CN106006736B - Using hydrogen from the method containing vanadium trioxide is prepared in vanadium solution - Google Patents
Using hydrogen from the method containing vanadium trioxide is prepared in vanadium solution Download PDFInfo
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- CN106006736B CN106006736B CN201610322651.1A CN201610322651A CN106006736B CN 106006736 B CN106006736 B CN 106006736B CN 201610322651 A CN201610322651 A CN 201610322651A CN 106006736 B CN106006736 B CN 106006736B
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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Abstract
The invention belongs to Non-ferrous Metallurgy field, more particularly to a kind of utilization hydrogen, from the method containing vanadium trioxide is prepared in vanadium solution, it is comprised the following steps that：It is 10 more than 6g/L, hydrogen ion concentration with vanadium concentration to use hydrogen‑5~10‑14Mol/L containing vanadium solution in high-temperature high-voltage reaction device stirring reaction more than 1 hour, described exists containing the vanadium in vanadium solution in the form of four valence states, obtains vanadium trioxide water slurry, wherein, reaction temperature be 50~300 DEG C, hydrogen partial pressure be more than 1MPa；Vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；Vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.Therefore, the present invention has the advantages that process is simple, environment-friendly, low production cost.
Description
Technical field
The invention belongs to Non-ferrous Metallurgy field, more particularly to a kind of oxidation of preparation three from vanadium solution is contained using hydrogen
The method of two vanadium.
Background technology
Vanadium trioxide is the important compound of vanadium, has important application in industries such as metallurgy, electronics, chemical industry.Three oxygen
Change two vanadium to can be used to produce vanadium iron and metal vanadium powder, also can be used 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, various 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 many
Poly- ammonium vanadate thermal decomposition cracking process, such as Chinese patent 200610020405.7, using the ammonia discharged when heating ammonium metavanadate
The nascent hydron that thermal cracking is produced 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, and reducing atmosphere is not only resulted in not enough, and without the row of the ammonia for cracking
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, this kind of 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, the method with industrial gas as reducing gas, in rotary kiln
In carry out reduction pyrolytic reaction to ammonium metavanadate or vanadic anhydride, obtain vanadium trioxide.The shortcoming of the method is：Reduction temperature
It is more than 900 DEG C to spend, and energy consumption is higher；Chinese patent CN200610020405.7 discloses a kind of vanadium sesquioxide powder that produces
Method.Its method is that powder ammonium vanadate or vanadic anhydride are added 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, and insulation reduces to prepare three oxidations two
Vanadium.The shortcoming of the technical scheme is：Reduction temperature is high, high energy consumption, and industrial gas consumption 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 is high.Ammonium metavanadate, poly ammonium vanadate be mostly by vanadium extraction industry obtained by containing vanadium solution through ammonium
Salt precipitation gained；Vanadic anhydride is ammonium metavanadate, poly vanadic acid through thermal decomposition gained.Therefore, if with ammonium metavanadate, poly vanadium
Sour ammonium needs two steps actually for raw material prepares vanadium trioxide：(1) ammonium metavanadate, poly vanadium are prepared through ammonium salt precipitation containing vanadium solution
Sour ammonium, (2) prepare vanadium trioxide as raw material with ammonium metavanadate, poly ammonium vanadate under high temperature and reducing atmosphere；If with
Vanadic anhydride needs three steps actually for raw material prepares vanadium trioxide：(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 with 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, existing vanadium trioxide preparation technology has that environmental pollution is serious.
In sum, existing vanadium trioxide preparation technology has that complex process, environmental pollution be serious, production cost is high
Inferior position.At present, it is badly in need of seeking a kind of process is simple, environment-friendly, low production cost vanadium trioxide preparation technology.
The content of the invention
Present invention seek to address that the defect of above-mentioned vanadium trioxide preparation technology, it is therefore an objective to provide a kind of process is simple, ring
Border is friendly, the vanadium trioxide preparation method of low production cost.
To achieve the above object, the technical solution adopted by the present invention is：Aoxidized from containing preparation three in vanadium solution using hydrogen
The method of two vanadium, it is comprised the following steps that：
It is 10 more than 6g/L, hydrogen ion concentration with vanadium concentration to use hydrogen-5~10-14Mol/L's is high in high temperature containing vanadium solution
Stirring reaction more than 1 hour in pressure reaction unit, described exists containing the vanadium in vanadium solution in the form of four valence states, obtains three oxygen
Change two vanadium water slurrys, wherein, reaction temperature is 50~300 DEG C, and hydrogen partial pressure is more than 1MPa；
Vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
Vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
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.
Due to using the above method, the present invention has the positive effect that：
1st, because the present invention directly from containing vanadium trioxide is prepared in vanadium solution compared with the prior art, can be eliminated
By preparing the operation of intermediate products ammonium vanadate or poly ammonium vanadate etc. through ammonium salt precipitation containing vanadium solution, technique is simplified, it is to avoid
The generation of ammonia nitrogen waste water and ammonia；Meanwhile, hydrogen is a kind of clean gas, does not result in environmental pollution, therefore the present invention has
Process is simple, environment-friendly advantage；
2nd, because reaction involved in the present invention is gas liquid reaction, temperature only needs 50~300 DEG C, and preferable temperature is 170~250
DEG C, and the existing technique institute for preparing vanadium trioxide by high price vanadium products such as, vanadic anhydrides with ammonium metavanadate, poly vanadic acid
The reaction being related to is gas-solid reaction, and required temperature is higher, generally higher than 500 DEG C, therefore, energy consumption cost of the invention is lower；Together
When, due to this invention simplifies technique, eliminating the operation for preparing ammonium metavanadate, poly vanadic acid by, vanadic anhydride etc., enter one
Step reduces production cost.Therefore, the present invention has the advantages that low production cost.
Therefore, the present invention has the advantages that process is simple, environment-friendly, low production cost.
Brief description of the drawings
Fig. 1 is a kind of process chart of the invention.
Specific 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：
Existing in the form of four valence states containing the vanadium in vanadium solution described in this specific embodiment.
Embodiment 1
Such as Fig. 1, a kind of utilization hydrogen is from the method containing vanadium trioxide is prepared in vanadium solution.It is comprised the concrete steps that：
(1) it is 35~50g/L to use hydrogen and vanadium concentration, and hydrogen ion concentration is 10-5~10-7Mol/L's exists containing vanadium solution
Temperature be 170~250 DEG C, hydrogen partial pressure be 2.5~3.5MPa, stirring reaction rotating speed be 800~1000r/min under conditions of,
Reacted 1.5~2.5 hours in high-temperature high-pressure reaction kettle, obtain vanadium trioxide water slurry；
(2) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(3) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
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 utilization hydrogen is from the method containing vanadium trioxide is prepared in vanadium solution.It is comprised the concrete steps that：
(1) it is 20~30g/L to use hydrogen and vanadium concentration, and hydrogen ion concentration is 10-10~10-14Mol/L containing vanadium solution
Temperature be 100~150 DEG C, hydrogen partial pressure be 1.5~2.5MPa, stirring reaction rotating speed be 500~800r/min under conditions of,
Reacted 1~3 hour in high-temperature high-pressure reaction kettle, obtain vanadium trioxide water slurry；
(2) vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
(3) vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
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 (4)
1., using hydrogen from the method containing vanadium trioxide is prepared in vanadium solution, it is comprised the following steps that：
It is 10 more than 6g/L, hydrogen ion concentration with vanadium concentration to use hydrogen-5~10-14Mol/L containing vanadium solution in high temperature high pressure reverse
Stirring reaction more than 1 hour in device is answered, described exists containing the vanadium in vanadium solution in the form of four valence states, obtains three oxidations two
Vanadium water slurry, wherein, reaction temperature is 50~300 DEG C, and hydrogen partial pressure is more than 1MPa；
Vanadium trioxide water slurry obtains vanadium trioxide filter cake and filtrate after separation of solid and liquid；
Vanadium trioxide filter cake is vacuum dried, obtains vanadium trioxide.
2. utilization hydrogen according to claim 1 is from the method containing vanadium trioxide is prepared in vanadium solution, it is characterised in that
Described vanadium concentration is 35~50g/L, is 10 containing hydrogen ion concentration in vanadium solution-5~10-7mol/L。
3. utilization hydrogen according to claim 1 is from the method containing vanadium trioxide is prepared in vanadium solution, it is characterised in that
Described reaction condition is：Temperature is 170~250 DEG C, and hydrogen partial pressure is more than 2.5MPa.
4. the method that utilization hydrogen according to claim 1 prepares vanadium trioxide from vanadium solution is contained, it is characterised in that
Described stirring reaction rotating speed is 500~1000r/min.
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| US2665970A (en) * | 1952-12-26 | 1954-01-12 | Ca Nat Research Council | Precipitation of vanadium oxides |
| JPS61141622A (en) * | 1984-12-13 | 1986-06-28 | Shinko Kagaku Kogyo Kk | Production of lower oxide of vanadium |
| CN1300002C (en) * | 2005-06-03 | 2007-02-14 | 武汉大学 | Process for preparing nano grade vanadium trioxide |
| CN1775661A (en) * | 2005-12-07 | 2006-05-24 | 冯良荣 | Method for preparing vanadium nitride |
| CN100457635C (en) * | 2006-12-12 | 2009-02-04 | 攀枝花市久欣钛业有限责任公司 | Production process of vanadium sesquioxide powder |
| CN101723460B (en) * | 2009-11-23 | 2010-12-08 | 中国科学院过程工程研究所 | Process for preparing chromium oxide from laterite-nickel ores |
| CN101700909B (en) * | 2009-11-25 | 2012-02-29 | 中国科学技术大学 | Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method |
| CN101717117B (en) * | 2009-12-29 | 2011-05-11 | 四川省川威集团有限公司 | Method for producing vanadium trioxide |
| CN102010004B (en) * | 2010-12-27 | 2012-05-30 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN104176778B (en) * | 2014-08-11 | 2016-01-06 | 武汉理工大学 | A kind of classifying porous barium oxide microballoon and its preparation method and application |
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