CN114149027B - Method for purifying vanadium pentoxide by melt volatilization - Google Patents
Method for purifying vanadium pentoxide by melt volatilization Download PDFInfo
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- CN114149027B CN114149027B CN202111347640.6A CN202111347640A CN114149027B CN 114149027 B CN114149027 B CN 114149027B CN 202111347640 A CN202111347640 A CN 202111347640A CN 114149027 B CN114149027 B CN 114149027B
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 298
- 238000000034 method Methods 0.000 title claims abstract description 61
- 239000007788 liquid Substances 0.000 claims abstract description 117
- 238000002844 melting Methods 0.000 claims abstract description 45
- 230000008018 melting Effects 0.000 claims abstract description 45
- 238000001816 cooling Methods 0.000 claims abstract description 41
- 239000012535 impurity Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000000498 cooling water Substances 0.000 claims description 24
- 239000003570 air Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 13
- 238000010924 continuous production Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052698 phosphorus Inorganic materials 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 abstract description 12
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000005587 bubbling Effects 0.000 abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000004530 micro-emulsion Substances 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000013043 chemical agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000009615 deamination Effects 0.000 description 2
- 238000006481 deamination reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PTXMVOUNAHFTFC-UHFFFAOYSA-N alumane;vanadium Chemical compound [AlH3].[V] PTXMVOUNAHFTFC-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of vanadium metallurgy, and discloses a method for purifying vanadium pentoxide by melt volatilization. The method comprises the following steps: (1) The vanadium pentoxide is melted to form a liquid molten pool at the temperature of 800-1500 ℃; (2) Maintaining the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Introducing gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.15-0.2 Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, and cooling to 120-450 ℃ to obtain vanadium pentoxide with the purity of not less than 99.9%. According to the difference of the melting point and saturated vapor pressure of the vanadium pentoxide and the impurity oxide, the invention adopts the gas supply bubbling at the bottom of the molten pool to accelerate the volatilization of the vanadium pentoxide vapor so as to separate and purify the vanadium pentoxide to prepare the high-purity vanadium pentoxide, and the process does not use chemistry or generate waste water, so that the process is simple and the production cost is low.
Description
Technical Field
The invention relates to the technical field of vanadium metallurgy, in particular to a method for purifying vanadium pentoxide by melting volatilization.
Background
Vanadium pentoxide is widely applied to the fields of steel, chemical industry, aerospace, energy and the like. With the development of the material field, the high-end vanadium-containing materials such as vanadium electrolyte, vanadium-aluminum alloy, metal vanadium, vanadium catalyst and the like have higher and higher purity requirements on the raw material vanadium pentoxide, and the market demand of the high-purity vanadium pentoxide also has a rapid growing trend. At present, the preparation of the high-purity vanadium pentoxide comprises a chemical precipitation method, a solution extraction method, a chlorination method and the like.
CN112209441a discloses a method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate, which comprises the steps of performing alkali dissolution of ammonium metavanadate, aging of vanadium liquid, hydrolysis of precipitated vanadium, re-dissolution of precipitated vanadium to obtain ammonium metavanadate with purity of more than 99.8%, and performing calcination deamination to obtain high-purity vanadium pentoxide. The method adopts the methods of secondary dissolution, primary adsorption impurity removal, secondary precipitation and primary calcination deamination to obtain the high-purity vanadium pentoxide, and chemical agents such as sodium hydroxide, sulfuric acid, ammonia water and the like are used in the process, so that the process has the defects of long process flow, large agent dosage and high treatment difficulty of the generated wastewater.
CN111057876a discloses a method for preparing high-purity vanadium pentoxide by microemulsion extraction, which comprises the steps of adjusting the pH, preparing the microemulsion, extracting, carrying microemulsion phase washing, back extracting, precipitating vanadium from alkaline ammonium salt, calcining and deaminizing to obtain the high-purity vanadium pentoxide, wherein organic extractant, kerosene, sodium hydroxide, sodium chloride, sulfuric acid, ammonium sulfate or ammonium chloride and other chemical agents are used in the process, so that the process also has the defects of long process flow, large agent consumption and large difficulty in treating the generated wastewater.
CN103130279B discloses a method for producing high-purity vanadium pentoxide by a chlorination method, which comprises the steps of uniformly mixing a vanadium-containing substance and a carbon simple substance, drying, adding the mixture into a reactor, and sequentially carrying out chlorination, rectification, hydrolysis and post-treatment to obtain the high-purity vanadium pentoxide.
In summary, the existing preparation method of the high-purity vanadium pentoxide has the problems of long process flow, large medicament consumption, environmental pollution, incomplete impurity removal and the like, so that the development of the preparation method of the high-purity vanadium pentoxide with simple process, safety, environmental protection and low cost is necessary.
Disclosure of Invention
The invention aims to solve the problems of long process flow, large medicament consumption, environmental pollution and incomplete impurity removal existing in the preparation method of high-purity vanadium pentoxide in the prior art, and provides a method for purifying the vanadium pentoxide by fusion volatilization, which ensures V according to the difference of the melting point and saturated vapor pressure of the vanadium pentoxide and the impurity oxide 2 O 5 Under the condition that decomposition reaction does not occur, the vanadium pentoxide is melted to form a liquid molten pool, the saturated vapor pressure of the vanadium pentoxide is rapidly increased after the temperature is higher than the melting point, the volatilization rate of the vanadium pentoxide is accelerated through bubbling of air supply at the bottom of the molten pool, and impurity elements are difficult to volatilize, so that the high-efficiency separation of heat exchange impurities of the vanadium pentoxide is realized, and the high-purity vanadium pentoxide is obtained through condensation and collection of the vanadium pentoxide vapor.
In order to achieve the above object, the present invention provides a method for purifying vanadium pentoxide by melt volatilization, comprising the steps of:
(1) The vanadium pentoxide is melted to form a liquid molten pool at the temperature of 800-1500 ℃;
(2) Maintaining the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor;
(3) Introducing gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.15-0.2 Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, and cooling to 120-450 ℃ to obtain vanadium pentoxide with the purity of not less than 99.9%.
Preferably, the method further comprises:
(4) When the liquid molten pool level is reduced to 0.05-0.10 times of the initial value of the liquid molten pool level in the step (1), emptying the residual materials in the liquid molten pool;
(5) Repeating the steps (1) - (4) for continuous production.
Preferably, in the step (1), the purity of the vanadium pentoxide is less than or equal to 99.5%, and the impurity content is more than or equal to 0.5% by mass.
More preferably, the impurity includes at least one of Fe, cr, mn, si, na, K, P and S.
Preferably, in step (1), vanadium pentoxide is melted at 850-1300 ℃ to form a liquid molten pool.
Preferably, in step (3), a gas is introduced into the liquid bath at a pressure of 0.16 to 0.19 Mpa.
Preferably, in step (3), the gas introduced into the liquid bath is at least one of argon, helium, oxygen, nitrogen or air.
Preferably, in step (3), the vanadium pentoxide vapour is cooled by circulating cooling water.
Preferably, the method is implemented in a vanadium pentoxide purification device comprising a melting furnace, a condenser and an exhaust gas treatment system which are arranged in sequence,
the top of the melting furnace is provided with a feed inlet, the periphery and the bottom of the melting furnace are provided with a plurality of heating elements, and the bottom of the melting furnace is also provided with a discharge hole and an air supply system;
the condenser comprises a cooling channel, a plurality of condenser partition plates are respectively arranged on the upper inner wall and the lower inner wall of the cooling channel at intervals, a cooling water inlet, a cooling water channel and a cooling water outlet are arranged on the outer side of the top of the cooling channel, and a plurality of collectors are continuously and detachably arranged at the bottom of the cooling channel.
Preferably, the interval between two adjacent condenser baffles is 20-80 cm.
Preferably, the bottom of the cooling channel is continuously and detachably provided with 3-8 collectors.
Preferably, the method comprises the steps of:
s1, adding vanadium pentoxide into the melting furnace from the charging port, closing the charging port, heating the melting furnace to raise the temperature, and melting the vanadium pentoxide to form a liquid molten pool at 800-1500 ℃;
s2, continuously heating the melting furnace to maintain the temperature of a liquid molten pool, and converting liquid vanadium pentoxide into vanadium pentoxide vapor;
s3, starting the gas supply system, introducing the gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.15-0.2 Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, cooling in the cooling channel to 120-450 ℃, and obtaining vanadium pentoxide with the purity of not less than 99.9% in the collector.
Preferably, the method further comprises:
s4, when the liquid molten pool level is reduced to 0.05-0.10 times of the initial value of the liquid molten pool level in the step S2, closing the air supply system, stopping heating, opening the discharge port, and emptying the residual materials in the liquid molten pool;
s5, closing the discharge hole, and repeating the steps S1 to S4 to perform continuous production.
According to the difference of the melting point and saturated vapor pressure of the vanadium pentoxide and the impurity oxide, the gas supply bubbling at the bottom of the molten pool is adopted to accelerate the volatilization of the vanadium pentoxide vapor so as to separate and purify the vanadium pentoxide, no chemical is used in the process, no wastewater is generated, the process is simple, the production cost is low, and the high-purity vanadium pentoxide can be obtained only through one-step heating volatilization separation, so that the method has obvious advantages in the aspects of safety, environmental protection and economic cost compared with other vanadium pentoxide production processes.
Drawings
FIG. 1 is a schematic diagram of a vanadium pentoxide purification apparatus according to the present invention.
Description of the reference numerals
10 a melting furnace; 11 charging ports; a heating element 12; 13, a discharge hole; 14 a gas supply system;
a 20 condenser; 21 cooling channels; 22 condenser baffles; 23 cooling water inlet; 24 cooling water channels; 25 a cooling water outlet; 26 collectors;
30 an exhaust gas treatment system.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The method for purifying vanadium pentoxide by melt volatilization provided by the invention comprises the following steps:
(1) The vanadium pentoxide is melted to form a liquid molten pool at the temperature of 800-1500 ℃;
(2) Maintaining the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor;
(3) Introducing gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.15-0.2 Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, and cooling to 120-450 ℃ to obtain vanadium pentoxide with the purity of not less than 99.9%.
In the method, vanadium pentoxide is melted at a specific temperature to form a liquid molten pool, then gas is introduced from the bottom of the liquid molten pool, the volatilization rate of the vanadium pentoxide vapor is accelerated by bubbling gas from the bottom of the liquid molten pool, the vanadium pentoxide vapor leaves the liquid molten pool, impurities are remained in the liquid molten pool, and then the volatilized vanadium pentoxide vapor is cooled to obtain high-purity vanadium pentoxide.
In a specific embodiment, to achieve continuous production, the method further comprises:
(4) When the liquid molten pool level is reduced to 0.05-0.10 times of the initial value of the liquid molten pool level in the step (1), emptying the residual materials in the liquid molten pool;
(5) Repeating the steps (1) - (4) for continuous production.
In the method of the present invention, the vanadium pentoxide may be vanadium pentoxide containing various impurities.
In a specific embodiment, in the step (1), the purity of the vanadium pentoxide is less than or equal to 99.5%, and the impurity content is more than or equal to 0.5% by mass;
in a preferred embodiment, the impurities in the vanadium pentoxide include at least one of Fe, cr, mn, si, na, K, P and S. Further, fe, cr, mn, si, P is present in the vanadium pentoxide in the form of oxides and Na, K, S are present in the vanadium pentoxide in the form of sulfates.
In the method of the invention, in order to ensure V 2 O 5 Can melt and form vapor without the impurities forming vapor, and the melting temperature needs to be controlled within a proper range.
In particular embodiments, in step (1), vanadium pentoxide may be melted to form a liquid melt pool at 800 ℃, 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃, or 1500 ℃.
In a preferred embodiment, in step (1), vanadium pentoxide is melted at a temperature of 850-1300 ℃ to form a liquid bath.
In the method of the invention, in order to provide sufficient gas into the liquid molten pool, simultaneously, the vanadium pentoxide vapor can be quickly volatilized without volatilizing impurities, thereby realizing V 2 O 5 And the air supply pressure needs to be reasonably controlled for full separation from impurities.
In a specific embodiment, in step (3), gas may be introduced into the liquid bath from the bottom of the liquid bath at a pressure of 0.15Mpa, 0.16Mpa, 0.17Mpa, 0.18Mpa, 0.19Mpa or 0.2 Mpa.
In a preferred embodiment, in step (3), a gas is introduced into the liquid bath at a pressure of from 0.16 to 0.19 Mpa.
In the method of the present invention, in the step (3), the gas may be a gas conventionally used in the art, which does not cause pollution to the environment.
In a specific embodiment, in step (3), the gas introduced into the liquid bath may be at least one of argon, helium, oxygen, nitrogen or air, preferably argon and oxygen.
In a preferred embodiment, in step (3), the vanadium pentoxide vapor may be cooled down by a common cooling medium, preferably by circulating cooling water.
The apparatus used to carry out the method is not limited as long as the present invention can be implemented.
In a specific embodiment, the method of the present invention may be implemented in a vanadium pentoxide purification apparatus as shown in fig. 1, which includes a melting furnace 10, a condenser 20 and an exhaust gas treatment system 30 disposed in this order,
the top of the melting furnace 10 is provided with a charging hole 11, the periphery and the bottom are provided with a plurality of heating elements 12, and the bottom of the melting furnace 10 is also provided with a discharging hole 13 and an air supply system 14;
the condenser 20 comprises a cooling channel 21, a plurality of condenser baffles 22 are respectively arranged on the upper inner wall and the lower inner wall of the cooling channel 21 at intervals, a cooling water inlet 23, a cooling water channel 24 and a cooling water outlet 25 are arranged on the outer side of the top of the cooling channel 21, and a plurality of collectors 26 are continuously and detachably arranged at the bottom of the cooling channel 21.
In the vanadium pentoxide purifying device, after vanadium pentoxide is added from a charging port 11, a heating element 12 heats a melting furnace 10, and the vanadium pentoxide is melted in the melting furnace 10 to form a liquid molten pool; then starting the gas supply system 14, introducing gas from the bottom of the liquid molten pool, enabling the vanadium pentoxide vapor to volatilize from the liquid molten pool rapidly and enter the cooling channel 21, cooling the vapor by a circulating cooling medium provided in the cooling water channel 24, and enabling the vapor to become vanadium pentoxide solid which falls into the collector 26 to obtain high-purity vanadium pentoxide; the exhaust gas treatment system 30 is used for treating pollutants such as dust. The plurality of collectors 26 are arranged continuously, that is, the plurality of collectors 26 are arranged next to one another, no interval exists between the two adjacent collectors 26, so that any part in the cooling channel 21 can be cooled and then falls down to form solid high-purity V 2 O 5 Can fall into the collector 26.
In a specific embodiment, the interval between two adjacent condenser baffles 22 is 20-80 cm. In the present invention, if the interval between adjacent two of the condenser baffles 22 is too small, the vapor flow resistance increases to cause an increase in residence time thereof in the cooler, decreasing production efficiency; if the spacing between adjacent two of the condenser baffles 22 is too great, the reduced vapor drag results in a reduced residence time in the condenser, failing to cool the vapor to a specified temperature by sufficient heat exchange to gain access to the collector. Therefore, in the present invention, the interval between two adjacent condenser baffles 22 is set at 20 to 80cm, and vapor is sufficiently heat-exchanged cooled to a specified temperature in the cooler and then enters the collector while ensuring proper production efficiency.
In a preferred embodiment, the spacing between two adjacent ones of the condenser baffles 22 is 30 to 60cm.
In another preferred embodiment, the bottom of the cooling channel 21 is continuously detachably provided with 3 to 8 collectors 26.
On the basis of the implementation of the invention by using the vanadium pentoxide purification device shown in fig. 1, the method comprises the following steps:
s1, adding vanadium pentoxide into the melting furnace 10 from the feed inlet 11, closing the feed inlet 11, and then heating the melting furnace 10 to raise the temperature, wherein the vanadium pentoxide is melted to form a liquid molten pool at 800-1500 ℃;
s2, continuously heating the melting furnace 10 to maintain the temperature of a liquid molten pool, and converting liquid vanadium pentoxide into vanadium pentoxide vapor;
s3, starting the gas supply system 14, introducing the gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.15-0.2 Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, cooling in the cooling channel 21 to 120-450 ℃, and obtaining vanadium pentoxide with the purity of not less than 99.9% in the collector 26.
In the method, the vanadium pentoxide material is added into the melting furnace 10 through the charging hole 11, then the melting furnace 10 is heated to 800-1500 ℃ through the heating element 12, so that the vanadium pentoxide is melted to form a liquid molten pool under the condition of 800-1500 ℃, then gas is introduced from the bottom of the liquid molten pool through the gas supply system 14, the pressure of the introduced gas is controlled to be 0.15-0.2 Mpa, the volatilization of the vanadium pentoxide vapor is promoted, the volatilized vapor enters the cooling channel 21, impurities are left in the melting furnace 10, and then the circulating cooling water in the cooling water channel 24 and other cooling mediums cool the vanadium pentoxide vapor to convert the vanadium pentoxide vapor into vanadium pentoxide solid, and the vanadium pentoxide solid falls into the collector 26 to obtain the high-purity vanadium pentoxide.
In a preferred embodiment, the method further comprises:
s4, when the liquid molten pool level is reduced to 0.05-0.10 times of the initial value of the liquid molten pool level in the step S2, closing the air supply system 14, stopping heating, opening the discharge port 13, and emptying the residual materials in the liquid molten pool;
s5, closing the discharge hole 13, and repeating the steps S1 to S4 to perform continuous production.
In the invention, after a liquid molten pool is formed, the vanadium pentoxide is volatilized from the liquid molten pool continuously along with continuous heating and continuous gas ventilation. When the liquid molten pool level is reduced to 0.05-0.10 times of the initial liquid molten pool level, the air supply system 14 is closed, heating is stopped, the rest materials are emptied, and the discharge port 13 is closed, so that vanadium pentoxide can be added again for continuous production.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
The examples of the present invention are all carried out in the following vanadium pentoxide purification apparatus.
As shown in fig. 1, the vanadium pentoxide purifying device comprises a melting furnace 10, a condenser 20 and a tail gas treatment system 30 which are sequentially arranged, wherein a charging hole 11 is arranged at the top of the melting furnace 10, a plurality of heating elements 12 are arranged at the periphery and the bottom of the melting furnace 10, and a discharging hole 13 and a gas supply system 14 are also arranged at the bottom of the melting furnace 10; the condenser 20 comprises a cooling channel 21, a plurality of condenser partition plates 22 are respectively arranged on the upper inner wall and the lower inner wall of the cooling channel 21 at intervals, the interval between every two adjacent condenser partition plates 22 is 20-80 cm, a cooling water inlet 23, a cooling water channel 24 and a cooling water outlet 25 are arranged on the outer side of the top of the cooling channel 21, and 3-8 collectors 26 are continuously and detachably arranged at the bottom of the cooling channel 21.
Example 1
(1) Adding vanadium pentoxide (the purity of the vanadium pentoxide is 96.4%, the content of Fe is 0.48%, the content of Cr is 0.59%, the content of Si is 0.62%, the content of Na is 1.74% and the content of P is 0.16% by mass) into the melting furnace 10 from the charging port 11, closing the charging port 11, and heating the melting furnace 10 to 1300 ℃ to enable the vanadium pentoxide to be completely melted to form a liquid molten pool; (2) Continuously heating to maintain the temperature of the liquid molten pool so as to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Starting a gas supply system 14, introducing argon into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.16Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, cooling to 230 ℃ in a cooling channel 21 by circulating cooling water, and obtaining high-purity vanadium pentoxide in a collector 26; (4) When the liquid molten pool level is reduced to 0.08 times of the initial value of the liquid molten pool in the step (1), the air supply system 14 is closed, heating is stopped, the discharge hole 13 is opened, and the residual materials in the liquid molten pool are emptied; (5) And (5) closing the discharge hole 13, and repeating the steps (1) - (4) to perform continuous production.
The purity of the high-purity vanadium pentoxide obtained by the detection was 99.90%, the content of Fe was 0.022% by mass, the content of Cr was 0.018% by mass, the content of Si was 0.009% by mass, the content of Na was 0.039% by mass, and the content of P was 0.002% by mass.
Example 2
(1) Adding vanadium pentoxide (the purity of the vanadium pentoxide is 98.1%, the content of Fe is 0.34%, the content of Mn is 0.69%, the content of Si is 0.51%, and the content of P is 0.25% by mass) into a melting furnace 10 from a charging port 11, closing the charging port 11, and heating the melting furnace 10 to 1150 ℃ to enable the vanadium pentoxide to be completely melted to form a liquid molten pool; (2) Continuously heating to maintain the temperature of the liquid molten pool so as to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Starting an air supply system 14, introducing oxygen into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.18Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, cooling to 170 ℃ in a cooling channel 21 by circulating cooling water, and obtaining high-purity vanadium pentoxide in a collector 26; (4) When the liquid molten pool level is reduced to 0.09 times of the initial value of the liquid molten pool in the step (1), the air supply system 14 is closed, heating is stopped, the discharge port 13 is opened, and the residual materials in the liquid molten pool are emptied; (5) And (5) closing the discharge hole 13, and repeating the steps (1) - (4) to perform continuous production.
The purity of the high-purity vanadium pentoxide obtained by detection is 99.96%, the content of Fe is 0.002 mass%, the content of Mn is 0.010 mass%, the content of Si is 0.017 mass%, and the content of P is 0.004 mass%.
Example 3
(1) Adding vanadium pentoxide (the purity of the vanadium pentoxide is 99.0%, the content of Fe is 0.14%, the content of Cr is 0.16%, the content of Si is 0.15%, the content of Na is 0.23%, the content of K is 0.12%, and the content of P is 0.18%) into a melting furnace 10 from a charging port 11, closing the charging port 11, and heating the melting furnace 10 to 870 ℃ to enable the vanadium pentoxide to be completely melted to form a liquid molten pool; (2) Continuously heating to maintain the temperature of the liquid molten pool so as to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Starting an air supply system 14, introducing oxygen into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.16Mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, cooling to 140 ℃ in a cooling channel 21 by circulating cooling water, and obtaining high-purity vanadium pentoxide in a collector 26; (4) When the liquid molten pool level is reduced to 0.06 times of the initial value of the liquid molten pool in the step (1), the air supply system 14 is closed, heating is stopped, the discharge port 13 is opened, and the residual materials in the liquid molten pool are emptied; (5) And (5) closing the discharge hole 13, and repeating the steps (1) - (4) to perform continuous production.
The purity of the high-purity vanadium pentoxide obtained by the detection was 99.97%, the content of Fe was 0.001 mass%, the content of Cr was 0.003 mass%, the content of Si was 0.011 mass%, the content of Na was 0.005 mass%, the content of K was 0.002 mass%, and the content of P was 0.002 mass%.
Comparative example 1
The process of example 3 was carried out, except that in step (1), the melting furnace 10 was heated to 700℃to completely melt vanadium pentoxide to form a liquid bath.
The purity of the vanadium pentoxide obtained by the detection was 99.72%, the content of Fe, cr, si, na, K, and P were 0.011, 0.007, 0.02, 0.094, 0.03, 0.09, and 0.09, respectively.
Comparative example 2
The procedure of example 3 was followed, except that in step (3), oxygen was introduced into the liquid bath from the bottom of the liquid bath at a pressure of 0.13 MPa.
The purity of the vanadium pentoxide obtained by the detection was 99.63%, the content of Fe, cr, si, na, K and P were 0.08%, 0.07%, 0.04%, 0.071%, 0.03%, 0.06% by mass, respectively.
Comparative example 3
The raw materials described in the example 3 are adopted, the high-purity vanadium pentoxide is prepared according to the method of multiple re-dissolution-precipitation of the existing production process, the vanadium pentoxide is dissolved by adopting sodium hydroxide, then sulfuric acid solution is added to adjust the pH value to 1.85, vanadium is precipitated at 95 ℃, ammonium vanadate is obtained after precipitation, the above operation is repeated for 5 times, and the ammonium vanadate is deaminated under the condition of 520 ℃.
The purity of the vanadium pentoxide obtained by the detection was 99.37%, the content of Fe was 0.09% by mass, the content of Cr was 0.06% by mass, the content of Si was 0.11% by mass, the content of Na was 0.13% by mass, the content of K was 0.06% by mass, and the content of P was 0.14% by mass.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (11)
1. A method for purifying vanadium pentoxide by melt volatilization, which is characterized by comprising the following steps:
(1) Melting vanadium pentoxide at 850-1300 ℃ to form a liquid molten pool;
(2) Maintaining the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor;
(3) Introducing gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.16-0.19 mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, and cooling to 120-450 ℃ to obtain vanadium pentoxide with the purity of not less than 99.9%.
2. The method according to claim 1, wherein the method further comprises:
(4) When the liquid molten pool level is reduced to 0.05-0.10 times of the initial value of the liquid molten pool level in the step (1), emptying the residual materials in the liquid molten pool;
(5) Repeating the steps (1) - (4), and carrying out continuous production.
3. The method according to claim 1, wherein in the step (1), the purity of the vanadium pentoxide is 99.5% or less and the impurity content is 0.5% or more.
4. A method according to claim 3, wherein the impurities comprise at least one of Fe, cr, mn, si, na, K, P and S.
5. The method of claim 1 wherein in step (3) the gas introduced into the liquid bath is at least one of argon, helium, oxygen, nitrogen or air.
6. The method according to claim 1, wherein in step (3), the vanadium pentoxide vapor is cooled down by circulating cooling water.
7. The method according to any one of claims 1 to 6, characterized in that the method is carried out in a vanadium pentoxide purification device comprising a melting furnace (10), a condenser (20) and an exhaust gas treatment system (30) arranged in this order,
the top of the melting furnace (10) is provided with a charging hole (11), the periphery and the bottom are provided with a plurality of heating elements (12), and the bottom of the melting furnace (10) is also provided with a discharging hole (13) and an air supply system (14);
the condenser (20) comprises a cooling channel (21), a plurality of condenser baffles (22) are respectively arranged on the upper inner wall and the lower inner wall of the cooling channel (21) at intervals, a cooling water inlet (23), a cooling water channel (24) and a cooling water outlet (25) are arranged on the outer side of the top of the cooling channel (21), and a plurality of collectors (26) are continuously and detachably arranged at the bottom of the cooling channel (21).
8. The method according to claim 7, wherein a spacing between two adjacent condenser baffles (22) is 20-80 cm.
9. Method according to claim 7, characterized in that the bottom of the cooling channel (21) is continuously detachably provided with 3-8 collectors (26).
10. The method according to claim 7, characterized in that it comprises the steps of:
s1, adding vanadium pentoxide into the melting furnace (10) from the feed inlet (11), closing the feed inlet (11), heating the melting furnace (10), and melting the vanadium pentoxide at 800-1500 ℃ to form a liquid molten pool;
s2, continuously heating the melting furnace (10) to maintain the temperature of a liquid molten pool, and converting liquid vanadium pentoxide into vanadium pentoxide vapor;
s3, starting the gas supply system (14), introducing the gas into the liquid molten pool from the bottom of the liquid molten pool at the pressure of 0.15-0.2 mpa, volatilizing vanadium pentoxide vapor from the liquid molten pool, cooling in the cooling channel (21) to 120-450 ℃, and obtaining vanadium pentoxide with the purity not lower than 99.9% in the collector (26).
11. The method according to claim 10, wherein the method further comprises:
s4, when the liquid molten pool level is reduced to 0.05-0.10 times of the initial value of the liquid molten pool level in the step S2, closing the air supply system (14), stopping heating, opening the discharge port (13), and emptying the residual materials in the liquid molten pool;
s5, closing the discharge hole (13), and repeating the steps S1-S4 to perform continuous production.
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| CN111994952A (en) * | 2020-10-10 | 2020-11-27 | 攀钢集团研究院有限公司 | Method for preparing high-purity vanadium pentoxide by vacuum sublimation of metallurgical-grade vanadium pentoxide |
| KR102248361B1 (en) * | 2020-11-17 | 2021-05-06 | 한국지질자원연구원 | Pyrometallurgical purification method of vanadium pentoxide and vanadium pentoxide prepared from the same |
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| CN111994952A (en) * | 2020-10-10 | 2020-11-27 | 攀钢集团研究院有限公司 | Method for preparing high-purity vanadium pentoxide by vacuum sublimation of metallurgical-grade vanadium pentoxide |
| KR102248361B1 (en) * | 2020-11-17 | 2021-05-06 | 한국지질자원연구원 | Pyrometallurgical purification method of vanadium pentoxide and vanadium pentoxide prepared from the same |
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