CN103101976B - A kind of preparation method of vanadium trioxide powder - Google Patents
A kind of preparation method of vanadium trioxide powder Download PDFInfo
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- CN103101976B CN103101976B CN201310053222.5A CN201310053222A CN103101976B CN 103101976 B CN103101976 B CN 103101976B CN 201310053222 A CN201310053222 A CN 201310053222A CN 103101976 B CN103101976 B CN 103101976B
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Abstract
The invention provides a kind of method that vanadate reduction prepares vanadous oxide powder.Method provided by the present invention comprises the steps: containing in the basic solution of vanadate, pass into direct current and carry out electrolytic reaction, obtain containing vanadium presoma, presoma is separated, washs, dries, then reduce in reducing atmosphere, obtain thick vanadous oxide, by the refining vanadium trioxide powder obtaining purity more than 99%.It is wide that the method has raw materials used suitability, and reaction process reduction temperature is low, and the product vanadous oxide quality better obtained, purity are high, and whole reaction process does not produce the feature such as obnoxious flavour and sewage.
Description
Technical field
The present invention relates to a kind of preparation method of chemical materials, particularly relate to a kind of method that low-temperature reduction prepares vanadous oxide.
Background technology
Vanadous oxide (V
2o
3) be a kind of important vanadium compound, have the character (also referred to as MST or MIT) of Metal-nonmetal transition, low temperature phase change feature is good, and sudden change of resistivity can reach 6 orders of magnitude, and also with lattice and anti-ferromagnetic change, low temperature is monocline antiferromagnetic semiconducter group.V
2o
3there are two transformation temperature: 150 ~ 170K and 500 ~ 530K.V
2o
3also be a kind of Body Effect material, during phase transformation, susceptibility, optical transmittance and reflectivity also produce sudden change.
Due to V
2o
3superior optical, electrical, magnetic properties, may be used for preparing various gas sensor, storage medium, resistive material etc.The another one main application of vanadous oxide produces vanadium iron, and directly vanadous oxide is made vanadium carbide or vanadium nitride etc. and directly add molten steel and prepare high-quality steel, in addition, vanadous oxide still prepares the important source material of vanadium metal.
Generally produce vanadous oxide by reduction ammonium vanadate or Vanadium Pentoxide in FLAKES in industry, reaction equation is as follows:
2NH
4VO
3+2H
2=2NH
3+V
2O
3+3H
2O
Because this reaction is a strong endothermic process, therefore, will expect the vanadous oxide of high-quality in industrial production, reduction reaction must be carried out under the high temperature of 800-900 DEG C.As CN1118765A discloses the method for a kind of industrial gas reduction ammonium vanadate or Vanadium Pentoxide in FLAKES, temperature of reaction 500-650 DEG C, reaction times 15-40min, but in actual industrial production implementation process, temperature of reaction usually will more than 900 DEG C.CN02092786A is also had to disclose a kind of method that vanadate direct-reduction produces barium oxide, using the vanadate of high-valence state as reaction raw materials, by controlling temperature of reaction 700-1500 DEG C, optionally can produce vanadous oxide, but the method temperature of reaction is high, and in reality, because product is the mixture of sodium hydroxide and vanadous oxide, be difficult to the sodium effectively removed in product by the method for washing, be therefore difficult to obtain the good vanadous oxide of quality.Visible temperature of reaction height is one of the subject matter during vanadous oxide is produced.
In addition, CN101717117A discloses a kind of method that solid carbon reducing agent prepares vanadous oxide, ammonium vanadate or Vanadium Pentoxide in FLAKES and binding agent, carbon dust are mixed and made into pelletizing, then reduce in reducing gas, 10-30min is reacted at 500-650 DEG C, then in inert atmosphere cooling obtain vanadous oxide, the binding agents such as the shortcoming of the method is dextrin, starch, water glass add the purity reducing vanadous oxide.CN1724385A discloses a kind of method that low temperature produces crystal formation vanadous oxide, although temperature of reaction only has 200-300 DEG C, but reaction needed is carried out under the high pressure of 3-15MPa, and need using organic reagent as reductive agent, the method not only requires high to conversion unit, and the use of organic reagent limits the scale operation of vanadous oxide.
The another one problem that vanadous oxide is produced is that raw materials for production are single, and only ammonium meta-vanadate, ammonium vanadate or Vanadium Pentoxide in FLAKES are used as the raw materials for production of vanadous oxide usually.As CN1724385A discloses a kind of method taking Vanadium Pentoxide in FLAKES as raw material preparation and have the vanadous oxide of crystal formation.The method makes Vanadium Pentoxide in FLAKES under the pressure condition of the temperature of 200 ~ 300 DEG C and 3 ~ 15MPa by solvent method, reaction is 0.5 ~ 5h, obtains vanadous oxide.It take Vanadium Pentoxide in FLAKES as the method that nano grade vanadium trioxide prepared by raw material that CN1300002C discloses a kind of.The method is first by V
2o
5and H
2c
2o
4the 2h that refluxes in dehydrated alcohol obtains VOC
2o
4ethanolic soln, then under the condition of High Temperature High Pressure reduction obtain nano level V
2o
3.The raw material also having above-mentioned CN1118765A, CN101717117A, CN1724385A used is also ammonium meta-vanadate, ammonium vanadate or Vanadium Pentoxide in FLAKES.
And CN1974407A discloses a kind of take vanadium tetraoxide as the method that vanadous oxide powder prepared by raw material, vanadium tetraoxide adds in reactor by the method, be heated to 550-600 DEG C, pass into reducing gas reaction 3min, obtain the good vanadous oxide powder of purity.Although the method reduces real reaction temperature, shorten the reaction times, because raw material vanadium tetraoxide is difficult to obtain, and price is more expensive, is therefore still difficult to the industrial production demand meeting vanadous oxide.
As can be seen from consulted reference materials, existing vanadous oxide production technology, or temperature of reaction is too high, or raw materials for production are limited, or product quality cannot ensure, a kind of reaction temperature of exploitation of therefore still needing and, the preparation method of the vanadous oxide that with low cost, adaptability to raw materials is wide.
Summary of the invention
When the object of the present invention is to provide a kind of mild condition, the method for vanadium trioxide powder is prepared in reduction.The principle preparing vanadous oxide provided by the present invention is: be dissolved in basic solution by the vanadate of high-valence state, the vanadate reduction of+5 valencys can be made to be the amorphous vanadium compound of+4 valencys, be referred to as presoma by electrolytic reduction.Because presoma does not have stable crystalline network, therefore can reduce at the temperature lower than titanium dioxide two vanadium reduction temperature and produce vanadous oxide.
Method provided by the present invention not only expands the raw material range preparing vanadous oxide, and greatly reduce reduction temperature, and obtained vanadous oxide purity is higher, more than 99%, whole process is simple, cost is low, thus significantly improves the utilising efficiency of resource, the energy.
The preparation method of vanadium trioxide powder provided by the present invention, comprises the steps:
A) containing in the basic solution of vanadate, pass into direct current and carry out electrolytic reduction;
B) by step a) reaction solution separation, washing, oven dry, obtain containing vanadium presoma;
C) by step b) gained reduces containing vanadium presoma in reducing gas, obtains thick vanadous oxide;
D) by step c) the thick vanadous oxide of gained is refining obtains vanadium trioxide powder.
Vanadous oxide preparation flow figure as shown in Figure 1.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step a) described in vanadate be vanadic acid sodium, potassium vanadate, ammonium meta-vanadate, ammonium poly-vanadate or its mixture.Be such as vanadic acid sodium or potassium vanadate, or the mixing of vanadic acid sodium and potassium vanadate, or be potassium vanadate, ammonium meta-vanadate mixes with ammonium poly-vanadate; Preferred vanadic acid sodium is or/and potassium vanadate; Preferred vanadic acid sodium further.The present invention's vanadate raw material used can be the vanadate of various+5 valencys, thus has expanded the raw material scope of application of the present invention, reduces reaction cost.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step a) described in vanadium concentration be 0.001-10mol/L.Be such as 0.002mol/L, 0.005mol/L, 0.008mol/L, 0.1mol/L, 0.3mol/L, 0.7mol/L, 1.2mol/L, 2mol/L, 3mol/L, 5mol/L, 8mol/L etc.; In order to take into account the quality of cost and product, step of the present invention a) described in vanadium concentration be preferably 0.001-5mol/L; More preferably 0.003-4.5mol/L.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step a) described in alkali be highly basic, more preferably inorganic strong alkali, be more preferably strong basicity soluble hydroxide or carbonate, be particularly preferably sodium hydroxide, potassium hydroxide, ammoniacal liquor, sodium carbonate, salt of wormwood, volatile salt or its mixture.Be such as sodium hydroxide or potassium hydroxide, or the mixing of sodium hydroxide and potassium hydroxide, or the mixing of sodium hydroxide and sodium carbonate, or the mixing of sodium hydroxide and salt of wormwood, or be sodium hydroxide, potassium hydroxide mixes with ammoniacal liquor; Preferred sodium hydroxide is or/and potassium hydroxide; Preferred sodium hydroxide further.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step a) described in alkali concn be 0.05-25mol/L.Be such as 0.07mol/L, 0.1mol/L, 0.15mol/L, 0.25mol/L, 0.4mol/L, 0.8mol/L, 1.5mol/L, 5mol/L, 8mol/L, 10mol/L, 14mol/L, 16mol/L, 20mol/L, 2mol/L3 etc.; Be preferably 0.05-15mol/L; More preferably 0.2-12mol/L.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step a) described in the negative electrode of electrolysis be glass-carbon electrode, Graphite Electrodes, activated carbon electrodes, coke electrodes, carbon black electrode or its mixture.Can be such as glass-carbon electrode or Graphite Electrodes or activated carbon electrodes, or the mixing of Graphite Electrodes and activated carbon electrodes, or glass-carbon electrode, Graphite Electrodes mix with activated carbon electrodes three's, or the mixing of wherein 4 kinds or 5 kinds electrodes; Preferred glass-carbon electrode is or/and Graphite Electrodes; Preferred glass-carbon electrode further.Because glass-carbon electrode has good chemical stability and higher overpotential of hydrogen evolution.
Preferably, the anode of described electrolysis is stainless steel electrode, nickel electrode, lead electrode or its mixture, such as, be stainless steel electrode or nickel electrode, or the mixing of stainless steel electrode and nickel electrode, or be stainless steel electrode, nickel electrode mixes with lead electrode; Preferred stainless steel electrode is or/and nickel electrode; Preferred stainless steel electrode further.Because stainless steel electrode not only can effectively reduce bath voltage, and cost of manufacture is lower.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step a) described in electrolytic current density be 20-900A/m
2.Be such as 25A/m
2, 30A/m
2, 50A/m
2, 90A/m
2, 110A/m
2, 150A/m
2, 200A/m
2, 300A/m
2, 500A/m
2, 700A/m
2, 850A/m
2deng; Preferred 20-800A/m
2; Preferred 50-500A/m further
2;
Preferably, described electrolysis system temperature is 20-95 DEG C.It is such as 22 DEG C, 25 DEG C, 32 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C etc.; Preferred 25-85 DEG C; Preferred 30-85 DEG C further;
Preferably, described electrolysis time is 0.5-50h.Be such as 0.7h, 1h, 1.8h, 2.5h, 3h, 10h, 15h, 25h, 30h, 40h, 46h etc.; Preferred 0.5-40h; In order to ensure the quality of product and improve reaction efficiency preferred 2-10h further further.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step c) described in reducing gas be hydrogen, carbon monoxide, methane, ammonia, Sweet natural gas, industrial gas or its mixture.Be such as hydrogen or carbon monoxide or ammonia, or be the mixture of above-mentioned two kinds of materials, or be the mixture wherein in 4, or be the mixture etc. of above-mentioned all substances; Preferred hydrogen, carbon monoxide, Sweet natural gas or its mixture; Preferred hydrogen is or/and Sweet natural gas further.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, step c) described in reduction temperature be 300-900 DEG C.It is such as 330 DEG C, 350 DEG C, 410 DEG C, 450 DEG C, 500 DEG C, 580 DEG C, 620 DEG C, 690 DEG C, 720 DEG C, 770 DEG C, 830 DEG C, 860 DEG C etc.; Preferred 400-900 DEG C; Preferred 700-900 DEG C further;
Preferably, the described recovery time is 0.5-8h.Be such as 0.7h, 1.0h, 1.3h, 1.8h, 2.5h, 3h, 5h, 7h etc.; Preferred 0.5-6h; For improving the efficiency preferred 0.5-3h further of reaction.
As optimal technical scheme, the preparation method of vanadium trioxide powder provided by the present invention, steps d) described in process for purification for using 50-80 DEG C of hot wash 5-20min.
Compared with prior art, the advantage that the method for the invention has is:
(1) adaptability to raw materials is wide, the vanadate of various+5 valencys, as vanadic acid sodium, and potassium vanadate, ammonium meta-vanadate, ammonium poly-vanadates etc. all can be used as reaction raw materials, reduce reaction cost;
(2) reduction temperature is low, and the presoma obtained due to electrolysis is amorphous state, and reduction temperature is lower, save energy;
(3) quality product is high, and the thick vanadous oxide that direct-reduction obtains, through hot wash, is removed residual impurity wherein, can be met the vanadous oxide of industrial requirement.
Accompanying drawing explanation
Fig. 1 is electrolytic preparation vanadium trioxide powder process flow sheet;
Fig. 2 is the XRD figure of the vanadous oxide powder of 800 DEG C of hydrogen reducing gained in embodiment 1.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
By 14g Na
3vO
4add in the electrolyzer of 200mL with 24g NaOH, add 100mL pure water stirring and dissolving, controlling electrolysis system temperature is 25 DEG C, take glassy carbon electrode as negative electrode (area 6cm
2), take stainless steel electrode as anode (area 8cm
2), logical direct current carries out electrolytic reaction, and control current density is 50A/m
2.Stop electrolytic reaction after 5h, by the electrolyte filtering containing electrolysate, after washing, obtain the unbodied containing vanadium presoma of black.Presoma is proceeded in closed tube furnace, first at N
2in atmosphere with the speed of 10 DEG C/min from room temperature to 800 DEG C, then at H
2800 DEG C of reduction 5h, last N in atmosphere
2conservation of nature is down to room temperature, obtains thick product vanadous oxide.Thick product washed 15min in 60 DEG C of hot water, filters, dry, obtain product vanadous oxide.V in icp analysis product
2o
3content 99.2%, its XRD figure as shown in Figure 2.
Embodiment 2
By 30g Na
3vO
4add in the electrolyzer of 200mL with 7g NaOH, add 100mL pure water stirring and dissolving, controlling electrolysis system temperature is 70 DEG C, take glassy carbon electrode as negative electrode (area 6cm
2), take lead electrode as anode (area 8cm
2), logical direct current carries out electrolytic reaction, and control current density is 300A/m
2.Stop electrolytic reaction after 10h, by the electrolyte filtering containing electrolysate, after washing, obtain the unbodied containing vanadium presoma of black.Presoma is proceeded in closed tube furnace, first at N
2in atmosphere with the speed of 10 DEG C/min from room temperature to 600 DEG C, then at H
2600 DEG C of reduction 4h, last N in atmosphere
2conservation of nature is down to room temperature, obtains thick product vanadous oxide.Thick product washed 20min in 50 DEG C of hot water, filters, dry, obtain product vanadous oxide.V in icp analysis product
2o
3content 99.0%.
Embodiment 3
By 18g Na
3vO
4with 8g Na
2cO
3add in the electrolyzer of 200mL, add 100mL pure water stirring and dissolving, controlling electrolysis system temperature is 45 DEG C, take Graphite Electrodes as negative electrode (area 6cm
2), take stainless steel electrode as anode (area 8cm
2), logical direct current carries out electrolytic reaction, and control current density is 150A/m
2.Stop electrolytic reaction after 7h, by the electrolyte filtering containing electrolysate, after washing, obtain the unbodied containing vanadium presoma of black.Presoma is proceeded in closed tube furnace, first at N
2in atmosphere with the speed of 15 DEG C/min from room temperature to 800 DEG C, then in CO atmosphere 800 DEG C reduction 1h, last N
2conservation of nature is down to room temperature, obtains thick product vanadous oxide.Thick product washed 10min in 70 DEG C of hot water, filters, dry, obtain product vanadous oxide.V in icp analysis product
2o
3content 99.5%.
Embodiment 4
By 27g K
3vO
4add in the electrolyzer of 200mL with 10g KOH, add 100mL pure water stirring and dissolving, controlling electrolysis system temperature is 85 DEG C, take activated carbon electrodes as negative electrode (area 6cm
2), take stainless steel electrode as anode (area 8cm
2), logical direct current carries out electrolytic reaction, and control current density is 350A/m
2.Stop electrolytic reaction after 12h, by the electrolyte filtering containing electrolysate, after washing, obtain the unbodied containing vanadium presoma of black.Presoma is proceeded in closed tube furnace, first at N
2in atmosphere with the speed of 14 DEG C/min from room temperature to 400 DEG C, then at H
2400 DEG C of reduction 6h, last N in atmosphere
2conservation of nature is down to room temperature, obtains thick product vanadous oxide.Thick product washed 20min in 50 DEG C of hot water, filters, dry, obtain product vanadous oxide.V in icp analysis product
2o
3content 99.1%.
Embodiment 5
By 0.1g Na
3vO
4add in the electrolyzer of 200mL with 2gNaOH, add 100mL pure water stirring and dissolving, controlling electrolysis system temperature is 30 DEG C, take Graphite Electrodes as negative electrode (area 6cm
2), take nickel electrode as anode (area 8cm
2), logical direct current carries out electrolytic reaction, and control current density is 20A/m
2.Stop electrolytic reaction after 40h, by the electrolyte filtering containing electrolysate, after washing, obtain the unbodied containing vanadium presoma of black.Presoma is proceeded in closed tube furnace, first at N
2in atmosphere with the speed of 20 DEG C/min from room temperature to 900 DEG C, then at H
2900 DEG C of reduction 0.5h, last N in atmosphere
2conservation of nature is down to room temperature, obtains thick product vanadous oxide.Thick product washed 5min in 80 DEG C of hot water, filters, dry, obtain product vanadous oxide.V in icp analysis product
2o
3content 99.6%.
Embodiment 6
By 160g Na
3vO
4add in the electrolyzer of 200mL with 90g NaOH, add 100mL pure water stirring and dissolving, controlling electrolysis system temperature is 85 DEG C, take Graphite Electrodes as negative electrode (area 6cm
2), take nickel electrode as anode (area 8cm
2), logical direct current carries out electrolytic reaction, and control current density is 800A/m
2.Stop electrolytic reaction after 2h, by the electrolyte filtering containing electrolysate, after washing, obtain the unbodied containing vanadium presoma of black.Presoma is proceeded in closed tube furnace, first at N
2in atmosphere with the speed of 10 DEG C/min from room temperature to 700 DEG C, then in Sweet natural gas 700 DEG C reduction 3h, last N
2conservation of nature is down to room temperature, obtains thick product vanadous oxide.Thick product washed 15min in 50 DEG C of hot water, filters, dry, obtain product vanadous oxide.V in icp analysis product
2o
3content 99.4%.
Found by research, in the preparation method of vanadous oxide powder provided by the invention, electrolytic solution vanadium concentration, alkali concn, electrolysis temperature, electrolysis time, current density, reduction temperature, the quality of recovery time to gained vanadous oxide powdered product all have a certain impact.As vanadium concentration 0.001-10mol/L, more than alkali concn 0.05mol/L, electrolysis temperature is less than 20-95 DEG C, and reduction temperature is 300 ~ 900 DEG C, and the recovery time is more than 0.5h, and the quality of products therefrom is higher.
Applicant states, the present invention illustrates detailed process flow of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process flow, does not namely mean that the present invention must rely on above-mentioned detailed process flow and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (32)
1. a preparation method for vanadium trioxide powder, comprises the steps:
A) containing in the basic solution of vanadate, pass into direct current and carry out electrolytic reduction;
B) by step a) reaction solution separation, washing, oven dry, obtain containing vanadium presoma;
C) by step b) gained reduces containing vanadium presoma in reducing gas, obtains thick vanadous oxide;
D) by step c) the thick vanadous oxide of gained is refining obtains vanadium trioxide powder;
Step a) described in vanadium concentration be 0.001-10mol/L; Described alkali concn is 0.05-25mol/L; Described electrolysis system temperature is 25-85 DEG C; Described electrolytic current density is 20-900A/m
2; Described electrolysis time is 2-40h.
2. the preparation method of vanadium trioxide powder as claimed in claim 1, is characterized in that, step a) described in vanadate be vanadic acid sodium, potassium vanadate, ammonium meta-vanadate, ammonium poly-vanadate or its mixture.
3. the preparation method of vanadium trioxide powder as claimed in claim 2, it is characterized in that, described vanadate is that vanadic acid sodium is or/and potassium vanadate.
4. the preparation method of vanadium trioxide powder as claimed in claim 3, it is characterized in that, described vanadate is vanadic acid sodium.
5. the preparation method of vanadium trioxide powder as claimed in claim 1, is characterized in that, step a) described in vanadium concentration be 0.001-5mol/L.
6. the preparation method of vanadium trioxide powder as claimed in claim 5, it is characterized in that, described vanadium concentration is 0.003-4.5mol/L.
7. the preparation method of vanadium trioxide powder as claimed in claim 1, is characterized in that, step a) described in alkali be highly basic.
8. the preparation method of vanadium trioxide powder as claimed in claim 7, it is characterized in that, described alkali is inorganic strong alkali.
9. the preparation method of vanadium trioxide powder as claimed in claim 1, it is characterized in that, described alkali is strong basicity soluble hydroxide or carbonate.
10. the preparation method of vanadium trioxide powder as claimed in claim 1, it is characterized in that, described alkali is sodium hydroxide, potassium hydroxide, ammoniacal liquor, sodium carbonate, salt of wormwood, volatile salt or its mixture.
The preparation method of 11. vanadium trioxide powders as claimed in claim 1, is characterized in that, step a) described in alkali concn be 0.05-15mol/L.
The preparation method of 12. vanadium trioxide powders as claimed in claim 11, it is characterized in that, described alkali concn is 0.2-12mol/L.
The preparation method of 13. vanadium trioxide powders as claimed in claim 1, is characterized in that, step a) described in the negative electrode of electrolysis be glass-carbon electrode, Graphite Electrodes, activated carbon electrodes, coke electrodes, carbon black electrode.
The preparation method of 14. vanadium trioxide powders as claimed in claim 13, is characterized in that, the negative electrode of described electrolysis is that glass-carbon electrode is or/and Graphite Electrodes.
The preparation method of 15. vanadium trioxide powders as claimed in claim 14, is characterized in that, the negative electrode of described electrolysis is glass-carbon electrode.
The preparation method of 16. vanadium trioxide powders as claimed in claim 1, is characterized in that, step a) described in the anode of electrolysis be stainless steel electrode, nickel electrode, lead electrode.
The preparation method of 17. vanadium trioxide powders as claimed in claim 16, is characterized in that, the anode of described electrolysis is that stainless steel electrode is or/and nickel electrode.
The preparation method of 18. vanadium trioxide powders as claimed in claim 17, is characterized in that, the anode of described electrolysis is stainless steel electrode.
The preparation method of 19. vanadium trioxide powders as claimed in claim 1, it is characterized in that, described electrolytic current density is 20-800A/m
2.
The preparation method of 20. vanadium trioxide powders as claimed in claim 19, it is characterized in that, described electrolytic current density is 50-500A/m
2.
The preparation method of 21. vanadium trioxide powders as claimed in claim 1, it is characterized in that, described electrolysis system temperature is 30-85 DEG C.
The preparation method of 22. vanadium trioxide powders as claimed in claim 1, it is characterized in that, described electrolysis time is 2-10h.
The preparation method of 23. a kind of vanadium trioxide powders as claimed in claim 1, is characterized in that, step c) described in reducing gas be hydrogen, carbon monoxide, methane, ammonia, Sweet natural gas, industrial gas or its mixture.
The preparation method of 24. vanadium trioxide powders as claimed in claim 23, is characterized in that, step c) described in reducing gas be hydrogen, carbon monoxide, Sweet natural gas or its mixture.
The preparation method of 25. vanadium trioxide powders as claimed in claim 24, is characterized in that, step c) described in reducing gas be that hydrogen is or/and Sweet natural gas.
The preparation method of 26. vanadium trioxide powders as claimed in claim 1, is characterized in that, step c) described in reduction temperature be 300-900 DEG C.
The preparation method of 27. vanadium trioxide powders as claimed in claim 26, it is characterized in that, described reduction temperature is 400-900 DEG C.
The preparation method of 28. vanadium trioxide powders as claimed in claim 27, it is characterized in that, described reduction temperature is 700-900 DEG C.
The preparation method of 29. vanadium trioxide powders as claimed in claim 1, is characterized in that, step c) described in recovery time be 0.5-8h.
The preparation method of 30. vanadium trioxide powders as claimed in claim 29, it is characterized in that, the described recovery time is 0.5-6h.
The preparation method of 31. vanadium trioxide powders as claimed in claim 30, it is characterized in that, the described recovery time is 0.5-3h.
The preparation method of 32. vanadium trioxide powders as claimed in claim 1, is characterized in that, steps d) described in process for purification for use 50-80 DEG C of hot wash 5-20min.
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| CN103695954B (en) * | 2013-12-12 | 2016-04-06 | 中国科学院过程工程研究所 | A kind of method being prepared vanadous oxide by vanadate Direct Electrolysis |
| CN103633309A (en) * | 2013-12-13 | 2014-03-12 | 黑龙江大学 | Preparation method of core-shell structure vanadium trioxide microspheres |
| CN106006734B (en) * | 2016-05-16 | 2017-06-13 | 武汉理工大学 | Method using vanadium trioxide is prepared containing vanadium solution |
| CN111892085A (en) * | 2020-07-21 | 2020-11-06 | 河北宏钛科技有限公司 | Vanadium trioxide preparation system and preparation method |
| CN112551580A (en) * | 2020-11-30 | 2021-03-26 | 鞍钢集团北京研究院有限公司 | Method for preparing vanadium trioxide by recycling electrolyte of positive electrode of failure vanadium battery |
| CN112408478B (en) * | 2020-12-02 | 2022-03-15 | 中国科学院过程工程研究所 | Preparation method of vanadium trioxide |
| CN116216779A (en) * | 2023-04-23 | 2023-06-06 | 攀钢集团钒钛资源股份有限公司 | Production method of low-sulfur vanadium trioxide |
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| CN1118765A (en) * | 1994-09-15 | 1996-03-20 | 攀枝花钢铁(集团)公司 | Method for producing V2O3 |
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