CN114180625B - Method for purifying vanadium pentoxide by negative pressure volatilization - Google Patents
Method for purifying vanadium pentoxide by negative pressure volatilization Download PDFInfo
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- CN114180625B CN114180625B CN202111347657.1A CN202111347657A CN114180625B CN 114180625 B CN114180625 B CN 114180625B CN 202111347657 A CN202111347657 A CN 202111347657A CN 114180625 B CN114180625 B CN 114180625B
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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 272
- 238000000034 method Methods 0.000 title claims abstract description 69
- 238000002844 melting Methods 0.000 claims abstract description 64
- 230000008018 melting Effects 0.000 claims abstract description 64
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 238000001816 cooling Methods 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 238000000746 purification Methods 0.000 claims abstract description 8
- 239000000498 cooling water Substances 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 12
- 238000010924 continuous production Methods 0.000 claims description 10
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 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 5
- 229920006395 saturated elastomer Polymers 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000011734 sodium Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000013043 chemical agent Substances 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
- 238000002360 preparation method Methods 0.000 description 3
- 239000000126 substance Substances 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
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000009615 deamination Effects 0.000 description 2
- 238000006481 deamination reaction Methods 0.000 description 2
- 238000000354 decomposition 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
- 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
- 239000002351 wastewater 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 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
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect 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
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 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
- 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 negative pressure 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, and converting the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) And (3) guiding the vanadium pentoxide vapor out of the liquid molten pool under the pressure of 10-50 kPa, and cooling the vanadium pentoxide vapor to 120-450 ℃ to obtain the vanadium pentoxide with the purity of more than 99.9%. The method for preparing the high-purity vanadium pentoxide by adopting negative pressure volatilization separation and purification is provided by utilizing the difference of the melting point and saturated vapor pressure of the vanadium pentoxide and the impurity oxide, and the high-purity vanadium pentoxide can be obtained by only one-step heating volatilization separation, so that the method has the advantages of simple process and low production cost, and has wide popularization and application prospects in vanadium oxide production enterprises at home and abroad.
Description
Technical Field
The invention relates to the technical field of vanadium metallurgy, in particular to a method for purifying vanadium pentoxide by negative pressure 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, incomplete impurity removal and the like in the prior art for preparing high-purity vanadium pentoxide, and provides a method for purifying vanadium pentoxide by negative pressure volatilization. The method utilizes the difference of the melting point and saturated vapor pressure of the vanadium pentoxide and the impurity oxide, and provides a method for preparing high-purity vanadium pentoxide by adopting negative pressure volatilization separation and purification.
In order to achieve the above object, the present invention provides a method for purifying vanadium pentoxide by negative pressure 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, and converting the liquid vanadium pentoxide into vanadium pentoxide vapor;
(3) And (3) guiding the vanadium pentoxide vapor out of the liquid molten pool under the pressure of 10-50 kPa, and cooling the vanadium pentoxide vapor to 120-450 ℃ to obtain the vanadium pentoxide with the purity of more than 99.9%.
Preferably, the method further comprises:
(4) When the liquid molten pool level is reduced to 0.05-0.1 time 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 900 to 1400 ℃.
Preferably, in step (3), vanadium pentoxide vapour is led from the liquid bath at a pressure of 20 to 50 kPa.
Preferably, in step (3), the vanadium pentoxide vapour is cooled by circulating cooling water.
Preferably, the method is carried out in a purification apparatus comprising a melting furnace, a condenser and a vacuum system arranged in this order,
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 outlet;
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 of the 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 vacuum system to control the pressure in the melting furnace to be 10-50 kPa, guiding the vanadium pentoxide vapor into the cooling channel from the melting furnace, cooling the vanadium pentoxide vapor to 120-450 ℃, and obtaining vanadium pentoxide with purity of more than 99.9% in the collector.
Preferably, the method further comprises:
s4, when the liquid molten pool level is reduced to 0.05-0.1 time of the initial value of the liquid molten pool level in the step S1, closing a vacuum system, stopping heating, opening the discharge port, and emptying the residual materials in the liquid molten pool in the melting furnace;
s5, repeating the steps S1 to S4, and carrying out continuous production.
The method of the invention ensures V according to the difference of the melting point and the saturated vapor pressure of the vanadium pentoxide and the impurity oxide 2 O 5 Under the condition of no decomposition reaction, the vanadium pentoxide is melted to form a liquid molten pool, the saturated vapor pressure of the vanadium pentoxide is rapidly increased and is violently volatilized after the temperature is higher than the melting point, and impurity elements are difficult to volatilize, so that the high-efficiency separation of vanadium impurities is realized, and the high-purity vanadium pentoxide is obtained through condensation and collection of the vanadium pentoxide.
Drawings
FIG. 1 is a schematic diagram of a 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;
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 vacuum 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 invention provides a method for purifying vanadium pentoxide by negative pressure volatilization, which 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, and converting the liquid vanadium pentoxide into vanadium pentoxide vapor;
(3) And (3) guiding the vanadium pentoxide vapor out of the liquid molten pool under the pressure of 10-50 kPa, and cooling the vanadium pentoxide vapor to 120-450 ℃ to obtain the vanadium pentoxide with the purity of more than 99.9%.
In the method of the invention, after the vanadium pentoxide is melted and volatilized at 800-1500 ℃, the vanadium pentoxide vapor is led out and cooled under the condition of 10-50 kPa, so that the phenomenon that the oxygen partial pressure is too low to lead V can be avoided 2 O 5 Producing O by decomposition 2 And low-valence vanadium oxide (VO 2 、V 2 O 3 Etc.), resulting in failure to obtain V 2 O 5 。
In a specific embodiment, the method further comprises: (4) When the liquid molten pool level is reduced to 0.05-0.1 times of the initial value of the liquid molten pool level in the step (1), emptying the residual materials in the liquid molten pool; and (5) repeating the steps (1) - (4) to realize continuous production.
The method of the invention can be applied to 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 impurity comprises 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 a specific embodiment, in step (1), the vanadium pentoxide may be melted at 800 ℃, 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃ or 1500 ℃.
In a preferred embodiment, in step (1), vanadium pentoxide is melted at 900 to 1400 ℃.
In the method of the invention, in order to ensure that the vanadium pentoxide vapor can volatilize under a negative pressure and violently, and simultaneously ensure that the vanadium pentoxide is not decomposed and impurity elements are not volatilized, the vanadium pentoxide vapor is led out in a proper pressure range so as to realize V 2 O 5 And separating impurities.
In particular embodiments, in step (3), vanadium pentoxide vapour may be withdrawn from the liquid bath at a pressure of 20kPa, 25kPa, 30kPa, 35kPa, 40kPa, 45kPa or 50 kPa.
In a preferred embodiment, in step (3), vanadium pentoxide vapour is led from the liquid bath at a pressure of 20 to 50 kPa.
In the process according to the invention, the vanadium pentoxide vapour is only required after its removal from the liquid bathCooling it to convert it into solid V 2 O 5 The high-purity vanadium pentoxide can be obtained by collecting.
In a specific embodiment, in the step (3), the vanadium pentoxide vapor can be cooled down 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 may be carried out in a purification apparatus as shown in fig. 1, which includes a melting furnace 10, a condenser 20 and a vacuum 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;
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 specific implementation process, the vanadium pentoxide is melted in the melting furnace 10 and forms vapor, then the vacuum system 30 provides negative pressure to guide the vanadium pentoxide vapor out of the melting furnace 10 into the cooling channel 21, impurities are remained in the melting furnace 10, and then the circulating cooling water in the cooling water channel 24 cools the vanadium pentoxide vapor to reduce the temperature, thus obtaining solid high-purity V 2 O 5 Falls into a collector, thereby realizing the purpose of purifying the vanadium pentoxide. 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.
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 carrying out the method according to the invention using the purification device according to the invention, 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 vacuum system 30 to control the pressure in the melting furnace 10 to be 10-50 kPa, guiding the vanadium pentoxide vapor from the melting furnace 10 into the cooling channel 21, cooling the vanadium pentoxide vapor to 120-450 ℃, and obtaining vanadium pentoxide with purity of more than 99.9% in the collector 26.
In the method, the vanadium pentoxide material is added into the melting furnace 10 through the charging port 11, then the melting furnace 10 is heated to 800-1500 ℃ through the heating element 12, so that the vanadium pentoxide is melted at 800-1500 ℃, then the vacuum system 30 provides negative pressure to control the pressure in the melting furnace 10 to 10-50 kPa, and the vanadium pentoxide vapor is removed from the melting furnace through the negative pressureThe melting furnace 10 is led out into a cooling channel 21, impurities are remained in the melting furnace 10, and then the circulating cooling water in a cooling water channel 24 cools the vanadium pentoxide vapor to reduce the temperature, thereby obtaining solid high-purity V 2 O 5 Falls into a collector.
In order to achieve continuous production with the process, in a preferred embodiment, the process further comprises:
s4, when the liquid molten pool level is reduced to 0.05-0.1 time of the initial value of the liquid molten pool level in the step S1, closing a vacuum system, stopping heating, opening the discharge hole 13, and emptying the residual materials in the liquid molten pool in the melting furnace 10; s5, repeating the steps S1 to S4, and carrying out continuous production.
The method has the advantages of no consumption of chemical agents, no pollution, low cost, simple process and the like, creatively utilizes the difference of the melting point and the saturated vapor pressure of the vanadium pentoxide and the impurity oxide, and obtains the high-purity vanadium pentoxide only through one-step heating, volatilizing and separating.
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 were all carried out using the following purification apparatus.
The purifying device comprises a melting furnace 10, a condenser 20 and a vacuum system 30 which are sequentially arranged, wherein a charging hole 11 is formed in the top of the melting furnace 10, a plurality of heating elements 12 are arranged on the periphery and the bottom of the melting furnace 10, and a discharging hole 13 is further formed in 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) Vanadium pentoxide (purity 98.2%, fe content 0.24% by mass, cr content 0.16% by mass, si content 0.35% by mass, na content 0.82% by mass) was fed into the melting furnace 10 from the feed port 11, the feed port 11 was closed, and the melting furnace 10 was heated to 900 ℃ to completely melt the vanadium pentoxide to form a liquid molten pool; (2) Continuously heating to maintain the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Starting a vacuum system 30 to control the pressure in the melting furnace 10 to be 24kPa, introducing vanadium pentoxide vapor into a cooling channel 21, and cooling to 360 ℃ by adopting circulating cooling water to obtain high-purity vanadium pentoxide; (4) When the liquid level of the molten pool is reduced to 0.08 times of the initial value, the vacuum system 30 is closed, heating is stopped, the discharge hole 13 is opened, and the materials in the melting furnace 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 is 99.94%, the content of Fe is 0.002% by mass, the content of Cr is 0.003% by mass, the content of Si is 0.008% by mass and the content of Na is 0.011% by mass.
Example 2
(1) Vanadium pentoxide (purity 99.3%, fe content 0.18%, mn content 0.22%, si content 0.09%, P content 0.13% by mass) was fed into the melting furnace 10 from the feed port 11, the feed port 11 was closed, and the melting furnace 10 was heated to 1400 ℃ to completely melt the vanadium pentoxide to form a liquid molten pool; (2) Continuously heating to maintain the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Starting a vacuum system 30 to control the pressure in the melting furnace 10 to be 46kPa, introducing vanadium pentoxide vapor into a cooling channel 21, and cooling to 270 ℃ by adopting circulating cooling water to obtain high-purity vanadium pentoxide; (4) When the liquid level of the molten pool is reduced to 0.07 times of the initial value, the vacuum system 30 is closed, heating is stopped, the discharge hole 13 is opened, and the materials in the melting furnace 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 is 99.98%, the content of Fe is 0.001% by mass, the content of Mn is 0.003% by mass, the content of Si is 0.005% by mass and the content of P is 0.004% by mass.
Example 3
(1) Vanadium pentoxide (purity: 97.8%, fe content: 0.37 mass%, cr content: 0.22 mass%, si content: 0.20 mass%, na content: 1.01 mass%, K content: 0.15 mass%, P content: 0.09 mass%) was fed into the melting furnace 10 from the feed port 11, the feed port 11 was closed, and the melting furnace 10 was heated to 1200 ℃ to completely melt the vanadium pentoxide to form a liquid molten pool; (2) Continuously heating to maintain the temperature of the liquid molten pool to convert the liquid vanadium pentoxide into vanadium pentoxide vapor; (3) Starting a vacuum system 30 to control the pressure in the melting furnace 10 to be 35kPa, introducing vanadium pentoxide vapor into a cooling channel 21, and cooling to 300 ℃ by adopting circulating cooling water to obtain high-purity vanadium pentoxide; (4) When the liquid level of the molten pool is reduced to 0.09 times of the initial value, the vacuum system 30 is closed, heating is stopped, the discharge hole 13 is opened, and the materials in the melting furnace 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 is 99.91%, the content of Fe is 0.002% by mass, the content of Cr is 0.004% by mass, the content of Si is 0.02% by mass, the content of Na is 0.04% by mass, the content of K is 0.002% by mass and the content of P is 0.001% by 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 high-purity vanadium pentoxide is 99.38%, the content of Fe is 0.13%, the content of Cr is 0.10%, the content of Si is 0.04%, the content of Na is 0.22%, the content of K is 0.07% and the content of P is 0.03% by mass.
Comparative example 2
The process of example 3 was carried out, except that in step (3), the vacuum system 30 was turned on to control the pressure in the melting furnace 10 to 8kPa.
The purity of the high-purity vanadium pentoxide is 99.20%, the content of Fe, cr, si, na, K and P is 0.17, 0.11, 0.05, 0.34, 0.08 and 0.03 respectively.
Comparative example 3
The process of example 3 was carried out, except that in step (3), the vacuum system 30 was turned on to control the pressure in the melting furnace 10 to 55kPa.
The purity of the high-purity vanadium pentoxide is 99.41%, the content of Fe is 0.009% by mass, the content of Cr is 0.07% by mass, the content of Si is 0.08% by mass, the content of Na is 0.31% by mass, the content of K is 0.06% by mass and the content of P is 0.04% 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 (12)
1. A method for purifying vanadium pentoxide by negative pressure volatilization, which is characterized by comprising 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, and converting the liquid vanadium pentoxide into vanadium pentoxide vapor;
(3) And (3) guiding the vanadium pentoxide vapor out of the liquid molten pool under the pressure of 10-50 kPa, and cooling the vanadium pentoxide vapor to 120-450 ℃ to obtain the vanadium pentoxide with the purity of more than 99.9%.
2. The method according to claim 1, characterized in that the method further comprises:
(4) When the liquid molten pool level is reduced to 0.05-0.1 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.
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 according to claim 1, wherein in step (1), vanadium pentoxide is melted at 900 to 1400 ℃.
6. The method according to claim 1, characterized in that in step (3) vanadium pentoxide vapour is led out of the liquid bath at a pressure of 20-50 kPa.
7. The method according to claim 1, wherein in step (3), the vanadium pentoxide vapor is cooled down by circulating cooling water.
8. The method according to any one of claims 1 to 7, characterized in that the method is carried out in a purification device comprising a melting furnace (10), a condenser (20) and a vacuum 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);
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).
9. A method according to claim 8, characterized in that the spacing between two of the condenser baffles (22) is 20-80 cm.
10. Method according to claim 8, characterized in that the bottom of the cooling channel (21) is continuously detachably provided with 3-8 collectors (26).
11. The method according to claim 8, characterized in that the method comprises the steps of:
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 vacuum system (30) to control the pressure in the melting furnace (10) to be 10-50 kPa, guiding vanadium pentoxide vapor from the melting furnace (10) into the cooling channel (21), cooling the vanadium pentoxide vapor to 120-450 ℃, and obtaining vanadium pentoxide with purity of more than 99.9% in the collector (26).
12. The method of claim 11, wherein the method further comprises:
s4, when the liquid molten pool level is reduced to 0.05-0.1 time of the initial value of the liquid molten pool level in the step S1, closing a vacuum system (30), stopping heating, opening a discharge hole (13), and emptying residual materials in the liquid molten pool in the melting furnace (10);
s5, repeating the steps S1 to S4, and carrying out continuous production.
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| CN101289226A (en) * | 2008-03-07 | 2008-10-22 | 昆明理工大学 | Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101289226A (en) * | 2008-03-07 | 2008-10-22 | 昆明理工大学 | Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate |
| 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 |
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