CN106006736A - Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution - Google Patents
Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution Download PDFInfo
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- CN106006736A CN106006736A CN201610322651.1A CN201610322651A CN106006736A CN 106006736 A CN106006736 A CN 106006736A CN 201610322651 A CN201610322651 A CN 201610322651A CN 106006736 A CN106006736 A CN 106006736A
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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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention belongs to the field of nonferrous metallurgy, and particularly relates to a method of using hydrogen for preparing vanadium trioxide from a vanadium-containing solution. The method includes the following steps that thevanadium-containing solution is subjected to stirring reaction for 1 hour or more in a high-temperature high-pressure reaction device, the concentration of hydrogen and vanadium is larger than 6 g/L, the concentration of hydrogen ions is 10<5>-10<14> mol/L, vanadium in the vanadium-containing solution exists in a tetravalent state, and vanadium trioxide water slurry is obtained, wherein the reaction temperature is 50-300 DEG C, and the hydrogen partial pressure is larger than 1 MPa; solid-liquid separation is carried out on the vanadium trioxide water slurry to obtain a vanadium trioxide filter cake and filter liquor; the vanadium trioxide filter cake is dried in vacuum to obtain vanadium trioxide. The method has the advantages of being simple in process, environmentally friendly and low in cost.
Description
Technical field
The invention belongs to Non-ferrous Metallurgy field, particularly relate to a kind of utilize hydrogen from containing vanadium solution is prepared Vanadium sesquioxide
Method.
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: utilize hydrogen from containing preparing Vanadium sesquioxide vanadium solution
Method, it specifically comprises the following steps that
Using hydrogen and vanadium concentration is 10 more than 6g/L, hydrogen ion concentration-5～10-14Mol/L containing vanadium solution at high-temperature high-voltage reaction
Stirring reaction more than 1 hour in device, described containing the vanadium in vanadium solution presented in four valence states, obtain Vanadium sesquioxide
Water slurry, wherein, reaction temperature is 50～300 DEG C, and hydrogen partial pressure is more than 1MPa；
Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
By such scheme, described vanadium concentration is 35～50g/L, is 10 containing hydrogen ion concentration in vanadium solution-5～10-7mol/L。
By such scheme, described reaction condition is: temperature is 170～250 DEG C, and hydrogen partial pressure is more than 2.5MPa.
By such scheme, described stirring reaction rotating speed is 500～1000r/min.
Owing to using said method, the present invention has the positive effect that:
1, compared with the prior art, can eliminate by containing vanadium directly from containing vanadium solution is prepared Vanadium sesquioxide due to the present invention
Solution prepares the operation of intermediate products ammonium vanadate or poly ammonium vanadate etc. through ammonium salt precipitation, simplify technique, it is to avoid ammonia nitrogen waste water
Generation with ammonia；Meanwhile, hydrogen is a kind of cleaning gas, does not results in environmental pollution, therefore the present invention have technique simple,
Eco-friendly advantage；
2, being gas liquid reaction due to reaction involved in the present invention, temperature only needs 50～300 DEG C, preferable temperature at 170～250 DEG C,
And existing with ammonium metavanadate, poly vanadic acid as involved by the technique that the high price vanadium products such as, vanadic anhydride prepare Vanadium sesquioxide
Reaction be gas-solid reaction, temperature required higher, generally higher than 500 DEG C, therefore, the energy consumption cost of the present invention is lower；Meanwhile,
Owing to this invention simplifies technique, eliminate and prepare ammonium metavanadate, poly vanadic acid by the operation of, vanadic anhydride etc., further
Reduce 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:
Described in this detailed description of the invention containing the vanadium in vanadium solution presented in four valence states.
Embodiment 1
Such as Fig. 1, a kind of utilize hydrogen from containing the method preparing Vanadium sesquioxide vanadium solution.It comprises the concrete steps that:
(1) using hydrogen and vanadium concentration is 35～50g/L, and hydrogen ion concentration is 10-5～10-7Mol/L containing vanadium solution in temperature is
170～250 DEG C, hydrogen partial pressure is 2.5～3.5MPa, under conditions of stirring reaction rotating speed is 800～1000r/min, high in high temperature
Pressure reaction kettle for reaction 1.5～2.5 hours, obtains Vanadium sesquioxide water slurry；
(2) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(3) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
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 utilize hydrogen from containing the method preparing Vanadium sesquioxide vanadium solution.It comprises the concrete steps that:
(1) using hydrogen and vanadium concentration is 20～30g/L, and hydrogen ion concentration is 10-10～10-14Mol/L containing vanadium solution in temperature is
100～150 DEG C, hydrogen partial pressure is 1.5～2.5MPa, under conditions of stirring reaction rotating speed is 500～800r/min, high in high temperature
Pressure reaction kettle for reaction 1～3 hours, obtains Vanadium sesquioxide water slurry；
(2) Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
(3) Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
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 (4)
1. utilizing hydrogen from containing the method preparing Vanadium sesquioxide vanadium solution, it specifically comprises the following steps that
Using hydrogen and vanadium concentration is 10 more than 6g/L, hydrogen ion concentration-5～10-14Mol/L containing vanadium solution at high-temperature high-voltage reaction
Stirring reaction more than 1 hour in device, described containing the vanadium in vanadium solution presented in four valence states, obtain Vanadium sesquioxide
Water slurry, wherein, reaction temperature is 50～300 DEG C, and hydrogen partial pressure is more than 1MPa；
Vanadium sesquioxide water slurry obtains Vanadium sesquioxide filter cake and filtrate after solid-liquid separation；
Vanadium sesquioxide filter cake is vacuum dried, obtains Vanadium sesquioxide.
The most according to claim 1 utilize hydrogen from containing the method preparing Vanadium sesquioxide vanadium solution, it is characterised in that institute
The vanadium concentration stated is 35～50g/L, is 10 containing hydrogen ion concentration in vanadium solution-5～10-7mol/L。
The most according to claim 1 utilize hydrogen from containing the method preparing Vanadium sesquioxide vanadium solution, it is characterised in that institute
The reaction condition stated is: temperature is 170～250 DEG C, and hydrogen partial pressure is more than 2.5MPa.
The most according to claim 1 utilize hydrogen from containing the method preparing Vanadium sesquioxide vanadium solution, it is characterised in that
Described stirring reaction rotating speed is 500～1000r/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610322651.1A CN106006736B (en) | 2016-05-16 | 2016-05-16 | Using hydrogen from the method containing vanadium trioxide is prepared in vanadium solution |
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| CN106006736B CN106006736B (en) | 2017-06-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107434259A (en) * | 2017-08-09 | 2017-12-05 | 河钢股份有限公司承德分公司 | A kind of method by preparing vanadium trioxide containing vanadium solution |
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| CN102010004A (en) * | 2010-12-27 | 2011-04-13 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN104176778A (en) * | 2014-08-11 | 2014-12-03 | 武汉理工大学 | Graded porous vanadium oxide microspheres and preparation method and application thereof |
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- 2016-05-16 CN CN201610322651.1A patent/CN106006736B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB738713A (en) * | 1952-12-26 | 1955-10-19 | Ca Nat Research Council | Precipitation of vanadium oxides from aqueous solutions |
| JPS61141622A (en) * | 1984-12-13 | 1986-06-28 | Shinko Kagaku Kogyo Kk | Production of lower oxide of vanadium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107434259A (en) * | 2017-08-09 | 2017-12-05 | 河钢股份有限公司承德分公司 | A kind of method by preparing vanadium trioxide containing vanadium solution |
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