CN107937737B - A method of reducing chromium content in high chromium calcium vanadate - Google Patents
A method of reducing chromium content in high chromium calcium vanadate Download PDFInfo
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- CN107937737B CN107937737B CN201711191213.7A CN201711191213A CN107937737B CN 107937737 B CN107937737 B CN 107937737B CN 201711191213 A CN201711191213 A CN 201711191213A CN 107937737 B CN107937737 B CN 107937737B
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- chromium
- calcium vanadate
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- vanadate
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of methods for reducing chromium content in high chromium calcium vanadate, belong to metallurgical technology field.The technical problem to be solved by the present invention is to higher for chromium content in current calcium vanadate, it is unfavorable for further preparing vanadium oxide product, a kind of method significantly reducing chromium content in high chromium calcium vanadate is provided.A method of reducing chromium content in high chromium calcium vanadate, comprising the following steps: A, add water to be beaten high chromium calcium vanadate, obtain slurry；B, sodium oxalate is added into slurry, after being stirred to react, is separated by solid-liquid separation, obtains low chromium calcium vanadate and de- chromium solution.The method of the present invention can effectively reduce the chromium content in calcium vanadate, and do not influence vanadium recovery by control sodium oxalate dosage and reaction condition, and vanadium and chromium in recyclable de- chromium solution, avoid the wasting of resources；The method of the present invention is easy to operate, mild condition, low in cost, is conducive to realize industrialization.
Description
Technical field
The invention belongs to metallurgical technology fields, and in particular to a method of reduce chromium content in high chromium calcium vanadate.
Background technique
Panxi Diqu possesses v-ti magnetite ore resources abundant, is the maximum vanadium and titanium resources location in China.Wherein, red lattice
Mine Fen Nankuang and Bei Kuang, be climb in the big v-ti magnetite mining area in Xisi (Tai Hekuang, Bai Makuang, mining heritages, Hongge Deposit) it is unique still
The mining area not large-scale developed and utilized.Red lattice south green ore iron, vanadium grade are suitable with the head grade in other mining areas Pan Xi, but chromium
Grade is 8~10 times of other mining areas.Studies have shown that " blast furnace ironmaking-vanadium extraction by converter blowing chromium " is current most industrialization prospect
Process flow is coexisted in slag using the process vanadium and chromium, is the raw material of further recycling vanadium, chromium.Vanadium chromium slag separation and Extraction
Studying main flow direction is to synchronize vanadium, chromium to be transformed into solution, further separates vanadium and chromium.Calcium salt precipitation method is molten from vanadium chromium
One of the method for Selective Separation vanadium in liquid, but obtained calcium vanadate chromium content is higher, is unfavorable for further preparing vanadium oxide production
Product.
It has not yet to see removing or reduces the relevant report of chromium content method in calcium vanadate, a kind of reduction vanadium need to be developed
The technology of chromium content in sour calcium.
Summary of the invention
In view of the above shortcomings of the prior art, chromium content in high chromium calcium vanadate is significantly reduced the present invention provides a kind of
Method, so that calcium vanadate is can satisfy the quality requirement for preparing vanadium oxide product.
A method of reducing chromium content in high chromium calcium vanadate, comprising the following steps:
A, add water to be beaten high chromium calcium vanadate, obtain slurry；
B, sodium oxalate is added into slurry, after being stirred to react, is separated by solid-liquid separation, obtains low chromium calcium vanadate and de- chromium solution.
Wherein, in the high chromium calcium vanadate of reduction described above in the method for chromium content, in step A, the high chromium calcium vanadate
Middle content of vanadium is with V2O5It is calculated as 32%~45%, chromium content is with Cr2O3It is calculated as 0.3%~1.0%, calcium content is calculated as 45% with CaO
~50%.
Wherein, in the high chromium calcium vanadate of reduction described above in the method for chromium content, in step A, the high chromium calcium vanadate
Solid-liquid mass ratio with water is 1:3~8.
Wherein, in the high chromium calcium vanadate of reduction described above in the method for chromium content, in step B, the sodium oxalate adds
Entering amount is C in sodium oxalate2O4 2-Mole and slurry in Ca2+Mole ratio be 0.3~0.5.
Wherein, described to be stirred to react in step B in the high chromium calcium vanadate of reduction described above in the method for chromium content
Temperature is 60~90 DEG C.
Wherein, described to be stirred to react in step B in the high chromium calcium vanadate of reduction described above in the method for chromium content
Time is 30~90min.
Wherein, in the high chromium calcium vanadate of reduction described above in the method for chromium content, in step B, the low chromium calcium vanadate
Middle chromium content is with Cr2O3It is calculated as≤0.2%.
Wherein, further comprising the steps of in the high chromium calcium vanadate of reduction described above in the method for chromium content:
C, chromium solution calcium salt precipitation method will be taken off obtained by step B separate vanadium, the chromium solution after obtaining calcium vanadate and precipitation, gained
Calcium vanadate is handled by step A and step B, and the chromium solution after gained precipitation further recycles chromium.
The beneficial effects of the present invention are:
Present approach provides a kind of techniques of chromium content in reduction calcium vanadate, pass through control sodium oxalate dosage and reaction
Condition can effectively reduce the chromium content in high chromium calcium vanadate, and not influence vanadium recovery, and oxidation is further prepared conducive to calcium vanadate
Vanadium；The vanadium and chromium in de- chromium solution have been recycled simultaneously, avoid the wasting of resources；The method of the present invention is easy to operate, mild condition, at
This is cheap, is conducive to realize industrialization.
Specific embodiment
Specifically, a kind of method for reducing chromium content in high chromium calcium vanadate, comprising the following steps:
A, add water to be beaten high chromium calcium vanadate, obtain slurry；
B, sodium oxalate is added into slurry, after being stirred to react, is separated by solid-liquid separation, obtains low chromium calcium vanadate and de- chromium solution.
Content of vanadium is in high chromium calcium vanadate with V2O5It is calculated as 32%~45%, calcium content is calculated as 45%~50% with CaO, but by
Contain content also in it with Cr2O3When being calculated as 0.3%~1.0% chromium, therefore further preparing vanadium oxide product, production will affect
Quality, it is therefore desirable to reduce its chromium content.
In step A of the present invention, it is first 1:3~8 by solid-liquid mass ratio by high chromium calcium vanadate and water, is formulated as slurry.
In step B of the present invention, it is because the solubility of calcium oxalate is small that sodium oxalate, which is added, into slurry, and sodium oxalate can be with Gao Ge
The reaction such as calcium hydroxide, calcium chromate, calcium vanadate in calcium vanadate slurry, enters vanadium, chromium in solution；Simultaneously again because of vanadium
Sour calcium solubility is smaller than calcium hydroxide, calcium chromate, therefore the additional amount of sodium oxalate is controlled the C in sodium oxalate2O4 2-Mole
With Ca in slurry2+Mole ratio be 0.3~0.5, by control sodium oxalate additional amount make itself and calcium hydroxide, calcium chromate
Reaction makes chromium enter solution, and reduction calcium vanadate as far as possible participates in the degree reacted, and reduces the quantity that vanadium enters solution, Jin Ercai
Low chromium calcium vanadate as much as possible can be obtained, the low chromium calcium vanadate of high-recovery is obtained by subsequent separation of solid and liquid.
Slurry is heated to 60~90 DEG C of reactions in the method for the present invention step B, is molten in order to be dispersed in high chromium calcium vanadate
In liquid, reacted conducive to the dissolution of calcium chromate and its with sodium oxalate.
In step B, the time being stirred to react is 30~90min；It has no special requirements to the revolving speed of stirring, as long as making body
Material can come into full contact under stirring in system.
The method of the present invention can effectively reduce the chromium content in calcium vanadate by control sodium oxalate dosage and reaction condition, walk
In rapid B, chromium content is in obtained low chromium calcium vanadate with Cr2O3It is calculated as≤0.2%.
In order to further recycling the vanadium and chromium in de- chromium solution, avoid the wasting of resources, the method for the present invention further include with
Lower step:
C, chromium solution calcium salt precipitation method will be taken off obtained by step B separate vanadium, the chromium solution after obtaining calcium vanadate and precipitation, gained
Calcium vanadate is handled by step A and step B, and the chromium solution after gained precipitation further recycles chromium；Vanadic acid is obtained through calcium salt precipitation method
When calcium is handled by step A and step B, can individually carry out, calcium vanadate can also be accumulated to it is a certain amount of after carry out again, can also be with
It is carried out after high chromium calcium vanadate mixing.
Content is mass percentage in the present invention.
Below by embodiment, invention is further described in detail, but does not therefore limit the scope of the present invention
Among the embodiment described range.
Embodiment 1
Take high chromium calcium vanadate (V2O540.43%, Cr2O30.63%, CaO48.32%) 200g, 600mL water, 70g grass is added
Sour sodium is stirred to react 90min at 90 DEG C, is separated by solid-liquid separation, obtains low chromium calcium vanadate 228.2g, wherein Cr2O3Content is 0.15%.
Embodiment 2
Take high chromium calcium vanadate (V2O540.43%, Cr2O30.63%, CaO48.32%) 200g, 800mL water, 92g grass is added
Sour sodium is stirred to react 60min at 70 DEG C, is separated by solid-liquid separation, obtains low chromium calcium vanadate 235.5g, wherein Cr2O3Content is 0.13%.
Embodiment 3
Take high chromium calcium vanadate (V2O540.43%, Cr2O30.63%, CaO48.32%) 200g, 1200mL water, 110g is added
Sodium oxalate is stirred to react 30min at 70 DEG C, is separated by solid-liquid separation, obtains low chromium calcium vanadate 242.8g, wherein Cr2O3Content is 0.12%.
In conclusion the method for reducing chromium content in high chromium calcium vanadate of the invention, can effectively reduce the chromium in calcium vanadate
Content, and vanadium recovery is not influenced, vanadium oxide is further prepared conducive to calcium vanadate；Recycled simultaneously vanadium in de- chromium solution and
Chromium avoids resources loss, can solve the problems, such as the technology of vanadium oxide preparation after vanadium chromium solution separation vanadium, chromium.
Claims (9)
1. the method for reducing chromium content in high chromium calcium vanadate, it is characterised in that: the following steps are included:
A, add water to be beaten high chromium calcium vanadate, obtain slurry；
B, sodium oxalate is added into slurry, after being stirred to react, is separated by solid-liquid separation, obtains low chromium calcium vanadate and de- chromium solution；The grass
The additional amount of sour sodium is C in sodium oxalate2O4 2-Mole and slurry in Ca2+Mole ratio be 0.3~0.5；The stirring
The temperature of reaction is 60~90 DEG C.
2. the method according to claim 1 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: described in step A
Chromium content is in high chromium calcium vanadate with Cr2O3It is calculated as 0.3%~1.0%.
3. the method according to claim 1 or 2 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: in step A,
The high chromium calcium vanadate and the solid-liquid mass ratio of water are 1:3~8.
4. the method according to claim 1 or 2 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: in step B,
The time being stirred to react is 30~90min.
5. the method according to claim 3 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: described in step B
The time being stirred to react is 30~90min.
6. the method according to claim 1 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: described in step B
Chromium content is in low chromium calcium vanadate with Cr2O3It is calculated as≤0.2%.
7. according to claim 1, the described in any item methods for reducing chromium content in high chromium calcium vanadate in 2,5 or 6, feature exist
In: further comprising the steps of:
C, chromium solution calcium salt precipitation method will be taken off obtained by step B separate vanadium, the chromium solution after obtaining calcium vanadate and precipitation, gained vanadic acid
Calcium is handled by step A and step B, and the chromium solution after gained precipitation further recycles chromium.
8. the method according to claim 3 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: further include following step
It is rapid:
C, chromium solution calcium salt precipitation method will be taken off obtained by step B separate vanadium, the chromium solution after obtaining calcium vanadate and precipitation, gained vanadic acid
Calcium is handled by step A and step B, and the chromium solution after gained precipitation further recycles chromium.
9. the method according to claim 4 for reducing chromium content in high chromium calcium vanadate, it is characterised in that: further include following step
It is rapid:
C, chromium solution calcium salt precipitation method will be taken off obtained by step B separate vanadium, the chromium solution after obtaining calcium vanadate and precipitation, gained vanadic acid
Calcium is handled by step A and step B, and the chromium solution after gained precipitation further recycles chromium.
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| CN201711191213.7A CN107937737B (en) | 2017-11-24 | 2017-11-24 | A method of reducing chromium content in high chromium calcium vanadate |
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| CN201711191213.7A CN107937737B (en) | 2017-11-24 | 2017-11-24 | A method of reducing chromium content in high chromium calcium vanadate |
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| CN107937737B true CN107937737B (en) | 2019-06-14 |
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| CN109628740A (en) * | 2019-02-25 | 2019-04-16 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for reducing chromium content in high chromium calcium vanadate |
| CN110423901B (en) * | 2019-09-11 | 2021-11-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for separating sodium vanadium chromium from vanadium chromium solution |
| CN112195347B (en) * | 2020-09-27 | 2022-07-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
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| US20040045834A1 (en) * | 2002-04-18 | 2004-03-11 | Bayer Aktiengesellschaft | Process for the utilization of vanadium bound in chromium ore as vanadium(V) oxide by electrolysis |
| CN100558643C (en) * | 2007-09-18 | 2009-11-11 | 攀钢集团攀枝花钢铁研究院 | A kind of preparation method of ammonium poly-vanadate |
| CN102703688B (en) * | 2012-05-07 | 2015-09-23 | 河北钢铁股份有限公司承德分公司 | The method of vanadium is reclaimed in vanadium titano-magnetite |
| CN104628033A (en) * | 2015-01-27 | 2015-05-20 | 河北钢铁股份有限公司承德分公司 | Method for preparing metavanadate |
| CN104805303B (en) * | 2015-05-21 | 2017-09-15 | 孟立新 | A kind of method that vanadium chromium slag acid system synchronously reclaims vanadium chromium |
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