CN105969984A - Preparation method of vanadium trioxide - Google Patents
Preparation method of vanadium trioxide Download PDFInfo
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- CN105969984A CN105969984A CN201610321602.6A CN201610321602A CN105969984A CN 105969984 A CN105969984 A CN 105969984A CN 201610321602 A CN201610321602 A CN 201610321602A CN 105969984 A CN105969984 A CN 105969984A
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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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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
- 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
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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Abstract
The invention belongs to the field of nonferrous metal metallurgy and particularly relates to a preparation method of vanadium trioxide. The preparation method comprises the following steps that (1) purification and impurity removal are conducted on vanadium-enriched liquid with the vanadium concentration being larger than 6 g/L and used for extracting vanadium from stone coal, and purification liquid and sediment slag are obtained; (2) pH regulation is conducted on the purification liquid through alkali liquid or acid liquid, and to-be-reduced liquid with the hydrogen ion concentration being 10<-4>-10<-14> mol/L is obtained; (3) under the condition that the hydrogen partial pressure is larger than 1 MPa, hydrogen and the to-be-reduced liquid are subjected to a stirring reaction in a high-temperature high-pressure reaction device for over an hour at the temperature of 50-300 DEG C, and vanadium trioxide water slurry is obtained; (4) after the vanadium trioxide water slurry is subjected to solid-liquid separation, a vanadium trioxide filter cake and filter liquid are obtained; and (5) vacuum drying is conducted on the vanadium trioxide filter cake, and vanadium trioxide is obtained. The preparation method has the advantages of being simple in technique, environmentally friendly and low in production cost.
Description
Technical field
The invention belongs to Non-ferrous Metallurgy field, particularly relate to the preparation method of a kind of Vanadium sesquioxide.
Background technology
Vanadium sesquioxide is the important compound of vanadium, has important application in industries such as metallurgy, electronics, chemical industry.Three oxidations two
Vanadium can be used for producing vanadium iron and metal vanadium powder, it is possible to as the raw material producing vanadium carbide and vanadium nitride；Due to have excellence light,
Electricity, magnetic property, Vanadium sesquioxide is at the multiple fields such as electricity, magnetic, photoswitch and gas sensor, storage material, resistance material
All it is with a wide range of applications.
At present, the method preparing Vanadium sesquioxide mainly has two kinds: a kind of is ammonium metavanadate or the poly vanadic acid of not additional reducing agent
Ammonium thermal decomposition cracking process, such as Chinese patent 200610020405.7, the thermal cracking of the ammonia discharged when utilizing heating ammonium metavanadate is produced
Raw nascent hydron reduces ammonium metavanadate, and this method does not use additional reducing gases, although can reduce departmental cost, but former
The ammonia cracking that material decomposites not exclusively, does not only result in reducing atmosphere inadequate, and does not has the eliminating of the ammonia of cracking can cause ring
Environment pollution.
Another kind prepares the direct high temperature reduction method that the method for Vanadium sesquioxide is additional reducing agent, how with C, NH3、H2、CH4、
CO or industrial gas etc. are reducing agent, the high price vfanadium compound such as thermal reduction ammonium metavanadate, poly ammonium vanadate, vanadic anhydride and obtain
Obtaining Vanadium sesquioxide, this kind of method is also the method preparing Vanadium sesquioxide being widely used at present.Chinese patent CN1118765A
Disclosing the production method of a kind of Vanadium sesquioxide, the method is with industrial gas as reducing gas, to ammonium metavanadate in rotary kiln
Or vanadic anhydride carries out reduction pyrolytic reaction, it is thus achieved that Vanadium sesquioxide.The shortcoming of the method is: reduction temperature be 900 DEG C with
On, energy consumption is higher；Chinese patent CN200610020405.7 discloses a kind of method producing vanadium sesquioxide powder.Its method
It is that powder body ammonium vanadate or vanadic anhydride are joined in external heat fluidized bed furnace boiler tube as furnace charge, makes the filling rate of boiler tube reach
10%～55%, it is passed through industrial gas, is heated to 600～650 DEG C, insulation reduction is to prepare Vanadium sesquioxide.This technical scheme
Shortcoming is: reduction temperature is high, and energy consumption is high, and industrial gas consumption is big, complex manufacturing.
From published data it can be seen that current Vanadium sesquioxide technology of preparing is mostly with ammonium metavanadate, poly ammonium vanadate
Or vanadic anhydride is raw material, reacting gained at certain temperature and reducing atmosphere, reaction temperature is generally higher than 500 DEG C, energy
Consumption height, production cost is high.Ammonium metavanadate, poly ammonium vanadate be mostly by vanadium extraction industry obtained by containing vanadium solution through ammonium salt precipitate
Gained；Vanadic anhydride is that ammonium metavanadate, poly vanadic acid are through thermal decomposition gained.Therefore, if with ammonium metavanadate, poly ammonium vanadate
Prepare Vanadium sesquioxide for raw material and actually need two steps: (1) prepares ammonium metavanadate, poly ammonium vanadate containing vanadium solution through ammonium salt precipitation,
(2) under high temperature and reducing atmosphere, Vanadium sesquioxide is prepared for raw material with ammonium metavanadate, poly ammonium vanadate；If with five oxidations
Two vanadium are that raw material is prepared Vanadium sesquioxide and actually needed three steps: (1) prepares ammonium metavanadate, poly vanadium containing vanadium solution through ammonium salt precipitation
Acid ammonium, (2) ammonium metavanadate, poly ammonium vanadate prepare vanadic anhydride through thermal decomposition, (3) with vanadic anhydride for raw material at height
Vanadium sesquioxide is prepared under temperature and reducing atmosphere.It can be seen that current Vanadium sesquioxide preparation technology is complex, multiple
Miscellaneous preparation technology also results in the increase of production cost.Meanwhile, ammonium metavanadate, the process of poly ammonium vanadate are prepared in ammonium salt precipitation
In can produce substantial amounts of ammonia nitrogen waste water, thermal decomposition ammonium metavanadate, poly ammonium vanadate are prepared the process of vanadic anhydride and can be discharged in a large number
Ammonia, environment all can be caused serious pollution by these waste water and waste gas；It addition, be former with ammonium metavanadate or poly ammonium vanadate
Material, can decomposite substantial amounts of ammonia during preparing Vanadium sesquioxide, and unreacted ammonia is discharged into the atmosphere equally can be right
Environment.Therefore, there is the problem that environmental pollution is serious in existing Vanadium sesquioxide preparation technology.
In sum, it is bad that existing Vanadium sesquioxide preparation technology exists that complex process, environmental pollution be serious, production cost is high
Gesture.At present, it is badly in need of seeking the Vanadium sesquioxide preparation technology that a kind of technique is simple, environmental friendliness, production cost are low.
Summary of the invention
Present invention seek to address that the defect of above-mentioned Vanadium sesquioxide preparation technology, it is therefore an objective to provide that a kind of technique is simple, environmental friendliness,
The Vanadium sesquioxide preparation method that production cost is low.
For achieving the above object, the technical solution used in the present invention is: the preparation method of a kind of Vanadium sesquioxide, includes following
Step:
(1) the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is more than 6g/L carries out purification and impurity removal operation, is purified liquid and precipitation slag；
(2) using alkali liquor or acid solution to carry out scavenging solution adjusting pH operation, obtaining hydrogen ion concentration is 10-4～10-14Mol/L treats also
Stock solution；
(3) using hydrogen and liquid to be restored is 50～300 DEG C in temperature, and hydrogen partial pressure is more than 1MPa, fills in high-temperature high-voltage reaction
Put stirring reaction more than 1 hour, obtain Vanadium sesquioxide water slurry；
(4) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(5) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
By such scheme, the vanadium concentration of described extracting vanadium from stone coal richness vanadium liquid is 35～50g/L.
By such scheme, the described hydrogen ion concentration in liquid to be restored is 10-4～10-7mol/L。
By such scheme, described hydrogen with the reaction condition of liquid to be restored is: temperature is 170～250 DEG C, and hydrogen partial pressure is 2.5
More than MPa, 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 exchanges desorption technique gained through resin ion,
Wherein the vanadium in extracting vanadium from stone coal richness vanadium liquid is presented in five valence states, the pH=1.0～3.0 of described extracting vanadium from stone coal leachate.
By such scheme, in described resin ion exchange, resin used is anion exchange resin.
By such scheme, strippant used in described desorption technique is the one or both in NaOH solution, NaCl solution
The mixed solution being obtained by mixing by a certain percentage.
By such scheme, described purification and impurity removal operation is: use alkali liquor or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9～11,
Obtain adjusting liquid after pH；After pH, liquid adds appropriate alkali solubility magnesium salt or calcium salt to adjusting, under the conditions of 60～100 DEG C, react 0.5～3
Hour, it is purified water slurry；Purify water slurry and be purified liquid and precipitation slag through solid-liquid separation.
Owing to using said method, the present invention has the positive effect that:
1, only need extracting vanadium from stone coal richness vanadium liquid just can directly be prepared after simple remove impurity processes from containing vanadium solution due to the present invention
Vanadium sesquioxide, compared with the prior art, eliminates and is prepared intermediate products ammonium vanadate or poly vanadium by containing vanadium solution through ammonium salt precipitation
The operation of acid ammonium etc., simplifies technique, it is to avoid the ammonia nitrogen waste water generation with ammonia；Meanwhile, hydrogen is a kind of cleaning gas,
Not resulting in environmental pollution, therefore the present invention has technique advantage simple, eco-friendly；
2, the main body reaction prepared due to Vanadium sesquioxide involved in the present invention is gas liquid reaction, and temperature only needs 50～300 DEG C,
Preferable temperature is at 170～250 DEG C, and existing prepares by high price vanadium products such as, vanadic anhydrides with ammonium metavanadate, poly vanadic acid
Reaction involved by the technique of Vanadium sesquioxide is gas-solid reaction, temperature required higher, generally higher than 500 DEG C, therefore, and this
Bright energy consumption cost is lower；Simultaneously as this invention simplifies technique, eliminate prepare ammonium metavanadate, poly vanadic acid by, five
The operation of V 2 O etc., reduce further production cost.Therefore, the present invention has the advantage that production cost is low.
Therefore, the present invention has the advantage that technique is simple, environmental friendliness, production cost are low.
Accompanying drawing explanation
Fig. 1 is a kind of process chart of the present invention.
Detailed description of the invention
The invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings, not the restriction to its protection domain:
Embodiment 1
Such as Fig. 1, the preparation method of a kind of Vanadium sesquioxide, it comprises the concrete steps that:
(1) the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is 35～50g/L is carried out purification and impurity removal operation, be purified liquid and precipitation slag；
(2) using alkali liquor or acid solution to carry out scavenging solution adjusting pH operation, obtaining hydrogen ion concentration is 10-4～10-7Mol/L treats also
Stock solution；
(3) using hydrogen and liquid to be restored is 170～250 DEG C in temperature, and hydrogen partial pressure is 3～4MPa, and stirring reaction rotating speed is
Under conditions of 800～1000r/min, react 3～4 hours in high-temperature high-pressure reaction kettle, obtain Vanadium sesquioxide water slurry；
(4) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(5) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
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 its intermediate ion is handed over
Changing resin used is D201 resin, the strippant used by desorption technique be mass fraction be 6%～10%NaOH solution, leach
Vanadium in liquid presented in five valence states, the pH=1.0～2.0 of leachate.
Described purification and impurity removal operation is: uses acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9～10, obtains adjusting liquid after pH；
To adjusting the MgCl adding 10～30g/L after pH in liquid2, react 1.5～3 hours under the conditions of 60～80 DEG C, be purified water slurry；
Purify water slurry and be purified liquid and precipitation slag through solid-liquid separation.
In the present embodiment, the rate of deposition of Vanadium sesquioxide is more than 98%, and the purity of Vanadium sesquioxide is more than 99%.
Embodiment 2
A kind of preparation method of Vanadium sesquioxide, it comprises the concrete steps that:
(1) the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is 15～25g/L is carried out purification and impurity removal operation, be purified liquid and precipitation slag；
(2) using alkali liquor or acid solution to carry out scavenging solution adjusting pH operation, obtaining hydrogen ion concentration is 10-12～10-14Mol/L treats
Reducing solution；
(3) using hydrogen and liquid to be restored is 180～300 DEG C in temperature, and hydrogen partial pressure is 3～5MPa, and stirring reaction rotating speed is
Under conditions of 500～800r/min, react 1～2.5 hour in high-temperature high-pressure reaction kettle, obtain Vanadium sesquioxide water slurry；
(4) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(5) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
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 its intermediate ion is handed over
Changing resin used is D314 resin, the strippant used by desorption technique be mass fraction be that 2%～4%`NaOH solution divides with quality
Number is the mixed solution that 8%～10%NaCl solution is obtained by mixing for 1:1 by volume, and the vanadium in leachate is with the form of five valence states
Exist, the pH=2.0～3.0 of leachate.
Described purification and impurity removal operation is: uses alkali liquor or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 10～11, obtains adjusting pH
Rear liquid；To adjusting, liquid adds after pH 15～40g/L CaCl2, react 0.5～1.5 hour under the conditions of 80～100 DEG C, be purified
Water slurry；Purify water slurry and be purified liquid and precipitation slag through solid-liquid separation.
In the present embodiment, the rate of deposition of Vanadium sesquioxide is more than 98%, and the purity of Vanadium sesquioxide is more than 99%.
Embodiment 3
A kind of preparation method of Vanadium sesquioxide, it comprises the concrete steps that:
(1) the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is 25～35g/L is carried out purification and impurity removal operation, be purified liquid and precipitation slag；
(2) using alkali liquor or acid solution to carry out scavenging solution adjusting pH operation, obtaining hydrogen ion concentration is 10-6～10-10Mol/L treats also
Stock solution；
(3) using hydrogen and liquid to be restored is 100～200 DEG C in temperature, and hydrogen partial pressure is 2～4MPa, and stirring reaction rotating speed is
Under conditions of 800～900r/min, react 1～2 hour in high-temperature high-pressure reaction kettle, obtain Vanadium sesquioxide water slurry；
(4) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(5) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
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 its intermediate ion is handed over
Changing resin used is D290 resin, the strippant used by desorption technique be mass fraction be mass fraction be 8%～10%NaCl molten
Liquid, the vanadium in leachate presented in five valence states, the pH=1.5～2.2 of leachate.
Described purification and impurity removal operation is: uses alkali liquor or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9.5～10.5, is adjusted
Liquid after pH；To adjusting, liquid adds after pH 20～30g/L CaCl2, react 1.0～2.0 hours under the conditions of 70～90 DEG C, obtain clean
Change water slurry；Purify water slurry and be purified liquid and precipitation slag through solid-liquid separation.
In the present embodiment, the rate of deposition of Vanadium sesquioxide is more than 98%, and the purity of Vanadium sesquioxide is more than 99%.
Claims (8)
1. a preparation method for Vanadium sesquioxide, includes following steps:
(1) the extracting vanadium from stone coal richness vanadium liquid that vanadium concentration is more than 6g/L carries out purification and impurity removal operation, is purified liquid and precipitation slag；
(2) using alkali liquor or acid solution to carry out scavenging solution adjusting pH operation, obtaining hydrogen ion concentration is 10-4～10-14Mol/L treats also
Stock solution；
(3) using hydrogen and liquid to be restored is 50～300 DEG C in temperature, and hydrogen partial pressure is more than 1MPa, fills in high-temperature high-voltage reaction
Put stirring reaction more than 1 hour, obtain Vanadium sesquioxide water slurry；
(4) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(5) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
The preparation method of Vanadium sesquioxide the most according to claim 1, it is characterised in that described extracting vanadium from stone coal richness vanadium liquid
Vanadium concentration is 35～50g/L.
The preparation method of Vanadium sesquioxide the most according to claim 1, it is characterised in that the described hydrogen in liquid to be restored from
Sub-concentration is 10-4～10-7mol/L。
The preparation method of Vanadium sesquioxide the most according to claim 1, it is characterised in that described hydrogen and liquid to be restored
Reaction condition is: temperature is 170～250 DEG C, and hydrogen partial pressure is more than 2.5MPa, and described stirring reaction rotating speed is 500～1000
r/min。
The preparation method of Vanadium sesquioxide the most according to claim 1 and 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 five valence states
Presented in, the pH=1.0～3.0 of described extracting vanadium from stone coal leachate.
The preparation method of Vanadium sesquioxide the most according to claim 5, it is characterised in that institute in described resin ion exchange
It is anion exchange resin with resin.
The preparation method of Vanadium sesquioxide the most according to claim 5, it is characterised in that used by described desorption technique
Strippant is the mixed solution that the one or both in NaOH solution, NaCl solution is obtained by mixing by a certain percentage.
The method that extracting vanadium from stone coal richness vanadium liquid the most according to claim 1 prepares Vanadium sesquioxide, it is characterised in that described is clean
Eliminating auxiliary work is: uses alkali liquor or acid solution regulation extracting vanadium from stone coal richness vanadium liquid pH to 9～11, obtains adjusting liquid after pH；To adjusting pH
Rear liquid adds appropriate alkali solubility magnesium salt or calcium salt, reacts 0.5～3 hour under the conditions of 60～100 DEG C, be purified water slurry；
Purify water slurry and be purified liquid and precipitation slag through solid-liquid separation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109722533A (en) * | 2019-03-06 | 2019-05-07 | 吉首大学 | A method of vanadium trioxide is prepared using extracting vanadium from stone coal pickle liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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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| CN101717117A (en) * | 2009-12-29 | 2010-06-02 | 四川省川威集团有限公司 | Method for producing vanadium trioxide |
| CN102092786A (en) * | 2009-12-10 | 2011-06-15 | 中国科学院过程工程研究所 | Method for cleanly preparing vanadium oxides |
| CN102092787A (en) * | 2010-12-30 | 2011-06-15 | 沈阳化工大学 | Method for continuously synthesizing vanadium trioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010057410A1 (en) * | 2008-11-18 | 2010-05-27 | Panzhihua New Steel & Vanadium Co., Ltd. | Clean production method of vanadium oxide |
| CN102092786A (en) * | 2009-12-10 | 2011-06-15 | 中国科学院过程工程研究所 | Method for cleanly preparing vanadium oxides |
| CN101717117A (en) * | 2009-12-29 | 2010-06-02 | 四川省川威集团有限公司 | Method for producing vanadium trioxide |
| CN102092787A (en) * | 2010-12-30 | 2011-06-15 | 沈阳化工大学 | Method for continuously synthesizing vanadium trioxide |
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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 |
| WO2019029615A1 (en) * | 2017-08-09 | 2019-02-14 | 河钢股份有限公司承德分公司 | Method for cleanly producing vanadium trioxide by vanadium-containing solution |
| CN109722533A (en) * | 2019-03-06 | 2019-05-07 | 吉首大学 | A method of vanadium trioxide is prepared using extracting vanadium from stone coal pickle liquor |
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