CN113336267A - Method for preparing vanadium trioxide by utilizing catalytic reduction of metal coating - Google Patents
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- CN113336267A CN113336267A CN202110511143.9A CN202110511143A CN113336267A CN 113336267 A CN113336267 A CN 113336267A CN 202110511143 A CN202110511143 A CN 202110511143A CN 113336267 A CN113336267 A CN 113336267A
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- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/464—Rhodium
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- B01J23/468—Iridium
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- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating. The technical scheme is as follows: dissolving pentavalent vanadium into a vanadium-rich solution with the vanadium concentration of 0.1-1 mol/L by using a sodium hydroxide solution, and adjusting the pH value to 4-6 by using a sulfuric acid solution; and then placing the vanadium-rich liquid in an autoclave, and stirring for 2-4 h at 200-300 ℃ under the hydrogen partial pressure of 1-3 MPa. The inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is one of palladium, platinum, rhodium and iridium. And cooling the stirred autoclave to below 50 ℃, releasing pressure, taking out slurry, carrying out suction filtration and drying to obtain vanadium trioxide. And returning the sodium hydroxide solution after suction filtration to the first step for recycling. The method has the characteristics of low energy consumption, low production cost, short production period, high reaction efficiency and high-efficiency recycling of the metal catalyst, and the purity of the product can be effectively ensured by adopting a catalytic reduction mode of the metal coating.
Description
Technical Field
The invention belongs to the technical field of preparation of vanadium trioxide. In particular to a method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating.
Background
Vanadium trioxide is a gray black vanadium oxide with high melting point and strong reducibility, and can be used for preparing sheet vanadium or powder vanadium, ferrovanadium, vanadium nitride, vanadium carbide and the like. In addition, vanadium trioxide can have phase transition due to temperature, and resistivity, magnetic susceptibility, light projection rate and reflectivity all change suddenly during phase transition, so that the vanadium trioxide has important application in aspects of thermoelectric switches, magnetic switches, optical switches, sensors, thin film materials and the like.
At present, the preparation method of vanadium trioxide is roughly divided into reduction roasting and liquid phase synthesis:
(1) reduction roasting: the vanadium trioxide reduction roasting preparation process usually adopts high valence vanadium products such as ammonium metavanadate, vanadate, vanadium pentoxide and the like as raw materials, and carbon monoxide, ammonia gas, coal gas, hydrogen or methane and other reducing gases are introduced for reduction roasting:
the patent technology of 'a method for continuously synthesizing vanadium trioxide' (CN102092787B) adopts poly-vanadate or vanadium pentoxide as raw materials, enters a multi-chamber boiling reactor after being preheated, is introduced with reducing gas, and generates the vanadium trioxide under the conditions that the reaction temperature is 600-750 ℃ and the reaction time in each chamber is 10-30 min.
A process for preparing vanadium trioxide by reduction roasting (CN101717117B) comprises mixing ammonium vanadate or vanadium pentoxide with binder and carbon powder to obtain pellets, introducing excessive reducing gas, reduction roasting at 500-650 deg.C, and cooling in inert atmosphere to obtain vanadium trioxide.
The patent of 'a production method of vanadium trioxide' (CN102583537B) is characterized in that an ammonia decomposition furnace is used for decomposing liquid ammonia into nitrogen and ammonia at 800-900 ℃, mixed gas is introduced into a push plate reduction furnace, vanadium pentoxide is added at the same time, the temperature in the furnace is kept at 620-680 ℃ for 20-40 min, and finally the vanadium trioxide is cooled in the furnace for 20-40 min to obtain the vanadium trioxide.
Most of reducing gases introduced in the existing reduction roasting have flammable and explosive potential safety hazards, and the high-temperature condition during roasting not only increases the production energy consumption, but also improves the danger coefficient of blasting. Therefore, if the vanadium trioxide can be synthesized by a liquid phase, the method has stronger practical significance.
(2) Liquid phase synthesis: the liquid phase synthesis of vanadium trioxide generally takes high-concentration vanadium-rich liquid as a raw material, and a reducing agent or gas is added under the condition of less than 400 ℃ to carry out liquid phase pressurization vanadium precipitation.
The patent technology of 'a method for preparing vanadium trioxide microsphere powder by tartaric acid induction' (CN103011290B) is characterized in that vanadium pentoxide and tartaric acid are uniformly mixed in water or alcohol according to a certain proportion, the reaction is carried out for 20-26 h at the temperature of 170-190 ℃, and the obtained solid is calcined for 3-4 h under the protection of inert gas and at the temperature of 500-600 ℃. Although the method has the known advantages, the method still needs anaerobic calcination at high temperature, the reduction degree of energy consumption is extremely limited, the reaction time is too long, and the efficiency is low.
The patent technology of 'a preparation method of vanadium trioxide powder' (CN105621485B) adopts a vanadium source, thioglycollic acid and water as raw materials, and carries out hydrothermal reaction for 16-32 hours under the conditions that the molar ratio of the vanadium source to the thioglycollic acid is 0.5-2: 1, the filling rate of a hydrothermal kettle is 0.6-0.85 and the temperature is 240-280 ℃, so that pure-phase vanadium trioxide powder with a better crystal form is prepared, but the adopted reducing agent thioglycollic acid is expensive, difficult to popularize industrially and low in efficiency.
Zhang Guobin et al (GuobinZhang, YiminZhang, ShenxuBao, JingHuang, Liuhong Zhang. anoveleco-friendly vanadium pretreatment hydrohydrogen reduction Technology [ J ]. Minerals,2017,7(10).) adopt a pressurized hydrogen reduction method to prepare vanadium trioxide, palladium chloride is used as an active hydrogen catalyst to enhance the reducibility of hydrogen, and the vanadium trioxide product with high vanadium deposition rate and purity is obtained by reacting in an autoclave for 2 hours under the conditions of the temperature of 250 ℃ and the partial pressure of the hydrogen of 4 MPa. Although the method has high efficiency and low energy consumption, the adopted palladium chloride can not be effectively recovered, and the problem of high production cost exists.
In conclusion, the method for synthesizing vanadium trioxide in a liquid phase has the problems of high production cost, high energy consumption, overlong reaction time and low efficiency, and the industrial application is seriously limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating, which has the advantages of low energy consumption, short production period, low cost, high reaction efficiency, high-efficiency cyclic utilization of a metal catalyst and high purity of the vanadium trioxide prepared by the method.
In order to achieve the above object, the invention adopts the technical scheme that:
completely dissolving pentavalent vanadium by using a sodium hydroxide solution to obtain a vanadium-rich solution with the vanadium concentration of 0.1-1 mol/L; and then regulating the pH value of the vanadium-rich liquid to 4-6 by using a sulfuric acid solution.
Secondly, according to the ratio of the volume of the liquid to the volume of the high-pressure kettle of 0.4-0.6: 1, putting the vanadium-rich liquid with the adjusted pH value into the high-pressure kettle; and introducing nitrogen into the autoclave to discharge air in the autoclave, and stirring for 2-4 hours at 200-300 ℃ under the condition of 1-3 MPa of hydrogen partial pressure.
The inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is one of palladium, platinum, rhodium and iridium.
Step three, cooling the stirred high-pressure kettle to below 50 ℃, releasing pressure, and taking out slurry in the high-pressure kettle; and carrying out suction filtration and drying on the slurry to obtain vanadium trioxide.
And returning the sodium hydroxide solution obtained by suction filtration to the first step for recycling.
The pentavalent vanadium is one of vanadium pentoxide powder, sodium orthovanadate powder, sodium metavanadate powder and sodium pyrovanadate powder; the purity of the pentavalent vanadium is more than 99%.
The rotating speed of the stirring is 300-800 r/min.
The drying is vacuum drying, the relative vacuum degree of the vacuum drying is-0.1 MPa, and the drying temperature of the vacuum drying is lower than 100 ℃.
Compared with the prior art, the invention has the following positive effects due to the adoption of the technical scheme:
(1) compared with the existing reduction roasting method, the method has the advantages that the adopted reaction temperature is 200-300 ℃, the reaction energy consumption is obviously reduced, the danger coefficient of explosion of the reducing gas in the reaction is also obviously reduced, the energy consumption is low, and the safety is high.
(2) Compared with the existing liquid phase synthesis method, the method of the invention adopts the metal coating mode, which not only can realize the cyclic and efficient utilization of the metal catalyst and reduce the production cost (about 1300 yuan can be saved for each ton of raw materials), but also can avoid the metal catalyst from entering the product, and effectively ensures the product purity.
(3) The existing catalyst adding mode is that catalyst powder is directly added into a solution, and a catalyst and a liquid phase are in a disturbed state during stirring, so that the method is a static catalysis process; the metal catalyst of the invention exists in the form of a metal coating, and hydrogen dissolved in a liquid phase can fully contact the metal coating, so that the invention is a dynamic catalysis process, can realize high-efficiency cyclic utilization of the metal catalyst and has high efficiency. Meanwhile, a catalytic reduction mode of the metal coating is adopted, so that the metal coating has a larger contact area, the probability of activating hydrogen is higher, and the high-purity and high-precipitation-rate vanadium trioxide can be obtained when the partial pressure of the hydrogen is below 3 MPa. The purity of the vanadium trioxide prepared by the method is more than 99%: the precipitation rate of vanadium trioxide is more than 99 percent.
(4) According to the invention, the pH value of the vanadium-rich liquid obtained after pentavalent vanadium is dissolved is adjusted, the vanadium-rich liquid is placed in an autoclave, stirred for 2-4 h under the conditions of 200-300 ℃ and 1-3 MPa of hydrogen partial pressure, and vanadium trioxide is obtained through cooling, pressure release, suction filtration and drying, so that the process is simple and the production period is short.
Therefore, the method has the characteristics of low energy consumption, low production cost, short production period, high reaction efficiency and high-efficiency recycling of the metal catalyst, and the purity of the product can be effectively ensured by adopting a catalytic reduction mode of the metal coating.
Drawings
FIG. 1 is an XRD pattern of vanadium trioxide prepared by catalytic reduction of a metal coating according to the present invention;
FIG. 2 is an SEM-EDS diagram of the vanadium trioxide shown in FIG. 1.
Detailed Description
The invention is further described with reference to the following drawings and detailed description, without limiting its scope:
in this embodiment:
the purity of the pentavalent vanadium is more than 99%.
The drying is vacuum drying, the relative vacuum degree of the vacuum drying is-0.1 MPa, and the drying temperature of the vacuum drying is lower than 100 ℃.
And returning the sodium hydroxide solution obtained by suction filtration to the first step for recycling.
The detailed description is omitted in the embodiments.
Example 1
A method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating. The method comprises the following specific steps:
completely dissolving pentavalent vanadium by using a sodium hydroxide solution to obtain a vanadium-rich solution with the vanadium concentration of 0.5-0.7 mol/L; and then regulating the pH value of the vanadium-rich liquid to 5-6 by using a sulfuric acid solution.
Secondly, according to the ratio of the volume of the liquid to the volume of the high-pressure kettle of 0.4-0.5: 1, putting the vanadium-rich liquid with the adjusted pH value into the high-pressure kettle; and introducing nitrogen into the autoclave to discharge air in the autoclave, and stirring for 2-3 hours at 250-280 ℃ under the condition of hydrogen partial pressure of 2-3 MPa.
The inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is palladium.
Step three, cooling the stirred high-pressure kettle to below 50 ℃, releasing pressure, and taking out slurry in the high-pressure kettle; and carrying out suction filtration and drying on the slurry to obtain vanadium trioxide.
The pentavalent vanadium is vanadium pentoxide powder.
The rotating speed of the stirring is 300-400 r/min.
Example 2
A method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating. The method comprises the following specific steps:
completely dissolving pentavalent vanadium by using a sodium hydroxide solution to obtain a vanadium-rich solution with the vanadium concentration of 0.7-1 mol/L; and then regulating the pH value of the vanadium-rich liquid to 4-5 by using a sulfuric acid solution.
Secondly, according to the ratio of the volume of the liquid to the volume of the high-pressure kettle of 0.5-0.6: 1, putting the vanadium-rich liquid with the adjusted pH value into the high-pressure kettle; and introducing nitrogen into the autoclave to discharge air in the autoclave, and stirring for 3-4 hours at 280-300 ℃ under the condition of 2-3 MPa of hydrogen partial pressure.
The inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is platinum.
Step three, cooling the stirred high-pressure kettle to below 50 ℃, releasing pressure, and taking out slurry in the high-pressure kettle; and carrying out suction filtration and drying on the slurry to obtain vanadium trioxide.
The pentavalent vanadium is sodium metavanadate powder.
The rotating speed of the stirring is 300-600 r/min.
Example 3
A method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating comprises the following specific steps:
completely dissolving pentavalent vanadium by using a sodium hydroxide solution to obtain a vanadium-rich solution with the vanadium concentration of 0.1-0.3 mol/L; and then regulating the pH value of the vanadium-rich liquid to 5-6 by using a sulfuric acid solution.
Secondly, according to the ratio of the volume of the liquid to the volume of the high-pressure kettle of 0.5-0.6: 1, putting the vanadium-rich liquid with the adjusted pH value into the high-pressure kettle; and introducing nitrogen into the autoclave to discharge air in the autoclave, and stirring for 2-3 hours at 200-230 ℃ and under the condition of 1-2 MPa of hydrogen partial pressure.
The inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is rhodium.
Step three, cooling the stirred high-pressure kettle to below 50 ℃, releasing pressure, and taking out slurry in the high-pressure kettle; and carrying out suction filtration and drying on the slurry to obtain vanadium trioxide.
The pentavalent vanadium is sodium orthovanadate powder.
The rotating speed of the stirring is 300-800 r/min.
Example 4
A method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating comprises the following specific steps:
completely dissolving pentavalent vanadium by using a sodium hydroxide solution to obtain a vanadium-rich solution with the vanadium concentration of 0.3-0.5 mol/L; and then regulating the pH value of the vanadium-rich liquid to 4-5 by using a sulfuric acid solution.
Secondly, according to the ratio of the volume of the liquid to the volume of the high-pressure kettle of 0.4-0.5: 1, putting the vanadium-rich liquid with the adjusted pH value into the high-pressure kettle; and introducing nitrogen into the autoclave to discharge air in the autoclave, and stirring for 3-4 hours at 230-250 ℃ and under the condition of 1-2 MPa of hydrogen partial pressure.
The inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is iridium.
Step three, cooling the stirred high-pressure kettle to below 50 ℃, releasing pressure, and taking out slurry in the high-pressure kettle; and carrying out suction filtration and drying on the slurry to obtain vanadium trioxide.
The pentavalent vanadium is sodium pyrovanadate powder.
The rotating speed of the stirring is 600-800 r/min.
Compared with the prior art, the embodiment of the invention has the following positive effects
(1) Compared with the existing reduction roasting method, the reduction roasting method has the advantages that the adopted reaction temperature is 200-300 ℃, the reaction energy consumption is obviously reduced, the danger coefficient of explosion of the reducing gas in the reaction is also obviously reduced, the energy consumption is low, and the safety is high.
(2) Compared with the existing liquid phase synthesis method, the method for preparing the metal catalyst by the metal coating can realize the cyclic and efficient utilization of the metal catalyst, reduce the production cost (about 1300 yuan can be saved for each ton of raw materials), prevent the metal catalyst from entering the product and effectively ensure the product purity.
(3) The existing catalyst adding mode is that catalyst powder is directly added into a solution, and a catalyst and a liquid phase are in a disturbed state during stirring, so that the method is a static catalysis process; the metal catalyst of the embodiment exists in the form of a metal coating, and hydrogen dissolved in a liquid phase can fully contact the metal coating, so that the process is a dynamic catalysis process, the high-efficiency cyclic utilization of the metal catalyst can be realized, and the efficiency is high. Meanwhile, a catalytic reduction mode of the metal coating is adopted, so that the metal coating has a larger contact area, the probability of activating hydrogen is higher, and the high-purity and high-precipitation-rate vanadium trioxide can be obtained when the partial pressure of the hydrogen is below 3 MPa. The purity of the prepared vanadium trioxide is more than 99%: the precipitation rate of vanadium trioxide is more than 99 percent.
The vanadium trioxide prepared by the specific embodiment is shown in the attached drawing: FIG. 1 is an XRD pattern of vanadium trioxide prepared by catalytic reduction of a metal coating in example 1; FIG. 2 is an SEM-EDS diagram of the vanadium trioxide shown in FIG. 1. As can be seen from FIG. 1, the prepared vanadium trioxide is vanadium trioxide crystal without any impurity; as can be seen from fig. 2, the vanadium trioxide crystals produced exhibited better rhombohedral shapes, in which the proportion of V, O element was close to the atomic ratio of vanadium trioxide.
(4) According to the specific embodiment, the pH value of the vanadium-rich liquid obtained after pentavalent vanadium is dissolved is adjusted, the vanadium-rich liquid is placed in an autoclave, the stirring is carried out for 2-4 hours under the conditions of 200-300 ℃ and 1-3 MPa of hydrogen partial pressure, and vanadium trioxide is obtained through cooling, pressure release, suction filtration and drying.
Therefore, the specific implementation mode has the characteristics of low energy consumption, low production cost, short production period, high reaction efficiency and high-efficiency recycling of the metal catalyst, and the product purity can be effectively ensured by adopting a catalytic reduction mode of the metal coating.
Claims (4)
1. A method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating is characterized in that the method for preparing the vanadium trioxide is as follows:
completely dissolving pentavalent vanadium by using a sodium hydroxide solution to obtain a vanadium-rich solution with the vanadium concentration of 0.1-1 mol/L; then regulating the pH value of the vanadium-rich liquid to 4-6 by using a sulfuric acid solution;
secondly, according to the ratio of the volume of the liquid to the volume of the high-pressure kettle of 0.4-0.6: 1, putting the vanadium-rich liquid with the adjusted pH value into the high-pressure kettle; introducing nitrogen into the autoclave to discharge air in the autoclave, and stirring for 2-4 hours at 200-300 ℃ and under the condition of 1-3 MPa of hydrogen partial pressure;
the inner wall of the high-pressure kettle and the surface of the stirring paddle are both metal coatings, and the metal of the metal coatings is one of palladium, platinum, rhodium and iridium;
step three, cooling the stirred high-pressure kettle to below 50 ℃, releasing pressure, and taking out slurry in the high-pressure kettle; carrying out suction filtration and drying on the slurry to obtain vanadium trioxide;
and returning the sodium hydroxide solution obtained by suction filtration to the first step for recycling.
2. The method for preparing vanadium trioxide by catalytic reduction of a metal coating according to claim 1, wherein the pentavalent vanadium is one of vanadium pentoxide powder, sodium orthovanadate powder, sodium metavanadate powder and sodium pyrovanadate powder; the purity of the pentavalent vanadium is more than 99%.
3. The method for preparing vanadium trioxide by utilizing catalytic reduction of a metal coating according to claim 1, wherein the stirring speed is 300-800 r/min.
4. The method for preparing vanadium trioxide by catalytic reduction of a metal coating according to claim 1, wherein the drying is vacuum drying, the relative vacuum degree of the vacuum drying is-0.1 MPa, and the drying temperature of the vacuum drying is lower than 100 ℃.
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| CN114132962A (en) * | 2021-12-13 | 2022-03-04 | 武汉科技大学 | Method for preparing vanadium trioxide by liquid-phase hydrogen reduction |
| CN117904673A (en) * | 2024-03-19 | 2024-04-19 | 四川大学 | Electrocatalyst and preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114132962A (en) * | 2021-12-13 | 2022-03-04 | 武汉科技大学 | Method for preparing vanadium trioxide by liquid-phase hydrogen reduction |
| CN117904673A (en) * | 2024-03-19 | 2024-04-19 | 四川大学 | Electrocatalyst and preparation and application thereof |
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