of leaching, ammoniacal liquor and the liquid-solid ratio containing grog after vanadium raw materials roasting are 2:1~10:1ml/g.
The present invention compares traditional roasting grog water logging/acid leaching process, and vanadium leaching rate is high, and impurity do not enter solution containing vanadium, can realize simple, the clean separation of vanadium.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
By V
2o
5content is that 12.8% vanadium slag leaches vanadium extraction at 900 DEG C of grogs that obtain after blank roasting at 30% ammonia soln, and extraction temperature is 160 DEG C, and leaching liquid-solid ratio is 5ml/g, and extraction time is 3h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 94.2%.
Embodiment 2
By V
2o
5content is that 2.1% vanadium titano-magnetite leaches vanadium extraction at 750 DEG C of grogs that obtain after sodium roasting at 15% ammonia soln, and extraction temperature is 140 DEG C, and leaching liquid-solid ratio is 8ml/g, and extraction time is 1h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 85.2%.
Embodiment 3
By V
2o
5content is that 10.6% vanadium slag leaches vanadium extraction at 800 DEG C of grogs that obtain after calcification baking at 20% ammonia soln, and extraction temperature is 150 DEG C, and leaching liquid-solid ratio is 4ml/g, and extraction time is 2h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 91.4%.
Embodiment 4
By V
2o
5content is that 1.6% bone coal leaches vanadium extraction at 850 DEG C of grogs that obtain after blank roasting at 25% ammonia soln, and extraction temperature is 130 DEG C, and leaching liquid-solid ratio is 6ml/g, and extraction time is 3h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 86.5%.
Embodiment 5
By V
2o
5content is that 8.7% vanadium containing catalysts leaches vanadium extraction at 750 DEG C of grogs that obtain after blank roasting at 10% ammonia soln, and extraction temperature is 120 DEG C, and leaching liquid-solid ratio is 6ml/g, and extraction time is 2h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 88.2%.
Embodiment 6
By V
2o
5content is that 7.5% vanadium containing catalysts leaches vanadium extraction at 700 DEG C of grogs that obtain after blank roasting at 35% ammonia soln, and extraction temperature is 180 DEG C, and leaching liquid-solid ratio is 3ml/g, and extraction time is 0.5h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 89.1%.
Embodiment 7
By V
2o
5content is that 8.3% vanadium containing catalysts leaches vanadium extraction at 780 DEG C of grogs that obtain after blank roasting at 5% ammonia soln, and extraction temperature is 50 DEG C, and leaching liquid-solid ratio is 10ml/g, and extraction time is 4h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 85.1%.
Embodiment 8
By V
2o
5content is that 8.7% vanadium containing catalysts leaches vanadium extraction at 780 DEG C of grogs that obtain after blank roasting at 1% ammonia soln, and extraction temperature is 110 DEG C, and leaching liquid-solid ratio is 6ml/g, and extraction time is 3h, obtains leached mud and ammonia soaks solution containing vanadium.Leached mud is through washing, dry, weigh and analyze the content of vanadium of residue, and the rate of recovery of Vanadium in Vanadium Residue is 86.9%.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (8)
1. containing a method for grog ammonia leaching and vanadium extraction after vanadium raw materials roasting, it is characterized in that, will in ammoniacal liquor, leach vanadium extraction containing grog after vanadium raw materials roasting, make vanadium enter solution with ammonium vanadate form, obtain leached mud and solution containing vanadium.
2. method according to claim 1, is characterized in that, the described vanadium raw materials that contains is vanadium titano-magnetite, bone coal, vanadium slag, contains the one kind or two or more mixture in chrome alum slag or vanadium containing catalysts; Wherein vanadium containing catalysts can be also the catalyzer that cannot reuse after using for the catalyzer before using.
3. method according to claim 1 and 2, is characterized in that, described roasting is the one kind or two or more combination in calcification baking, sodium roasting, blank roasting.
4. according to the method described in claim 1-3 any one, it is characterized in that, the mass concentration of described ammoniacal liquor is 0.1~40%, is preferably 1~30%.
5. according to the method described in claim 1-4 any one, it is characterized in that, the temperature of described leaching is normal temperature~180 DEG C, is preferably 120~150 DEG C.
6. according to the method described in claim 1-5 any one, it is characterized in that, the time of described leaching is more than 0.5h, to be preferably 1~4h.
7. according to the method described in claim 1-6 any one, it is characterized in that, in the process of described leaching, ammoniacal liquor and the liquid-solid ratio containing grog after vanadium raw materials roasting are 2:1~10:1ml/g, are preferably 3:1~6:1ml/g.
8. method according to claim 1, is characterized in that, comprises the steps:, by leaching vanadium extraction in the ammoniacal liquor that is 0.1~40% in mass concentration containing grog after vanadium raw materials roasting, to make vanadium enter solution with ammonium vanadate form, obtains leached mud and solution containing vanadium;
Wherein, the temperature of leaching is normal temperature~180 DEG C, and the time of leaching is more than 0.5h, and in the process of leaching, ammoniacal liquor and the liquid-solid ratio containing grog after vanadium raw materials roasting are 2:1~10:1ml/g.
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Cited By (9)
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CN105779758A (en) * | 2016-03-03 | 2016-07-20 | 中国科学院过程工程研究所 | Method for extracting vanadium from vanadium-contained raw material clinker via ammonium oxalate leaching |
CN107090551A (en) * | 2017-04-25 | 2017-08-25 | 中国科学院过程工程研究所 | A kind of method of the direct vanadium extraction of vanadium titano-magnetite |
CN108893597A (en) * | 2018-08-03 | 2018-11-27 | 中南大学 | The technique of zinc is recycled from willemite resource |
CN109019687A (en) * | 2018-09-28 | 2018-12-18 | 东北大学 | A method of vanadic anhydride and chrome green are prepared using chromium type high vanadium slag |
CN109207745A (en) * | 2017-07-07 | 2019-01-15 | 中国科学院过程工程研究所 | A method of it leaches from ammonium oxalate containing separation ammonium metavanadate in vanadium raw materials roasting clinker solution |
CN110129552A (en) * | 2019-06-21 | 2019-08-16 | 东北大学 | A method of vanadic sulfide material is prepared using containing vanadium leachate |
CN111519032A (en) * | 2020-06-12 | 2020-08-11 | 攀钢集团研究院有限公司 | Vanadium slag treatment method |
CN114350982A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by using calcified roasting clinker and recycling leaching washing liquid |
CN115725862A (en) * | 2022-11-22 | 2023-03-03 | 东北大学 | Method for enhancing vanadium extraction of vanadium shale by microwave suspension roasting-alkali mixing curing |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105779758A (en) * | 2016-03-03 | 2016-07-20 | 中国科学院过程工程研究所 | Method for extracting vanadium from vanadium-contained raw material clinker via ammonium oxalate leaching |
CN107090551A (en) * | 2017-04-25 | 2017-08-25 | 中国科学院过程工程研究所 | A kind of method of the direct vanadium extraction of vanadium titano-magnetite |
CN109207745A (en) * | 2017-07-07 | 2019-01-15 | 中国科学院过程工程研究所 | A method of it leaches from ammonium oxalate containing separation ammonium metavanadate in vanadium raw materials roasting clinker solution |
CN108893597A (en) * | 2018-08-03 | 2018-11-27 | 中南大学 | The technique of zinc is recycled from willemite resource |
CN109019687A (en) * | 2018-09-28 | 2018-12-18 | 东北大学 | A method of vanadic anhydride and chrome green are prepared using chromium type high vanadium slag |
CN110129552A (en) * | 2019-06-21 | 2019-08-16 | 东北大学 | A method of vanadic sulfide material is prepared using containing vanadium leachate |
CN111519032A (en) * | 2020-06-12 | 2020-08-11 | 攀钢集团研究院有限公司 | Vanadium slag treatment method |
CN114350982A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by using calcified roasting clinker and recycling leaching washing liquid |
CN114350982B (en) * | 2021-11-30 | 2023-09-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium and recycling leaching washing liquid by calcified roasting clinker |
CN115725862A (en) * | 2022-11-22 | 2023-03-03 | 东北大学 | Method for enhancing vanadium extraction of vanadium shale by microwave suspension roasting-alkali mixing curing |
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