CN105969984B - A kind of preparation method of vanadium trioxide - Google Patents
A kind of preparation method of vanadium trioxide Download PDFInfo
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C01G31/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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Abstract
The invention belongs to Non-ferrous Metallurgy field, more particularly to a kind of preparation method of vanadium trioxide, include following steps：(1) purification and impurity removal operation is carried out to extracting vanadium from stone coal richness vanadium liquid of the vanadium concentration more than 6g/L, is purified liquid and precipitation slag；(2) scavenging solution is carried out using alkali lye or acid solution adjusting pH operations, obtains hydrogen ion concentration as 10‑4~10‑14Mol/L liquid to be restored；(3) use hydrogen and liquid to be restored in temperature for 50~300 DEG C, hydrogen partial pressure is more than 1MPa, stirring reaction more than 1 hour in high-temperature high-voltage reaction device, obtains vanadium trioxide water slurry；(4) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；(5) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.The present invention has the advantages of technique is simple, environment-friendly, production cost is low.
Description
Technical field
The invention belongs to Non-ferrous Metallurgy field, more particularly to a kind of preparation method of vanadium trioxide.
Background technology
Vanadium trioxide is the important compound of vanadium, there is important application in industries such as metallurgy, electronics, chemical industry.Three oxygen
Change two vanadium to can be used for producing vanadium iron and metal vanadium powder, also can be as the raw material for producing vanadium carbide and vanadium nitride；Due to excellent
Light, electricity, magnetic property, vanadium trioxide is in electricity, magnetic, photoswitch and gas sensor, storage material, a variety of necks such as resistance material
Domain is all with a wide range of applications.
At present, the method for preparing vanadium trioxide mainly has two kinds：A kind of is the not ammonium metavanadate of additional reducing agent or more
Poly- ammonium vanadate thermally decomposes cracking process, such as Chinese patent 200610020405.7, utilizes the ammonia discharged when heating ammonium metavanadate
Nascent hydron caused by thermal cracking reduces ammonium metavanadate, and this method do not use additional also Primordial Qi, although can reduce part into
This, but the ammonia cracking that raw material decomposes go out is incomplete, does not only result in that reducing atmosphere is inadequate, and without the row of the ammonia cracked
Except environmental pollution can be caused.
The method that another kind prepares vanadium trioxide is the direct high temperature reduction method of additional reducing agent, more with C, NH3、H2、
CH4, CO or industrial gas etc. be reducing agent, the high price vfanadium compound such as thermal reduction ammonium metavanadate, poly ammonium vanadate, vanadic anhydride
And vanadium trioxide is obtained, such a method is also the method for preparing vanadium trioxide being widely used at present.Chinese patent
CN1118765A discloses a kind of production method of vanadium trioxide, and this method is using industrial gas as reducing gas, in rotary kiln
In carry out reduction pyrolytic reaction to ammonium metavanadate or vanadic anhydride, obtain vanadium trioxide.The shortcomings that this method is：Reduction temperature
Spend for more than 900 DEG C, energy consumption is higher；Chinese patent CN200610020405.7 discloses a kind of vanadium sesquioxide powder that produces
Method.Its method is to be added to powder ammonium vanadate or vanadic anhydride in external heat fluidized bed furnace boiler tube as furnace charge, makes stove
The filling rate of pipe reaches 10%~55%, is passed through industrial gas, is heated to 600~650 DEG C, insulation is reduced to prepare three oxidations two
Vanadium.The shortcomings that technical scheme is：Reduction temperature is high, and high energy consumption, industrial gas dosage is big, complex manufacturing.
Can be seen that current vanadium trioxide technology of preparing from published data is mostly with ammonium metavanadate, poly
Ammonium vanadate or vanadic anhydride are raw material, and at certain temperature and reducing atmosphere obtained by reaction, reaction temperature is generally higher than 500
DEG C, high energy consumption, production cost height.Ammonium metavanadate, poly ammonium vanadate are mostly by containing vanadium solution through ammonium obtained by vanadium extraction industry
Salt precipitation gained；Vanadic anhydride is ammonium metavanadate, poly vanadic acid through thermal decomposition gained.Therefore, if with ammonium metavanadate, poly vanadium
Sour ammonium prepares vanadium trioxide for raw material needs two steps actually：(1) ammonium metavanadate, poly vanadium are prepared through ammonium salt precipitation containing vanadium solution
Sour ammonium, (2) under high temperature and reducing atmosphere prepare vanadium trioxide using ammonium metavanadate, poly ammonium vanadate as raw material；If with
Vanadic anhydride prepares vanadium trioxide for raw material needs three steps actually：(1) containing vanadium solution through ammonium salt precipitation prepare ammonium metavanadate,
Poly ammonium vanadate, (2) ammonium metavanadate, poly ammonium vanadate prepare vanadic anhydride through thermal decomposition, and (3) are using vanadic anhydride as raw material
Vanadium trioxide is prepared under high temperature and reducing atmosphere.As can be seen that current vanadium trioxide preparation technology is more multiple
Miscellaneous, complicated preparation technology also results in the increase of production cost.Meanwhile prepare ammonium metavanadate, poly ammonium vanadate in ammonium salt precipitation
During can produce substantial amounts of ammonia nitrogen waste water, thermal decomposition ammonium metavanadate, poly ammonium vanadate prepare the process meeting of vanadic anhydride
Substantial amounts of ammonia is discharged, these waste water and waste gas can all cause serious pollution to environment；In addition, with ammonium metavanadate or poly vanadium
Sour ammonium is raw material, and substantial amounts of ammonia can be decomposited during vanadium trioxide is prepared, and unreacted ammonia is discharged into air
In environment can equally be polluted.Therefore, there is the problem of environmental pollution is serious in existing vanadium trioxide preparation technology.
In summary, there is complex process in existing vanadium trioxide preparation technology, environmental pollution is serious, production cost is high
Inferior position.At present, it is badly in need of seeking the vanadium trioxide preparation technology that a kind of technique is simple, environment-friendly, production cost is low.
The content of the invention
Present invention seek to address that the defects of above-mentioned vanadium trioxide preparation technology, it is therefore an objective to provide that a kind of technique is simple, ring
The vanadium trioxide preparation method that border is friendly, production cost is low.
To achieve the above object, the technical solution adopted by the present invention is：A kind of preparation method of vanadium trioxide, includes
Following steps：
(1) purification and impurity removal operation is carried out to extracting vanadium from stone coal richness vanadium liquid of the vanadium concentration more than 6g/L, is purified liquid and precipitation
Slag；
(2) scavenging solution is carried out using alkali lye or acid solution adjusting pH operations, obtains hydrogen ion concentration as 10-4~10-14mol/L
Liquid to be restored；
(3) use hydrogen and liquid to be restored in temperature for 50~300 DEG C, hydrogen partial pressure is more than 1MPa, in high temperature high pressure reverse
Stirring reaction more than 1 hour in device is answered, obtains vanadium trioxide water slurry；
(4) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(5) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
By such scheme, the vanadium concentration of described extracting vanadium from stone coal richness vanadium liquid is 35~50g/L.
By such scheme, the hydrogen ion concentration in described liquid to be restored is 10-4~10-7mol/L。
By such scheme, the reaction condition of described hydrogen and liquid to be restored is：Temperature is 170~250 DEG C, hydrogen partial pressure
For more than 2.5MPa, described stirring reaction rotating speed is 500~1000r/min.
By such scheme, described extracting vanadium from stone coal richness vanadium liquid is that extracting vanadium from stone coal leachate exchange-desorbs work through resin ion
Obtained by skill, wherein the vanadium in extracting vanadium from stone coal richness vanadium liquid exists in the form of five valence states, the pH=of described extracting vanadium from stone coal leachate
1.0~3.0.
By such scheme, resin used is anion exchange resin during described resin ion exchanges.
By such scheme, in described desorption technique strippant used be NaOH solution, one kind in NaCl solution or
The two mixed solution being obtained by mixing by a certain percentage.
By such scheme, described purification and impurity removal operation is：Using alkali lye or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9
~11, obtain liquid after tune pH；Appropriate alkali solubility magnesium salts or calcium salt are added in liquid after to tune pH, it is anti-under the conditions of 60~100 DEG C
Answer 0.5~3 hour, be purified water slurry；Purification water slurry is purified liquid and precipitation slag through separation of solid and liquid.
Due to being had the positive effect that using the above method, the present invention：
1st, due to the present invention only need to extracting vanadium from stone coal richness vanadium liquid through simple removal of impurities processing after can be directly from containing vanadium solution
In prepare vanadium trioxide, compared with the prior art, eliminate by preparing intermediate products vanadic acid through ammonium salt precipitation containing vanadium solution
The process of ammonium or poly ammonium vanadate etc., simplifies technique, avoids the generation of ammonia nitrogen waste water and ammonia；Meanwhile hydrogen is a kind of
Clean gas, environmental pollution will not be caused, therefore the present invention has the advantages of technique is simple, environment-friendly；
2nd, because main body reaction prepared by vanadium trioxide involved in the present invention is gas liquid reaction, temperature only needs 50~
300 DEG C, preferable temperature at 170~250 DEG C, and it is existing pressed with ammonium metavanadate, poly vanadic acid, the production of the high price vanadium such as vanadic anhydride
The reaction that product prepare involved by the technique of vanadium trioxide is gas-solid reaction, and required temperature is higher, generally higher than 500 DEG C, therefore,
The energy consumption cost of the present invention is lower；Simultaneously as this invention simplifies technique, eliminate prepare ammonium metavanadate, poly vanadic acid by,
The process of vanadic anhydride etc., reduce further production cost.Therefore, the present invention has the advantages of production cost is low.
Therefore, the present invention has the advantages of technique is simple, environment-friendly, production cost is low.
Brief description of the drawings
Fig. 1 is a kind of process chart of the present invention.
Embodiment
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System：
Embodiment 1
Such as Fig. 1, a kind of preparation method of vanadium trioxide, it is comprised the concrete steps that：
(1) purification and impurity removal operation is carried out to the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is 35~50g/L, is purified liquid with sinking
Mud；
(2) scavenging solution is carried out using alkali lye or acid solution adjusting pH operations, obtains hydrogen ion concentration as 10-4~10-7mol/L
Liquid to be restored；
(3) use hydrogen and liquid to be restored in temperature for 170~250 DEG C, hydrogen partial pressure is 3~4MPa, and stirring reaction turns
Under conditions of speed is 800~1000r/min, is reacted 3~4 hours in high-temperature high-pressure reaction kettle, obtain vanadium trioxide water slurry；
(4) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(5) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
Described extracting vanadium from stone coal richness vanadium liquid is that extracting vanadium from stone coal leachate exchanges-desorption technique gained through resin ion, wherein
Resin used in ion exchange is D201 resins, and the strippant used in desorption technique is that mass fraction is 6%~10%NaOH solution,
Vanadium in leachate exists in the form of five valence states, pH=1.0~2.0 of leachate.
Described purification and impurity removal operation is：Extracting vanadium from stone coal richness vanadium liquid pH to 9~10 is adjusted using acid solution, obtained after adjusting pH
Liquid；10~30g/L MgCl is added after to tune pH in liquid2, reacted 1.5~3 hours under the conditions of 60~80 DEG C, be purified water
Slurry；Purification water slurry is purified liquid and precipitation slag through separation of solid and liquid.
The rate of deposition of vanadium trioxide is more than 98% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Embodiment 2
A kind of preparation method of vanadium trioxide, it is comprised the concrete steps that：
(1) purification and impurity removal operation is carried out to the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is 15~25g/L, is purified liquid with sinking
Mud；
(2) scavenging solution is carried out using alkali lye or acid solution adjusting pH operations, obtains hydrogen ion concentration as 10-12~10-14mol/L
Liquid to be restored；
(3) use hydrogen and liquid to be restored in temperature for 180~300 DEG C, hydrogen partial pressure is 3~5MPa, and stirring reaction turns
Under conditions of speed is 500~800r/min, is reacted 1~2.5 hour in high-temperature high-pressure reaction kettle, obtain vanadium trioxide water
Slurry；
(4) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(5) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
Described extracting vanadium from stone coal richness vanadium liquid is that extracting vanadium from stone coal leachate exchanges-desorption technique gained through resin ion, wherein
Resin used in ion exchange is D314 resins, and the strippant used in desorption technique is that mass fraction is 2%~4%`NaOH solution
It is that 8%~10%NaCl solution is 1 by volume with mass fraction:1 mixed solution being obtained by mixing, the vanadium in leachate is with five
The form of valence state is present, pH=2.0~3.0 of leachate.
Described purification and impurity removal operation is：Using alkali lye or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 10~11, obtain
Liquid after tune pH；After to tune pH 15~40g/L CaCl are added in liquid2, react 0.5~1.5 hour, obtain under the conditions of 80~100 DEG C
To purification water slurry；Purification water slurry is purified liquid and precipitation slag through separation of solid and liquid.
The rate of deposition of vanadium trioxide is more than 98% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Embodiment 3
A kind of preparation method of vanadium trioxide, it is comprised the concrete steps that：
(1) purification and impurity removal operation is carried out to the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is 25~35g/L, is purified liquid with sinking
Mud；
(2) scavenging solution is carried out using alkali lye or acid solution adjusting pH operations, obtains hydrogen ion concentration as 10-6~10-10mol/L
Liquid to be restored；
(3) use hydrogen and liquid to be restored in temperature for 100~200 DEG C, hydrogen partial pressure is 2~4MPa, and stirring reaction turns
Under conditions of speed is 800~900r/min, is reacted 1~2 hour in high-temperature high-pressure reaction kettle, obtain vanadium trioxide water slurry；
(4) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(5) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
Described extracting vanadium from stone coal richness vanadium liquid is that extracting vanadium from stone coal leachate exchanges-desorption technique gained through resin ion, wherein
Resin used in ion exchange is D290 resins, the strippant used in desorption technique be mass fraction be mass fraction be 8%~
10%NaCl solution, the vanadium in leachate exist in the form of five valence states, pH=1.5~2.2 of leachate.
Described purification and impurity removal operation is：Using alkali lye or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9.5~10.5, obtain
Liquid after to tune pH；After to tune pH 20~30g/L CaCl are added in liquid2, reacted 1.0~2.0 hours under the conditions of 70~90 DEG C,
It is purified water slurry；Purification water slurry is purified liquid and precipitation slag through separation of solid and liquid.
The rate of deposition of vanadium trioxide is more than 98% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Claims (8)
1. a kind of preparation method of vanadium trioxide, includes following steps：
(1) purification and impurity removal operation is carried out to extracting vanadium from stone coal richness vanadium liquid of the vanadium concentration more than 6g/L, is purified liquid and precipitation slag；
(2) scavenging solution is carried out using alkali lye or acid solution adjusting pH operations, obtains hydrogen ion concentration as 10-4~10-14Mol/L's treats
Reducing solution；
(3) use hydrogen and liquid to be restored in temperature for 50~300 DEG C, hydrogen partial pressure is more than 1MPa, is filled in high-temperature high-voltage reaction
Put stirring reaction more than 1 hour, obtain vanadium trioxide water slurry；
(4) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(5) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
2. the preparation method of vanadium trioxide according to claim 1, it is characterised in that described extracting vanadium from stone coal richness vanadium liquid
Vanadium concentration be 35~50g/L.
3. the preparation method of vanadium trioxide according to claim 1, it is characterised in that the hydrogen in described liquid to be restored
Ion concentration is 10-4~10-7mol/L。
4. the preparation method of vanadium trioxide according to claim 1, it is characterised in that described hydrogen and liquid to be restored
Reaction condition be：Temperature is 170~250 DEG C, and hydrogen partial pressure be more than 2.5MPa, described stirring reaction rotating speed for 500~
1000r/min。
5. the preparation method of vanadium trioxide according to claim 1 or 2, it is characterised in that described extracting vanadium from stone coal richness vanadium
Liquid is that extracting vanadium from stone coal leachate exchanges-desorption technique gained through resin ion, and wherein the vanadium in extracting vanadium from stone coal richness vanadium liquid is with pentavalent
The form of state is present, pH=1.0~3.0 of described extracting vanadium from stone coal leachate.
6. the preparation method of vanadium trioxide according to claim 5, it is characterised in that during described resin ion exchanges
Resin used is anion exchange resin.
7. the preparation method of vanadium trioxide according to claim 5, it is characterised in that used in described desorption technique
The mixed solution that is obtained by mixing by a certain percentage of one or both of the strippant for NaOH solution, in NaCl solution.
8. the preparation method of vanadium trioxide according to claim 1, it is characterised in that described purification and impurity removal operation is：
Using alkali lye or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9~11, liquid after tune pH is obtained；Added in right amount in liquid after to tune pH
Alkali solubility magnesium salts or calcium salt, reacted 0.5~3 hour under the conditions of 60~100 DEG C, be purified water slurry；Water slurry is purified through solid-liquid
Isolated scavenging solution and precipitation slag.
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| WO2023279144A1 (en) * | 2021-07-08 | 2023-01-12 | Avanti Materials Ltd | Recovery of vanadium from alkaline slag materials |
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| CN107522228A (en) * | 2017-08-09 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of method by the vanadium trioxide of clean manufacturing containing vanadium solution |
| CN109722533B (en) * | 2019-03-06 | 2020-09-01 | 吉首大学 | Method for preparing vanadium trioxide by using stone coal vanadium extraction pickle liquor |
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| CN101412539B (en) * | 2008-11-18 | 2010-12-08 | 攀钢集团研究院有限公司 | Clean production process for vanadium oxide |
| CN102092786B (en) * | 2009-12-10 | 2014-04-02 | 中国科学院过程工程研究所 | Method for cleanly preparing vanadium oxides |
| CN101717117B (en) * | 2009-12-29 | 2011-05-11 | 四川省川威集团有限公司 | Method for producing vanadium trioxide |
| CN102092787B (en) * | 2010-12-30 | 2012-07-18 | 沈阳化工大学 | Method for continuously synthesizing vanadium trioxide |
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