CN113582229B - Ammonium metavanadate one-step pyrolysis and carbon permeation reduction process - Google Patents
Ammonium metavanadate one-step pyrolysis and carbon permeation reduction process Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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Abstract
A one-step pyrolysis and carbon permeation reduction process for ammonium metavanadate comprises the following steps: (1) Mixing ammonium metavanadate, sodium carbonate and polyvinylpyrrolidone, and performing ball milling for activation to obtain activated ammonium metavanadate; (2) And (2) uniformly mixing the activated ammonium metavanadate obtained in the step (1) with graphene, vacuumizing, and then heating for reaction to obtain vanadium trioxide. According to the method, the particle size of the raw material ammonium metavanadate is controlled through ball milling, the raw material ammonium metavanadate is activated, and a small amount of sodium carbonate and polyvinylpyrrolidone are added to pretreat the ammonium metavanadate, so that the subsequent permeation reduction of graphene is facilitated. The method adds the graphene, reacts under a vacuum condition, is beneficial to the permeation of carbon atoms in the graphene, can reduce the reaction temperature, enables the permeation and reduction reaction to be carried out in one step, is simple and convenient to operate, and is beneficial to industrial production.
Description
Technical Field
The invention belongs to the technical field of chemical metallurgy, and particularly relates to a one-step pyrolysis and carbon permeation reduction process for ammonium metavanadate.
Background
Ammonium metavanadate with molecular formula of NH 4 VO 3 White or slightly yellowish crystalline powder, relative density 2.326, molecular weight 116.98, slightly soluble in cold water, hot ethanol and diethyl ether, in hot water and dilute ammonium hydroxide. When burned in air, the vanadium pentoxide becomes vanadium pentoxide.
Ammonium metavanadate is an intermediate product for extracting vanadium, and is mainly used for preparing vanadium pentoxide (powder or flake), and further producing metal vanadium, ferrovanadium alloy or other vanadium-based alloys. It can also be used as chemical reagent, catalyst, drier, mordant, etc. The ceramic industry is widely used as a glaze.
The vanadium ore resources in China are more, and the total reserve is V 2 O 5 And the calculation result is 2596 ten thousand tons, which is third in the world. The vanadium ore is widely distributed, and the reserves of the Panzhihua region in Sichuan are most abundant and account for 49 percent of the total reserves in China; the second is the Hebei Chengde region, which accounts for 21%, and other vanadium ore reserves have larger scale in Hunan, hubei, henan, shaanxi, guizhou, gansu provinces and other provinces.
However, in the prior art, the preparation of vanadium trioxide by using ammonium metavanadate firstly pyrolyzes the ammonium metavanadate into vanadium pentoxide, and then the vanadium pentoxide is fired and reduced at 950-1050 ℃ to obtain the vanadium trioxide, the reaction is carried out in two steps, the reaction temperature is high, and the operation is inconvenient.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a one-step pyrolysis and carbon permeation reduction process for ammonium metavanadate, which has the advantages of low reaction temperature, one-step reaction and simple and convenient operation.
The invention adopts the technical scheme that the one-step pyrolysis and carbon permeation reduction process of ammonium metavanadate comprises the following steps of:
(1) Ammonium metavanadate pretreatment: mixing ammonium metavanadate, sodium carbonate and polyvinylpyrrolidone according to a mass ratio of 100:0.1-0.2:0.1-0.2, and performing ball milling for activation to obtain activated ammonium metavanadate;
further, in the step (1), the rotating speed of the ball mill is 20-30 r/min, and the ball milling is carried out for 10-30 hours. In the ball milling process, the ammonium metavanadate is activated, so that the graphene can permeate in the subsequent reaction and the reaction can be completed. If the rotating speed of the ball mill is too high, the centrifugal force of the ball is too large, and after a certain degree, the steel ball always rotates along with the ball mill, so that the activation effect cannot be achieved. If the rotating speed of the ball mill is too low, the subsequent graphene permeation is not facilitated. The ball milling time is too short, so that the activation cannot be fully performed, the ball milling time is too long, the effect is improved limitedly, and the production efficiency is reduced.
Research shows that a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on ammonium metavanadate, so that subsequent graphene permeation reduction is facilitated, the temperature of subsequent decomposition and permeation reduction can be reduced, and one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out.
In the ball milling process, the process of activation and the process of ball milling to reduce the particle size of the raw materials are both performed, so that the ball milling speed and time need to be controlled, the ammonium metavanadate is likely to have a smaller size due to too fast ball milling speed or too long ball milling time, and when the size of the ammonium metavanadate after ball milling is smaller, agglomeration is likely to occur in the subsequent reaction process, so that the powder components are not uniformly dispersed; when the ball milling speed is too slow or the time is too short, the size of the ammonium metavanadate may be too large, and when the size of the ammonium metavanadate after ball milling is too large, the permeation and reduction degree of the graphene can be affected, so that the reaction is insufficient, or the reaction temperature needs to be increased to meet the requirement of sufficient reaction.
(2) One-step decomposition and reduction: and (2) uniformly mixing the activated ammonium metavanadate obtained in the step (1) with graphene, vacuumizing, and heating to 700-800 ℃ for reaction for 2-5 hours to obtain vanadium trioxide.
Further, in the step (2), the molar ratio of ammonium metavanadate to carbon atoms of the graphene is 1:0.26-0.30, and mixing uniformly. If the amount of added graphene is too small, vanadium pentoxide which is a pyrolysis product of ammonium metavanadate cannot react completely, and if the amount of added graphene is too large, vanadium oxide with a lower valence state is generated, so that the purity of vanadium trioxide is influenced. Research shows that the molar ratio of ammonium metavanadate to carbon atoms of ammonium metavanadate and graphene is 1:0.26 to 0.30, which can ensure the complete reaction of the vanadium pentoxide and can not influence the purity of the vanadium trioxide. The invention selects graphene, and does not select common carbon powder, because the graphene has a special molecular structure and can play the roles of activation and reduction, and if the graphene is changed into the common carbon powder, the reaction can be realized only by increasing the heating temperature.
In the step (2), the vacuum degree is controlled to be 50-100Pa through vacuumizing, the graphene is favorably permeated and reduced under the vacuum condition, when the vacuum degree is poor, the permeation of the graphene is influenced, so that the reduction is insufficient, the purity of a final product is not high, and the quality is not good.
According to the invention, the graphene is added and reacts under a vacuum condition, so that the penetration of carbon atoms in the graphene is facilitated, the reaction temperature can be reduced, the penetration and reduction reaction can be carried out in one step, the operation is simple and convenient, and the industrial production is facilitated.
The purity of the vanadium trioxide obtained by the method is more than or equal to 99.90 percent.
According to the invention, the particle size of the raw material ammonium metavanadate is controlled through ball milling, the raw material ammonium metavanadate is activated, and a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on the ammonium metavanadate, so that the subsequent graphene permeation reduction is facilitated, the subsequent decomposition and permeation reduction temperature can be reduced, and the one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out. The method adds the graphene, reacts under a vacuum condition, is beneficial to the permeation of carbon atoms in the graphene, can reduce the reaction temperature, enables the permeation and reduction reaction to be carried out in one step, is simple and convenient to operate, and is beneficial to industrial production. The obtained vanadium trioxide has high purity.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The one-step pyrolysis and carbon permeation reduction process of ammonium metavanadate in the embodiment comprises the following steps:
(1) Ammonium metavanadate pretreatment: mixing ammonium metavanadate, sodium carbonate and polyvinylpyrrolidone according to a mass ratio of 100:0.1:0.1, mixing, and carrying out ball milling for activation to obtain activated ammonium metavanadate;
in the step (1), the rotating speed of the ball mill is 20r/min, and the ball milling is carried out for 30 hours. In the ball milling process, the ammonium metavanadate is activated, so that the graphene is favorably permeated in the subsequent reaction, and the complete reaction is favorably realized. If the rotating speed of the ball mill is too high, the centrifugal force of the ball is too large, and after a certain degree, the steel ball always rotates along with the ball mill, so that the activation effect cannot be achieved. If the rotating speed of the ball mill is too low, the subsequent graphene permeation is not facilitated. The ball milling time is too short, so that the activation cannot be fully performed, the ball milling time is too long, the effect is improved limitedly, and the production efficiency is reduced.
Research shows that a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on ammonium metavanadate, so that subsequent graphene permeation reduction is facilitated, the temperature of subsequent decomposition and permeation reduction can be reduced, and one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out.
In the ball milling process, the process of activation and the process of ball milling to reduce the particle size of the raw materials are both performed, so that the ball milling speed and time need to be controlled, the ammonium metavanadate is likely to have a smaller size due to too fast ball milling speed or too long ball milling time, and when the size of the ammonium metavanadate after ball milling is smaller, agglomeration is likely to occur in the subsequent reaction process, so that the powder components are not uniformly dispersed; the ball milling speed is too slow or the time is too short, so that the size of the ammonium metavanadate is possibly too large, and when the size of the ammonium metavanadate after ball milling is too large, the permeation and reduction degree of the graphene can be influenced, so that the reaction is insufficient, or the requirement of sufficient reaction can be met only by increasing the reaction temperature.
(2) One-step decomposition and reduction: and (2) uniformly mixing the activated ammonium metavanadate obtained in the step (1) with graphene, vacuumizing, and heating to 800 ℃ for reaction for 2 hours to obtain vanadium trioxide.
In the step (2), the molar ratio of ammonium metavanadate to carbon atoms of the ammonium metavanadate and the graphene is 1: mixing at a ratio of 0.26. If the amount of added graphene is too small, vanadium pentoxide which is a pyrolysis product of ammonium metavanadate cannot react completely, and if the amount of added graphene is too large, vanadium oxide with a lower valence state is generated, so that the purity of vanadium trioxide is influenced. The graphene is selected, and common carbon powder is not selected, because the graphene has a special molecular structure and can play the roles of activation and reduction, and if the graphene is changed into the common carbon powder, the reaction can be realized only by increasing the heating temperature.
In the step (2), the vacuum degree is controlled to be 50Pa by vacuumizing, the graphene is favorably permeated and reduced under the vacuum condition, when the vacuum degree is not good, the permeation of the graphene is influenced, the reduction is insufficient, and the final product is not high in purity and poor in quality.
According to the invention, the graphene is added and reacts under a vacuum condition, so that the penetration of carbon atoms in the graphene is facilitated, the reaction temperature can be reduced, the penetration and reduction reaction can be carried out in one step, the operation is simple and convenient, and the industrial production is facilitated.
The purity of the vanadium trioxide obtained by the method is 99.92%.
According to the invention, the particle size of the raw material ammonium metavanadate is controlled through ball milling, the raw material ammonium metavanadate is activated, and a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on the ammonium metavanadate, so that the subsequent graphene permeation reduction is facilitated, the temperature of the subsequent decomposition and permeation reduction can be reduced, and the one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out. The method adds the graphene, reacts under a vacuum condition, is beneficial to the permeation of carbon atoms in the graphene, can reduce the reaction temperature, enables the permeation and reduction reaction to be carried out in one step, is simple and convenient to operate, and is beneficial to industrial production. The obtained vanadium trioxide has high purity.
Example 2
The one-step pyrolysis and carbon infiltration reduction process of ammonium metavanadate in the embodiment comprises the following steps:
(1) Ammonium metavanadate pretreatment: mixing ammonium metavanadate, sodium carbonate and polyvinylpyrrolidone according to a mass ratio of 100: 0.2:0.2, mixing, and performing ball milling for activation to obtain activated ammonium metavanadate;
in the step (1), the rotating speed of the ball mill is 30r/min, and the ball milling is carried out for 10 hours. In the ball milling process, the ammonium metavanadate is activated, so that the graphene is favorably permeated in the subsequent reaction, and the complete reaction is favorably realized. If the rotating speed of the ball mill is too high, the centrifugal force of the ball is too large, and after a certain degree, the steel ball always rotates along with the ball mill, so that the activation effect cannot be achieved. If the rotating speed of the ball mill is too low, the subsequent graphene permeation is not facilitated. The ball milling time is too short, the activation cannot be fully carried out, the ball milling time is too long, the improvement on the effect is limited, and the production efficiency is reduced.
Research shows that a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on ammonium metavanadate, so that subsequent graphene permeation reduction is facilitated, the temperature of subsequent decomposition and permeation reduction can be reduced, and one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out.
In the ball milling process, the process of activation and the process of ball milling to reduce the particle size of the raw materials are both performed, so that the ball milling speed and time need to be controlled, the ammonium metavanadate is likely to have a smaller size due to too fast ball milling speed or too long ball milling time, and when the size of the ammonium metavanadate after ball milling is smaller, agglomeration is likely to occur in the subsequent reaction process, so that the powder components are not uniformly dispersed; when the ball milling speed is too slow or the time is too short, the size of the ammonium metavanadate may be too large, and when the size of the ammonium metavanadate after ball milling is too large, the permeation and reduction degree of the graphene can be affected, so that the reaction is insufficient, or the reaction temperature needs to be increased to meet the requirement of sufficient reaction.
(2) One-step decomposition and reduction: and (2) uniformly mixing the activated ammonium metavanadate obtained in the step (1) with graphene, vacuumizing, and heating to 700 ℃ for reaction for 5 hours to obtain vanadium trioxide.
In the step (2), the molar ratio of ammonium metavanadate to carbon atoms of the ammonium metavanadate and the graphene is 1:0.30, and mixing uniformly. If the amount of added graphene is too small, vanadium pentoxide which is a pyrolysis product of ammonium metavanadate cannot react completely, and if the amount of added graphene is too large, vanadium oxide with a lower valence state is generated, so that the purity of vanadium trioxide is influenced. The graphene is selected, and common carbon powder is not selected, because the graphene has a special molecular structure and can play the roles of activation and reduction, and if the graphene is changed into the common carbon powder, the reaction can be realized only by increasing the heating temperature.
In the step (2), the vacuum degree is controlled to be 100Pa by vacuumizing, the graphene is favorably permeated and reduced under the vacuum condition, when the vacuum degree is not good, the permeation of the graphene is influenced, the reduction is insufficient, and the final product is not high in purity and poor in quality.
The method adds the graphene, reacts under a vacuum condition, is beneficial to the permeation of carbon atoms in the graphene, can reduce the reaction temperature, enables the permeation and reduction reaction to be carried out in one step, is simple and convenient to operate, and is beneficial to industrial production.
The purity of the vanadium trioxide obtained by the method is 99.90%.
According to the invention, the particle size of the raw material ammonium metavanadate is controlled through ball milling, the raw material ammonium metavanadate is activated, and a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on the ammonium metavanadate, so that the subsequent graphene permeation reduction is facilitated, the temperature of the subsequent decomposition and permeation reduction can be reduced, and the one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out. According to the invention, the graphene is added and reacts under a vacuum condition, so that the penetration of carbon atoms in the graphene is facilitated, the reaction temperature can be reduced, the penetration and reduction reaction can be carried out in one step, the operation is simple and convenient, and the industrial production is facilitated. The obtained vanadium trioxide has high purity.
Example 3
The one-step pyrolysis and carbon permeation reduction process of ammonium metavanadate in the embodiment comprises the following steps:
(1) Ammonium metavanadate pretreatment: mixing ammonium metavanadate, sodium carbonate and polyvinylpyrrolidone according to a mass ratio of 100:0.1:0.2, mixing, and carrying out ball milling for activation to obtain activated ammonium metavanadate;
in the step (1), the rotating speed of the ball mill is 25r/min, and the ball milling is carried out for 20 hours. In the ball milling process, the ammonium metavanadate is activated, so that the graphene is favorably permeated in the subsequent reaction, and the complete reaction is favorably realized. If the rotating speed of the ball mill is too high, the centrifugal force of the ball is too large, and after a certain degree, the steel ball always rotates along with the ball mill, so that the activation effect cannot be achieved. If the rotating speed of the ball mill is too low, the subsequent graphene permeation is not facilitated. The ball milling time is too short, so that the activation cannot be fully performed, the ball milling time is too long, the effect is improved limitedly, and the production efficiency is reduced.
Research shows that a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on ammonium metavanadate, so that subsequent graphene permeation reduction is facilitated, the temperature of subsequent decomposition and permeation reduction can be reduced, and one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out.
In the ball milling process, the process of activation and the process of ball milling to reduce the particle size of the raw materials are both performed, so that the ball milling speed and time need to be controlled, the ammonium metavanadate is likely to have a smaller size due to too fast ball milling speed or too long ball milling time, and when the size of the ammonium metavanadate after ball milling is smaller, agglomeration is likely to occur in the subsequent reaction process, so that the powder components are not uniformly dispersed; when the ball milling speed is too slow or the time is too short, the size of the ammonium metavanadate may be too large, and when the size of the ammonium metavanadate after ball milling is too large, the permeation and reduction degree of the graphene can be affected, so that the reaction is insufficient, or the reaction temperature needs to be increased to meet the requirement of sufficient reaction.
(2) One-step decomposition and reduction: and (2) uniformly mixing the activated ammonium metavanadate obtained in the step (1) with graphene, vacuumizing, and heating to the temperature of 750 ℃ for reaction for 3 hours to obtain vanadium trioxide.
In the step (2), the molar ratio of ammonium metavanadate to carbon atoms of the ammonium metavanadate and the graphene is 1:0.28 is mixed uniformly. If the amount of added graphene is too small, vanadium pentoxide which is a pyrolysis product of ammonium metavanadate cannot react completely, and if the amount of added graphene is too large, vanadium oxide with a lower valence state is generated, so that the purity of vanadium trioxide is influenced. The invention selects graphene, and does not select common carbon powder, because the graphene has a special molecular structure and can play the roles of activation and reduction, and if the graphene is changed into the common carbon powder, the reaction can be realized only by increasing the heating temperature.
In the step (2), the vacuum degree is controlled to be 80Pa through vacuumizing, the graphene is favorably permeated and reduced under the vacuum condition, when the vacuum degree is poor, the permeation of the graphene is influenced, so that the reduction is insufficient, and the final product is low in purity and poor in quality.
According to the invention, the graphene is added and reacts under a vacuum condition, so that the penetration of carbon atoms in the graphene is facilitated, the reaction temperature can be reduced, the penetration and reduction reaction can be carried out in one step, the operation is simple and convenient, and the industrial production is facilitated.
The purity of the vanadium trioxide obtained by the method is 99.93%.
According to the invention, the particle size of the raw material ammonium metavanadate is controlled through ball milling, the raw material ammonium metavanadate is activated, and a small amount of sodium carbonate and polyvinylpyrrolidone are added to carry out pretreatment (activation) on the ammonium metavanadate, so that the subsequent graphene permeation reduction is facilitated, the subsequent decomposition and permeation reduction temperature can be reduced, and the one-step pyrolysis and carbon permeation reduction can be smoothly and fully carried out. The method adds the graphene, reacts under a vacuum condition, is beneficial to the permeation of carbon atoms in the graphene, can reduce the reaction temperature, enables the permeation and reduction reaction to be carried out in one step, is simple and convenient to operate, and is beneficial to industrial production. The obtained vanadium trioxide has high purity.
Comparative example 1
This comparative example was carried out in the same manner as in example 1 except that sodium carbonate and polyvinylpyrrolidone were not added in step (1). Heating the step (2) to 800 ℃ for reaction for 2 hours, and thus, vanadium trioxide cannot be obtained. The temperature is increased to 900 ℃ for 2 hours, and vanadium trioxide can be obtained. It is shown that the addition of sodium carbonate and polyvinylpyrrolidone can lower the reaction temperature.
Comparative example 2
In this comparative example, the same parameters as in example 1 were used except that the rotational speed of the ball mill in step (1) was 10r/min and the ball milling was carried out for 10 hours. And (3) heating the obtained product in the step (2) to 800 ℃ for reaction for 2 hours, wherein the purity of the obtained vanadium trioxide is only 70%. The ball milling can promote the penetration of the graphene, so that the reaction is faster and more sufficient.
Comparative example 3
In the comparative example, the parameters were the same as those in example 1 except that the graphene was replaced with the common carbon powder in the step (2). Heating the step (2) to 800 ℃ for reaction for 2 hours, and thus, vanadium trioxide cannot be obtained. The temperature is increased to 950 ℃ for reaction for 2 hours, and vanadium trioxide can be obtained. Indicating that the addition of graphene can lower the reaction temperature.
Comparative example 4
This comparative example was conducted in the same manner as example 1 except that no vacuum was applied in step (2). Heating the step (2) to 800 ℃ for reaction for 2 hours, and thus, vanadium trioxide cannot be obtained.
Claims (2)
1. A one-step pyrolysis and carbon permeation reduction process for ammonium metavanadate is characterized by comprising the following steps of:
(1) Ammonium metavanadate pretreatment: ammonium metavanadate, sodium carbonate and polyvinylpyrrolidone are mixed according to a mass ratio of 100:0.1-0.2:0.1-0.2, and performing ball milling for activation to obtain activated ammonium metavanadate;
(2) One-step decomposition and reduction: uniformly mixing the activated ammonium metavanadate obtained in the step (1) with graphene, vacuumizing, and heating to 700-800 ℃ for reacting for 2-5 hours to obtain vanadium trioxide;
in the step (1), the rotating speed of the ball mill is 20-30 r/min, and the ball milling is carried out for 10-30 hours;
in the step (2), the molar ratio of ammonium metavanadate to carbon atoms of the ammonium metavanadate and the graphene is 1: mixing at a ratio of 0.26-0.30;
in the step (2), vacuumizing to control the vacuum degree to be 50-100Pa.
2. The one-step pyrolysis and carbon permeation reduction process of ammonium metavanadate according to claim 1, wherein in the step (1), the rotation speed of a ball mill is 22-38 r/min, and the ball milling is carried out for 15-25 hours.
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GB600833A (en) * | 1942-04-28 | 1948-04-20 | Cie De Prod Chim Et Electro Me | Method of extraction of vanadium from bauxites and manufacture of ferro-vanadium |
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