CN107434259A - A kind of method by preparing vanadium trioxide containing vanadium solution - Google Patents
A kind of method by preparing vanadium trioxide containing vanadium solution Download PDFInfo
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- CN107434259A CN107434259A CN201710674293.5A CN201710674293A CN107434259A CN 107434259 A CN107434259 A CN 107434259A CN 201710674293 A CN201710674293 A CN 201710674293A CN 107434259 A CN107434259 A CN 107434259A
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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Abstract
The present invention relates to a kind of method by preparing vanadium trioxide containing vanadium solution, methods described is：CO is passed through in containing vanadium solution2And H2, reacted under conditions of heating is pressurizeed, separation of solid and liquid after the completion of reaction, obtain vanadium trioxide solid and separating liquid.The inventive method uses CO2And H2Composite gas solve the technical barrier for generating sodium hydroxide in vanadate hydrogen reduction and causing reduction reaction to be difficult to being reacted containing vanadium solution；The reduction efficiency of vanadate is improved, has obtained the vanadium trioxide product that purity is more than 99%；The generation of ammonia nitrogen waste water is effectively avoided simultaneously, is realized recycling for water resource, has been reached the purpose of wastewater zero discharge.The present invention has the characteristics that technological process is short, production is efficient, product is high-end, environment-friendly, cost is low, suitable for industrialization promotion.
Description
Technical field
The present invention relates to vanadium chemical field, and in particular to a kind of method by preparing vanadium trioxide containing vanadium solution.
Background technology
Barium oxide is mainly for the production of alloy, colouring agent, all-vanadium redox flow battery electrolyte, sulfuric acid and the stone of ceramics printing and dyeing
The industries such as the metallurgy such as the catalyst of oiling work, electronics, dyestuff, the energy, chemical industry.Barium oxide mainly has vanadic anhydride (V2O5)、
Vanadium trioxide (V2O3) and vanadium dioxide (VO2) etc., the preparation technology of different oxides is different.
In vanadium metallurgical industry, using vanadic anhydride as the primary product of vanadium, contained containing vanadium mineral by hydrometallurgy
Vanadium solution, the impurity element in solution is removed by chemical subtraction, then by precipitation, calcining and other processes, it is higher that purity is made
Vanadic anhydride industrial products.Conventional precipitation method has hydrolysis precipitation, ammonium salt precipitation and calcium, iron precipitation etc., at present industry
On generally using acid ammonium salt precipitation method, the method is that alkalescence after cleaning contains sulphur acid for adjusting pH value 5- is added in vanadium solution
When 6, ammonium salt is added, then with sulphur acid for adjusting pH value 1.8-2.5, bisque ammonium poly-vanadate is generated under heating, stirring condition, should
The product purity that method obtains is high, and ammonium salt consumption is low, and precipitation rate is high, but a large amount of acid ammonia nitrogen waste waters, place are produced in production process
It is high to manage cost.
Vanadium trioxide is the desirable feedstock for producing VN alloy and vanadium iron, at present, produces the general of vanadium trioxide
It is for raw material, with reducibility gas such as natural gas, coal gas, hydrogen with ammonium metavanadate, ammonium poly-vanadate, vanadic anhydride etc. all over method
Reduced at 800-1000 DEG C, obtain the vanadium trioxide product of grade more than 64%, the production procedure length of this method, be produced into
This height, prepared by raw material equally exists the problems such as ammonia nitrogen waste water is difficult to processing.
CN103922404B discloses a kind of method that vanadic anhydride prepares vanadium trioxide, by by vanadic anhydride
It is well mixed with carbon dust 2 ︰ 1 in molar ratio ratio；Mixed raw material is pressed into material block, then carbon dust is covered on material block；
The material block of shaping is fired into 3-5h at 950 DEG C -1050 DEG C and obtains vanadium trioxide.The invention reduction temperature is more than 900 DEG C, energy consumption
It is higher, it is unfavorable for promoting.
CN103695954B discloses a kind of method that vanadium trioxide is prepared by vanadate Direct Electrolysis, using vanadate as
Raw material, using alkali metal or alkaline earth metal chloride as fused salt, 150 DEG C -250 DEG C are warming up under nitrogen or argon gas atmosphere, constant temperature
12h-24h removes the moisture in fused salt, then heats to 500 DEG C -1000 DEG C, is electrolysed, tank voltage 2.5-5.0V, during electrolysis
Between be 3h-12h, under the cathode portion obtain product vanadium trioxide product.But energy consumption is equally existed during electrolytic preparation
The problem of too high.
CN106006736A discloses a kind of method for preparing vanadium trioxide from containing vanadium solution using hydrogen, using hydrogen
Gas is more than 6g/L, hydrogen ion concentration 10 with vanadium concentration-4-10-14Containing vanadium solution in high-temperature high-voltage reaction device in 50-300
DEG C, more than hydrogen partial pressure 1MPa react more than 1 hour, obtain vanadium trioxide product.This method there is severe reaction conditions,
The incomplete shortcoming of reduction reaction, while the sodium hydroxide solution of the big volume low-concentration of by-product, it is difficult to recycle, it is necessary to using it
He is handled method.
In summary, the industry urgently develops that a kind of production procedure is short, and energy consumption is low, and no ammonia nitrogen waste water produces and reduction reaction
What can efficiently be carried out prepares vanadium trioxide new method.
The content of the invention
In view of problems of the prior art, the invention provides a kind of side by preparing vanadium trioxide containing vanadium solution
Method, solve the technical barrier for generating sodium hydroxide in vanadate hydrogen reduction and causing reduction reaction to be difficult to, carry
The high reduction efficiency of vanadate, has obtained purity and has been more than 99% vanadium trioxide product, while effectively avoided ammonia nitrogen waste water
Generation, have the characteristics that technological process it is short, production cleaning, product is high-end, cost is low, suitable for industrialization promotion.
To use following technical scheme up to this purpose, the present invention：
The present invention provides a kind of method by preparing vanadium trioxide containing vanadium solution, and methods described is：To in containing vanadium solution
It is passed through CO2And H2, reacted under conditions of heating is pressurizeed, separation of solid and liquid after the completion of reaction, obtain vanadium trioxide solid and separation
Liquid.
The hydrogen reduction reaction formula of typical vanadate is：
2HXVO4 (3-X)-+2H2(g)=V2O3+(6-2X)OH-+(2X-1)H2O (wherein X is 0-2)
Hydroxide ion can be produced in hydrogen reduction by vanadate it can be seen from reaction equation, makes the alkalescence of solution
Gradually enhancing, causes the trend of hydrogen reducing vanadate to die down, and reduction difficulty gradually increases, and reduction reaction can not be properly completed.
Present invention selection is passed through CO2And H2Composite gas containing vanadium solution with reacting, CO2Can effectively it consume raw in reduction process
Into hydroxide ion, reduce the pH value containing vanadium solution, improve the reactivity of vanadate, solve vanadate hydrogen reducing mistake
The technical barrier for generating sodium hydroxide in journey and causing reduction reaction to be difficult to, and then reaction temperature and hydrogen partial pressure are obtained
To be greatly lowered, it is more beneficial for mitigating the temperature and pressure load of equipment, while reduces energy consumption.
According to the present invention, described containing vanadium solution is to be obtained through sodium roasting, wet-leaching or other approach containing vanadium mineral
Alkaline solution containing vanadium.
It is described containing containing any one in sodium vanadate, sodium pyrovanadate or sodium metavanadate in vanadium solution according to the present invention.
According to the present invention, the concentration containing vanadium in vanadium solution is 20-60g/L, for example, can be 20g/L, 25g/L,
Specific point value between 30g/L, 35g/L, 40g/L, 45g/L, 50g/L, 55g/L or 60g/L, and above-mentioned numerical value, is limited to a piece
Width and the consideration for simplicity, the present invention no longer exclusive list.
According to the present invention, the concentration containing sodium in vanadium solution is 9-94g/L, such as can be 9g/L, 10g/L, 15g/
L, 20g/L, 30g/L, 45g/L, 50g/L, 56g/L, 60g/L, 64g/L, 72g/L, 81g/L, 88g/L or 94g/L, and it is above-mentioned
Specific point value between numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the concentration≤50mg/L containing silicon in vanadium solution, concentration≤15mg/L of phosphorus, the concentration of chromium≤
30mg/L。
According to the present invention, the temperature of the reaction is 80-180 DEG C, for example, can be 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C,
Specific point value between 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C or 180 DEG C, and above-mentioned numerical value, is limited to a piece
Width and the consideration for simplicity, the present invention no longer exclusive list.
According to the present invention, CO in the course of reaction2Partial pressure be 0.5-1MPa, such as can be 0.5MPa,
0.55MPa, 0.6MPa, 0.65MPa, 0.7MPa, 0.75MPa, 0.8MPa, 0.85MPa, 0.9MPa, 0.95MPa or 1MPa, with
And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, H in the course of reaction2Partial pressure be 1-2.5MPa, such as can be 1MPa, 1.2MPa,
Specific point value between 1.5MPa, 1.7MPa, 1.9MPa, 2MPa, 2.3MPa or 2.5MPa, and above-mentioned numerical value, as space is limited
And the consideration for simplicity, the present invention no longer exclusive list.
According to the present invention, the time of the reaction is 0.5-3h, for example, can be 0.5h, 0.8h, 1h, 1.2h, 1.5h,
Specific point value between 1.8h, 2h, 2.2h, 2.5h, 2.8h or 3h, and above-mentioned numerical value, examining as space is limited and for simplicity
Consider, the present invention no longer exclusive list.
According to the present invention, stirred in the course of reaction with 300-800r/min speed to being stirred containing vanadium solution
Can speed up the process of reaction, the mixing speed can be 300r/min, 350r/min, 400r/min, 450r/min,
500r/min, 550r/min, 600r/min, 650r/min, 700r/min, 750r/min or 800r/min, and above-mentioned numerical value
Between specific point value, as space is limited and the consideration for simplicity, the present invention no longer exclusive list.
The vanadium trioxide solid is dried the present invention under protective atmosphere, obtains pure vanadium trioxide
Product.
According to the present invention, the protective atmosphere is the group of any one or at least two in nitrogen, argon gas or helium
Close, such as can be any one in nitrogen, argon gas or helium, typical but non-limiting is combined as：Nitrogen and argon gas；Nitrogen
Gas and helium；Argon gas and helium；Nitrogen, argon gas and helium.
According to the present invention, the temperature of the drying is 105-350 DEG C, for example, can be 105 DEG C, 125 DEG C, 150 DEG C, 175
DEG C, 200 DEG C, 235 DEG C, 250 DEG C, 275 DEG C, 300 DEG C, 325 DEG C or the specific point value between 350 DEG C, and above-mentioned numerical value, be limited to
Length and the consideration for simplicity, the present invention no longer exclusive list.
The present invention is passed through CO into the separating liquid2Carry out acidification reaction, obtain after separation of solid and liquid sodium bicarbonate crystal and
Filtrate.
According to the present invention, the temperature of the acidification reaction is 15-30 DEG C, for example, can be 15 DEG C, 18 DEG C, 20 DEG C, 23 DEG C,
Specific point value between 25 DEG C, 28 DEG C or 30 DEG C, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is not
Exclusive list again.
According to the present invention, the time of the acidification reaction is 0.5-2h, for example, can be 0.5h, 0.8h, 1h, 1.2h,
Specific point value between 1.5h, 1.8h or 2h, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is no longer
Exclusive list.
According to the present invention, the pH of the reaction end of the acidification reaction is 7.5-8.3, for example, can be 7.5,7.6,7.7,
7.8th, the specific point value between 7.9,8.0,8.1,8.2 or 8.3, and above-mentioned numerical value, as space is limited and for simplicity consideration,
The present invention no longer exclusive list.
According to the present invention, separating liquid is stirred with 100-300r/min speed during the acidification reaction, stirred
The speed mixed can be 100r/min, 120r/min, 150r/min, 170r/min, 200r/min, 230r/min, 250r/min,
Specific point value between 280r/min or 300r/min, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention
No longer exclusive list.
By acidified reaction, the filtrate that is obtained after separation of solid and liquid is back to the circulation of vanadate solution preparation section to be made the present invention
With.
Preferably, prepared by the filtrate return vanadium extraction of wet method containing vanadium mineral into vanadate solution process to recycle.
The present invention from means well known in the art carry out separation of solid and liquid, such as can be filtering, suction filtration, centrifugation with
And sedimentation etc., but it is non-be only limitted to this, separation process should be advisable in order to operate.
As preferable technical scheme, the method for the present invention by preparing vanadium trioxide containing vanadium solution includes following step
Suddenly：
(1) it is passed through CO in containing vanadium solution2And H2, reacted under conditions of heating is pressurizeed, separation of solid and liquid after the completion of reaction,
Obtain vanadium trioxide solid and separating liquid；
(2) step (1) the vanadium trioxide solid is dried under protective atmosphere, obtains three pure oxidations
Two vanadium products；
(3) it is passed through CO into step (1) described separating liquid2Acidification reaction is carried out, sodium acid carbonate crystalline substance is obtained after separation of solid and liquid
Body and filtrate, the filtrate are back to the recycling of vanadate solution preparation section.
Compared with prior art, the present invention at least has the advantages that：
(1) the inventive method uses CO2And H2Composite gas react in high-pressure reactor with containing vanadium solution, can be effective
The pH value containing vanadium solution is reduced, improves the reactivity of vanadate, generation sodium hydroxide is made during solving vanadate reduction
The technical barrier being difficult into reduction reaction so that reaction temperature and hydrogen partial pressure are significantly lowered, and are more beneficial for subtracting
The temperature and pressure load of light equipment.
(2) present invention is eliminated containing vanadium using the vanadium trioxide product that high-quality has directly been prepared containing vanadium solution
Solution prepares the series of processes process such as intermediate products, then high temperature reduction through ammonium salt precipitation, shortens technological process, and source solves
The pollution problem of acid ammonia nitrogen waste water, has that technological process is short, production cost is low, advantages of environment protection.
(3) present invention can realize the efficient reduction to vanadate, and its percent reduction is more than 99%, while obtains purity and be more than
99% vanadium trioxide product.
(4) the inventive method is by using CO2Filtrate after acidifying reduction, obtains pure sodium bicarbonate crystal, takes off
Solution after sodium can return to the vanadium extraction of wet method containing vanadium mineral and prepare the recycling of vanadate solution process, realize following for water resource
Ring utilizes, and has reached the purpose of wastewater zero discharge.
Brief description of the drawings
Fig. 1 is the process chart that a kind of embodiment of the present invention provides.
The present invention is described in more detail below.But following examples is only the simple example of the present invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are defined by claims.
Embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by embodiment.
As shown in figure 1, the technological process that a kind of embodiment of the present invention provides can be：Obtained to wet method vanadium extraction
Containing being passed through CO in vanadium solution2And H2, reacted under conditions of heating is pressurizeed, vanadium trioxide slurry, solid-liquid obtained after the completion of reaction
Separation, obtains vanadium trioxide solid and separating liquid；Vanadium trioxide solid is dried under protective atmosphere, obtains three
V 2 O product；CO is passed through into separating liquid2Acidification reaction is carried out, sodium bicarbonate crystal and filtrate are obtained after separation of solid and liquid,
Gained filtrate is back to wet method vanadium extraction prepared in the process of vanadate and recycle.
For the present invention is better described, technical scheme is readily appreciated, of the invention is typical but non-limiting
Embodiment is as follows：
Embodiment 1
(1) it is passed through CO into the solution containing sodium pyrovanadate that vanadium concentration is 46g/L2And H2, at 120 DEG C, CO2Partial pressure 0.5MPa,
H2Partial pressure 2MPa, under conditions of speed of agitator is 500r/min, reacted 2 hours in high-temperature high-voltage reaction device, after the completion of reaction
Filtering, obtains vanadium trioxide solid and separating liquid；
(2) the vanadium trioxide solid for obtaining step (1) is dried under 105 DEG C, nitrogen atmosphere, obtains three oxidations
Two vanadium products；
(3) at 15 DEG C, CO is passed through in the separating liquid obtained to step (1)2Acidification reaction is carried out, with 200r/min speed
Degree stirring, reaction end pH value are 8.0, are separated by filtration to obtain sodium bicarbonate crystal and filtrate after reacting 1.5h；The filter that will be obtained
Liquid returns to sodium vanadate solution preparation section and recycled.
By detection, the percent reduction of vanadate is 99.3% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Embodiment 2
(1) it is to be passed through CO containing in burnt meta-acid sodium solution for 32g/L to vanadium concentration2And H2, at 150 DEG C, CO2Partial pressure 1MPa, H2
Partial pressure 2.5MPa, under conditions of speed of agitator is 700r/min, reacted 3 hours in high-temperature high-voltage reaction device, after the completion of reaction
Filtering, obtains vanadium trioxide solid and separating liquid；
(2) the vanadium trioxide solid for obtaining step (1) is dried under 280 DEG C, nitrogen atmosphere, obtains three oxidations
Two vanadium products；
(3) at 25 DEG C, CO is passed through in the separating liquid obtained to step (1)2Acidification reaction is carried out, with 250r/min speed
Degree stirring, reaction end pH value are 8.2, are separated by filtration to obtain sodium bicarbonate crystal and filtrate after reacting 2h；The filtrate that will be obtained
Sodium pyrovanadate solution preparation section is returned to recycle.
By detection, the percent reduction of vanadate is 99.1% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Embodiment 3
(1) it is passed through CO into the solution containing sodium metavanadate that vanadium concentration is 25g/L2And H2, at 100 DEG C, CO2Partial pressure 0.8MPa,
H2Partial pressure 2.2MPa, under conditions of speed of agitator is 350r/min, reacted 3 hours in high-temperature high-voltage reaction device, reaction is completed
After filter, obtain vanadium trioxide solid and separating liquid；
(2) the vanadium trioxide solid for obtaining step (1) is dried under 200 DEG C, argon gas atmosphere, obtains three oxidations
Two vanadium products；
(3) at 20 DEG C, CO is passed through in the separating liquid obtained to step (1)2Acidification reaction is carried out, with 100r/min speed
Degree stirring, reaction end pH value are 7.8, are separated by filtration to obtain sodium bicarbonate crystal and filtrate after reacting 1h；The filtrate that will be obtained
Sodium metavanadate solution preparation section is returned to recycle.
By detection, the percent reduction of vanadate is 99.1% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Embodiment 4
(1) it is passed through CO into the solution containing sodium metavanadate that vanadium concentration is 38g/L2And H2, at 180 DEG C, CO2Partial pressure 0.7MPa,
H2Partial pressure 1.5MPa, under conditions of speed of agitator is 800r/min, reacts 1.5 hours, reacted in high-temperature high-voltage reaction device
Into rear filtering, vanadium trioxide solid and separating liquid are obtained；
(2) the vanadium trioxide solid for obtaining step (1) is dried under 300 DEG C, nitrogen atmosphere, obtains three oxidations
Two vanadium products；
(3) at 30 DEG C, CO is passed through in the separating liquid obtained to step (1)2Acidification reaction is carried out, with 300r/min speed
Degree stirring, reaction end pH value are 8.3, are separated by filtration to obtain sodium bicarbonate crystal and filtrate after reacting 0.5h；The filter that will be obtained
Liquid returns to sodium metavanadate solution preparation section and recycled.
By detection, the percent reduction of vanadate is 99.2% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Embodiment 5
(1) it is passed through CO into the solution containing sodium vanadate that vanadium concentration is 20g/L2And H2, at 80 DEG C, CO2Partial pressure 1MPa, H2
Partial pressure 2.5MPa, under conditions of speed of agitator is 300r/min, reacted 3 hours in high-temperature high-voltage reaction device, after the completion of reaction
Filtering, obtains vanadium trioxide solid and separating liquid；
(2) the vanadium trioxide solid for obtaining step (1) is dried under 120 DEG C, nitrogen atmosphere, obtains three oxidations
Two vanadium products；
(3) at 18 DEG C, CO is passed through in the separating liquid obtained to step (1)2Acidification reaction is carried out, with 100r/min speed
Degree stirring, reaction end pH value are 7.5, are separated by filtration to obtain sodium bicarbonate crystal and filtrate after reacting 2h；The filtrate that will be obtained
Sodium vanadate solution preparation section is returned to recycle.
By detection, the percent reduction of vanadate is 99.3% in the present embodiment, and the purity of vanadium trioxide is more than 99%.
Comparative example 1
(1) solution containing sodium pyrovanadate in Example 1 is as raw material, measures its pH as 10, and vanadium concentration is 46g/L, to
This, which contains in sodium pyrovanadate solution, is passed through H2, at 120 DEG C, H2Partial pressure 2MPa, under conditions of speed of agitator is 500r/min, in high temperature
Reacted 2 hours in high-pressure reactor, filtered after the completion of reaction, obtain vanadium trioxide solid and separating liquid；
(2) with the step of embodiment 1 (2).
By detection, the percent reduction of vanadate is 91.2% in this comparative example, and the purity of vanadium trioxide is more than 99%.
Comparative example 2
Compared with comparative example 1, except by H in step (1)2Partial pressure replace with outside 2.5MPa, other conditions and comparative example 1
It is identical.
By detection, the percent reduction of vanadate is 92.9% in this comparative example, and the purity of vanadium trioxide is more than 99%.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
- A kind of 1. method by preparing vanadium trioxide containing vanadium solution, it is characterised in that methods described is：To containing logical in vanadium solution Enter CO2And H2, reacted under conditions of heating is pressurizeed, separation of solid and liquid after the completion of reaction, obtain vanadium trioxide solid and separation Liquid.
- 2. the method as described in claim 1, it is characterised in that the vanadium solution that contains is through sodium roasting, wet method containing vanadium mineral The alkaline solution containing vanadium that leaching or other approach obtain.
- 3. the method as described in claim 1, it is characterised in that it is described contain vanadium solution in containing sodium vanadate, sodium pyrovanadate or Any one in sodium metavanadate.
- 4. the method as described in claim 1, it is characterised in that the concentration containing vanadium in vanadium solution is 20-60g/L, sodium Concentration is 9-94g/L；Preferably, the concentration≤50mg/L containing silicon in vanadium solution, concentration≤15mg/L of phosphorus, concentration≤30mg/L of chromium.
- 5. the method as described in claim 1, it is characterised in that the temperature of the reaction is 80-180 DEG C；Preferably, CO in the course of reaction2Partial pressure be 0.5-1MPa, H2Partial pressure be 1-2.5MPa；Preferably, the time of the reaction is 0.5-3h；Preferably, in the course of reaction with 300-800r/min speed to being stirred containing vanadium solution.
- 6. the method as described in claim 1, it is characterised in that carry out the vanadium trioxide solid under protective atmosphere Dry, obtain vanadium trioxide product；Preferably, the protective atmosphere is any one in nitrogen, argon gas or helium or at least two combination；Preferably, the temperature of the drying is 105-350 DEG C.
- 7. the method as described in claim 1, it is characterised in that be passed through CO into the separating liquid2Carry out acidification reaction, solid-liquid Sodium bicarbonate crystal and filtrate are obtained after separation.
- 8. method as claimed in claim 7, it is characterised in that the temperature of the acidification reaction is 15-30 DEG C；Preferably, the time of the acidification reaction is 0.5-2h；Preferably, the pH of the reaction end of the acidification reaction is 7.5-8.3；Preferably, separating liquid is stirred with 100-300r/min speed during the acidification reaction.
- 9. method as claimed in claim 7, it is characterised in that the filtrate is back to the circulation of vanadate solution preparation section Use；Preferably, prepared by the filtrate return vanadium extraction of wet method containing vanadium mineral into vanadate solution process to recycle.
- 10. the method as described in claim any one of 1-9, it is characterised in that the described method comprises the following steps：(1) it is passed through CO in containing vanadium solution2And H2, react, separation of solid and liquid after the completion of reaction, obtain under conditions of heating is pressurizeed Vanadium trioxide solid and separating liquid；(2) the vanadium trioxide solid for obtaining step (1) is dried under protective atmosphere, obtains vanadium trioxide production Product；(3) it is passed through CO in the separating liquid obtained to step (1)2Carry out acidification reaction, obtain after separation of solid and liquid sodium bicarbonate crystal and Filtrate, the filtrate are back to the recycling of vanadate solution preparation section.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314083A (en) * | 2018-04-04 | 2018-07-24 | 河钢股份有限公司承德分公司 | A method of by preparing vanadium trioxide 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 |
| CN114956174A (en) * | 2022-06-28 | 2022-08-30 | 中国科学院过程工程研究所 | Method for preparing vanadium pentoxide from sodium orthovanadate |
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| CN106006735A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method for preparing vanadium trioxide through bone coal vanadium extracting vanadium-rich liquid |
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| CN108314083A (en) * | 2018-04-04 | 2018-07-24 | 河钢股份有限公司承德分公司 | A method of by preparing vanadium trioxide containing vanadium solution |
| CN108314083B (en) * | 2018-04-04 | 2020-11-03 | 河钢股份有限公司承德分公司 | Method for preparing vanadium trioxide from 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 |
| CN114956174A (en) * | 2022-06-28 | 2022-08-30 | 中国科学院过程工程研究所 | Method for preparing vanadium pentoxide from sodium orthovanadate |
| CN114956174B (en) * | 2022-06-28 | 2023-08-08 | 中国科学院过程工程研究所 | Method for preparing vanadium pentoxide from sodium orthovanadate |
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