CN105950877A - Method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water - Google Patents
Method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water Download PDFInfo
- Publication number
- CN105950877A CN105950877A CN201610370654.2A CN201610370654A CN105950877A CN 105950877 A CN105950877 A CN 105950877A CN 201610370654 A CN201610370654 A CN 201610370654A CN 105950877 A CN105950877 A CN 105950877A
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- CN
- China
- Prior art keywords
- vanadium
- remove impurity
- wastewater
- slag
- reclaim
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
Abstract
The invention discloses a method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water. The method comprises the following steps: (a) the impurity removing slag is leached by using the vanadium precipitation waste water to obtain acid vanadium-contained leaching liquid; (b) ion exchange resins are used for absorbing vanadium enriched in the acid vanadium-contained leaching liquid to form vanadium-contained resins; (c) the vanadium-contained resins are desorbed by alkali solution to obtain vanadium-contained desorbing liquid; and (d) the vanadium precipitation treatment is performed for the vanadium-contained desorbing liquid to obtain ammonium metavanadate or ammonium vanadate; and vanadium oxides are prepared by calcining ammonium metavanadate or ammonium vanadate. The method for recovering vanadium in silicon removing slag can effectively recover vanadium in the impurity removing slag; and the vanadium precipitation waste water is used.
Description
Technical field
The present invention relates to a kind of chemical substance recovery method, be specifically related to one and utilize vanadium wastewater to reclaim remove impurity
In slag, the method for vanadium, belongs to chemical field.
Background technology
Containing in navajoite vanadium extracting process, vanadium leachate can with impurity Si, P, As etc. more or less, because of
This must carry out deep impurity-removing operation in preparation high-purity vanadium oxide product process, and leachate is through chemical precipitation
A certain amount of remove impurity slag (including dephosphorization underflow slag, arsenic removal slag and desilication slag) can be produced after method remove impurity, the quantity of slag with
Impurity content changes.What this impurity-removing method was difficult to avoid that damages with certain vanadium, cause in remove impurity slag containing 3%～
The vanadium of 10% (mass percent).
Recovery currently for the vanadium in remove impurity slag does not also have reasonable method.
Summary of the invention
It is an object of the present invention to provide a kind of method of vanadium in high efficiente callback remove impurity slag, and remove in recovery
In miscellaneous slag during vanadium, it is also possible to make full use of vanadium wastewater, there is the effect of a kind of waste's reclamation
Really.
The present invention is achieved in that
A kind of utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, comprise the following steps:
A. by vanadium wastewater, remove impurity slag is leached, obtain acid containing vanadium leachate；
B. acid containing the vanadium formation resin Han vanadium in vanadium leachate described in spent ion exchange resin adsorption and enrichment；
C. obtain containing vanadium stripping liquid with the resin Han vanadium described in alkaline solution desorbing；
D. carry out precipitation process to containing vanadium stripping liquid, obtain ammonium metavanadate or ammonium poly-vanadate, ammonium metavanadate or many
Ammonium vanadate prepares barium oxide after calcining.
Further scheme is, described remove impurity slag is for prepare vanadium goods or high-purity vanadium oxide containing navajoite or vanadium slag
Product produces in remove impurity or purge process.
Further scheme is, described vanadium wastewater is to carry out precipitation under acid condition to operate the water-soluble of generation
Liquid, including at least one in Upper-liquor of Precipitating Vanadate Process or wash water.
Further scheme is, in step a: leach remove impurity slag by vanadium wastewater, during need
Stir.
Further scheme is, in step a, leaches remove impurity slag by vanadium wastewater, and the time controls
30～90min.
Further scheme is, in step a, leaches remove impurity slag by vanadium wastewater, vanadium wastewater
With the consumption weight liquid-solid ratio of remove impurity slag it is: (1 to 10): 1.
Further scheme is, ion exchange resin is anion exchange resin.
Further scheme is, in step c, alkaline solution, including sodium hydroxide, potassium hydroxide, carbon
Acid sodium, potassium carbonate, sodium bicarbonate aqueous solution in one.
Further scheme is, in step c, during desorbing, the anion concentration of alkaline solution used controls 2
To 3mol/L, the vanadium hydraulic control V content after desorbing is more than 20g/L.
In the recovery desilication slag of the present invention, the method for vanadium has the advantage that
(1) vanadium in energy efficient recovery remove impurity slag, the response rate is more than 90%；
(2) vanadium wastewater can be made to be obtained by, it is to avoid to pollute.
Detailed description of the invention
Hereinafter, the vanadium wastewater that utilizes combining the exemplary embodiment specific descriptions present invention is reclaimed remove impurity
The method of vanadium in slag.
Method comprises the following steps according to an exemplary embodiment of the present invention:
Step a:
Use vanadium wastewater that remove impurity slag is leached, obtain acid containing vanadium leachate.
Wherein, remove impurity slag is for carrying out during preparing vanadium goods or high-purity vanadium oxide product containing navajoite or vanadium slag
The slag produced in remove impurity or purge process, the content of vanadium in this remove impurity slag is generally 3～10wt%.Used
Vanadium wastewater can be at least one in the Upper-liquor of Precipitating Vanadate Process that produces of acid precipitation operation or wash water；Control acid
The leaching time is 30～90min, to guarantee that the vanadium in remove impurity slag can leach effectively.Meanwhile, in order to fully beat
Remove miscellaneous slag and make it be fully contacted with vanadium wastewater, being preferably stirred during whole acidleach.
Step b:
Use anion exchange resin to adsorb and be enriched with described acidity and contain the vanadium in vanadium leachate, obtain containing vanadium tree
Fat.
Step c:
Use the resin Han vanadium described in alkali liquor desorbing, obtain containing vanadium stripping liquid.
Step d:
Carry out precipitation process by described containing vanadium stripping liquid, obtain ammonium metavanadate or ammonium poly-vanadate, by ammonium metavanadate
Or prepare qualified barium oxide (such as vanadic anhydride product) after ammonium poly-vanadate calcining.Wherein, precipitation processes
Can carry out by such as adding the ammonium salt such as ammonium sulfate or ammonium chloride, calcining can use Muffle furnace to carry out, precipitation
Being techniques known in the art means with calcining, therefore not to repeat here.
Below in conjunction with concrete example, the detailed description of the invention of the present invention is further described, the most therefore will
Limit the invention among described example ranges.Further, unless otherwise noted, this specification relates to
Percentage ratio is all weight percentage.
Embodiment 1
Take in the vanadium wastewater (pH=3) that 200g desilication slag (containing vanadium 3.17%) joins 600ml, stirring
Persistently leach filtration washing after 30min, obtain containing vanadium leachate 542ml (the wherein 11.07g/L Han vanadium).So
Adsorb with 717 anion exchange resin afterwards and be enriched with containing the vanadium in vanadium leachate, obtaining containing vanadium resin.With
Sodium hydroxide solution 300ml desorbing resin Han vanadium of 2mol/L, it is thus achieved that 268mL containing vanadium stripping liquid (wherein
Containing vanadium 22.17g/L).Ammonium metavanadate is obtained to containing addition 25g ammonium sulfate precipitation in vanadium stripping liquid.By metavanadic acid
Ammonium calcines 2h deamination in 500 DEG C in being placed in Muffle furnace, it is thus achieved that vanadic anhydride 9.12g, wherein containing V2O5
99.07wt%.
Embodiment 2
Take in the vanadium wastewater (pH=2.5) that 200g dephosphorization underflow slag (containing vanadium 7.15%) joins 900ml,
Filtration washing after 90min is persistently leached in stirring, obtains containing vanadium leachate 965ml (the wherein 14.51g/L Han vanadium).
Then adsorb with D201 anion exchange resin and be enriched with containing the vanadium in vanadium leachate, obtaining containing vanadium resin.With
Sodium hydroxide solution 400ml desorbing resin Han vanadium of 3mol/L, it is thus achieved that 356mL containing vanadium stripping liquid (wherein
Containing vanadium 39.40g/L).Ammonium poly-vanadate is obtained to containing addition 56g ammonium sulfate precipitation in vanadium stripping liquid.By many vanadic acid
Ammonium calcines 2h deamination in 500 DEG C in being placed in Muffle furnace, it is thus achieved that vanadic anhydride 24.92g, wherein containing V2O5
99.54wt%.
Embodiment 3
Take in the vanadium wastewater (pH=2.8) that 200g arsenic removal slag (containing vanadium 5.10%) joins 700ml, stir
Mix and persistently leach filtration washing after 60min, obtain containing vanadium leachate 730ml (the wherein 12.01g/L Han vanadium).
Then adsorb with 717 anion exchange resin and be enriched with containing the vanadium in vanadium leachate, obtaining containing vanadium resin.With
Sodium hydroxide solution 300ml desorbing resin Han vanadium of 2mol/L, with obtain 285mL containing vanadium stripping liquid (its
In the 29.8g/L Han vanadium).Ammonium metavanadate is obtained to containing addition 30g ammonium sulfate precipitation in vanadium stripping liquid.By inclined vanadium
Acid ammonium calcines 2h deamination in 500 DEG C in being placed in Muffle furnace, it is thus achieved that vanadic anhydride 15.07g, wherein containing V2O5
99.26wt%.
The vanadium recovery of the inventive method is high, technique is simple, environmental friendliness, and the product purity obtained is high.
Though the present invention of having specifically described, it will be appreciated by those skilled in the art that, without departing from
In the case of the spirit and scope of the present invention, the present invention can be made various forms of change.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, and above-described embodiment is only
For the present invention preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, it should
Understanding, those skilled in the art can be designed that a lot of other amendments and embodiment, and these are revised and real
The mode of executing will fall within spirit disclosed in the present application and spirit.
Claims (9)
1. one kind utilizes vanadium wastewater to reclaim the method for vanadium in remove impurity slag, it is characterised in that comprise the following steps:
A. by vanadium wastewater, remove impurity slag is leached, obtain acid containing vanadium leachate；
B. acid containing the vanadium formation resin Han vanadium in vanadium leachate described in spent ion exchange resin adsorption and enrichment；
C. obtain containing vanadium stripping liquid with the resin Han vanadium described in alkaline solution desorbing；
D. carry out precipitation process to containing vanadium stripping liquid, obtain ammonium metavanadate or ammonium poly-vanadate, ammonium metavanadate or many
Ammonium vanadate prepares barium oxide after calcining.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
In described remove impurity slag for preparing remove impurity or purification mistake in vanadium goods or high-purity vanadium oxide product containing navajoite or vanadium slag
Journey produces.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
Under described vanadium wastewater is acid condition, carry out the aqueous solution that precipitation operation produces, including Upper-liquor of Precipitating Vanadate Process or
At least one in wash water.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
In step a: by vanadium wastewater, remove impurity slag is leached, during need stirring.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
In leaching remove impurity slag by vanadium wastewater, the time controls 30～90min.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
In step a, by vanadium wastewater, remove impurity slag is leached, vanadium wastewater and the consumption weight liquid of remove impurity slag
Gu ratio is: (1 to 10): 1.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
It is anion exchange resin in described ion exchange resin.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
In step c, alkaline solution, including sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, bicarbonate
One in the aqueous solution of sodium.
The most according to claim 1, utilize vanadium wastewater to reclaim the method for vanadium in remove impurity slag, its feature exists
In step c, during desorbing, the anion concentration of alkaline solution used controls at 2 to 3mol/L, after desorbing
Vanadium hydraulic control V content is more than 20g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610370654.2A CN105950877A (en) | 2016-05-27 | 2016-05-27 | Method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water |
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| CN201610370654.2A CN105950877A (en) | 2016-05-27 | 2016-05-27 | Method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502747A (en) * | 2017-10-13 | 2017-12-22 | 重庆大学 | It is a kind of with microemulsion from vanadium wastewater extracting vanadium method |
| CN107739832A (en) * | 2017-10-25 | 2018-02-27 | 成都先进金属材料产业技术研究院有限公司 | The method for reclaiming vanadium in oxygen-enriched air roasting acidity precipitation waste liquid |
| CN108285239A (en) * | 2018-04-11 | 2018-07-17 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of process for treating waste liquor and system |
| CN110438336A (en) * | 2019-09-09 | 2019-11-12 | 宁夏京成天宝饲料添加剂有限公司 | A method of extracting vanadic anhydride from containing descloizite |
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| CN102337410A (en) * | 2011-10-19 | 2012-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium from dephosphorization base flow residues |
| CN102337411A (en) * | 2011-10-19 | 2012-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium and chromium from high-chromium low-vanadium vanadium precipitation wastewater |
| CN102337409A (en) * | 2011-10-19 | 2012-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium from dephosphorization bottom flow residues |
| CN102876895A (en) * | 2012-10-09 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium and chromium from low-concentration pentavalent vanadium and hexavalent chromium mixed liquor |
| CN103572062A (en) * | 2013-10-17 | 2014-02-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium from desilication slag |
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2016
- 2016-05-27 CN CN201610370654.2A patent/CN105950877A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102337410A (en) * | 2011-10-19 | 2012-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium from dephosphorization base flow residues |
| CN102337411A (en) * | 2011-10-19 | 2012-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium and chromium from high-chromium low-vanadium vanadium precipitation wastewater |
| CN102337409A (en) * | 2011-10-19 | 2012-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium from dephosphorization bottom flow residues |
| CN102876895A (en) * | 2012-10-09 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium and chromium from low-concentration pentavalent vanadium and hexavalent chromium mixed liquor |
| CN103572062A (en) * | 2013-10-17 | 2014-02-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium from desilication slag |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502747A (en) * | 2017-10-13 | 2017-12-22 | 重庆大学 | It is a kind of with microemulsion from vanadium wastewater extracting vanadium method |
| CN107739832A (en) * | 2017-10-25 | 2018-02-27 | 成都先进金属材料产业技术研究院有限公司 | The method for reclaiming vanadium in oxygen-enriched air roasting acidity precipitation waste liquid |
| CN108285239A (en) * | 2018-04-11 | 2018-07-17 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of process for treating waste liquor and system |
| CN110438336A (en) * | 2019-09-09 | 2019-11-12 | 宁夏京成天宝饲料添加剂有限公司 | A method of extracting vanadic anhydride from containing descloizite |
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Application publication date: 20160921 |
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