CN108517424A - A method of being ultrasonically treated precipitation - Google Patents
A method of being ultrasonically treated precipitation Download PDFInfo
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- CN108517424A CN108517424A CN201810307106.4A CN201810307106A CN108517424A CN 108517424 A CN108517424 A CN 108517424A CN 201810307106 A CN201810307106 A CN 201810307106A CN 108517424 A CN108517424 A CN 108517424A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The present invention relates to a kind of method being ultrasonically treated precipitation, the method is：Vanadium solution will be contained to be added in reaction vessel, ammonium salt is added, heated after adjusting pH, after reaching predetermined temperature, stop heating；It opens ultrasonic generator to be ultrasonically treated the liquid in reaction vessel, device is closed after the completion of processing, is separated by solid-liquid separation after static, obtains vanadium product.The present invention carries out precipitation using ultrasonication containing vanadium solution, realize mechanical agitation and vibration of ultrasonic wave stirring collective effect, instead of traditional steam heating and simple mechanical agitation, precipitation process solid-liquid mass transfer effect is preferable, precipitation efficiency and vanadium yield are obviously improved, reduce a ton vanadium waste treating capacity simultaneously, precipitation processing, with good economic efficiency and application prospect can be carried out well to high-concentration and low-concentration qualifying liquid.
Description
Technical field
The present invention relates to vanadium chemical fields, and in particular to a method of being ultrasonically treated precipitation.
Background technology
Precipitation technology is vanadium extraction one vital key link of entire production technology, is directly related to leaching, waste water
With precipitation three processes operational effect, overall cost and economic benefit, for this purpose, invention low-cost high-efficiency benefit precipitation method is mesh
One of the emphasis of preceding numerous scientific workers' research.
Currently, main precipitation technique includes hydrolysis precipitation method, calcium vanadate and ferric vandate precipitation method, ammonium salt precipitation method etc..
It is sodium vanadate solution as solution acidic increase gradually hydrolyzes to hydrolyze precipitation method, produces the process of more sodium vanadates.It is industrial earliest
In this way, China before the 1980s also in this way.Hydrolyze precipitation method the advantages of be it is easy to operate,
It is with short production cycle, production cost is low, allow vanadium concentration wide range fluctuate, the disadvantage is that hydrolysis precipitation obtained by red cake be thick
Vanadium, product purity is relatively low, acid consumption is big, sewage quantity is big, and essentially ammonium salt precipitation is replaced, but hydrolyzing precipitation may be for
The specific vanadium solution system that certain impurity contents are high, symbiosis difficulty separate substance content is high has preferable precipitation effect.Calcium vanadate and
Ferric vandate precipitation method is to containing the lower solution of vanadium concentration, and pH value is under conditions of 5.1-11, after milk of lime or calcium chloride is added,
It heats, stir to get white vanadic acid calcium precipitate.Also can ferrous sulfate, ferric sulfate or ferric trichloride be added in acid condition
Precipitating reagent, heating, stirring can be obtained yellow and precipitated to black ferric vandate.Both intermediate processings are enriched with from low concentration solution
The method of vanadium, using being subject to certain restrictions.
Ammonium salt precipitation method is to produce the method that high-grade vanadic anhydride uses, and the pH value of vanadium solution is different, vanadium
Polymerized form in the solution is also different, and ammonium metavanadate is settled out from weakly alkaline solution, and is then precipitated from acid solution
Go out ammonium poly-vanadate, therefore ammonium salt precipitation is divided into the precipitation of alkalescent ammonium salt, faintly acid ammonium salt precipitation according to precipitation process pH value difference
With acid ammonium salt precipitation.It is industrial generally using acid ammonium salt precipitation method at present.
CN106241871A discloses a kind of high concentration vanadium liquid acid ammonium salt precipitation method, and the method is：Configuration is certain
Concentration ammonium salt solution is used in combination acid that its pH value is adjusted to 2-3；Keep heating, stirring；It is slowly added to high concentration vanadium liquid and acid adding is kept
PH value 2-3；Sustained response filtering to after precipitating completely, that is, obtain ammonium poly-vanadate.105400968 A of CN disclose a kind of acidity
Ammonium salt precipitation method technique：In acid adding tank after an acid adding, sulfuric acid is added into ammonium tank is added in the qualifying liquid for leaching process production
Ammonium carries out precipitation operation subsequently into settling tank by adding steam, secondary acid adding and stirring manual operation.Precipitation is completed
Afterwards, upper liquid enters supernatant tank and is settled, and gained supernatant enters wastewater disposal basin, carries out wastewater treatment, more vanadium of gained
Sour ammonium (APV) underflow enters APV and collects tank；The APV underflows of precipitation gained also collect tank into APV in settling tank, then pass through pump
It is conveyed into plate and frame filter press and carries out washing and filter pressing.Filtrate portion obtained by plate compression machine operation enters leaching process and is returned
With another part enters wastewater disposal basin；The another part of gained is product ammonium poly-vanadate (APV), and work is restored as dry
Sequence raw material.CN105400968A discloses a kind of low-cost high-efficiency precipitation method, includes the following steps：A, vanadium immersion liquid is taken, is added
Sulfuric acid；B, ammonium sulfate is added into treated the vanadium immersion liquid of a steps acid adding；C, b step is added to the solution after ammonium sulfate, be passed through
Steam, adjusting solution ph are 1.8-2.5, stir evenly rear stratification, detach, obtain supernatant and precipitation；D, by step c
Obtained supernatant fraction returns in vanadium immersion liquid, instead of sulfuric acid and part of sulfuric acid ammonium.
Although the above method has the characteristics that ton, vanadium waste yield is few, acid consumption is few, consumption ammonium amount is few, still with tradition
Acid precipitation technique it is the same, due to the use of steam heat so that ton vanadium waste yield it is larger, increase processing waste water cost
And environmental protection pressure.And simple mechanical agitation is only carried out during precipitation, react uneven equal, precipitation efficiency is low, and product refers to
Mark is poor, and unstable product quality thereby reduces economic benefit, it is difficult to obtain industrialization promotion.
Invention content
In view of problems of the prior art, the purpose of the present invention is to provide a kind of sides using ultrasonic wave precipitation
Method, use vibration of ultrasonic wave heating stirring for means carry out precipitation, reduce a ton vanadium waste treating capacity, improve precipitation efficiency and
Vanadium yield, remarkable in economical benefits is promoted, while obtaining the vanadium product of high quality, is had a good application prospect.
The present invention provides a kind of methods using ultrasonic wave precipitation, the described method comprises the following steps：
(1) vanadium solution will be contained to be added in reaction vessel, ammonium salt is added, heated after adjusting pH, after reaching predetermined temperature, stopped
Heating；
(2) it opens ultrasonic generator to be ultrasonically treated the liquid in reaction vessel, dress is closed after the completion of processing
It sets, is separated by solid-liquid separation after static, obtains vanadium product.
Ultrasonic wave is the sound wave that frequency is higher than 20000 hertz, since ultrasonic frequency is very high, so ultrasonic wave and general sound
Wave is compared, its power is very big.When ultrasonic wave is propagated in a liquid, due to the high vibration of liquid particle, meeting exists
Liquid internal generates small cavity.These small cavities swell and are closed rapidly, can make that fierce shock work occurs between liquid particle
With to generate thousands of pressure to a atmospheric pressure up to ten thousand.This violent interaction, can make the temperature of liquid rapid between particle
It so increases, plays good stirring action, to make two kinds of immiscible liquid (Ru Shui and oil) emulsify, and accelerate molten
The dissolving of matter promotes chemical reaction.It is this that by ul-trasonic irradiation, caused various effects are known as the sky of ultrasonic wave in a liquid
Change acts on.
The present invention carries out precipitation in the way of ultrasonication, the technique that precipitation is heated instead of conventional vapor, from source
It is few that ton vanadium waste yield is realized on head, the processing of ton vanadium waste is low；Simultaneously because the cavitation of ultrasonic wave, realizes machinery
Stirring and vibration of ultrasonic wave stir collective effect, and compared with the simple mechanical agitation of tradition, solid-liquid mass transfer effect is good.Profit of the invention
With vibration of ultrasonic wave agitating and heating simultaneously instead of steam heating and simple mechanical agitation, and it is equal to high-concentration and low-concentration qualifying liquid
Precipitation processing can be carried out well, and there is uniform, at low cost reaction, vanadium extraction production efficiency height, good product quality, mixed economy
The various features such as high efficiency.
According to the present invention, the reaction vessel is the reaction kettle of with closure, and the reaction kettle is placed on chuck heating dress
In setting.
According to the present invention, a concentration of 5-80g/L containing vanadium in vanadium solution, preferably 20-50g/L；Such as can be
It is specific between 5g/L, 10g/L, 20g/L, 30g/L, 40g/L, 50g/L, 60g/L, 70g/L or 80g/L and above-mentioned numerical value
Point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the ammonium in step (1) in ammonium salt and the molar ratio containing the vanadium in vanadium solution are 1:(0.8-5), example
Such as can be 1:0.8、1:1、1:2、1:3、1:4 or 1:Specific point value between 5 and above-mentioned numerical value, as space is limited and for
Concise consideration, the present invention no longer exclusive list.
According to the present invention, step (1) described ammonium salt is arbitrary in ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate or ammonium hydrogen carbonate
It is a kind of or at least two combination, such as can be any one in ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate or ammonium hydrogen carbonate,
Typical but non-limiting is combined as：Ammonium sulfate and ammonium hydrogen sulfate, ammonium sulfate and ammonium hydrogen carbonate, ammonium carbonate and ammonium hydrogen carbonate etc.,
As space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the pH that solution is adjusted in step (1) is 1.9-2.1 or 7-9, when the pH is 1.9-2.1, is sunk
Ammonium poly-vanadate is obtained after vanadium；When the pH is 7-9, ammonium metavanadate is obtained after precipitation.Within the above range by pH controls, it helps
In obtaining vanadium product high-quality, that purity is high.
According to the present invention, the temperature heated in step (1) is 70-90 DEG C, for example, can be 70 DEG C, 73 DEG C, 75 DEG C, 78
DEG C, 80 DEG C, 83 DEG C, 85 DEG C, 88 DEG C or the specific point value between 90 DEG C and above-mentioned numerical value, as space is limited and for concise
Consider, the present invention no longer exclusive list.
According to the present invention, the power of step (2) described supersound process is 150-350W, for example, can be 150W, 180W,
Specific point value between 200W, 230W, 250W, 280W, 300W, 330W or 350W and above-mentioned numerical value, as space is limited and for
Concise consideration, the present invention no longer exclusive list.
According to the present invention, time of step (2) described supersound process is 20-45min, for example, can be 20min, 25min,
Specific point value between 30min, 35min, 40min or 45min and above-mentioned numerical value, as space is limited and for concise consideration,
The present invention no longer exclusive list.
According to the present invention, step (2) described ultrasonic generator be set to reaction vessel bottom and/or side to it
In liquid carry out vibrations agitating and heating.
Described be separated by solid-liquid separation of step (2) of the present invention selects mode commonly used in the art to carry out, such as can be filtering, take out
Filter, centrifugation etc., but it is non-be only limitted to this, other suitable solid-liquid separation methods are equally applicable to the present invention.
The method of the present invention for being ultrasonically treated precipitation includes the following steps as a preferred technical solution,：
(1) being added in the closed reactor being placed in chuck heating device containing vanadium solution by a concentration of 5-80g/L of vanadium,
Ammonium salt is added, the molar ratio of control ammonium vanadium is 1:(0.8-5), adjusting pH are 1.9-2.1 or 7-9, are then heated to 70-90 DEG C,
After reaching predetermined temperature, stop heating；
(2) ultrasonic generator is opened, in reactor bottom and/or side to liquid ultrasonic treatment 20- therein
45min, power 150-350W close device, are separated by solid-liquid separation after static, obtain vanadium product after the completion of processing.
For this purpose, the present invention uses following technical scheme：
Compared with prior art, the present invention at least has the advantages that：
(1) present invention uses vibration of ultrasonic wave heating stirring to carry out precipitation for means, adds instead of traditional handicraft steam
The mode of heat reduces because entering the moisture in reaction system in steam heating process, reduces a ton vanadium waste treating capacity, ton vanadium
60 yuan or so of wastewater treatment cost savings；The solid-liquid mass transfer of vibration of ultrasonic wave stirring simultaneously is preferable, is stirred with simple tradition machinery
It compares, precipitation efficiency improves 5-15%, and vanadium yield improves 0.19-0.95%, and remarkable in economical benefits is promoted.
(2) present invention carries out precipitation using ultrasonication, and entire reaction process uniformly carries out, and improves product quality,
It can be evenly distributed, the vanadium product that granularity is small, purity is high.
(2) present invention can carry out precipitation processing well to high-concentration and low-concentration containing vanadium solution, preferably solve biography
System technique precipitation is difficult to realize the technical bottleneck of high concentration precipitation.
Description of the drawings
Fig. 1 is the schematic device used in the ultrasonic high-efficiency precipitation that a kind of specific implementation mode of the present invention provides；
In figure：1- ultrasonic generators, 2- reaction kettles, 3- precipitation reaction solutions, 4- reaction kettle sealing covers, 5- mechanical agitations
Paddle.
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 subject to claims.
Specific implementation mode
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
As shown in Figure 1, ultrasonic high-efficiency precipitation process of the present invention can be realized with following device：Precipitation reaction solution
3 are placed in reaction kettle 2, and sealing cover 4 is arranged in 2 top of reaction kettle, and mechanical agitation paddle 5 immerses precipitation reaction solution 3 through sealing cover 4,
Ultrasonic generator 1 is set to the bottom and/or side of reaction kettle 2.
For the present invention is better described, it is easy to understand technical scheme of the present invention, of the invention is typical but non-limiting
Embodiment is as follows：
Embodiment 1
A method of using ultrasonic high-efficiency precipitation, include the following steps：
(1) a concentration of 21g/L of 2000mL are added containing vanadium solution in reaction kettle, reaction kettle is placed on chuck heating dress
It sets, according to ammonium vanadium 1:Ammonium sulfate is added in 3 molar ratio, and it is 1.9 to adjust PH using sulfuric acid solution；After solution is heated to 90 DEG C,
Stop heating；
(2) ultrasonic generator is opened, vibrations agitating and heating precipitation is carried out to the liquid in reaction kettle using ultrasonic wave
Processing, control sonification power are 200W, and time 25min, precipitation temperature is 97 DEG C, and device is closed after the completion of processing, quiet
It is separated by solid-liquid separation after only, obtains vanadium product.
After the completion of the present embodiment precipitation, the residual content of vanadium of static rear precipitation supernatant and sediment ammonium poly-vanadate quality are measured,
As a result it shows：Supernatant content of vanadium is 0.08g/l, and precipitation rate is 99.62%, applies mechanical agitation phase merely with the same terms
Than precipitation rate improves 0.19%；Sediment ammonium poly-vanadate quality：V2O589.15%, S content 0.10%, potassium sodium content 0.7%.
Embodiment 2
A method of using ultrasonic high-efficiency precipitation, include the following steps：
(1) a concentration of 23g/L of 2000mL are added containing vanadium solution in reaction kettle, reaction kettle is placed on chuck heating dress
It sets, according to ammonium vanadium 1:Ammonium sulfate is added in 3.5 molar ratio, and it is 2.0 to adjust PH using sulfuric acid solution；Solution is heated to 86 DEG C
Afterwards, stop heating；
(2) ultrasonic generator is opened, vibrations agitating and heating precipitation is carried out to the liquid in reaction kettle using ultrasonic wave
Processing, control sonification power are 250W, and time 30min, precipitation temperature is 97 DEG C, and device is closed after the completion of processing, quiet
It is separated by solid-liquid separation after only, obtains vanadium product.
After the completion of the present embodiment precipitation, the residual content of vanadium of static rear precipitation supernatant and sediment ammonium poly-vanadate quality are measured,
As a result it shows：Supernatant content of vanadium is 0.08g/l, and precipitation rate is 99.65%, applies mechanical agitation phase merely with the same terms
Than precipitation rate improves 0.22%；Sediment ammonium poly-vanadate quality：V2O589.10%, S content 0.098%, potassium sodium content
0.71%.
Embodiment 3
A method of using ultrasonic high-efficiency precipitation, include the following steps：
(1) a concentration of 25g/L of 2000mL are added containing vanadium solution in reaction kettle, reaction kettle is placed on chuck heating dress
It sets, according to ammonium vanadium 1:Ammonium hydrogen sulfate is added in 5 molar ratio, and it is 2.1 to adjust PH using sulfuric acid solution；Solution is heated to 80 DEG C
Afterwards, stop heating；
(2) ultrasonic generator is opened, vibrations agitating and heating precipitation is carried out to the liquid in reaction kettle using ultrasonic wave
Processing, control sonification power are 250W, and time 40min, precipitation temperature is 97 DEG C, and device is closed after the completion of processing, quiet
It is separated by solid-liquid separation after only, obtains vanadium product.
After the completion of the present embodiment precipitation, the residual content of vanadium of static rear precipitation supernatant and sediment ammonium poly-vanadate quality are measured,
As a result it shows：Supernatant content of vanadium is 0.10g/l, and precipitation rate is 99.60%, applies mechanical agitation phase merely with the same terms
Than precipitation rate improves 0.95%；Sediment ammonium poly-vanadate quality：V2O589.20%, S content 0.11%, potassium sodium content
0.70%.
Embodiment 4
A method of using ultrasonic high-efficiency precipitation, include the following steps：
(1) a concentration of 30g/L of 2000mL are added containing vanadium solution in reaction kettle, reaction kettle is placed on chuck heating dress
It sets, according to ammonium vanadium 1:Ammonium sulfate is added in 4 molar ratio, and it is 2.1 to adjust PH using sulfuric acid solution；After solution is heated to 77 DEG C,
Stop heating；
(2) ultrasonic generator is opened, vibrations agitating and heating precipitation is carried out to the liquid in reaction kettle using ultrasonic wave
Processing, control sonification power are 300W, and time 35min, precipitation temperature is 97 DEG C, and device is closed after the completion of processing, quiet
It is separated by solid-liquid separation after only, obtains vanadium product.
After the completion of the present embodiment precipitation, the residual content of vanadium of static rear precipitation supernatant and sediment ammonium poly-vanadate quality are measured,
As a result it shows：Supernatant content of vanadium is 0.11g/l, and precipitation rate is 99.63%, applies mechanical agitation phase merely with the same terms
Than precipitation rate improves 0.23%；Sediment ammonium poly-vanadate quality：V2O589.50%, S content 0.10%, potassium sodium content
0.97%.
Embodiment 5
A method of using ultrasonic high-efficiency precipitation, include the following steps：
(1) a concentration of 35g/L of 2000mL are added containing vanadium solution in reaction kettle, reaction kettle is placed on chuck heating dress
It sets, according to ammonium vanadium 1:Ammonium sulfate is added in 1 molar ratio, and it is 8 to adjust PH using ammonium hydroxide；After solution is heated to 72 DEG C, stop adding
Heat；
(2) ultrasonic generator is opened, vibrations agitating and heating precipitation is carried out to the liquid in reaction kettle using ultrasonic wave
Processing, control sonification power are 350W, and time 35min, precipitation temperature is 97 DEG C, and device is closed after the completion of processing, quiet
It is separated by solid-liquid separation after only, obtains vanadium product.
After the completion of the present embodiment precipitation, the residual content of vanadium of static rear precipitation supernatant and sediment ammonium metavanadate quality are measured,
As a result it shows：Supernatant content of vanadium is 0.13g/l, and precipitation rate is 99.63%, applies mechanical agitation phase merely with the same terms
Than precipitation rate improves 0.77%；Sediment ammonium metavanadate quality：V2O589.27%, S content 0.12%, potassium sodium content
0.70%.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, 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 also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of method being ultrasonically treated precipitation, which is characterized in that the described method comprises the following steps：
(1) it will contain in vanadium solution addition reaction vessel, ammonium salt is added, is heated after adjusting pH, and after reaching predetermined temperature, stop adding
Heat；
(2) it opens ultrasonic generator to be ultrasonically treated the liquid in reaction vessel, device is closed after the completion of processing, it is quiet
It is separated by solid-liquid separation after only, obtains vanadium product.
2. the method as described in claim 1, which is characterized in that the reaction vessel is the reaction kettle with sealing cover, described
Reaction kettle is placed in chuck heating device.
3. method as claimed in claim 1 or 2, which is characterized in that a concentration of 5-80g/L containing vanadium in vanadium solution, it is excellent
It is selected as 20-50g/L.
4. method as described in any one of claims 1-3, which is characterized in that ammonium in step (1) in ammonium salt and contain vanadium solution
In vanadium molar ratio be 1:(0.8-5)；
Preferably, step (1) described ammonium salt be ammonium sulfate, ammonium hydrogen sulfate, ammonium carbonate or ammonium hydrogen carbonate in any one or extremely
Few two kinds of combination.
5. method according to any one of claims 1-4, which is characterized in that the pH for adjusting solution in step (1) is 1.9-2.1
Or 7-9.
6. method as described in any one in claim 1-5, which is characterized in that the temperature heated in step (1) is 70-90 DEG C.
7. method as claimed in any one of claims 1 to 6, which is characterized in that the power of step (2) described supersound process is
150-350W。
8. such as claim 1-7 any one of them methods, which is characterized in that the time of step (2) described supersound process is 20-
45min。
9. such as claim 1-8 any one of them methods, which is characterized in that step (2) the ultrasonic generator setting
Vibrations agitating and heating is carried out to liquid therein in the bottom of reaction vessel and/or side.
10. such as claim 1-9 any one of them methods, which is characterized in that the described method comprises the following steps：
(1) being added in the closed reactor being placed in chuck heating device containing vanadium solution by a concentration of 5-80g/L of vanadium, is added
The molar ratio of ammonium salt, control ammonium vanadium is 1:(0.8-5), adjusting pH are 1.9-2.1 or 7-9, are then heated to 70-90 DEG C, are reached
After predetermined temperature, stop heating；
(2) ultrasonic generator is opened, in reactor bottom and/or side to liquid ultrasonic treatment 20-45min therein,
Control power is 150-350W, and device is closed after the completion of processing, is separated by solid-liquid separation after static, obtains vanadium product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247952A (en) * | 2021-04-29 | 2021-08-13 | 武汉理工大学 | Method for preparing high-purity vanadium pentoxide from vanadium-rich liquid by utilizing ultrasonic waves |
| CN116119716A (en) * | 2022-12-13 | 2023-05-16 | 中核沽源铀业有限责任公司 | Ammonium molybdate preparation method and device |
| CN116254427A (en) * | 2023-03-10 | 2023-06-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for controlling granularity of vanadium precipitation product |
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| CN107522218A (en) * | 2017-10-19 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of ultrasound-enhanced calcium vanadate ammonium leaching and the method for preparing nano-calcium carbonate |
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
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| CN113247952A (en) * | 2021-04-29 | 2021-08-13 | 武汉理工大学 | Method for preparing high-purity vanadium pentoxide from vanadium-rich liquid by utilizing ultrasonic waves |
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